#------------------------------------------------------------------------------
#$Date: 2025-04-30 03:53:31 +0200 (Wed, 30 Apr 2025) $
#$Revision: 299463 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023484.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_2023484
loop_
_publ_author_name
'Guseynova, Saadet N.'
'Samigullina, Aida I.'
'Demir, Cemile Baydere'
'Dege, Necmi'
'Sepay, Nayim'
'Zangrando, Ennio'
'Hasanov, Khudayar I.'
'Belay, Alebel N.'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of
2,2-dichloro-3,3-diethoxy-1-(4-fluorophenyl)propan-1-ol
;
_journal_coeditor_code OI2015
_journal_issue 5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 444
_journal_page_last 447
_journal_paper_doi 10.1107/S2056989025002154
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration ad
_chemical_formula_iupac 'C13 H17 Cl2 F O3'
_chemical_formula_moiety 'C13 H17 Cl2 F O3'
_chemical_formula_sum 'C13 H17 Cl2 F O3'
_chemical_formula_weight 311.16
_chemical_name_systematic
;
2,2-Dichloro-3,3-diethoxy-1-(4-fluorophenyl)propan-1-ol
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/2
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.5608(3)
_cell_length_b 10.8048(3)
_cell_length_c 12.8872(4)
_cell_measurement_reflns_used 13434
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 77.57
_cell_measurement_theta_min 3.44
_cell_volume 1470.52(7)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0316
_diffrn_reflns_av_unetI/netI 0.0203
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 15942
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.771
_diffrn_reflns_theta_min 5.342
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 4.099
_exptl_absorpt_correction_T_max 0.81000
_exptl_absorpt_correction_T_min 0.61074
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.405
_exptl_crystal_description block
_exptl_crystal_F_000 648
_exptl_crystal_size_max 0.150
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.080
_refine_diff_density_max 0.168
_refine_diff_density_min -0.183
_refine_ls_abs_structure_details
;
Flack x determined using 1296 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.001(6)
_refine_ls_extinction_coef 0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 241
_refine_ls_number_reflns 3123
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0247
_refine_ls_R_factor_gt 0.0247
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.5017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0654
_refine_ls_wR_factor_ref 0.0654
_reflns_number_gt 3111
_reflns_number_total 3123
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oi2015.cif
_cod_data_source_block I
_cod_database_code 2023484
_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 0.578
_shelx_estimated_absorpt_t_max 0.735
_shelx_hkl_file
;
0 0 1 2.29 0.58
0 0 2 7891.35 156.59
0 0 3 1.93 1.88
0 0 4 4679.42 99.16
0 0 5 4.38 2.16
0 0 6 3794.15 87.06
0 0 7 7.26 3.67
0 0 8 1580.28 48.11
0 0 9 2.91 1.47
0 0 9 3.86 3.87
0 0 -9 3.88 1.69
0 0 -9 0.21 1.25
0 0 10 330.87 11.31
0 0 10 308.69 20.29
0 0 -10 297.51 11.74
