#------------------------------------------------------------------------------
#$Date: 2025-01-15 03:28:41 +0100 (Wed, 15 Jan 2025) $
#$Revision: 297318 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023346.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023346
loop_
_publ_author_name
'Gienau, Trevor J.'
'Clay, Malachi'
'Brennessel, William W.'
'Reed, Carly R.'
_publ_section_title
;
(2,9-Dimethyl-1,10-phenanthroline)bis[2-(pyridin-2-yl)phenyl]iridium(III)
hexafluorophosphate and
(2,9-dimethyl-1,10-phenanthroline)bis[5-methyl-2-(pyridin-2-yl)phenyl]iridium(III)
hexafluorophosphate--diethyl ether--acetonitrile (1/0.61/0.78)
;
_journal_coeditor_code ZV2036
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024012039
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '[Ir (C14 H12 N2) (C11 H8 N)2] P F6'
_chemical_formula_moiety 'C36 H28 Ir N4 +, F6 P -'
_chemical_formula_sum 'C36 H28 F6 Ir N4 P'
_chemical_formula_weight 853.79
_chemical_name_systematic
;
(2,9-Dimethyl-1,10-phenanthroline)bis[2-(pyridin-2-yl)phenyl]iridium(III)
hexafluorophosphate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 11.41300(10)
_cell_length_b 17.16270(10)
_cell_length_c 31.7109(2)
_cell_measurement_reflns_used 61784
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 80.0580
_cell_measurement_theta_min 4.7630
_cell_volume 6211.46(8)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 1.5-ac6-015 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5-ac6-015 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0421
_diffrn_reflns_av_unetI/netI 0.0142
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -39
_diffrn_reflns_number 101540
_diffrn_reflns_theta_full 74.504
_diffrn_reflns_theta_max 80.468
_diffrn_reflns_theta_min 4.774
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 9.430
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.55763
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.826
_exptl_crystal_description block
_exptl_crystal_F_000 3344
_exptl_crystal_size_max 0.269
_exptl_crystal_size_mid 0.248
_exptl_crystal_size_min 0.143
_refine_diff_density_max 1.116
_refine_diff_density_min -0.679
_refine_ls_extinction_coef 0.000151(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.164
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 436
_refine_ls_number_reflns 6757
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.164
_refine_ls_R_factor_all 0.0245
_refine_ls_R_factor_gt 0.0241
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+11.8694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0595
_refine_ls_wR_factor_ref 0.0598
_reflns_number_gt 6668
_reflns_number_total 6757
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zv2036.cif
_cod_data_source_block 1
_cod_database_code 2023346
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.186
_shelx_estimated_absorpt_t_max 0.346
_shelx_hkl_file
;
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7 -10 20 2984.34 467.581 14
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7 -10 -20 3705.17 462.474 26
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7 10 20 2817.86 416.641 30
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7 -10 20 2846.03 397.436 30
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7 -10 -20 3367.78 461.741 24
7 -10 21 2623.30 378.436 34
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7 10 21 3661.00 441.026 30
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7 -10 21 2042.01 342.571 30
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7 -10 22 13685.9 913.071 34
7 -10 22 17048.9 1074.93 31
7 10 22 15178.0 1015.41 31
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7 10 -22 14895.7 887.541 32
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7 10 23 3402.38 451.947 31
7 -10 23 3991.92 437.234 34
7 -10 23 3856.22 484.829 31
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7 10 -23 4353.31 414.502 32
7 -10 23 4026.44 484.911 14
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7 -10 -23 3591.45 433.572 24
7 10 24 1737.56 315.294 31
7 -10 24 1917.58 294.165 34
7 -10 24 1797.24 312.112 31
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7 -10 -24 2071.39 314.449 24
-7 10 -25 1977.21 309.676 33
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-7 -10 -25 2123.40 324.596 18
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7 10 26 17867.9 963.517 31
7 -10 26 16113.9 899.020 34
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7 -10 -26 19786.5 971.167 24
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7 10 27 1500.54 238.838 31
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7 11 6 15250.3 1463.42 8
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7 11 -8 1774.11 325.697 29
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7 -11 8 1965.16 364.083 23
7 -11 -8 1495.50 346.851 23
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7 -11 -8 2149.52 424.535 26
7 11 9 46991.6 2890.66 9
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7 11 -10 271.423 192.390 12
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14 -1 -1 35839.8 1469.48 23
14 -1 -1 35738.7 1468.62 26
14 -1 1 39193.7 1490.62 26
14 1 -1 35987.7 1465.72 26
14 1 1 38018.3 1482.00 26
