#------------------------------------------------------------------------------
#$Date: 2025-04-05 13:40:53 +0200 (Sat, 05 Apr 2025) $
#$Revision: 299190 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023408.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_2023408
loop_
_publ_author_name
'Mewis, Ryan E.'
'Hulme, Matthew C.'
'Marron, Jack'
'Langley, Stuart K.'
'Sutcliffe, Oliver B.'
'Benjamin, Sophie L.'
_publ_section_title
;
Synthesis and crystal structures of five fluorinated diphenidine
derivatives.
;
_journal_coeditor_code EE2011
_journal_issue 'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 229
_journal_page_last 234
_journal_paper_doi 10.1107/S2056989025001288
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '2C16 H18 F2 N +, 2Cl -, C H2 Cl2'
_chemical_formula_moiety '2(C16 H18 F2 N +), 2(Cl -), C H2 Cl2'
_chemical_formula_sum 'C33 H38 Cl4 F4 N2'
_chemical_formula_weight 680.45
_chemical_name_systematic
;
[1-(2,6-Difluorophenyl)-2-phenylethyl](ethyl)azanium chloride
dichloromethane hemisolvate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 92.130(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 22.9963(14)
_cell_length_b 7.8729(5)
_cell_length_c 19.0330(10)
_cell_measurement_reflns_used 8967
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max 26.43
_cell_measurement_theta_min 2.99
_cell_volume 3443.5(4)
_computing_cell_refinement CrysAlisPro
_computing_data_collection CrysAlisPro
_computing_data_reduction CrysAlisPro
_computing_molecular_graphics
;
X-SEED (Barbour, 2020)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur'
_diffrn_measurement_method 'scans in phi and omega'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0212
_diffrn_reflns_av_unetI/netI 0.0175
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 12738
_diffrn_reflns_theta_full 24.997
_diffrn_reflns_theta_max 24.997
_diffrn_reflns_theta_min 3.293
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 0.390
_exptl_absorpt_correction_T_max 0.962
_exptl_absorpt_correction_T_min 0.911
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.313
_exptl_crystal_description Block
_exptl_crystal_F_000 1416
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.249
_refine_diff_density_min -0.223
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 224
_refine_ls_number_reflns 3034
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0343
_refine_ls_R_factor_gt 0.0310
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+2.8401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0750
_refine_ls_wR_factor_ref 0.0768
_reflns_number_gt 2813
_reflns_number_total 3034
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ee2011.cif
_cod_data_source_block II
_cod_depositor_comments
'Adding full bibliography for 2023405--2023409.cif.'
_cod_original_sg_symbol_H-M 'I 2/a'
_cod_database_code 2023408
_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_hkl_file
;
-31 1 2 2.07 2.18
-31 1 4 23.88 3.65
-31 2 1 6.08 2.38
-30 0 0 160.34 8.74
-30 0 2 5.06 2.46
-30 0 4 82.81 6.25
-30 0 6 5.34 2.20
-30 0 8 0.26 1.89
-30 1 -1 1.31 2.08
-30 1 1 5.16 2.29
-30 1 3 3.37 2.12
-30 1 5 93.23 6.37
-30 2 -2 -1.01 2.10
-30 2 0 3.89 2.19
-30 2 2 1.26 1.93
-30 3 -3 2.89 2.22
-29 0 -3 -0.20 1.99