0 0 -11 0.75 1.78
0 0 11 0.61 1.79
0 0 11 0.54 3.52
0 0 -11 4.53 4.34
0 0 -12 725.59 37.62
0 0 12 744.54 21.58
0 0 12 785.15 21.36
0 0 -12 755.32 22.37
0 0 13 0.11 1.51
0 0 13 -1.15 1.87
0 0 -13 -0.28 1.63
0 0 13 -0.65 1.98
0 0 14 344.01 11.07
0 0 14 335.55 11.54
0 0 -14 351.24 12.03
0 0 14 337.06 11.45
0 0 15 0.15 1.07
0 0 15 -0.63 1.33
0 0 16 185.78 5.71
0 -1 0 1.67 0.49
0 -1 1 1449.32 29.77
0 1 1 1411.13 29.75
0 -1 -1 1436.05 31.03
0 1 2 2060.15 44.14
0 -1 2 2075.24 44.18
0 -1 3 2269.26 49.88
0 1 3 2231.98 49.76
0 1 4 281.49 11.54
0 -1 4 276.40 11.48
0 1 5 2744.31 63.42
0 -1 5 2688.49 63.40
0 -1 6 187.99 11.48
0 1 6 205.50 11.79
0 -1 7 2601.13 68.23
0 1 7 2830.36 69.12
0 1 8 799.99 30.34
0 -1 8 739.44 29.57
0 1 -9 523.90 15.71
0 1 -9 497.58 15.66
0 -1 -9 497.44 15.65
0 -1 -9 488.15 15.50
0 -1 -9 495.41 15.48
0 -1 9 521.96 15.56
0 -1 -9 544.32 27.88
0 1 9 523.84 16.00
0 -1 9 526.69 15.87
0 1 9 546.77 15.16
0 -1 9 576.47 15.41
0 1 9 538.84 25.78
0 -1 9 563.41 26.39
0 -1 -10 33.22 3.64
0 1 -10 36.97 3.79
0 1 -10 30.97 3.65
0 -1 -10 37.18 3.78
0 -1 -10 36.00 3.87
0 -1 10 36.57 3.67
0 -1 -10 32.95 7.73
0 1 10 39.71 7.61
0 -1 10 37.59 7.35
0 1 10 39.13 3.68
0 -1 10 33.45 3.49
0 1 10 41.00 4.09
0 -1 10 37.04 3.88
0 -1 -11 457.72 15.85
0 1 -11 477.95 16.00
0 -1 -11 481.14 15.87
0 1 -11 485.53 16.05
0 1 11 469.84 16.07
0 -1 11 484.21 15.52
0 -1 -11 476.73 28.71
0 -1 11 454.94 14.79
0 1 11 475.04 14.94
0 1 11 464.80 26.41
0 -1 11 474.94 26.77
0 1 -12 16.07 3.02
0 1 -12 12.58 2.73
0 -1 -12 14.85 2.80
0 -1 -12 14.48 6.02
0 1 -12 19.97 6.17
0 -1 12 14.00 2.81
0 -1 12 11.72 2.60
0 -1 12 14.25 2.68
0 1 12 16.67 2.81
0 1 12 13.79 2.90
0 1 -13 43.63 4.26
0 1 13 39.80 4.16
0 -1 13 37.76 3.63
0 1 13 41.59 3.80
0 -1 13 39.50 4.15
0 -1 13 41.15 4.00
0 -1 14 0.65 1.52
0 1 14 2.83 1.57
0 -1 14 1.23 1.60
0 1 14 0.35 1.51
0 -1 15 29.08 2.70
0 1 15 29.37 2.71
0 -1 15 30.27 2.63
0 1 15 28.46 2.69
0 -1 15 25.56 2.60
0 1 16 6.19 1.06
0 -1 16 6.84 1.08
0 -2 0 175.77 6.81
0 2 1 272.04 7.25
0 -2 1 283.71 7.32
0 2 2 9077.99 182.07
0 -2 2 9351.56 182.22
0 -2 -2 9258.67 185.19
0 2 3 183.88 7.91
0 -2 3 183.32 7.87
0 -2 -3 179.35 8.97
0 2 4 3202.61 71.15
0 -2 4 3327.96 71.50
0 -2 -4 3183.64 73.53
0 -2 5 125.08 8.14
0 2 5 119.87 7.96
0 -2 -5 115.71 8.84
0 2 6 507.18 20.12
0 -2 6 546.17 20.90
0 -2 -6 527.25 22.32
0 -2 -7 19.67 4.71
0 -2 7 14.18 3.80
0 2 7 17.56 4.11
0 2 -8 80.65 4.75
0 -2 -8 82.80 5.13
0 -2 -8 78.61 9.53
0 -2 8 99.02 9.88
0 2 8 97.34 9.56
0 -2 8 83.46 4.88
0 -2 8 100.26 5.10
0 -2 9 605.31 17.41
0 -2 9 585.26 16.90
0 -2 -9 565.67 17.14
0 -2 -9 559.82 17.40
0 2 -9 567.41 17.10
0 2 -9 589.52 17.15
0 -2 -9 572.04 16.88
0 -2 -9 638.11 30.57
0 2 9 607.47 16.52
0 -2 9 644.54 16.86
0 -2 9 645.03 28.44
0 2 9 596.80 27.37
0 -2 10 41.60 4.06
0 2 10 37.19 3.99
0 -2 10 35.86 3.66
0 -2 10 35.88 3.68
0 -2 -10 37.91 3.93
0 2 -10 38.31 3.88
0 2 -10 38.09 3.86
0 -2 -10 36.35 3.70
0 -2 -10 45.03 8.38
0 2 10 38.26 3.56
0 -2 10 38.35 3.64
0 -2 10 37.63 7.51
0 2 10 42.52 7.80
0 -2 11 264.91 10.53
0 2 -11 296.28 11.82
0 -2 -11 296.94 11.65