-14 1 -1 38840.1 1476.77 35
14 -1 2 1327.65 205.113 23
14 -1 2 1698.86 223.609 26
14 1 2 2056.87 242.050 26
14 -1 -2 1518.62 223.455 26
-14 1 -2 1608.94 214.237 35
14 -1 3 16801.8 789.789 23
14 -1 3 15396.0 763.901 26
14 1 3 15024.1 759.162 26
-14 1 -3 15799.1 772.073 35
14 1 4 53.9905 88.1607 26
14 -1 4 181.809 108.169 23
14 -1 -4 220.666 117.887 23
14 -1 4 157.403 95.3140 26
14 1 -4 55.2246 92.2890 26
-14 1 -4 275.187 125.504 35
14 -1 5 33630.6 1317.34 23
14 -1 -5 34049.9 1326.33 23
14 1 5 33750.1 1311.41 23
14 1 -5 35052.7 1329.82 23
14 -1 5 31871.1 1289.85 26
14 1 -5 35253.5 1339.14 26
14 1 5 34430.7 1321.21 26
-14 1 -5 34600.8 1344.32 35
14 -1 6 2596.54 233.835 23
14 -1 -6 2178.40 225.506 23
14 1 6 2434.02 224.725 23
14 1 -6 2235.39 223.546 23
14 -1 -6 2159.63 233.240 26
14 -1 6 1938.86 202.533 26
14 1 -6 2189.23 222.970 26
14 1 6 2269.58 224.638 26
-14 1 -6 2161.73 235.120 35
14 -1 7 478.978 97.9346 23
14 -1 -7 311.286 97.6268 23
14 1 7 314.656 84.5339 23
14 1 -7 384.392 93.5040 23
14 -1 -7 525.197 118.305 26
14 -1 7 339.569 82.5137 26
14 1 -7 328.994 98.8622 26
14 1 7 313.794 87.6173 26
-14 1 -7 636.088 128.714 35
14 -1 -8 180.527 70.9644 23
14 1 -8 458.096 90.1826 23
14 -1 -8 385.760 103.256 26
14 1 -8 450.487 95.9968 26
-14 1 -8 338.058 106.936 35
14 -1 -9 36574.9 1340.52 26
-14 1 -9 41355.2 1419.36 35
-14 1 -10 556.664 107.850 35
-14 1 -11 12462.2 536.829 35
14 -2 0 30511.2 1259.40 23
14 -2 0 30986.2 1259.01 26
14 2 0 29710.1 1241.40 26
-14 2 0 29022.0 1215.09 35
-14 -2 0 30650.4 1211.94 35
14 2 1 348.131 127.890 26
14 -2 1 480.508 143.930 23
14 -2 -1 521.244 140.905 23
14 -2 -1 401.963 139.616 26
14 -2 1 468.798 147.989 26
-14 2 -1 292.306 120.871 35
-14 -2 -1 376.895 123.318 35
14 -2 2 2773.73 279.352 23
14 -2 -2 2392.21 269.093 26
14 -2 2 2910.14 282.502 26
14 2 2 2939.34 281.497 26
-14 2 -2 2565.99 264.427 35
-14 -2 -2 2257.72 246.569 35
14 2 -3 525.960 131.526 26
14 2 3 750.857 152.860 26
14 -2 3 822.837 163.522 23
14 -2 -3 720.692 154.213 26
14 -2 3 636.131 140.166 26
-14 2 -3 584.770 141.822 35
-14 -2 -3 800.247 148.230 35
14 -2 4 42985.8 1580.64 23
14 -2 -4 43386.9 1586.32 23
14 -2 4 39310.8 1533.41 26
14 2 -4 41945.2 1569.51 26
14 2 4 41673.1 1571.29 26
-14 2 -4 40732.3 1563.38 35
-14 -2 -4 42533.0 1559.04 35
14 -2 5 1626.33 199.222 23
14 -2 -5 1643.75 203.795 23
14 -2 5 1828.41 202.803 26
14 2 -5 1993.75 215.104 26
14 2 5 1833.71 205.213 26
-14 2 -5 1533.96 206.354 35
-14 -2 -5 2009.85 218.436 35
14 -2 6 8692.98 470.321 23
14 -2 -6 8421.93 474.395 23
14 2 6 8928.74 468.903 23
14 -2 -6 9802.25 519.777 26
14 -2 6 7785.47 428.033 26
14 2 -6 8273.32 466.202 26
14 2 6 9202.17 484.344 26
-14 2 -6 9250.07 500.109 35
-14 -2 -6 10130.2 506.626 35
14 -2 7 2469.15 208.022 23
14 -2 -7 2471.33 214.263 23
14 2 7 2643.13 207.783 23
14 2 -7 2418.07 207.594 23
14 -2 -7 2979.70 252.882 26
14 2 -7 2583.61 218.242 26
14 2 7 2470.52 215.129 26
-14 2 -7 2400.87 230.322 35
-14 -2 -7 2719.68 238.835 35
14 -2 -8 16134.2 691.531 26
-14 2 -8 15543.5 694.446 35
-14 -2 -8 15950.4 689.998 35
14 -2 -9 764.342 111.623 26
-14 2 -9 887.479 129.575 35
-14 2 -10 8737.06 431.500 35
-14 -2 -10 10002.7 442.683 35
14 -3 0 4210.88 346.185 23
14 -3 0 3880.80 339.092 26
14 3 0 4411.46 344.096 26
-14 3 0 3892.19 316.754 35
-14 -3 0 4853.13 332.068 35
14 -3 1 30785.8 1228.69 23
14 -3 -1 30408.5 1224.63 23
14 -3 -1 30788.6 1222.72 26
14 -3 1 29453.5 1201.24 26
14 3 1 29685.5 1205.33 26
-14 3 -1 26949.0 1151.77 35
-14 -3 -1 30603.7 1157.35 35
-14 3 1 28184.8 1161.98 35
-14 -3 1 29932.0 1152.50 35
14 3 2 158.476 99.6978 26
14 -3 2 146.150 91.7208 23
14 -3 -2 149.119 103.620 26
14 -3 2 305.858 105.991 26
-14 3 -2 237.787 104.543 35
-14 -3 -2 216.511 88.7699 35
-14 3 2 157.889 91.0156 35
-14 -3 2 284.182 97.3616 35
14 3 -2 271.105 100.940 32
14 -3 3 8375.16 492.519 23
14 -3 -3 8455.75 493.197 23
14 -3 -3 7997.52 492.956 26
14 -3 3 7289.14 449.962 26
14 3 -3 8697.00 486.544 26
14 3 3 8921.29 497.397 26
-14 3 -3 6933.57 443.085 35
-14 -3 -3 8070.58 446.678 35
14 3 -3 8123.93 471.922 32
14 -3 4 1213.27 178.751 23
14 -3 -4 1409.74 186.806 23
14 -3 -4 1529.59 205.652 26
14 3 -4 1679.36 196.271 26
14 -3 4 1208.78 166.272 26
14 3 4 1793.25 206.364 26
-14 3 -4 1663.71 193.877 35
-14 -3 -4 1701.13 186.102 35
14 3 -4 1703.46 198.252 32
14 -3 5 71912.9 2485.59 23
14 -3 -5 77124.7 2512.57 23
14 -3 5 66340.3 2415.19 26
14 3 -5 76597.2 2490.21 26
14 3 5 78172.5 2513.62 26
-14 3 -5 69506.8 2470.11 35
-14 -3 -5 78267.9 2477.11 35
14 3 6 93.6053 76.9238 26
14 -3 6 99.1919 66.2329 23
14 -3 -6 25.8130 70.3053 23
14 3 -6 59.5730 62.3636 26
-14 3 -6 169.562 85.8823 35
-14 -3 -6 36.1659 64.3989 35
14 3 7 226.037 79.2188 26
14 -3 -7 134.666 61.6926 23
14 3 -7 191.363 64.6290 23
14 -3 -7 313.870 97.8176 26
14 3 -7 66.0207 55.2794 26
-14 3 -7-11.7753 71.2193 35
-14 -3 -7 142.710 68.4460 35
14 -3 -8 312.394 87.9422 26
-14 3 -8 286.255 81.5867 35
-14 -3 -8 405.036 84.8920 35
14 -4 0 28100.8 1099.40 23
14 -4 0 28204.8 1083.59 26
-14 -4 0 26091.0 984.553 35
14 -4 1 2088.70 227.059 23
14 -4 1 1848.95 209.782 26
14 -4 -1 2032.86 223.790 26
14 4 1 2514.28 237.727 26
-14 4 -1 1693.63 196.332 35
-14 -4 -1 2252.73 194.373 35
-14 4 1 1672.50 199.678 35
-14 -4 1 2094.39 187.732 35
14 -4 2 3504.59 288.615 23