-29 0 -1 -1.08 1.74
-29 0 1 -1.34 1.84
-29 0 3 -0.32 1.77
-29 0 5 2.30 1.92
-29 0 7 1.86 1.99
-29 0 9 0.98 1.70
-29 0 11 -2.78 2.24
-29 1 -4 5.88 2.51
-29 -1 -2 21.64 3.56
-29 1 -2 18.83 3.35
-29 1 0 5.97 2.55
-29 -1 0 13.24 3.12
-29 1 2 7.09 2.44
-29 -1 2 14.70 3.06
-29 -1 4 57.12 5.31
-29 1 4 61.39 5.11
-29 1 6 4.85 2.19
-29 -1 6 6.71 2.66
-29 -1 8 10.51 2.68
-29 1 8 7.16 2.33
-29 2 -5 15.12 3.20
-29 2 -3 158.07 8.55
-29 2 -1 3.48 2.15
-29 2 1 34.21 3.93
-29 2 3 142.71 7.52
-29 3 -4 1.37 1.85
-29 3 -2 22.72 3.43
-28 0 -6 92.72 6.81
-28 0 -4 -0.13 1.80
-28 0 -2 21.37 3.52
-28 0 0 28.77 3.99
-28 0 2 24.06 3.44
-28 0 4 24.31 3.45
-28 0 6 40.21 4.29
-28 0 8 0.31 1.69
-28 0 10 84.71 5.98
-28 0 12 20.53 3.24
-28 -1 -5 21.50 3.79
-28 1 -5 24.07 3.68
-28 -1 -3 15.09 3.26
-28 1 -3 13.28 2.86
-28 -1 -1 48.11 4.87
-28 1 -1 49.23 4.64
-28 1 1 53.41 4.76
-28 -1 1 57.89 5.11
-28 -1 3 67.99 5.53
-28 1 3 68.70 5.30
-28 1 5 1.29 1.76
-28 -1 5 2.06 1.84
-28 1 7 46.96 4.38
-28 -1 7 59.25 5.21
-28 -1 9 9.62 2.66
-28 1 9 8.68 2.31
-28 -1 11 3.79 2.31
-28 2 -6 6.92 2.97
-28 2 -4 49.85 4.82
-28 -2 -2 17.09 3.14
-28 2 -2 21.16 3.33
-28 -2 0 10.26 2.83
-28 2 0 8.66 2.45
-28 -2 2 0.95 2.02
-28 2 2 0.92 1.57
-28 -2 4 11.13 2.78
-28 2 4 8.87 2.18
-28 -2 6 3.16 2.32
-28 3 -7 4.96 2.56
-28 3 -5 25.73 3.72
-28 3 -3 0.85 1.92
-28 3 -1 2.21 1.79
-28 4 -6 23.95 3.54
-27 0 -7 1.43 2.12
-27 0 -5 3.55 2.38
-27 0 -3 3.70 2.22
-27 0 -1 2.06 1.95
-27 0 1 -3.41 2.00
-27 0 3 1.11 1.66
-27 0 5 1.61 1.94
-27 0 7 3.21 1.86
-27 0 9 3.64 2.26
-27 0 11 1.23 1.66
-27 0 13 -4.61 2.07
-27 1 -8 2.36 1.98
-27 -1 -6 -0.04 2.21
-27 1 -6 3.28 2.38
-27 1 -4 26.89 3.76
-27 -1 -4 30.53 3.95
-27 -1 -2 1.63 1.69
-27 1 -2 3.23 2.01
-27 1 0 7.34 2.44
-27 -1 0 4.55 2.12
-27 1 2 3.74 1.86
-27 -1 2 5.54 2.43
-27 1 4 5.93 2.07
-27 -1 4 8.33 2.63
-27 -1 6 12.25 2.72
-27 1 6 6.56 2.10
-27 1 8 1.62 1.60
-27 -1 8 0.86 1.91
-27 1 10 3.53 1.89
-27 -1 10 7.24 2.54
-27 -1 12 12.18 2.72
-27 2 -7 2.59 2.32
-27 -2 -5 30.81 4.16
-27 2 -5 22.06 3.43
-27 -2 -3 36.33 4.45
-27 2 -3 30.35 4.00
-27 2 -1 11.43 2.39
-27 -2 -1 15.71 2.92
-27 -2 1 32.70 4.08
-27 2 1 30.70 3.53
-27 -2 3 76.30 5.80
-27 2 3 72.65 5.12
-27 -2 5 2.32 2.33
-27 2 5 0.98 1.78
-27 -2 7 16.50 3.05
-27 -2 9 19.96 3.34
-27 3 -8 13.00 2.84
-27 3 -6 4.03 2.27
-27 3 -4 69.86 5.45
-27 3 -2 21.82 3.18
-27 -3 -2 27.93 3.89
-27 -3 0 12.30 3.10
-27 3 0 6.36 2.05
-27 3 2 60.70 4.65
-27 -3 2 63.88 5.61
-27 -3 4 13.11 2.86
-27 -3 6 1.19 1.83
-27 4 -7 10.82 2.59
-27 4 -5 33.18 3.97
-26 0 -8 7.06 2.52
-26 0 -6 47.96 4.81
-26 0 -4 161.81 8.36
-26 0 -2 4.08 2.21
-26 0 0 36.23 3.93
-26 0 2 76.11 5.47
-26 0 4 9.54 2.59
-26 0 6 160.40 7.89
-26 0 8 5.83 2.11
-26 0 10 12.13 2.58
-26 0 12 6.84 2.14
-26 0 14 52.79 4.78
-26 -1 -9 13.05 3.40
-26 1 -9 17.93 3.55
-26 -1 -7 6.25 2.64
-26 1 -7 4.33 2.32
-26 1 -5 2.34 2.19
-26 -1 -5 0.43 2.03
-26 1 -3 4.46 2.21
-26 -1 -3 7.52 2.65
-26 -1 -1 59.05 5.03
-26 1 -1 60.07 4.87
-26 -1 1 5.58 2.22
-26 1 1 8.02 2.30
-26 1 3 47.28 4.12
-26 -1 3 43.05 4.36
-26 -1 5 5.55 2.31
-26 1 5 2.85 1.87
-26 -1 7 27.85 3.58
-26 1 7 26.24 3.30
-26 -1 9 110.38 6.73
-26 1 9 111.12 6.40
-26 -1 11 38.10 4.15
-26 1 11 42.30 3.99
-26 -1 13 26.87 3.56
-26 2 -10 7.13 2.58
-26 -2 -8 16.84 3.68