0 -2 -11 297.89 11.95
0 2 -11 316.42 12.04
0 -2 11 305.90 11.59
0 -2 11 312.67 11.87
0 -2 11 293.07 11.82
0 2 11 302.76 12.22
0 -2 -11 338.25 23.51
0 -2 11 337.42 21.85
0 2 11 313.48 21.03
0 2 11 313.15 11.27
0 -2 11 321.97 11.40
0 -2 -12 181.42 9.02
0 -2 -12 177.03 8.74
0 2 -12 200.38 9.31
0 -2 12 200.03 8.97
0 -2 12 193.18 9.19
0 2 12 193.88 9.35
0 -2 -12 175.54 17.52
0 -2 12 193.29 8.55
0 2 12 199.21 8.56
0 -2 12 198.16 9.11
0 2 13 115.75 6.79
0 -2 13 120.63 6.77
0 -2 13 114.73 6.35
0 2 13 113.47 6.02
0 -2 13 108.78 5.92
0 2 -13 116.42 6.60
0 -2 -13 121.70 6.82
0 -2 13 112.36 6.60
0 -2 14 2.42 1.54
0 -2 14 1.27 1.43
0 2 14 0.88 1.53
0 -2 14 2.50 1.73
0 -2 15 0.60 1.14
0 2 15 0.91 1.22
0 -2 15 0.51 1.32
0 2 15 0.46 1.18
0 2 16 26.57 1.83
0 -3 0 1.71 1.39
0 -3 1 4375.41 90.99
0 -3 -1 4229.41 90.81
0 -3 2 2345.75 49.03
0 3 2 2319.91 49.02
0 -3 -2 2348.45 53.97
0 3 3 4561.74 95.69
0 -3 3 4703.14 95.80
0 -3 -3 4640.14 100.58
0 -3 4 2536.83 56.63
0 3 4 2441.55 56.39
0 -3 -4 2478.37 60.54
0 3 5 1722.49 44.46
0 -3 5 1820.65 44.95
0 -3 -5 1756.22 48.26
0 3 6 6.28 2.42
0 -3 6 6.36 2.65
0 -3 -6 3.68 2.51
0 -3 -7 89.16 9.69
0 3 7 105.33 9.29
0 -3 7 110.04 9.37
0 -3 7 96.56 4.56
0 3 8 13.27 2.00
0 -3 8 14.84 2.09
0 3 -8 14.88 2.16
0 -3 -8 27.16 3.21
0 -3 -8 14.09 2.18
0 -3 -8 15.09 2.11
0 3 -8 11.47 1.95
0 -3 -8 11.59 2.10
0 -3 -8 19.02 5.45
0 -3 8 13.67 2.31
0 -3 8 15.48 2.17
0 -3 8 13.12 4.22
0 3 8 14.05 4.05
0 -3 8 14.52 2.22
0 -3 9 8.14 1.92
0 -3 -9 7.41 2.27
0 -3 9 10.76 2.21
0 -3 -9 8.56 4.25
0 -3 9 11.58 2.32
0 -3 -9 6.70 1.90
0 -3 -9 13.32 2.20
0 3 -9 3.39 1.51
0 3 -9 4.88 1.77
0 -3 9 7.14 1.85
0 -3 9 4.80 3.71
0 3 9 7.76 3.61
0 3 9 7.43 1.82
0 -3 10 66.21 4.85
0 3 10 71.84 5.37
0 -3 10 74.41 5.27
0 -3 10 71.10 5.05
0 -3 10 67.23 5.11
0 -3 -10 69.58 5.10
0 3 -10 67.66 4.98
0 3 -10 71.92 5.15
0 -3 -10 68.16 4.92
0 -3 -10 75.36 10.68
0 -3 10 71.73 9.82
0 3 10 82.74 10.26
0 -3 10 73.85 4.83
0 3 10 71.57 4.81
0 -3 11 181.86 8.54
0 3 11 201.73 9.67
0 -3 11 206.24 9.43
0 -3 11 206.97 9.15
0 -3 -11 208.09 18.73
0 -3 11 223.50 9.75
0 -3 -11 212.95 9.47
0 -3 -11 209.80 9.22
0 3 -11 214.10 9.41
0 -3 11 233.13 9.21
0 3 11 215.00 8.91
0 3 -12 22.47 3.11
0 -3 -12 21.52 3.06
0 -3 12 22.91 3.19
0 3 12 25.74 3.47
0 -3 12 24.66 3.19
0 -3 -12 30.91 7.41
0 -3 12 25.09 3.43
0 -3 12 23.40 2.85
0 3 12 24.04 2.99
0 -3 12 27.60 3.07
0 3 13 1.42 1.76
0 -3 13 1.09 1.55
0 -3 13 1.47 1.70
0 3 13 2.03 1.75
0 -3 13 2.82 1.77
0 3 13 2.75 1.47
0 -3 13 2.53 1.44
0 -3 -13 1.77 1.44
0 3 -13 3.54 1.54
0 3 14 367.51 11.82
0 -3 14 380.61 11.48
0 3 14 398.37 11.79
0 -3 14 372.29 11.75
0 3 -15 107.92 4.32
0 3 15 96.36 4.45
0 -3 15 98.70 4.34
0 3 15 94.83 4.44
0 3 15 98.85 4.56
0 -4 0 2507.44 58.77
0 -4 -1 963.12 28.13
0 -4 1 987.65 28.37
0 -4 2 755.87 23.99
0 -4 -2 727.50 23.90
0 -4 -3 86.43 7.34
0 -4 3 82.58 3.67
0 -4 3 90.88 5.07
0 4 3 83.81 4.94
0 -4 -4 687.61 25.20
0 -4 4 701.31 20.40
0 4 4 653.38 20.17
0 -4 -5 208.96 13.33
0 4 5 195.75 10.49
0 -4 5 200.39 10.47
0 4 6 116.02 8.85
0 4 6 114.87 4.68
0 -4 6 123.82 4.80