14 -4 2 3193.54 264.017 26
14 -4 -2 3709.78 302.684 26
14 4 -2 4012.88 295.078 26
14 4 2 3340.04 278.943 26
-14 4 -2 2934.09 236.338 35
-14 -4 -2 3008.84 227.282 35
-14 4 2 2808.84 233.280 35
-14 -4 2 3435.94 238.354 35
14 -4 -3 6007.25 383.053 23
14 -4 3 5414.21 339.342 26
14 -4 -3 5938.36 392.218 26
14 4 -3 5942.80 364.366 26
14 4 3 6428.00 388.443 26
14 -4 3 4855.06 350.405 23
-14 4 -3 4637.78 310.558 35
-14 -4 -3 5744.03 320.138 35
-14 4 3 4509.36 310.064 35
-14 -4 3 6063.81 323.144 35
14 4 -3 6544.11 382.707 32
14 -4 4 16198.6 679.381 26
14 -4 -4 18831.2 788.566 26
14 4 -4 17470.1 727.180 26
14 4 4 18328.7 761.346 26
14 -4 4 18747.6 762.935 23
14 -4 -4 17746.4 758.037 23
-14 4 -4 14830.7 671.067 35
-14 -4 -4 16576.5 672.848 35
-14 4 4 15497.2 678.682 35
-14 -4 4 16256.0 666.125 35
14 4 -4 17664.9 741.064 32
14 4 -5 87.9634 64.3396 26
14 4 5 171.515 80.9551 26
14 -4 5 36.8930 63.0088 23
14 -4 -5 63.6181 65.1891 23
14 4 -5 24.9216 59.5392 32
14 -4 6 12275.5 549.204 23
14 -4 -6 12748.1 562.200 23
14 4 6 13947.2 591.890 26
14 4 7 200.324 63.9271 26
14 -4 -7 224.351 79.9958 26
14 -4 -8 6519.45 342.292 26
14 -5 0 157.725 88.0686 23
14 -5 0 140.585 78.5243 26
14 5 -1 24689.2 905.969 32
14 -5 1 19402.9 846.314 26
14 -5 -1 21128.4 884.494 26
14 5 -1 22870.3 889.859 26
14 -5 1 22293.2 905.563 23
14 -5 -2 989.036 150.488 26
14 5 -2 1333.81 153.142 26
14 -5 2 1283.94 165.324 23
14 5 2 1179.08 156.801 26
14 -5 -3 17769.4 757.087 26
14 5 -3 17104.4 713.128 26
14 -5 3 18248.2 748.973 23
14 -5 -3 17865.6 751.510 23
14 5 3 17437.5 745.814 26
14 5 -4 1954.69 181.381 32
14 -5 -4 1425.06 171.954 26
14 -5 4 1413.47 159.086 23
14 -5 -4 1619.91 168.740 23
14 5 4 1990.68 184.510 26
14 5 -5 35454.9 1272.57 32
14 -5 -5 34650.3 1297.91 26
14 5 5 38009.3 1294.09 26
14 -6 0 37345.0 1331.43 23
14 6 0 38025.1 1314.75 26
14 -6 1 507.543 96.3753 23
0 0 0 0.00 0.00 0
TITL Faces in Pbca
REM Pbca (#61 in standard setting)
CELL 1.54184 11.413004 17.162696 31.710909 90.0000 90.0000 90.0000
ZERR 6.00 0.000055 0.000091 0.000161 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N F P Ir
UNIT 252.00 252.00 36.00 36.00 6.00 6.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.14 0.25 0.27
TREF
HKLF 4
END
;
_shelx_hkl_checksum 15090
_shelx_res_file
;
TITL brocr22_a.res in Pbca
brocr22.res
created by SHELXL-2019/3 at 11:15:03 on 18-Jun-2024
REM Old TITL BROCR22_auto in Pbca
REM SHELXT solution in Pbca: R1 0.053, Rweak 0.002, Alpha 0.059
REM 2.261 for 695 systematic absences, Orientation as input
REM Formula found by SHELXT: C36 N4 F6 P Ir
CELL 1.54184 11.413 17.1627 31.7109 90 90 90
ZERR 8 0.0001 0.0001 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H F Ir N P
UNIT 288 224 48 8 32 8
L.S. 12
PLAN 5
SIZE 0.269 0.248 0.143
TEMP -173
CONF
BOND $H
list 4
MORE -1
fmap 2
acta 149.008
REM
REM
REM
WGHT 0.022900 11.869400
EXTI 0.000151
FVAR 1.44762
IR1 4 0.510637 0.494050 0.356823 11.00000 0.01142 0.01540 =
0.01044 -0.00022 -0.00051 0.00033
N1 5 0.649978 0.546667 0.327603 11.00000 0.01338 0.01432 =
0.01394 -0.00076 0.00061 0.00136
N2 5 0.362444 0.443192 0.380331 11.00000 0.01200 0.02395 =
0.01185 -0.00205 -0.00074 -0.00188
N3 5 0.636676 0.401083 0.370838 11.00000 0.01339 0.01576 =
0.01475 0.00306 0.00096 -0.00036
N4 5 0.567838 0.522966 0.421621 11.00000 0.01456 0.02216 =
0.01176 0.00028 -0.00040 -0.00237
C1 1 0.473753 0.466966 0.296369 11.00000 0.01642 0.01821 =
0.01092 -0.00094 -0.00157 0.00275
C2 1 0.380587 0.422568 0.280991 11.00000 0.01443 0.02204 =
0.01746 -0.00211 -0.00059 0.00061
AFIX 43
H2 2 0.320529 0.406073 0.299715 11.00000 -1.20000
AFIX 0
C3 1 0.374615 0.402173 0.238556 11.00000 0.01922 0.02605 =
0.01927 -0.00524 -0.00480 -0.00068
AFIX 43
H3 2 0.311915 0.370417 0.228920 11.00000 -1.20000
AFIX 0
C4 1 0.458897 0.427524 0.210074 11.00000 0.02742 0.02664 =
0.01461 -0.00497 -0.00354 0.00039
AFIX 43
H4 2 0.454588 0.412515 0.181280 11.00000 -1.20000
AFIX 0
C5 1 0.549297 0.474880 0.224009 11.00000 0.02521 0.02428 =
0.01305 -0.00286 0.00196 -0.00108
AFIX 43
H5 2 0.606228 0.493618 0.204648 11.00000 -1.20000
AFIX 0
C6 1 0.556471 0.495092 0.266873 11.00000 0.01809 0.01463 =
0.01517 -0.00029 -0.00044 0.00209
C7 1 0.652708 0.540570 0.284592 11.00000 0.01690 0.01637 =
0.01396 0.00038 0.00050 0.00238
C8 1 0.743824 0.574186 0.261730 11.00000 0.02276 0.01827 =
0.01495 -0.00052 0.00183 -0.00085
AFIX 43
H8 2 0.743229 0.572399 0.231788 11.00000 -1.20000
AFIX 0
C9 1 0.835320 0.610235 0.282786 11.00000 0.02164 0.01756 =
0.02089 -0.00100 0.00531 -0.00199
AFIX 43
H9 2 0.898527 0.632459 0.267446 11.00000 -1.20000
AFIX 0
C10 1 0.833741 0.613559 0.326435 11.00000 0.01897 0.01814 =
0.02315 0.00032 -0.00178 -0.00224
AFIX 43
H10 2 0.896565 0.636951 0.341467 11.00000 -1.20000
AFIX 0
C11 1 0.739132 0.582236 0.347725 11.00000 0.01852 0.01660 =
0.01597 -0.00023 -0.00182 0.00026
AFIX 43
H11 2 0.736895 0.585921 0.377606 11.00000 -1.20000
AFIX 0
C12 1 0.394575 0.579734 0.345474 11.00000 0.01806 0.02003 =
0.01454 -0.00381 -0.00443 0.00872
C13 1 0.415354 0.652102 0.326843 11.00000 0.02378 0.02175 =
0.01757 -0.00072 -0.00256 0.00429
AFIX 43
H13 2 0.492169 0.664552 0.317475 11.00000 -1.20000
AFIX 0
C14 1 0.325330 0.706787 0.321661 11.00000 0.03792 0.02202 =
0.02348 -0.00171 -0.00619 0.00909