-26 2 -8 12.79 2.96
-26 -2 -6 46.40 5.02
-26 2 -6 54.68 4.96
-26 2 -4 14.25 3.00
-26 -2 -4 14.88 3.09
-26 -2 -2 -1.55 2.05
-26 2 -2 1.34 1.71
-26 -2 0 3.66 2.23
-26 2 0 3.71 1.82
-26 2 2 3.37 1.86
-26 -2 2 1.04 1.85
-26 -2 4 16.59 3.05
-26 2 4 19.35 2.85
-26 2 6 43.08 3.90
-26 -2 6 51.87 4.78
-26 -2 8 12.34 2.94
-26 -2 10 17.61 3.11
-26 -2 12 5.58 2.30
-26 3 -9 4.18 2.39
-26 3 -7 21.50 3.43
-26 3 -5 8.36 2.52
-26 -3 -5 8.82 2.81
-26 -3 -3 5.85 2.66
-26 3 -3 10.75 2.56
-26 -3 -1 6.06 2.67
-26 3 -1 6.80 2.05
-26 3 1 2.83 1.71
-26 -3 1 6.88 2.45
-26 3 3 9.26 2.17
-26 -3 3 11.79 2.68
-26 -3 5 1.76 2.17
-26 -3 7 6.03 2.49
-26 -3 9 41.06 4.69
-26 4 -8 13.00 2.96
-26 4 -6 100.25 6.52
-26 4 -4 20.64 3.12
-26 4 -2 31.86 3.66
-26 -4 -2 33.99 4.26
-26 -4 0 175.16 9.24
-26 -4 2 26.41 3.92
-26 -4 4 4.93 2.41
-25 0 -11 2.57 2.34
-25 0 -9 3.52 2.56
-25 0 -7 4.90 2.45
-25 0 -5 0.92 2.02
-25 0 -3 -1.86 1.88
-25 0 -1 -0.19 1.74
-25 0 1 0.71 1.77
-25 0 3 1.28 1.78
-25 0 5 1.55 1.63
-25 0 7 1.93 1.95
-25 0 9 2.16 1.87
-25 0 11 2.26 1.80
-25 0 13 0.21 1.55
-25 0 15 2.30 1.86
-25 1 -10 104.52 7.25
-25 -1 -10 122.06 7.85
-25 1 -8 6.42 2.63
-25 -1 -8 3.07 2.39
-25 -1 -6 39.24 4.39
-25 1 -6 37.03 4.24
-25 -1 -4 12.76 2.83
-25 1 -4 16.29 3.00
-25 -1 -2 53.74 4.83
-25 1 -2 51.63 4.48
-25 1 0 155.20 7.59
-25 -1 0 146.87 7.72
-25 -1 2 -1.48 1.99
-25 1 2 -0.86 1.55
-25 1 4 74.65 5.02
-25 -1 4 71.22 5.26
-25 1 6 207.93 8.53
-25 -1 6 214.10 9.18
-25 -1 8 8.97 2.40
-25 1 8 5.81 2.00
-25 -1 10 6.95 2.28
-25 1 10 8.74 2.22
-25 -1 12 39.91 4.33
-25 1 12 48.98 4.16
-25 -1 14 2.52 2.12
-25 -1 16 21.03 3.47
-25 2 -11 5.52 2.56
-25 -2 -9 14.08 3.41
-25 2 -9 11.62 2.87
-25 -2 -7 100.13 6.93
-25 2 -7 106.30 6.78
-25 -2 -5 3.73 2.48
-25 2 -5 3.06 2.41
-25 -2 -3 97.27 6.52
-25 2 -3 109.70 6.49
-25 -2 -1 51.35 4.77
-25 2 -1 50.32 4.33
-25 -2 1 11.15 2.72
-25 2 1 9.11 2.43
-25 -2 3 85.56 5.91
-25 2 3 86.80 5.35
-25 -2 5 1.59 2.06
-25 2 5 1.90 1.48
-25 2 7 2.50 1.72
-25 -2 7 4.54 2.35
-25 -2 9 68.83 5.39
-25 -2 11 33.53 4.10
-25 -2 13 14.05 2.85
-25 3 -10 143.72 8.42
-25 -3 -8 7.67 2.89
-25 3 -8 4.78 2.42
-25 3 -6 1.32 2.16
-25 -3 -6 3.93 2.44
-25 -3 -4 111.07 7.15
-25 3 -4 107.60 6.43
-25 3 -2 1.74 2.02
-25 -3 -2 -1.07 2.04
-25 3 0 4.82 1.85
-25 -3 0 1.11 2.12
-25 3 2 147.53 6.89
-25 -3 2 147.59 8.08
-25 -3 4 15.15 3.03
-25 3 4 12.70 2.31
-25 -3 6 46.55 4.68
-25 -3 8 89.87 6.44
-25 -3 10 42.02 4.61
-25 4 -9 4.30 2.52
-25 4 -7 14.76 2.93
-25 4 -5 1.35 1.93
-25 -4 -5 4.00 2.56
-25 4 -3 33.71 3.69
-25 -4 -3 35.44 4.48
-25 -4 -1 10.28 2.90
-25 4 -1 12.47 2.35
-25 -4 1 7.93 2.60
-25 -4 3 81.44 6.35
-25 -4 5 7.09 2.92
-25 -4 7 12.21 3.12
-25 5 -8 35.00 4.22
-24 0 -12 3.92 2.47
-24 0 -10 583.82 17.74
-24 0 -8 287.29 11.51
-24 0 -6 1.48 1.96
-24 0 -4 218.36 9.26
-24 0 -2 8.15 2.33
-24 0 0 15.47 2.79
-24 0 2 148.14 7.21
-24 0 4 4.72 1.90
-24 0 6 16.68 2.74
-24 0 8 107.58 6.18
-24 0 10 1.52 1.77
-24 0 12 3.11 1.83
-24 0 14 5.01 2.00
-24 0 16 26.14 3.52
-24 -1 -11 8.71 2.84
-24 1 -11 9.75 3.08
-24 -1 -9 64.14 5.63
-24 1 -9 55.65 5.40
-24 1 -7 73.19 5.63
-24 -1 -7 76.37 5.90
-24 -1 -5 7.90 2.64
-24 1 -5 13.89 2.88
-24 1 -3 30.56 3.56
-24 -1 -3 29.45 3.55
-24 1 -1 5.87 2.05
-24 -1 -1 7.18 2.22
-24 1 1 12.45 2.38
-24 -1 1 17.58 2.89