0 -4 -6 118.35 10.78
0 4 7 398.86 11.06
0 -4 7 389.76 10.98
0 -4 -7 386.97 21.48
0 -4 7 360.97 11.98
0 4 7 412.82 18.98
0 -4 7 420.74 19.15
0 -4 -7 364.18 11.91
0 -4 7 383.58 12.12
0 -4 7 371.91 11.64
0 -4 -8 783.25 20.82
0 -4 -8 886.33 36.49
0 -4 8 804.01 22.06
0 -4 8 938.96 33.03
0 4 8 887.39 32.36
0 -4 8 846.57 22.16
0 -4 -8 801.32 21.19
0 -4 -8 829.07 22.81
0 -4 -8 778.96 20.79
0 4 -8 844.00 21.46
0 4 -8 864.32 21.67
0 -4 8 849.40 21.96
0 -4 8 839.51 21.69
0 -4 -8 865.11 22.24
0 -4 8 925.80 21.13
0 4 8 841.25 20.80
0 -4 -9 274.60 9.85
0 -4 9 305.47 11.26
0 -4 -9 293.79 10.69
0 -4 -9 281.94 10.34
0 4 -9 309.95 10.89
0 4 -9 311.53 11.02
0 -4 9 294.14 11.02
0 -4 9 299.59 10.92
0 -4 9 302.77 11.35
0 4 9 312.72 18.99
0 -4 9 319.07 19.33
0 -4 9 326.85 10.51
0 4 9 311.29 10.35
0 -4 -9 307.34 11.37
0 -4 -9 359.56 22.92
0 -4 -10 1174.08 28.94
0 4 -10 1169.55 28.96
0 -4 -10 1116.02 28.39
0 -4 10 1136.04 28.98
0 -4 10 1103.63 29.05
0 -4 10 1148.88 29.36
0 -4 -10 1179.23 46.96
0 -4 10 1148.81 29.61
0 -4 10 1221.65 28.44
0 4 10 1201.76 28.41
0 -4 -11 73.83 5.13
0 4 -11 72.79 5.06
0 -4 -11 72.28 4.98
0 4 11 68.86 5.39
0 -4 11 69.62 5.27
0 -4 11 71.27 5.19
0 -4 11 70.70 5.11
0 -4 -11 72.18 10.92
0 -4 11 76.71 5.59
0 4 11 72.37 4.77
0 -4 11 75.13 4.77
0 -4 12 121.01 6.52
0 4 12 119.28 5.96
0 -4 12 119.77 5.90
0 -4 -12 125.19 6.43
0 4 -12 119.95 6.27
0 -4 12 97.38 5.79
0 -4 12 115.33 6.75
0 4 12 109.41 6.62
0 4 13 98.29 5.75
0 -4 13 104.03 5.60
0 4 14 10.17 1.94
0 -4 -14 11.63 1.70
0 -4 14 11.88 1.94
0 4 14 12.87 2.09
0 4 15 0.88 0.94
0 4 15 1.19 0.88
0 4 -15 1.12 0.96
0 4 15 0.42 0.91
0 -5 0 2.00 1.92
0 -5 1 385.55 17.00
0 -5 -1 372.84 16.92
0 -5 2 2460.31 51.67
0 -5 2 2584.39 62.82
0 -5 -2 2602.08 63.27
0 -5 3 3939.98 79.96
0 -5 -3 3933.02 92.76
0 -5 -4 19.11 4.20
0 -5 -5 2949.44 58.87
0 -5 -5 3007.38 75.92
0 -5 6 855.88 21.49
0 -5 -6 802.94 21.11
0 -5 -6 871.14 33.94
0 -5 7 1075.80 23.43
0 -5 7 950.00 25.12
0 -5 -7 1048.81 39.88
0 -5 -7 994.66 25.23
0 -5 7 1049.60 25.68
0 -5 -7 949.47 24.64
0 -5 7 982.46 24.81
0 -5 8 80.63 4.31
0 5 8 81.06 4.42
0 -5 -8 83.43 5.32
0 -5 8 73.13 5.04
0 -5 -8 86.18 10.93
0 -5 8 76.53 4.95
0 -5 8 82.85 5.38
0 -5 -8 72.62 4.73
0 -5 -9 11.16 2.02
0 -5 9 16.56 2.81
0 -5 9 14.44 2.65
0 -5 -9 11.02 1.91
0 -5 -9 20.53 3.12
0 -5 9 20.29 2.93
0 -5 -9 14.65 5.50
0 5 9 12.63 2.00
0 -5 9 14.22 2.04
0 -5 -10 803.83 37.85
0 -5 10 789.81 21.67
0 -5 10 769.09 21.98
0 -5 -10 721.18 20.10
0 5 10 814.17 20.34
0 -5 10 814.90 20.18
0 -5 -10 807.77 20.75
0 -5 11 76.17 5.33
0 -5 -11 76.96 11.15
0 5 11 78.33 5.58
0 -5 11 81.71 5.46
0 5 12 22.04 3.05
0 -5 12 21.07 2.82
0 -5 12 19.33 2.88
0 5 13 5.14 1.77
0 -5 13 4.81 1.73
0 5 14 7.02 1.45
0 5 14 5.26 1.46
0 -5 -14 8.26 1.43
0 -5 14 6.04 1.44
0 5 -15 7.32 0.98
0 5 15 6.42 1.04
0 -6 0 995.86 33.99
0 -6 1 6138.35 135.29
0 -6 -1 6345.28 136.74
0 -6 1 5973.74 120.98
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12 5 2 96.29 3.78
12 5 3 51.04 2.51
-12 -5 3 60.34 3.02
-12 -5 4 64.84 2.96
12 6 0 42.39 2.19
13 0 0 -0.19 0.92
13 0 1 323.86 8.63
13 0 2 59.48 2.76