AFIX 43
H14 2 0.341283 0.755710 0.308878 11.00000 -1.20000
AFIX 0
C15 1 0.212443 0.689209 0.335302 11.00000 0.03139 0.03127 =
0.02750 -0.00807 -0.00604 0.01461
AFIX 43
H15 2 0.151613 0.726569 0.332250 11.00000 -1.20000
AFIX 0
C16 1 0.188565 0.617519 0.353287 11.00000 0.02161 0.03311 =
0.02058 -0.00760 -0.00362 0.00893
AFIX 43
H16 2 0.111499 0.605614 0.362596 11.00000 -1.20000
AFIX 0
C17 1 0.278630 0.562420 0.357732 11.00000 0.01818 0.02615 =
0.01275 -0.00545 -0.00241 0.00491
C18 1 0.262138 0.486068 0.376997 11.00000 0.01543 0.02941 =
0.01207 -0.00674 -0.00088 0.00279
C19 1 0.156425 0.454920 0.391375 11.00000 0.01568 0.03962 =
0.02048 -0.00806 0.00026 -0.00084
AFIX 43
H19 2 0.086445 0.484707 0.389581 11.00000 -1.20000
AFIX 0
C20 1 0.153772 0.380640 0.408228 11.00000 0.01686 0.04569 =
0.01995 -0.00466 0.00225 -0.01044
AFIX 43
H20 2 0.081877 0.359062 0.417796 11.00000 -1.20000
AFIX 0
C21 1 0.256748 0.337622 0.411124 11.00000 0.02671 0.02824 =
0.01810 -0.00220 0.00459 -0.00812
AFIX 43
H21 2 0.256365 0.286435 0.422525 11.00000 -1.20000
AFIX 0
C22 1 0.359592 0.371131 0.397021 11.00000 0.02041 0.02260 =
0.01541 -0.00142 -0.00031 -0.00216
AFIX 43
H22 2 0.430497 0.342410 0.399172 11.00000 -1.20000
AFIX 0
C23 1 0.670102 0.340731 0.346551 11.00000 0.01794 0.01580 =
0.01800 0.00430 0.00174 -0.00105
C24 1 0.770899 0.296508 0.355954 11.00000 0.01740 0.01742 =
0.02749 0.00242 0.00214 0.00081
AFIX 43
H24 2 0.795756 0.256781 0.337108 11.00000 -1.20000
AFIX 0
C25 1 0.832845 0.310400 0.391892 11.00000 0.01439 0.02466 =
0.02914 0.00893 0.00004 0.00012
AFIX 43
H25 2 0.900264 0.280176 0.398306 11.00000 -1.20000
AFIX 0
C26 1 0.796382 0.369557 0.419296 11.00000 0.01447 0.02872 =
0.01975 0.00783 -0.00022 -0.00042
C27 1 0.852504 0.382778 0.458904 11.00000 0.01591 0.04337 =
0.02291 0.00861 -0.00318 0.00432
AFIX 43
H27 2 0.917596 0.351582 0.466879 11.00000 -1.20000
AFIX 0
C28 1 0.814045 0.439016 0.485039 11.00000 0.02166 0.05072 =
0.01747 0.00459 -0.00717 0.00216
AFIX 43
H28 2 0.851634 0.446614 0.511451 11.00000 -1.20000
AFIX 0
C29 1 0.717557 0.487329 0.473559 11.00000 0.01924 0.03504 =
0.01427 0.00223 -0.00187 -0.00201
C30 1 0.676105 0.546284 0.500123 11.00000 0.02646 0.03893 =
0.01551 -0.00292 -0.00405 -0.00243
AFIX 43
H30 2 0.712731 0.555431 0.526566 11.00000 -1.20000
AFIX 0
C31 1 0.583169 0.590435 0.487929 11.00000 0.02421 0.03119 =
0.01449 -0.00494 0.00072 -0.00291
AFIX 43
H31 2 0.553931 0.629698 0.506237 11.00000 -1.20000
AFIX 0
C32 1 0.529894 0.578487 0.448424 11.00000 0.01905 0.02492 =
0.01416 -0.00139 0.00175 -0.00386
C33 1 0.659517 0.476508 0.434517 11.00000 0.01472 0.02577 =
0.01310 0.00318 -0.00161 -0.00250
C34 1 0.698938 0.415164 0.407185 11.00000 0.01024 0.02374 =
0.01598 0.00516 -0.00045 -0.00181
C35 1 0.597380 0.315993 0.309740 11.00000 0.02520 0.01590 =
0.02526 -0.00236 -0.00328 -0.00003
AFIX 137
H35A 2 0.514957 0.312952 0.318246 11.00000 -1.50000
H35B 2 0.623651 0.264746 0.299921 11.00000 -1.50000
H35C 2 0.605828 0.354052 0.286903 11.00000 -1.50000
AFIX 0
C36 1 0.428951 0.630296 0.437089 11.00000 0.03115 0.02836 =
0.01803 -0.00694 -0.00136 0.00640
AFIX 137
H36A 2 0.447145 0.658624 0.411067 11.00000 -1.50000
H36B 2 0.415152 0.667579 0.459963 11.00000 -1.50000
H36C 2 0.358563 0.598554 0.432826 11.00000 -1.50000
AFIX 0
P1 6 0.562515 0.187083 0.444620 11.00000 0.02072 0.02970 =
0.01914 0.00513 0.00287 -0.00293
F1 3 0.536413 0.218211 0.397593 11.00000 0.03734 0.02957 =
0.01993 0.00421 0.00337 0.00451
F2 3 0.588037 0.156832 0.491221 11.00000 0.02599 0.08846 =
0.02337 0.02204 0.00550 0.00763
F3 3 0.697404 0.175930 0.433033 11.00000 0.02652 0.03444 =
0.02732 0.00292 0.00875 0.00240
F4 3 0.587755 0.274912 0.458894 11.00000 0.04099 0.04075 =
0.04291 -0.01886 0.00304 0.00324
F5 3 0.426990 0.198774 0.455783 11.00000 0.02083 0.07807 =
0.03986 0.02866 0.00528 0.00102
F6 3 0.536347 0.100193 0.429212 11.00000 0.05635 0.02481 =
0.06957 0.01338 -0.02563 -0.01290
HKLF 4
REM brocr22_a.res in Pbca
REM wR2 = 0.0598, GooF = S = 1.164, Restrained GooF = 1.164 for all data
REM R1 = 0.0241 for 6668 Fo > 4sig(Fo) and 0.0245 for all 6757 data
REM 436 parameters refined using 0 restraints
END
WGHT 0.0229 11.8698
REM Highest difference peak 1.116, deepest hole -0.679, 1-sigma level 0.096
Q1 1 0.4597 0.5534 0.3528 11.00000 0.05 1.12
Q2 1 0.4999 0.4397 0.3596 11.00000 0.05 0.94
Q3 1 0.5514 0.5514 0.3581 11.00000 0.05 0.88
Q4 1 0.4965 0.5041 0.2132 11.00000 0.05 0.62
Q5 1 0.4979 0.4777 0.3207 11.00000 0.05 0.59
;
_shelx_res_checksum 36302
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir Ir1 0.51064(2) 0.49405(2) 0.35682(2) 0.01242(5) Uani d 1 . .
N N1 0.64998(18) 0.54667(12) 0.32760(6) 0.0139(4) Uani d 1 . .
N N2 0.36244(18) 0.44319(13) 0.38033(6) 0.0159(4) Uani d 1 . .
N N3 0.63668(18) 0.40108(12) 0.37084(6) 0.0146(4) Uani d 1 . .
N N4 0.56784(19) 0.52297(13) 0.42162(6) 0.0162(4) Uani d 1 . .
C C1 0.4738(2) 0.46697(15) 0.29637(7) 0.0152(5) Uani d 1 . .
C C2 0.3806(2) 0.42257(15) 0.28099(8) 0.0180(5) Uani d 1 . .
H H2 0.320529 0.406073 0.299715 0.022 Uiso calc 1 . .
C C3 0.3746(2) 0.40217(16) 0.23856(8) 0.0215(5) Uani d 1 . .
H H3 0.311915 0.370417 0.228920 0.026 Uiso calc 1 . .
C C4 0.4589(3) 0.42752(16) 0.21007(8) 0.0229(5) Uani d 1 . .