-24 1 3 16.18 2.66
-24 -1 3 11.39 2.60
-24 -1 5 168.34 7.91
-24 1 5 172.91 7.50
-24 -1 7 32.32 3.74
-24 1 7 25.72 3.06
-24 -1 9 63.54 5.00
-24 1 9 56.01 4.39
-24 1 11 19.31 2.85
-24 -1 11 21.22 3.19
-24 1 13 1.33 1.48
-24 -1 13 3.06 2.20
-24 -1 15 33.43 3.91
-24 -1 17 27.12 3.85
-24 2 -12 2.10 2.37
-24 2 -10 0.60 2.03
-24 -2 -10 4.72 2.29
-24 2 -8 12.04 2.80
-24 -2 -8 13.46 3.00
-24 2 -6 41.48 4.15
-24 -2 -6 42.23 4.49
-24 -2 -4 86.80 6.03
-24 2 -4 91.69 5.83
-24 -2 -2 148.30 7.79
-24 2 -2 144.19 7.22
-24 -2 0 59.79 4.95
-24 2 0 55.75 4.39
-24 2 2 10.58 2.17
-24 -2 2 16.23 2.99
-24 -2 4 2.85 1.93
-24 2 4 3.08 1.79
-24 -2 6 4.79 2.08
-24 2 6 4.94 1.71
-24 -2 8 7.15 2.38
-24 2 8 4.97 1.68
-24 -2 10 -0.58 1.79
-24 -2 12 17.06 3.10
-24 -2 14 -2.57 2.27
-24 -2 14 -0.06 1.54
-24 3 -11 3.10 2.37
-24 -3 -9 30.36 4.20
-24 3 -9 23.88 3.65
-24 -3 -7 17.29 3.24
-24 3 -7 10.03 2.54
-24 3 -5 15.02 2.78
-24 -3 -5 16.74 3.22
-24 3 -3 24.65 3.20
-24 -3 -3 21.74 3.42
-24 -3 -1 17.03 3.10
-24 3 -1 21.42 2.89
-24 -3 1 8.51 2.54
-24 3 1 5.36 1.88
-24 -3 3 85.15 5.92
-24 3 3 88.05 5.07
-24 -3 5 14.36 3.01
-24 3 5 17.87 2.47
-24 -3 7 19.11 3.09
-24 -3 9 36.98 4.14
-24 -3 11 6.86 2.64
-24 4 -10 11.86 3.03
-24 -4 -8 12.77 3.15
-24 4 -8 5.01 2.31
-24 -4 -6 94.28 6.64
-24 4 -6 88.25 5.92
-24 -4 -4 6.68 2.65
-24 4 -4 13.23 2.60
-24 4 -2 7.96 1.99
-24 -4 -2 13.92 3.13
-24 4 0 70.39 4.58
-24 -4 0 74.33 5.77
-24 -4 2 1.63 1.94
-24 -4 4 2.80 2.16
-24 -4 6 37.67 4.31
-24 -4 8 4.00 2.19
-24 -4 10 2.41 2.13
-24 5 -9 34.28 4.24
-24 5 -7 52.22 4.70
-24 -5 -5 4.97 2.34
-24 -5 -3 52.28 5.09
-24 -5 -1 98.09 6.91
-24 -5 1 43.79 4.72
-24 -5 3 0.32 1.93
-24 -5 5 141.07 8.28
-23 0 -13 4.08 2.65
-23 0 -11 6.08 2.86
-23 0 -9 4.08 2.41
-23 0 -7 2.46 2.10
-23 0 -5 2.73 1.94
-23 0 -3 2.13 2.16
-23 0 -1 0.17 1.62
-23 0 1 0.74 1.61
-23 0 3 0.14 1.53
-23 0 5 0.76 1.58
-23 0 7 1.92 1.65
-23 0 9 0.94 1.83
-23 0 11 -2.36 1.86
-23 0 13 0.91 1.62
-23 0 15 3.90 2.03
-23 0 17 2.11 1.80
-23 1 -12 37.98 4.68
-23 -1 -12 34.11 4.53
-23 -1 -10 26.23 3.92
-23 1 -10 19.07 3.48
-23 1 -8 131.29 7.46
-23 -1 -8 133.72 7.57
-23 -1 -6 35.84 4.11
-23 1 -6 43.94 4.30
-23 1 -4 6.10 2.20
-23 -1 -4 6.32 2.24
-23 1 -2 80.59 5.23
-23 -1 -2 81.28 5.40
-23 1 0 120.92 6.20
-23 -1 0 116.90 6.53
-23 1 2 4.25 1.77
-23 -1 2 2.39 1.78
-23 -1 4 6.13 2.16
-23 1 4 9.33 2.19
-23 1 6 79.28 4.95
-23 -1 6 76.25 5.16
-23 -1 8 3.60 1.86
-23 1 8 1.96 1.35
-23 1 10 54.38 4.15
-23 -1 10 58.77 4.61
-23 1 12 13.70 2.31
-23 -1 12 15.94 2.83
-23 -1 12 17.07 2.48
-23 -1 14 24.47 3.38
-23 1 14 26.44 3.13
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28 2 -6 3.46 2.05
28 2 -4 14.14 3.24
28 2 -2 3.29 2.13
28 2 6 7.68 2.33
28 2 8 2.17 1.93
28 3 -7 44.80 4.49
28 3 -5 7.11 2.75
28 3 -5 -1.55 2.06
28 3 -3 6.04 2.48
28 3 -1 50.01 4.91
28 3 1 4.97 2.51
28 3 5 25.29 3.81
28 3 7 4.77 2.66
28 4 -4 0.97 1.98
28 4 -2 2.26 2.06
28 4 0 27.81 3.67
28 4 6 40.53 4.72
29 0 9 0.61 1.99
29 1 -4 49.88 4.67
29 1 8 2.31 2.45
29 2 -5 4.99 2.34
29 2 -3 147.09 7.98
29 2 -1 37.06 4.34
29 3 -6 2.59 1.99
29 3 -4 3.65 2.57
29 4 -1 0.98 1.80
30 1 -3 2.31 2.18
30 2 -4 25.51 3.93
30 2 -2 4.28 2.74
0 0 0 0.00 0.00
TITL OS-4 in Ia
REM Ia (#9 in standard setting)
CELL 0.71073 22.996344 7.872904 19.033033 90.0000 92.1297 90.0000