13 0 -2 61.57 2.83
13 0 3 10.68 1.22
13 -1 3 87.47 3.33
13 -1 2 13.34 1.36
13 1 -2 13.95 1.42
13 -1 1 103.32 3.95
13 -1 0 2.83 1.09
13 1 0 3.55 1.07
13 1 1 106.13 4.01
13 -1 -2 8.65 1.19
13 1 2 8.69 1.19
13 1 3 82.00 3.17
13 -2 2 166.23 4.90
13 2 -2 170.74 5.05
13 -2 1 27.10 1.85
13 -2 0 56.01 2.71
13 2 0 51.25 2.63
13 -2 -1 23.21 1.74
13 2 1 20.56 1.67
13 -2 -2 166.82 4.92
13 2 2 161.38 4.82
13 -3 1 18.54 1.45
13 3 -1 21.23 1.52
13 -3 0 0.06 0.67
13 3 0 0.26 0.66
13 -3 -1 12.83 1.27
13 3 1 15.05 1.27
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 56179
_shelx_res_file
;
TITL GF5_a.res in P2(1)2(1)2(1)
shelx.res
created by SHELXL-2019/2 at 20:02:15 on 05-Dec-2024
CELL 1.54184 10.5608 10.8048 12.8872 90 90 90
ZERR 4 0.0001 0.0001 0.0001 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 Cl F O
UNIT 52 68 8 4 12
EQIV $1 1-X,0.5+Y,0.5-Z
L.S. 10
PLAN 5
SIZE 0.15 0.08 0.12
TEMP -173
CONF
HTAB O1 O2_$1
HTAB O1 O3_$1
BOND
BOND $H
fmap 2
acta
WGHT 0.033200 0.501700
EXTI 0.002198
FVAR 0.96586
CL1 3 0.213245 0.290369 0.370039 11.00000 0.02327 0.02939 =
0.03612 0.00581 0.00838 0.00382
CL2 3 0.300118 0.136876 0.199281 11.00000 0.02670 0.02181 =
0.04432 -0.00790 -0.00735 -0.00018
F1 4 -0.116688 0.503285 0.006125 11.00000 0.03303 0.04701 =
0.03805 0.00367 -0.00910 0.01088
O1 5 0.385466 0.481111 0.268195 11.00000 0.03216 0.02093 =
0.03918 0.00057 -0.00522 -0.00886
H1 2 0.429937 0.530638 0.236369 11.00000 0.06658
O2 5 0.465881 0.131106 0.382225 11.00000 0.02926 0.02319 =
0.02420 -0.00018 0.00348 -0.00006
O3 5 0.556864 0.255017 0.261447 11.00000 0.01702 0.02802 =
0.02700 -0.00200 0.00153 -0.00203
C1 1 0.460894 0.248895 0.335295 11.00000 0.02213 0.02234 =
0.02646 -0.00244 0.00416 -0.00081
H1A 2 0.468951 0.314987 0.388041 11.00000 0.03205
C2 1 0.335629 0.269696 0.275325 11.00000 0.02006 0.02095 =
0.03055 -0.00323 0.00317 -0.00153
C3 1 0.343196 0.384038 0.203777 11.00000 0.02194 0.02459 =
0.02808 -0.00186 0.00131 -0.00311
H3 2 0.409727 0.362828 0.149444 11.00000 0.03300
C4 1 0.219369 0.415428 0.150135 11.00000 0.02260 0.02312 =
0.02778 0.00219 0.00260 -0.00200
C5 1 0.133627 0.495911 0.196643 11.00000 0.02910 0.02172 =
0.02899 -0.00022 0.00122 -0.00163
H5 2 0.152583 0.530267 0.261318 11.00000 0.02439
C6 1 0.019995 0.525906 0.148524 11.00000 0.02738 0.02418 =
0.03227 0.00360 0.00286 0.00341
H6 2 -0.043756 0.580081 0.177335 11.00000 0.03647
C7 1 -0.004901 0.474120 0.052748 11.00000 0.02604 0.03214 =
0.03201 0.00901 -0.00154 0.00142
C8 1 0.076966 0.394916 0.003101 11.00000 0.03298 0.03586 =
0.02697 -0.00073 -0.00064 0.00351
H8 2 0.055443 0.361216 -0.067695 11.00000 0.04252
C9 1 0.190327 0.366375 0.052707 11.00000 0.02755 0.03250 =
0.02747 -0.00082 0.00272 0.00199
H9 2 0.248026 0.310176 0.020522 11.00000 0.03129
C10 1 0.433598 0.124011 0.490595 11.00000 0.03097 0.04439 =
0.02291 0.00210 0.00226 0.00528
H10A 2 0.477139 0.194286 0.527835 11.00000 0.03268
H10B 2 0.339199 0.135200 0.499942 11.00000 0.05508
C11 1 0.472817 -0.000089 0.530608 11.00000 0.03779 0.04097 =
0.02808 0.00498 0.00021 -0.00373