H H4 0.454588 0.412515 0.181280 0.027 Uiso calc 1 . .
C C5 0.5493(2) 0.47488(16) 0.22401(8) 0.0208(5) Uani d 1 . .
H H5 0.606228 0.493618 0.204648 0.025 Uiso calc 1 . .
C C6 0.5565(2) 0.49509(13) 0.26687(8) 0.0160(5) Uani d 1 . .
C C7 0.6527(2) 0.54057(14) 0.28459(8) 0.0157(5) Uani d 1 . .
C C8 0.7438(2) 0.57419(15) 0.26173(8) 0.0187(5) Uani d 1 . .
H H8 0.743229 0.572399 0.231788 0.022 Uiso calc 1 . .
C C9 0.8353(2) 0.61024(15) 0.28279(8) 0.0200(5) Uani d 1 . .
H H9 0.898527 0.632459 0.267446 0.024 Uiso calc 1 . .
C C10 0.8337(2) 0.61356(15) 0.32644(8) 0.0201(5) Uani d 1 . .
H H10 0.896565 0.636951 0.341467 0.024 Uiso calc 1 . .
C C11 0.7391(2) 0.58224(15) 0.34773(8) 0.0170(5) Uani d 1 . .
H H11 0.736895 0.585921 0.377606 0.020 Uiso calc 1 . .
C C12 0.3946(2) 0.57973(15) 0.34547(8) 0.0175(5) Uani d 1 . .
C C13 0.4154(2) 0.65210(16) 0.32684(8) 0.0210(5) Uani d 1 . .
H H13 0.492169 0.664552 0.317475 0.025 Uiso calc 1 . .
C C14 0.3253(3) 0.70679(17) 0.32166(9) 0.0278(6) Uani d 1 . .
H H14 0.341283 0.755710 0.308878 0.033 Uiso calc 1 . .
C C15 0.2124(3) 0.68921(18) 0.33530(9) 0.0301(7) Uani d 1 . .
H H15 0.151613 0.726569 0.332250 0.036 Uiso calc 1 . .
C C16 0.1886(3) 0.61752(18) 0.35329(8) 0.0251(6) Uani d 1 . .
H H16 0.111499 0.605614 0.362596 0.030 Uiso calc 1 . .
C C17 0.2786(2) 0.56242(16) 0.35773(7) 0.0190(5) Uani d 1 . .
C C18 0.2621(2) 0.48607(16) 0.37700(8) 0.0190(5) Uani d 1 . .
C C19 0.1564(2) 0.45492(18) 0.39137(8) 0.0253(6) Uani d 1 . .
H H19 0.086445 0.484707 0.389581 0.030 Uiso calc 1 . .
C C20 0.1538(2) 0.38064(19) 0.40823(9) 0.0275(6) Uani d 1 . .
H H20 0.081877 0.359062 0.417796 0.033 Uiso calc 1 . .
C C21 0.2567(3) 0.33762(17) 0.41112(8) 0.0244(6) Uani d 1 . .
H H21 0.256365 0.286435 0.422525 0.029 Uiso calc 1 . .
C C22 0.3596(2) 0.37113(15) 0.39702(8) 0.0195(5) Uani d 1 . .
H H22 0.430497 0.342410 0.399172 0.023 Uiso calc 1 . .
C C23 0.6701(2) 0.34073(14) 0.34655(8) 0.0172(5) Uani d 1 . .
C C24 0.7709(2) 0.29651(16) 0.35595(8) 0.0208(5) Uani d 1 . .
H H24 0.795756 0.256781 0.337108 0.025 Uiso calc 1 . .
C C25 0.8328(2) 0.31040(16) 0.39189(9) 0.0227(5) Uani d 1 . .
H H25 0.900264 0.280176 0.398306 0.027 Uiso calc 1 . .
C C26 0.7964(2) 0.36956(16) 0.41930(8) 0.0210(5) Uani d 1 . .
C C27 0.8525(2) 0.38278(19) 0.45890(9) 0.0274(6) Uani d 1 . .
H H27 0.917596 0.351582 0.466879 0.033 Uiso calc 1 . .
C C28 0.8140(3) 0.4390(2) 0.48504(9) 0.0299(7) Uani d 1 . .
H H28 0.851634 0.446614 0.511451 0.036 Uiso calc 1 . .
C C29 0.7176(2) 0.48733(17) 0.47356(8) 0.0229(6) Uani d 1 . .
C C30 0.6761(3) 0.54628(19) 0.50012(8) 0.0270(6) Uani d 1 . .
H H30 0.712731 0.555431 0.526566 0.032 Uiso calc 1 . .
C C31 0.5832(2) 0.59043(17) 0.48793(8) 0.0233(5) Uani d 1 . .
H H31 0.553931 0.629698 0.506237 0.028 Uiso calc 1 . .
C C32 0.5299(2) 0.57849(16) 0.44842(8) 0.0194(5) Uani d 1 . .
C C33 0.6595(2) 0.47651(16) 0.43452(8) 0.0179(5) Uani d 1 . .
C C34 0.6989(2) 0.41516(15) 0.40718(8) 0.0167(5) Uani d 1 . .
C C35 0.5974(2) 0.31599(15) 0.30974(9) 0.0221(5) Uani d 1 . .
H H35A 0.514957 0.312952 0.318246 0.033 Uiso calc 1 . .
H H35B 0.623651 0.264746 0.299921 0.033 Uiso calc 1 . .
H H35C 0.605828 0.354052 0.286903 0.033 Uiso calc 1 . .
C C36 0.4290(3) 0.63030(17) 0.43709(9) 0.0258(6) Uani d 1 . .
H H36A 0.447145 0.658624 0.411067 0.039 Uiso calc 1 . .
H H36B 0.415152 0.667579 0.459963 0.039 Uiso calc 1 . .
H H36C 0.358563 0.598554 0.432826 0.039 Uiso calc 1 . .
P P1 0.56252(6) 0.18708(4) 0.44462(2) 0.02319(15) Uani d 1 . .
F F1 0.53641(16) 0.21821(10) 0.39759(5) 0.0289(4) Uani d 1 . .
F F2 0.58804(17) 0.15683(15) 0.49122(6) 0.0459(5) Uani d 1 . .
F F3 0.69740(15) 0.17593(10) 0.43303(5) 0.0294(4) Uani d 1 . .
F F4 0.58775(18) 0.27491(12) 0.45889(6) 0.0415(5) Uani d 1 . .
F F5 0.42699(16) 0.19877(14) 0.45578(6) 0.0463(5) Uani d 1 . .