ZERR 10.00 0.001423 0.000494 0.001019 0.0000 0.0052 0.0000
LATT -2
SYMM x+1/2,-y, z
SFAC C H N F
UNIT 170.00 220.00 10.00 20.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 49054
_shelx_res_file
;
REM reset to Ia #9
REM
REM
REM
REM OS-4 in Ia #9
REM R1 = 0.0340 for 6060 Fo > 4sig(Fo) and 0.0404 for all 6890 data
REM 391 parameters refined using 4 restraints
REM Highest difference peak 0.242, deepest hole -0.262, 1-sigma level 0.038
REM OS-4 in Ia #9
REM R1 = 0.0316 for 5045 Fo > 4sig(Fo) and 0.0359 for all 5573 data
REM 407 parameters refined using 4 restraints
REM Highest difference peak 0.258, deepest hole -0.191, 1-sigma level 0.039
REM OS-4 in Ia #9
REM wR2 = 0.0736, GooF = S = 1.038, Restrained GooF = 1.042 for all data
REM R1 = 0.0295 for 5045 Fo > 4sig(Fo) and 0.0339 for all 5573 data
REM 407 parameters refined using 24 restraints
REM Instructions for potential hydrogen bonds
REM Highest difference peak 0.192, deepest hole -0.231, 1-sigma level 0.033
REM OS-4 in Ia #9
REM wR2 = 0.0886, GooF = S = 1.045, Restrained GooF = 1.045 for all data
REM R1 = 0.0349 for 2813 Fo > 4sig(Fo) and 0.0382 for all 3034 data
REM 211 parameters refined using 0 restraints
REM Highest difference peak 0.727, deepest hole -0.218, 1-sigma level 0.041
REM OS-4 in Ia #9
REM wR2 = 0.0776, GooF = S = 1.073, Restrained GooF = 1.073 for all data
REM R1 = 0.0314 for 2813 Fo > 4sig(Fo) and 0.0346 for all 3034 data
REM 215 parameters refined using 0 restraints
REM Highest difference peak 0.250, deepest hole -0.228, 1-sigma level 0.036
TITL OS-4 in Ia #9
C:\Users\stula\Desktop\OS4-II~1\os4.res
created by SHELXL-2018/3 at 10:17:41 on 29-Jan-2025
CELL 0.71073 22.9963 7.8729 19.0330 90.000 92.130 90.000
ZERR 4.0000 0.0014 0.0005 0.0010 0.000 0.005 0.000
LATT 2
SYMM 0.5-X, Y, -Z
SFAC C H N F CL
UNIT 132 152 8 16 16
MERG 2
OMIT -2 50
SHEL 7.00 0.77
FMAP 2
GRID
PLAN 4
TEMP -100
HTAB N1 CL1
L.S. 20
ACTA
WGHT 0.034300 2.840100
FVAR 0.31637 0.70743
CL1 5 0.286405 0.609901 0.162227 11.00000 0.02983 0.03802 =
0.02123 -0.00054 0.00001 0.00784
CL1S 5 0.313258 0.288208 0.008594 11.00000 0.04910 0.05581 =
0.05809 -0.02505 -0.01914 0.02620
F1 4 0.055196 1.141291 0.115353 11.00000 0.04865 0.04052 =
0.05067 -0.00129 0.00228 0.02136
F2 4 0.176558 0.698700 0.049077 11.00000 0.06686 0.06288 =
0.04020 -0.01576 -0.01129 0.04160
N1 3 0.195736 0.904369 0.178781 11.00000 0.02611 0.02682 =
0.02107 0.00105 -0.00276 0.00252
C1 1 0.131686 0.881666 0.162642 11.00000 0.02460 0.02645 =
0.02393 0.00037 -0.00222 0.00190
AFIX 13
H1 2 0.110554 0.967062 0.191048 11.00000 -1.20000
AFIX 0
C9 1 0.116294 0.915622 0.086018 11.00000 0.02168 0.02534 =
0.02544 0.00225 -0.00267 -0.00111
C3 1 0.050358 0.668890 0.175581 11.00000 0.03395 0.02679 =
0.03127 0.01034 -0.00438 -0.00385
C13 1 0.124139 0.848866 -0.038480 11.00000 0.03665 0.05236 =
0.02799 -0.00614 -0.00137 -0.00359
AFIX 43
H13 2 0.140233 0.779839 -0.073793 11.00000 -1.20000
AFIX 0
C12 1 0.086113 0.978389 -0.055615 11.00000 0.03248 0.05562 =
0.02868 0.01188 -0.00797 -0.01210
AFIX 43
H12 2 0.075593 0.999429 -0.103567 11.00000 -1.20000
AFIX 0
C11 1 0.063154 1.077735 -0.004197 11.00000 0.02709 0.03811 =
0.04485 0.01786 -0.00823 -0.00280
AFIX 43
H11 2 0.037235 1.168104 -0.016069 11.00000 -1.20000