H11A 2 0.436484 -0.063804 0.491535 11.00000 0.03808
H11B 2 0.451518 -0.004451 0.603532 11.00000 0.05017
H11C 2 0.564963 -0.007986 0.519684 11.00000 0.04573
C12 1 0.679113 0.282032 0.305124 11.00000 0.01943 0.02475 =
0.03160 -0.00236 -0.00013 -0.00362
H12A 2 0.708523 0.210193 0.349463 11.00000 0.02920
H12B 2 0.671232 0.360570 0.349934 11.00000 0.04103
C13 1 0.769697 0.303075 0.216708 11.00000 0.02210 0.03468 =
0.03742 0.00534 0.00387 -0.00305
H13A 2 0.854461 0.315066 0.243193 11.00000 0.03450
H13B 2 0.740554 0.375873 0.179824 11.00000 0.04791
H13C 2 0.771638 0.229735 0.171885 11.00000 0.03969
HKLF 4
REM GF5_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0654, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0247 for 3111 Fo > 4sig(Fo) and 0.0247 for all 3123 data
REM 241 parameters refined using 0 restraints
END
WGHT 0.0332 0.5017
REM Highest difference peak 0.168, deepest hole -0.183, 1-sigma level 0.039
Q1 1 0.0423 0.4584 0.0207 11.00000 0.05 0.17
Q2 1 0.2753 0.4049 0.1758 11.00000 0.05 0.16
Q3 1 0.2255 0.1872 0.3661 11.00000 0.05 0.16
Q4 1 0.2127 0.2132 0.1921 11.00000 0.05 0.15
Q5 1 0.2092 0.2750 0.2831 11.00000 0.05 0.15
;
_shelx_res_checksum 77999
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'
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
Cl Cl1 0.21324(5) 0.29037(5) 0.37004(4) 0.02959(15) Uani d 1 . .
Cl Cl2 0.30012(5) 0.13688(5) 0.19928(5) 0.03094(15) Uani d 1 . .
F F1 -0.11669(14) 0.50329(16) 0.00613(12) 0.0394(4) Uani d 1 . .
O O1 0.38547(17) 0.48111(15) 0.26820(14) 0.0308(4) Uani d 1 . .
H H1 0.430(4) 0.531(4) 0.236(3) 0.067(13) Uiso d 1 . .
O O2 0.46588(15) 0.13111(14) 0.38223(12) 0.0255(3) Uani d 1 . .
O O3 0.55686(14) 0.25502(14) 0.26145(12) 0.0240(3) Uani d 1 . .
C C1 0.4609(2) 0.2489(2) 0.33530(17) 0.0236(4) Uani d 1 . .
H H1A 0.469(3) 0.315(3) 0.388(2) 0.032(7) Uiso d 1 . .
C C2 0.3356(2) 0.2697(2) 0.27532(18) 0.0239(4) Uani d 1 . .
C C3 0.3432(2) 0.3840(2) 0.20378(18) 0.0249(4) Uani d 1 . .
H H3 0.410(3) 0.363(3) 0.149(2) 0.033(8) Uiso d 1 . .
C C4 0.2194(2) 0.41543(19) 0.15014(17) 0.0245(4) Uani d 1 . .
C C5 0.1336(2) 0.4959(2) 0.19664(19) 0.0266(4) Uani d 1 . .
H H5 0.153(3) 0.530(3) 0.261(2) 0.024(7) Uiso d 1 . .
C C6 0.0200(2) 0.5259(2) 0.14852(19) 0.0279(5) Uani d 1 . .
H H6 -0.044(3) 0.580(3) 0.177(2) 0.036(8) Uiso d 1 . .
C C7 -0.0049(2) 0.4741(2) 0.05275(19) 0.0301(5) Uani d 1 . .
C C8 0.0770(2) 0.3949(2) 0.00310(18) 0.0319(5) Uani d 1 . .
H H8 0.055(3) 0.361(3) -0.068(3) 0.043(8) Uiso d 1 . .
C C9 0.1903(2) 0.3664(2) 0.05271(18) 0.0292(5) Uani d 1 . .
H H9 0.248(3) 0.310(3) 0.021(2) 0.031(7) Uiso d 1 . .
C C10 0.4336(2) 0.1240(3) 0.49060(18) 0.0328(5) Uani d 1 . .
H H10A 0.477(3) 0.194(3) 0.528(2) 0.033(7) Uiso d 1 . .
H H10B 0.339(4) 0.135(4) 0.500(3) 0.055(10) Uiso d 1 . .
C C11 0.4728(3) -0.0001(3) 0.5306(2) 0.0356(6) Uani d 1 . .
H H11A 0.436(3) -0.064(3) 0.492(3) 0.038(8) Uiso d 1 . .
H H11B 0.452(3) -0.004(3) 0.604(3) 0.050(9) Uiso d 1 . .
H H11C 0.565(3) -0.008(3) 0.520(3) 0.046(9) Uiso d 1 . .
C C12 0.67911(19) 0.2820(2) 0.30512(18) 0.0253(4) Uani d 1 . .