F F6 0.5363(2) 0.10019(11) 0.42921(8) 0.0502(6) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ir1 0.01142(7) 0.01540(7) 0.01044(7) 0.00033(3) -0.00051(3) -0.00022(3)
N1 0.0134(9) 0.0143(9) 0.0139(9) 0.0014(7) 0.0006(7) -0.0008(7)
N2 0.0120(9) 0.0239(11) 0.0118(9) -0.0019(8) -0.0007(7) -0.0020(8)
N3 0.0134(9) 0.0158(10) 0.0147(10) -0.0004(8) 0.0010(8) 0.0031(8)
N4 0.0146(10) 0.0222(10) 0.0118(9) -0.0024(8) -0.0004(8) 0.0003(8)
C1 0.0164(11) 0.0182(12) 0.0109(11) 0.0027(9) -0.0016(9) -0.0009(9)
C2 0.0144(11) 0.0220(12) 0.0175(12) 0.0006(9) -0.0006(9) -0.0021(10)
C3 0.0192(12) 0.0261(13) 0.0193(13) -0.0007(10) -0.0048(10) -0.0052(10)
C4 0.0274(14) 0.0266(13) 0.0146(12) 0.0004(11) -0.0035(10) -0.0050(10)
C5 0.0252(13) 0.0243(13) 0.0130(12) -0.0011(11) 0.0020(10) -0.0029(10)
C6 0.0181(13) 0.0146(11) 0.0152(12) 0.0021(9) -0.0004(10) -0.0003(8)
C7 0.0169(11) 0.0164(11) 0.0140(11) 0.0024(9) 0.0005(9) 0.0004(9)
C8 0.0228(12) 0.0183(12) 0.0150(11) -0.0008(10) 0.0018(10) -0.0005(9)
C9 0.0216(13) 0.0176(12) 0.0209(12) -0.0020(10) 0.0053(10) -0.0010(10)
C10 0.0190(12) 0.0181(12) 0.0231(13) -0.0022(10) -0.0018(10) 0.0003(10)
C11 0.0185(12) 0.0166(12) 0.0160(11) 0.0003(9) -0.0018(10) -0.0002(9)
C12 0.0181(12) 0.0200(12) 0.0145(11) 0.0087(10) -0.0044(9) -0.0038(9)
C13 0.0238(13) 0.0218(13) 0.0176(12) 0.0043(10) -0.0026(10) -0.0007(10)
C14 0.0379(16) 0.0220(13) 0.0235(13) 0.0091(12) -0.0062(12) -0.0017(11)
C15 0.0314(15) 0.0313(15) 0.0275(15) 0.0146(12) -0.0060(12) -0.0081(12)
C16 0.0216(14) 0.0331(15) 0.0206(13) 0.0089(12) -0.0036(10) -0.0076(11)
C17 0.0182(13) 0.0261(14) 0.0128(11) 0.0049(10) -0.0024(9) -0.0055(9)
C18 0.0154(12) 0.0294(14) 0.0121(11) 0.0028(10) -0.0009(9) -0.0067(10)
C19 0.0157(12) 0.0396(16) 0.0205(13) -0.0008(11) 0.0003(10) -0.0081(11)
C20 0.0169(13) 0.0457(17) 0.0199(13) -0.0104(12) 0.0022(10) -0.0047(12)
C21 0.0267(14) 0.0282(14) 0.0181(12) -0.0081(11) 0.0046(11) -0.0022(10)
C22 0.0204(12) 0.0226(13) 0.0154(12) -0.0022(10) -0.0003(10) -0.0014(9)
C23 0.0179(12) 0.0158(11) 0.0180(11) -0.0011(9) 0.0017(10) 0.0043(9)
C24 0.0174(12) 0.0174(12) 0.0275(14) 0.0008(10) 0.0021(10) 0.0024(10)
C25 0.0144(12) 0.0247(13) 0.0291(14) 0.0001(10) 0.0000(10) 0.0089(11)
C26 0.0145(12) 0.0287(14) 0.0197(12) -0.0004(10) -0.0002(10) 0.0078(10)
C27 0.0159(12) 0.0434(17) 0.0229(14) 0.0043(12) -0.0032(10) 0.0086(12)
C28 0.0217(14) 0.0507(19) 0.0175(13) 0.0022(13) -0.0072(11) 0.0046(12)
C29 0.0192(13) 0.0350(15) 0.0143(12) -0.0020(11) -0.0019(10) 0.0022(10)
C30 0.0265(14) 0.0389(17) 0.0155(13) -0.0024(13) -0.0041(10) -0.0029(11)
C31 0.0242(13) 0.0312(14) 0.0145(12) -0.0029(11) 0.0007(10) -0.0049(10)
C32 0.0191(12) 0.0249(13) 0.0142(11) -0.0039(10) 0.0018(10) -0.0014(10)
C33 0.0147(11) 0.0258(13) 0.0131(11) -0.0025(10) -0.0016(9) 0.0032(10)
C34 0.0102(11) 0.0237(12) 0.0160(11) -0.0018(9) -0.0004(9) 0.0052(9)
C35 0.0252(13) 0.0159(12) 0.0253(13) 0.0000(10) -0.0033(11) -0.0024(10)
C36 0.0312(15) 0.0284(14) 0.0180(13) 0.0064(12) -0.0014(11) -0.0069(11)
P1 0.0207(3) 0.0297(4) 0.0191(3) -0.0029(3) 0.0029(3) 0.0051(3)
F1 0.0373(9) 0.0296(9) 0.0199(8) 0.0045(8) 0.0034(7) 0.0042(7)
F2 0.0260(9) 0.0885(17) 0.0234(9) 0.0076(10) 0.0055(7) 0.0220(10)
F3 0.0265(8) 0.0344(9) 0.0273(8) 0.0024(7) 0.0088(7) 0.0029(7)
F4 0.0410(11) 0.0407(11) 0.0429(11) 0.0032(9) 0.0030(9) -0.0189(9)
F5 0.0208(9) 0.0781(15) 0.0399(11) 0.0010(9) 0.0053(8) 0.0287(10)
F6 0.0563(13) 0.0248(10) 0.0696(15) -0.0129(9) -0.0256(12) 0.0134(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ir1 N3 . . 84.45(8) y
N1 Ir1 N4 . . 95.28(8) y
N2 Ir1 N1 . . 174.13(8) y
N2 Ir1 N3 . . 99.10(8) y
N2 Ir1 N4 . . 90.07(8) y
N3 Ir1 N4 . . 77.38(8) y
C1 Ir1 N1 . . 80.44(9) y
C1 Ir1 N2 . . 94.33(9) y
C1 Ir1 N3 . . 99.31(9) y
C1 Ir1 N4 . . 174.88(9) y
C12 Ir1 N1 . . 96.20(10) y
C12 Ir1 N2 . . 80.36(10) y
C12 Ir1 N3 . . 178.62(9) y
C12 Ir1 N4 . . 101.33(9) y
C12 Ir1 C1 . . 82.01(10) y
C7 N1 Ir1 . . 115.75(16) ?
C11 N1 Ir1 . . 124.85(17) ?
C11 N1 C7 . . 119.3(2) ?
C18 N2 Ir1 . . 115.82(18) ?
C22 N2 Ir1 . . 123.77(18) ?
C22 N2 C18 . . 120.4(2) ?
C23 N3 Ir1 . . 129.02(17) ?
C23 N3 C34 . . 117.9(2) ?
C34 N3 Ir1 . . 112.38(16) ?
C32 N4 Ir1 . . 130.48(18) ?
C32 N4 C33 . . 117.8(2) ?
C33 N4 Ir1 . . 111.72(16) ?
C2 C1 Ir1 . . 128.08(19) ?
C2 C1 C6 . . 117.6(2) ?
C6 C1 Ir1 . . 114.25(18) ?
C1 C2 H2 . . 119.6 ?
C3 C2 C1 . . 120.8(2) ?
C3 C2 H2 . . 119.6 ?
C2 C3 H3 . . 119.5 ?
C4 C3 C2 . . 121.0(2) ?
C4 C3 H3 . . 119.5 ?
C3 C4 H4 . . 120.3 ?
C5 C4 C3 . . 119.5(2) ?
C5 C4 H4 . . 120.3 ?
C4 C5 H5 . . 120.1 ?
C4 C5 C6 . . 119.8(2) ?
C6 C5 H5 . . 120.1 ?