AFIX 0
C14 1 0.138060 0.822742 0.031559 11.00000 0.03009 0.03576 =
0.03139 -0.00282 -0.00572 0.00739
C10 1 0.078538 1.043415 0.064851 11.00000 0.02419 0.02659 =
0.03557 0.00310 0.00089 0.00025
C4 1 0.009034 0.745528 0.216516 11.00000 0.04329 0.03927 =
0.03724 0.00500 0.00288 -0.00605
AFIX 43
H4 2 0.021169 0.820557 0.253303 11.00000 -1.20000
PART 1
AFIX 0
C15 1 0.219557 1.075144 0.155813 21.00000 0.02291 0.02972 =
0.04131 0.01402 -0.01001 -0.01126
AFIX 23
H15A 2 0.195508 1.167814 0.174557 21.00000 -1.20000
H15B 2 0.217609 1.082569 0.103855 21.00000 -1.20000
PART 0
AFIX 0
C8 1 0.031745 0.559747 0.122521 11.00000 0.04513 0.03026 =
0.04046 0.00391 -0.00481 -0.00528
AFIX 43
H8 2 0.059436 0.506416 0.093985 11.00000 -1.20000
AFIX 0
C2 1 0.114387 0.704524 0.188340 11.00000 0.03306 0.02939 =
0.03493 0.00779 -0.00562 -0.00139
AFIX 23
H2A 2 0.137251 0.617767 0.163763 11.00000 -1.20000
H2B 2 0.124134 0.695173 0.239296 11.00000 -1.20000
AFIX 0
C7 1 -0.027035 0.527569 0.110659 11.00000 0.05630 0.04260 =
0.04990 0.01037 -0.01780 -0.02012
AFIX 43
H7 2 -0.039328 0.451887 0.074176 11.00000 -1.20000
AFIX 0
C5 1 -0.049643 0.713646 0.204231 11.00000 0.03726 0.05044 =
0.05986 0.01960 0.01012 0.00004
AFIX 43
H5 2 -0.077544 0.767277 0.232379 11.00000 -1.20000
AFIX 0
C6 1 -0.067709 0.604216 0.151228 11.00000 0.03486 0.05465 =
0.06646 0.03149 -0.01295 -0.01434
AFIX 43
H6 2 -0.107970 0.581969 0.142816 11.00000 -1.20000
PART 1
AFIX 0
C16 1 0.283475 1.096298 0.183104 21.00000 0.03262 0.03546 =
0.03968 0.00178 -0.00073 -0.00854
AFIX 137
H16A 2 0.285642 1.081935 0.234280 21.00000 -1.50000
H16B 2 0.297386 1.209892 0.171032 21.00000 -1.50000
H16C 2 0.307818 1.010445 0.161259 21.00000 -1.50000
PART 0
AFIX 0
C1S 1 0.250000 0.413592 0.000000 10.50000 0.02862 0.02726 =
0.03402 0.00000 -0.00699 0.00000
AFIX 23
H1S1 2 0.252617 0.487565 -0.041826 10.50000 -1.20000
H1S2 2 0.247383 0.487565 0.041827 10.50000 -1.20000
PART 2
AFIX 0
C16A 1 0.193164 1.211546 0.184325 -21.00000 0.04025 0.03087 =
0.04298 -0.00185 -0.00980 -0.01000
AFIX 137
H16D 2 0.155523 1.220984 0.158750 -21.00000 -1.50000
H16E 2 0.216492 1.313058 0.175641 -21.00000 -1.50000
H16F 2 0.186879 1.201409 0.234797 -21.00000 -1.50000
PART 0
AFIX 0
H1B 2 0.216212 0.818822 0.161242 11.00000 0.03590
H1A 2 0.200952 0.892572 0.227309 11.00000 0.03359
PART 2
C15A 1 0.224832 1.056556 0.159397 -21.00000 0.05315 0.04158 =
0.01451 0.00646 -0.00880 0.02385
AFIX 23
H15C 2 0.227354 1.060956 0.107617 -21.00000 -1.20000
H15D 2 0.264950 1.056010 0.180153 -21.00000 -1.20000
AFIX 0
HKLF 4
REM OS-4 in Ia #9
REM wR2 = 0.0768, GooF = S = 1.066, Restrained GooF = 1.066 for all data
REM R1 = 0.0310 for 2813 Fo > 4sig(Fo) and 0.0343 for all 3034 data
REM 224 parameters refined using 0 restraints
END
WGHT 0.0343 2.8337
REM Highest difference peak 0.249, deepest hole -0.223, 1-sigma level 0.035
Q1 1 0.1234 0.8941 0.1201 11.00000 0.05 0.25
Q2 1 0.1354 0.9060 0.0625 11.00000 0.05 0.21
Q3 1 0.2883 0.2026 -0.0028 11.00000 0.05 0.21
Q4 1 0.0800 0.6907 0.1820 11.00000 0.05 0.20
;
_shelx_res_checksum 73593
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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 0.28641(2) 0.60990(5) 0.16223(2) 0.02972(12) Uani d 1 . .