H H12A 0.709(3) 0.210(3) 0.349(2) 0.029(7) Uiso d 1 . .
H H12B 0.671(3) 0.361(3) 0.350(3) 0.041(8) Uiso d 1 . .
C C13 0.7697(2) 0.3031(2) 0.2167(2) 0.0314(5) Uani d 1 . .
H H13A 0.854(3) 0.315(3) 0.243(2) 0.035(8) Uiso d 1 . .
H H13B 0.741(3) 0.376(3) 0.180(3) 0.048(9) Uiso d 1 . .
H H13C 0.772(3) 0.230(3) 0.172(2) 0.040(8) Uiso 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
Cl1 0.0233(2) 0.0294(3) 0.0361(3) 0.0038(2) 0.0084(2) 0.0058(2)
Cl2 0.0267(3) 0.0218(2) 0.0443(3) -0.0002(2) -0.0073(2) -0.0079(2)
F1 0.0330(8) 0.0470(9) 0.0381(8) 0.0109(7) -0.0091(6) 0.0037(7)
O1 0.0322(9) 0.0209(7) 0.0392(9) -0.0089(7) -0.0052(7) 0.0006(7)
O2 0.0293(7) 0.0232(7) 0.0242(7) -0.0001(6) 0.0035(6) -0.0002(6)
O3 0.0170(7) 0.0280(8) 0.0270(7) -0.0020(6) 0.0015(6) -0.0020(6)
C1 0.0221(10) 0.0223(10) 0.0265(10) -0.0008(8) 0.0042(8) -0.0024(8)
C2 0.0201(9) 0.0209(10) 0.0305(10) -0.0015(8) 0.0032(8) -0.0032(8)
C3 0.0219(9) 0.0246(10) 0.0281(10) -0.0031(8) 0.0013(8) -0.0019(9)
C4 0.0226(10) 0.0231(10) 0.0278(10) -0.0020(8) 0.0026(8) 0.0022(8)
C5 0.0291(11) 0.0217(10) 0.0290(11) -0.0016(9) 0.0012(9) -0.0002(9)
C6 0.0274(11) 0.0242(10) 0.0323(11) 0.0034(9) 0.0029(9) 0.0036(9)
C7 0.0260(11) 0.0321(12) 0.0320(11) 0.0014(9) -0.0015(9) 0.0090(10)
C8 0.0330(12) 0.0359(13) 0.0270(12) 0.0035(10) -0.0006(9) -0.0007(10)
C9 0.0275(11) 0.0325(11) 0.0275(10) 0.0020(10) 0.0027(9) -0.0008(9)
C10 0.0310(12) 0.0444(14) 0.0229(11) 0.0053(11) 0.0023(9) 0.0021(10)
C11 0.0378(14) 0.0410(14) 0.0281(12) -0.0037(11) 0.0002(10) 0.0050(10)
C12 0.0194(10) 0.0248(10) 0.0316(10) -0.0036(8) -0.0001(8) -0.0024(9)
C13 0.0221(11) 0.0347(12) 0.0374(12) -0.0030(9) 0.0039(9) 0.0053(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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 '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
C3 O1 H1 . . 112(3) ?
C1 O2 C10 . . 117.08(18) ?
C1 O3 C12 . . 113.31(17) ?
O3 C1 O2 . . 108.00(16) ?
O3 C1 C2 . . 105.90(17) ?
O2 C1 C2 . . 112.15(17) ?
O3 C1 H1A . . 111.9(18) ?
O2 C1 H1A . . 110.7(18) ?
C2 C1 H1A . . 108.2(18) ?
C3 C2 C1 . . 111.72(17) ?
C3 C2 Cl2 . . 109.13(16) ?
C1 C2 Cl2 . . 109.77(14) ?
C3 C2 Cl1 . . 110.15(15) ?
C1 C2 Cl1 . . 107.12(15) ?
Cl2 C2 Cl1 . . 108.90(11) ?
O1 C3 C4 . . 112.01(18) ?
O1 C3 C2 . . 105.07(18) ?
C4 C3 C2 . . 113.98(17) ?
O1 C3 H3 . . 110.7(17) ?
C4 C3 H3 . . 109.4(17) ?
C2 C3 H3 . . 105.5(18) ?
C5 C4 C9 . . 118.8(2) ?
C5 C4 C3 . . 120.3(2) ?
C9 C4 C3 . . 120.9(2) ?
C6 C5 C4 . . 121.1(2) ?
C6 C5 H5 . . 119.4(17) ?
C4 C5 H5 . . 119.6(17) ?
C7 C6 C5 . . 118.0(2) ?
C7 C6 H6 . . 117.2(19) ?
C5 C6 H6 . . 124.9(19) ?
F1 C7 C8 . . 119.0(2) ?
F1 C7 C6 . . 117.8(2) ?
C8 C7 C6 . . 123.3(2) ?
C7 C8 C9 . . 117.7(2) ?
C7 C8 H8 . . 120(2) ?
C9 C8 H8 . . 122(2) ?
C8 C9 C4 . . 121.2(2) ?
C8 C9 H9 . . 119.4(18) ?