C1 C6 C7 . . 115.5(2) ?
C5 C6 C1 . . 121.1(2) ?
C5 C6 C7 . . 123.2(2) ?
N1 C7 C6 . . 114.0(2) ?
N1 C7 C8 . . 120.3(2) ?
C8 C7 C6 . . 125.7(2) ?
C7 C8 H8 . . 120.1 ?
C9 C8 C7 . . 119.8(2) ?
C9 C8 H8 . . 120.1 ?
C8 C9 H9 . . 120.3 ?
C10 C9 C8 . . 119.3(2) ?
C10 C9 H9 . . 120.3 ?
C9 C10 H10 . . 120.6 ?
C11 C10 C9 . . 118.8(2) ?
C11 C10 H10 . . 120.6 ?
N1 C11 C10 . . 122.3(2) ?
N1 C11 H11 . . 118.8 ?
C10 C11 H11 . . 118.8 ?
C13 C12 Ir1 . . 127.9(2) ?
C13 C12 C17 . . 117.6(2) ?
C17 C12 Ir1 . . 114.48(19) ?
C12 C13 H13 . . 119.3 ?
C12 C13 C14 . . 121.4(3) ?
C14 C13 H13 . . 119.3 ?
C13 C14 H14 . . 120.1 ?
C15 C14 C13 . . 119.8(3) ?
C15 C14 H14 . . 120.1 ?
C14 C15 H15 . . 119.9 ?
C16 C15 C14 . . 120.2(3) ?
C16 C15 H15 . . 119.9 ?
C15 C16 H16 . . 120.1 ?
C15 C16 C17 . . 119.8(3) ?
C17 C16 H16 . . 120.1 ?
C12 C17 C18 . . 115.2(2) ?
C16 C17 C12 . . 121.1(3) ?
C16 C17 C18 . . 123.6(3) ?
N2 C18 C17 . . 114.1(2) ?
N2 C18 C19 . . 119.5(3) ?
C19 C18 C17 . . 126.3(3) ?
C18 C19 H19 . . 120.1 ?
C20 C19 C18 . . 119.9(3) ?
C20 C19 H19 . . 120.1 ?
C19 C20 H20 . . 120.1 ?
C19 C20 C21 . . 119.8(3) ?
C21 C20 H20 . . 120.1 ?
C20 C21 H21 . . 120.8 ?
C22 C21 C20 . . 118.4(3) ?
C22 C21 H21 . . 120.8 ?
N2 C22 C21 . . 122.0(3) ?
N2 C22 H22 . . 119.0 ?
C21 C22 H22 . . 119.0 ?
N3 C23 C24 . . 121.6(2) ?
N3 C23 C35 . . 120.6(2) ?
C24 C23 C35 . . 117.7(2) ?
C23 C24 H24 . . 119.8 ?
C25 C24 C23 . . 120.4(3) ?
C25 C24 H24 . . 119.8 ?
C24 C25 H25 . . 120.3 ?
C24 C25 C26 . . 119.5(2) ?
C26 C25 H25 . . 120.3 ?
C25 C26 C27 . . 121.9(3) ?
C25 C26 C34 . . 117.8(2) ?
C34 C26 C27 . . 120.3(3) ?
C26 C27 H27 . . 119.7 ?
C28 C27 C26 . . 120.6(3) ?
C28 C27 H27 . . 119.7 ?
C27 C28 H28 . . 119.6 ?
C27 C28 C29 . . 120.8(3) ?
C29 C28 H28 . . 119.6 ?
C30 C29 C28 . . 121.9(3) ?
C30 C29 C33 . . 117.6(3) ?
C33 C29 C28 . . 120.5(3) ?
C29 C30 H30 . . 120.1 ?
C31 C30 C29 . . 119.7(2) ?
C31 C30 H30 . . 120.1 ?
C30 C31 H31 . . 119.7 ?
C30 C31 C32 . . 120.6(3) ?
C32 C31 H31 . . 119.7 ?
N4 C32 C31 . . 121.7(3) ?
N4 C32 C36 . . 121.0(2) ?
C31 C32 C36 . . 117.3(2) ?
N4 C33 C29 . . 122.6(2) ?
N4 C33 C34 . . 118.9(2) ?
C29 C33 C34 . . 118.5(2) ?
N3 C34 C26 . . 122.5(2) ?
N3 C34 C33 . . 118.2(2) ?
C26 C34 C33 . . 119.3(2) ?
C23 C35 H35A . . 109.5 ?
C23 C35 H35B . . 109.5 ?
C23 C35 H35C . . 109.5 ?
H35A C35 H35B . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
C32 C36 H36A . . 109.5 ?
C32 C36 H36B . . 109.5 ?
C32 C36 H36C . . 109.5 ?
H36A C36 H36B . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
F2 P1 F1 . . 179.64(13) ?
F2 P1 F3 . . 89.89(10) ?
F2 P1 F4 . . 90.67(13) ?
F2 P1 F5 . . 90.71(10) ?
F2 P1 F6 . . 90.78(13) ?
F3 P1 F1 . . 90.29(9) ?
F3 P1 F4 . . 90.26(10) ?
F3 P1 F5 . . 179.38(11) ?
F3 P1 F6 . . 89.88(12) ?
F4 P1 F1 . . 89.01(11) ?
F5 P1 F1 . . 89.11(10) ?
F5 P1 F4 . . 89.62(12) ?
F6 P1 F1 . . 89.53(11) ?
F6 P1 F4 . . 178.54(12) ?
F6 P1 F5 . . 90.23(13) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ir1 N1 . 2.050(2) y
Ir1 N2 . 2.044(2) y
Ir1 N3 . 2.194(2) y
Ir1 N4 . 2.212(2) y
Ir1 C1 . 2.017(2) y
Ir1 C12 . 2.012(2) y
N1 C7 . 1.368(3) ?
N1 C11 . 1.347(3) ?
N2 C18 . 1.365(3) ?
N2 C22 . 1.346(3) ?
N3 C23 . 1.346(3) ?
N3 C34 . 1.375(3) ?
N4 C32 . 1.348(3) ?
N4 C33 . 1.378(3) ?
C1 C2 . 1.396(3) ?
C1 C6 . 1.414(4) ?
C2 H2 . 0.9500 ?
C2 C3 . 1.392(4) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.389(4) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.386(4) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.405(3) ?
C6 C7 . 1.460(4) ?
C7 C8 . 1.393(4) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.385(4) ?
C9 H9 . 0.9500 ?
C9 C10 . 1.385(4) ?
C10 H10 . 0.9500 ?
C10 C11 . 1.382(4) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.396(4) ?
C12 C17 . 1.411(4) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.401(4) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.392(5) ?
C15 H15 . 0.9500 ?
C15 C16 . 1.383(5) ?
C16 H16 . 0.9500 ?
C16 C17 . 1.404(4) ?
C17 C18 . 1.458(4) ?
C18 C19 . 1.396(4) ?
C19 H19 . 0.9500 ?
C19 C20 . 1.383(4) ?
C20 H20 . 0.9500 ?
C20 C21 . 1.391(4) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.381(4) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.410(4) ?
C23 C35 . 1.494(4) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.362(4) ?
C25 H25 . 0.9500 ?
C25 C26 . 1.400(4) ?
C26 C27 . 1.428(4) ?
C26 C34 . 1.413(3) ?
C27 H27 . 0.9500 ?
C27 C28 . 1.346(4) ?
C28 H28 . 0.9500 ?
C28 C29 . 1.426(4) ?