Cl Cl1S 0.31326(2) 0.28821(7) 0.00859(3) 0.05486(16) Uani d 1 . .
F F1 0.05520(5) 1.14129(13) 0.11535(6) 0.0466(3) Uani d 1 . .
F F2 0.17656(5) 0.69870(15) 0.04908(5) 0.0570(3) Uani d 1 . .
N N1 0.19574(5) 0.90437(17) 0.17878(7) 0.0248(3) Uani d 1 . .
C C1 0.13169(6) 0.88167(19) 0.16264(7) 0.0251(3) Uani d 1 . .
H H1 0.110554 0.967062 0.191048 0.030 Uiso calc 1 . .
C C9 0.11629(6) 0.91562(18) 0.08602(7) 0.0242(3) Uani d 1 . .
C C3 0.05036(7) 0.6689(2) 0.17558(8) 0.0308(3) Uani d 1 . .
C C13 0.12414(8) 0.8489(2) -0.03848(9) 0.0391(4) Uani d 1 . .
H H13 0.140233 0.779839 -0.073793 0.047 Uiso calc 1 . .
C C12 0.08611(7) 0.9784(2) -0.05562(9) 0.0392(4) Uani d 1 . .
H H12 0.075593 0.999429 -0.103567 0.047 Uiso calc 1 . .
C C11 0.06315(7) 1.0777(2) -0.00420(9) 0.0369(4) Uani d 1 . .
H H11 0.037235 1.168104 -0.016069 0.044 Uiso calc 1 . .
C C14 0.13806(7) 0.8227(2) 0.03156(8) 0.0326(4) Uani d 1 . .
C C10 0.07854(6) 1.04341(19) 0.06485(8) 0.0288(3) Uani d 1 . .
C C4 0.00903(8) 0.7455(2) 0.21652(9) 0.0399(4) Uani d 1 . .
H H4 0.021169 0.820557 0.253303 0.048 Uiso calc 1 . .
C C15 0.2196(4) 1.0751(12) 0.1558(4) 0.0316(19) Uani d 0.707(5) A 1
H H15A 0.195508 1.167814 0.174557 0.038 Uiso calc 0.707(5) A 1
H H15B 0.217609 1.082569 0.103855 0.038 Uiso calc 0.707(5) A 1
C C8 0.03174(8) 0.5597(2) 0.12252(9) 0.0388(4) Uani d 1 . .
H H8 0.059436 0.506416 0.093985 0.047 Uiso calc 1 . .
C C2 0.11439(7) 0.7045(2) 0.18834(9) 0.0326(4) Uani d 1 . .
H H2A 0.137251 0.617767 0.163763 0.039 Uiso calc 1 . .
H H2B 0.124134 0.695173 0.239296 0.039 Uiso calc 1 . .
C C7 -0.02704(9) 0.5276(3) 0.11066(10) 0.0501(5) Uani d 1 . .
H H7 -0.039328 0.451887 0.074176 0.060 Uiso calc 1 . .
C C5 -0.04964(8) 0.7136(3) 0.20423(11) 0.0490(5) Uani d 1 . .
H H5 -0.077544 0.767277 0.232379 0.059 Uiso calc 1 . .
C C6 -0.06771(8) 0.6042(3) 0.15123(11) 0.0524(5) Uani d 1 . .
H H6 -0.107970 0.581969 0.142816 0.063 Uiso calc 1 . .
C C16 0.28347(10) 1.0963(3) 0.18310(13) 0.0360(7) Uani d 0.707(5) A 1
H H16A 0.285642 1.081935 0.234280 0.054 Uiso calc 0.707(5) A 1
H H16B 0.297386 1.209892 0.171032 0.054 Uiso calc 0.707(5) A 1
H H16C 0.307818 1.010445 0.161259 0.054 Uiso calc 0.707(5) A 1
C C1S 0.250000 0.4136(3) 0.000000 0.0302(5) Uani d 1 . .
H H1S1 0.252617 0.487565 -0.041826 0.036 Uiso calc 0.5 . .
H H1S2 0.247383 0.487565 0.041827 0.036 Uiso calc 0.5 . .
C C16A 0.1932(3) 1.2115(7) 0.1843(3) 0.0383(18) Uani d 0.293(5) A 2
H H16D 0.155523 1.220984 0.158750 0.057 Uiso calc 0.293(5) A 2
H H16E 0.216492 1.313058 0.175641 0.057 Uiso calc 0.293(5) A 2
H H16F 0.186879 1.201409 0.234797 0.057 Uiso calc 0.293(5) A 2
H H1B 0.2162(8) 0.819(2) 0.1612(9) 0.036(5) Uiso d 1 . .
H H1A 0.2010(7) 0.893(2) 0.2273(10) 0.034(5) Uiso d 1 . .