C4 C9 H9 . . 119.4(18) ?
O2 C10 C11 . . 108.5(2) ?
O2 C10 H10A . . 108.3(18) ?
C11 C10 H10A . . 112.6(17) ?
O2 C10 H10B . . 110(2) ?
C11 C10 H10B . . 110(2) ?
H10A C10 H10B . . 108(3) ?
C10 C11 H11A . . 111(2) ?
C10 C11 H11B . . 108(2) ?
H11A C11 H11B . . 113(3) ?
C10 C11 H11C . . 108(2) ?
H11A C11 H11C . . 105(3) ?
H11B C11 H11C . . 111(3) ?
O3 C12 C13 . . 107.75(19) ?
O3 C12 H12A . . 109.9(16) ?
C13 C12 H12A . . 110.4(16) ?
O3 C12 H12B . . 108.3(18) ?
C13 C12 H12B . . 110.6(18) ?
H12A C12 H12B . . 110(2) ?
C12 C13 H13A . . 110.0(19) ?
C12 C13 H13B . . 107(2) ?
H13A C13 H13B . . 111(3) ?
C12 C13 H13C . . 109.7(18) ?
H13A C13 H13C . . 107(3) ?
H13B C13 H13C . . 112(3) ?
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
Cl1 C2 . 1.792(2) ?
Cl2 C2 . 1.778(2) ?
F1 C7 . 1.362(3) ?
O1 C3 . 1.410(3) ?
O1 H1 . 0.82(5) ?
O2 C1 . 1.410(3) ?
O2 C10 . 1.440(3) ?
O3 C1 . 1.392(3) ?
O3 C12 . 1.438(3) ?
C1 C2 . 1.549(3) ?
C1 H1A . 0.99(3) ?
C2 C3 . 1.544(3) ?
C3 C4 . 1.518(3) ?
C3 H3 . 1.02(3) ?
C4 C5 . 1.391(3) ?
C4 C9 . 1.397(3) ?
C5 C6 . 1.389(3) ?
C5 H5 . 0.93(3) ?
C6 C7 . 1.380(4) ?
C6 H6 . 0.97(3) ?
C7 C8 . 1.374(4) ?
C8 C9 . 1.392(3) ?
C8 H8 . 1.01(4) ?
C9 H9 . 0.96(3) ?
C10 C11 . 1.495(4) ?
C10 H10A . 1.01(3) ?
C10 H10B . 1.01(4) ?
C11 H11A . 0.94(3) ?
C11 H11B . 0.97(4) ?
C11 H11C . 0.99(4) ?
C12 C13 . 1.505(3) ?
C12 H12A . 1.01(3) ?
C12 H12B . 1.03(3) ?
C13 H13A . 0.97(3) ?
C13 H13B . 0.97(4) ?
C13 H13C . 0.98(3) ?
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
O1 H1 O2 3_655 0.82(5) 2.17(5) 2.975(2) 165(4) yes
O1 H1 O3 3_655 0.82(5) 2.43(5) 3.046(2) 133(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
C12 O3 C1 O2 . . . . -80.7(2) ?
C12 O3 C1 C2 . . . . 158.94(17) ?
C10 O2 C1 O3 . . . . 145.47(19) ?
C10 O2 C1 C2 . . . . -98.2(2) ?
O3 C1 C2 C3 . . . . -49.1(2) ?
O2 C1 C2 C3 . . . . -166.62(17) ?
O3 C1 C2 Cl2 . . . . 72.14(18) ?
O2 C1 C2 Cl2 . . . . -45.4(2) ?
O3 C1 C2 Cl1 . . . . -169.77(14) ?
O2 C1 C2 Cl1 . . . . 72.67(18) ?
C1 C2 C3 O1 . . . . -52.0(2) ?
Cl2 C2 C3 O1 . . . . -173.54(14) ?
Cl1 C2 C3 O1 . . . . 66.95(19) ?
C1 C2 C3 C4 . . . . -174.97(18) ?
Cl2 C2 C3 C4 . . . . 63.5(2) ?
Cl1 C2 C3 C4 . . . . -56.0(2) ?
O1 C3 C4 C5 . . . . -28.8(3) ?
C2 C3 C4 C5 . . . . 90.3(2) ?
O1 C3 C4 C9 . . . . 149.9(2) ?
C2 C3 C4 C9 . . . . -91.0(2) ?
C9 C4 C5 C6 . . . . 1.1(3) ?
C3 C4 C5 C6 . . . . 179.8(2) ?
C4 C5 C6 C7 . . . . -0.5(3) ?
C5 C6 C7 F1 . . . . 179.7(2) ?
C5 C6 C7 C8 . . . . -0.1(4) ?
F1 C7 C8 C9 . . . . -179.8(2) ?
C6 C7 C8 C9 . . . . -0.1(4) ?
C7 C8 C9 C4 . . . . 0.7(4) ?
C5 C4 C9 C8 . . . . -1.2(3) ?
C3 C4 C9 C8 . . . . -179.9(2) ?
C1 O2 C10 C11 . . . . -167.2(2) ?
C1 O3 C12 C13 . . . . -172.42(18) ?