C29 C30 . 1.399(4) ?
C29 C33 . 1.416(4) ?
C30 H30 . 0.9500 ?
C30 C31 . 1.360(4) ?
C31 H31 . 0.9500 ?
C31 C32 . 1.408(4) ?
C32 C36 . 1.499(4) ?
C33 C34 . 1.436(4) ?
C35 H35A . 0.9800 ?
C35 H35B . 0.9800 ?
C35 H35C . 0.9800 ?
C36 H36A . 0.9800 ?
C36 H36B . 0.9800 ?
C36 H36C . 0.9800 ?
P1 F1 . 1.6118(17) ?
P1 F2 . 1.5932(19) ?
P1 F3 . 1.5943(18) ?
P1 F4 . 1.600(2) ?
P1 F5 . 1.599(2) ?
P1 F6 . 1.597(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C10 H10 F1 8_765 0.95 2.39 3.243(3) 149.6 yes
C11 H11 F3 8_765 0.95 2.46 3.229(3) 138.3 yes
C22 H22 F1 . 0.95 2.45 3.311(3) 150.4 yes
C27 H27 F2 4_556 0.95 2.36 3.192(3) 146.0 yes
C31 H31 F4 5_666 0.95 2.55 3.463(3) 160.4 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ir1 N1 C7 C6 . . . . -1.7(3) ?
Ir1 N1 C7 C8 . . . . -179.89(18) ?
Ir1 N1 C11 C10 . . . . 176.85(19) ?
Ir1 N2 C18 C17 . . . . -1.2(3) ?
Ir1 N2 C18 C19 . . . . 178.51(18) ?
Ir1 N2 C22 C21 . . . . -177.47(19) ?
Ir1 N3 C23 C24 . . . . 165.04(18) ?
Ir1 N3 C23 C35 . . . . -18.1(3) ?
Ir1 N3 C34 C26 . . . . -170.57(19) ?
Ir1 N3 C34 C33 . . . . 12.2(3) ?
Ir1 N4 C32 C31 . . . . -176.17(19) ?
Ir1 N4 C32 C36 . . . . 3.6(4) ?
Ir1 N4 C33 C29 . . . . 175.2(2) ?
Ir1 N4 C33 C34 . . . . -4.1(3) ?
Ir1 C1 C2 C3 . . . . -173.0(2) ?
Ir1 C1 C6 C5 . . . . 173.9(2) ?
Ir1 C1 C6 C7 . . . . -1.6(3) ?
Ir1 C12 C13 C14 . . . . -178.8(2) ?
Ir1 C12 C17 C16 . . . . 177.60(19) ?
Ir1 C12 C17 C18 . . . . 0.7(3) ?
N1 C7 C8 C9 . . . . 3.5(4) ?
N2 C18 C19 C20 . . . . -1.0(4) ?
N3 C23 C24 C25 . . . . 4.8(4) ?
N4 C33 C34 N3 . . . . -5.6(3) ?
N4 C33 C34 C26 . . . . 177.1(2) ?
C1 C2 C3 C4 . . . . -2.2(4) ?
C1 C6 C7 N1 . . . . 2.2(3) ?
C1 C6 C7 C8 . . . . -179.8(2) ?
C2 C1 C6 C5 . . . . -4.0(4) ?
C2 C1 C6 C7 . . . . -179.5(2) ?
C2 C3 C4 C5 . . . . -1.0(4) ?
C3 C4 C5 C6 . . . . 1.6(4) ?
C4 C5 C6 C1 . . . . 0.9(4) ?
C4 C5 C6 C7 . . . . 176.0(2) ?
C5 C6 C7 N1 . . . . -173.2(2) ?
C5 C6 C7 C8 . . . . 4.8(4) ?
C6 C1 C2 C3 . . . . 4.6(4) ?
C6 C7 C8 C9 . . . . -174.4(2) ?
C7 N1 C11 C10 . . . . 0.4(4) ?
C7 C8 C9 C10 . . . . -1.2(4) ?
C8 C9 C10 C11 . . . . -1.5(4) ?
C9 C10 C11 N1 . . . . 1.9(4) ?
C11 N1 C7 C6 . . . . 175.0(2) ?
C11 N1 C7 C8 . . . . -3.2(4) ?
C12 C13 C14 C15 . . . . 0.1(4) ?
C12 C17 C18 N2 . . . . 0.3(3) ?
C12 C17 C18 C19 . . . . -179.4(2) ?
C13 C12 C17 C16 . . . . -3.1(4) ?
C13 C12 C17 C18 . . . . 180.0(2) ?
C13 C14 C15 C16 . . . . -1.1(4) ?
C14 C15 C16 C17 . . . . 0.0(4) ?
C15 C16 C17 C12 . . . . 2.2(4) ?
C15 C16 C17 C18 . . . . 178.8(2) ?
C16 C17 C18 N2 . . . . -176.5(2) ?
C16 C17 C18 C19 . . . . 3.8(4) ?
C17 C12 C13 C14 . . . . 2.0(4) ?
C17 C18 C19 C20 . . . . 178.6(2) ?
C18 N2 C22 C21 . . . . 0.3(4) ?
C18 C19 C20 C21 . . . . 0.6(4) ?
C19 C20 C21 C22 . . . . 0.2(4) ?
C20 C21 C22 N2 . . . . -0.7(4) ?
C22 N2 C18 C17 . . . . -179.1(2) ?
C22 N2 C18 C19 . . . . 0.6(4) ?
C23 N3 C34 C26 . . . . 0.9(3) ?
C23 N3 C34 C33 . . . . -176.3(2) ?
C23 C24 C25 C26 . . . . -0.6(4) ?
C24 C25 C26 C27 . . . . 175.1(3) ?
C24 C25 C26 C34 . . . . -3.0(4) ?
C25 C26 C27 C28 . . . . -178.6(3) ?
C25 C26 C34 N3 . . . . 3.0(4) ?
C25 C26 C34 C33 . . . . -179.8(2) ?
C26 C27 C28 C29 . . . . -0.9(5) ?
C27 C26 C34 N3 . . . . -175.2(2) ?
C27 C26 C34 C33 . . . . 2.0(4) ?
C27 C28 C29 C30 . . . . -179.9(3) ?
C27 C28 C29 C33 . . . . 0.6(5) ?
C28 C29 C30 C31 . . . . -179.5(3) ?
C28 C29 C33 N4 . . . . -178.3(3) ?
C28 C29 C33 C34 . . . . 0.9(4) ?
C29 C30 C31 C32 . . . . -1.4(4) ?
C29 C33 C34 N3 . . . . 175.1(2) ?
C29 C33 C34 C26 . . . . -2.2(4) ?
C30 C29 C33 N4 . . . . 2.1(4) ?
C30 C29 C33 C34 . . . . -178.6(3) ?
C30 C31 C32 N4 . . . . 0.6(4) ?
C30 C31 C32 C36 . . . . -179.2(3) ?
C32 N4 C33 C29 . . . . -2.9(4) ?
C32 N4 C33 C34 . . . . 177.8(2) ?
C33 N4 C32 C31 . . . . 1.5(4) ?
C33 N4 C32 C36 . . . . -178.7(2) ?
C33 C29 C30 C31 . . . . 0.1(4) ?
C34 N3 C23 C24 . . . . -4.8(3) ?
C34 N3 C23 C35 . . . . 172.1(2) ?
C34 C26 C27 C28 . . . . -0.5(4) ?
C35 C23 C24 C25 . . . . -172.2(2) ?