C C15A 0.2248(10) 1.057(3) 0.1594(10) 0.037(6) Uani d 0.293(5) A 2
H H15C 0.227354 1.060956 0.107617 0.044 Uiso calc 0.293(5) A 2
H H15D 0.264950 1.056010 0.180153 0.044 Uiso calc 0.293(5) A 2
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 0.0298(2) 0.0380(2) 0.02123(18) 0.00784(16) 0.00001(14) -0.00054(15)
Cl1S 0.0491(3) 0.0558(3) 0.0581(3) 0.0262(2) -0.0191(2) -0.0251(2)
F1 0.0486(6) 0.0405(6) 0.0507(6) 0.0214(5) 0.0023(5) -0.0013(5)
F2 0.0669(7) 0.0629(7) 0.0402(6) 0.0416(6) -0.0113(5) -0.0158(5)
N1 0.0261(7) 0.0268(7) 0.0211(7) 0.0025(6) -0.0028(5) 0.0011(6)
C1 0.0246(7) 0.0264(8) 0.0239(7) 0.0019(6) -0.0022(6) 0.0004(6)
C9 0.0217(7) 0.0253(8) 0.0254(7) -0.0011(6) -0.0027(6) 0.0023(6)
C3 0.0340(8) 0.0268(8) 0.0313(8) -0.0038(7) -0.0044(7) 0.0103(7)
C13 0.0366(9) 0.0524(11) 0.0280(8) -0.0036(8) -0.0014(7) -0.0061(8)
C12 0.0325(9) 0.0556(11) 0.0287(8) -0.0121(8) -0.0080(7) 0.0119(8)
C11 0.0271(8) 0.0381(9) 0.0448(10) -0.0028(7) -0.0082(7) 0.0179(8)
C14 0.0301(8) 0.0358(9) 0.0314(8) 0.0074(7) -0.0057(6) -0.0028(7)
C10 0.0242(7) 0.0266(8) 0.0356(8) 0.0002(6) 0.0009(6) 0.0031(7)
C4 0.0433(10) 0.0393(10) 0.0372(9) -0.0060(8) 0.0029(8) 0.0050(8)
C15 0.023(2) 0.030(3) 0.041(3) -0.011(3) -0.0100(19) 0.014(2)
C8 0.0451(10) 0.0303(9) 0.0405(10) -0.0053(8) -0.0048(8) 0.0039(7)
C2 0.0331(9) 0.0294(8) 0.0349(9) -0.0014(7) -0.0056(7) 0.0078(7)
C7 0.0563(12) 0.0426(11) 0.0499(11) -0.0201(9) -0.0178(9) 0.0104(9)
C5 0.0373(10) 0.0504(11) 0.0599(12) 0.0000(9) 0.0101(9) 0.0196(10)
C6 0.0349(10) 0.0546(12) 0.0665(13) -0.0143(9) -0.0130(9) 0.0315(11)
C16 0.0326(14) 0.0355(14) 0.0397(14) -0.0085(10) -0.0007(10) 0.0018(10)
C1S 0.0286(11) 0.0273(11) 0.0340(12) 0.000 -0.0070(9) 0.000
C16A 0.040(3) 0.031(3) 0.043(3) -0.010(3) -0.010(3) -0.002(3)
C15A 0.053(9) 0.042(8) 0.015(5) 0.024(5) -0.009(4) 0.006(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
C15A N1 C1 . . 120.8(11) ?
C1 N1 C15 . . 114.0(4) ?
N1 C1 C9 . . 111.62(12) ?
N1 C1 C2 . . 107.84(12) ?
C9 C1 C2 . . 114.45(13) ?
C14 C9 C10 . . 114.19(14) ?
C14 C9 C1 . . 123.60(13) ?
C10 C9 C1 . . 122.21(13) ?
C8 C3 C4 . . 118.70(16) ?
C8 C3 C2 . . 120.46(15) ?
C4 C3 C2 . . 120.84(15) ?
C12 C13 C14 . . 117.66(16) ?
C11 C12 C13 . . 120.75(15) ?
C12 C11 C10 . . 118.49(15) ?
F2 C14 C13 . . 118.30(14) ?
F2 C14 C9 . . 116.80(14) ?
C13 C14 C9 . . 124.89(15) ?
F1 C10 C11 . . 118.07(14) ?
F1 C10 C9 . . 117.92(14) ?
C11 C10 C9 . . 124.01(15) ?
C5 C4 C3 . . 120.64(17) ?
N1 C15 C16 . . 110.2(7) ?
C3 C8 C7 . . 120.44(18) ?
C3 C2 C1 . . 112.35(13) ?
C6 C7 C8 . . 120.56(18) ?
C6 C5 C4 . . 120.15(19) ?
C7 C6 C5 . . 119.51(18) ?
Cl1S C1S Cl1S . 2 111.79(12) ?
N1 C15A C16A . . 111.2(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
Cl1S C1S . 1.7606(13) ?
F1 C10 . 1.3580(18) ?
F2 C14 . 1.3516(18) ?
N1 C15A . 1.43(2) ?
N1 C1 . 1.5040(19) ?
N1 C15 . 1.522(8) ?
C1 C9 . 1.512(2) ?
C1 C2 . 1.535(2) ?
C9 C14 . 1.378(2) ?
C9 C10 . 1.379(2) ?
C3 C8 . 1.382(2) ?
C3 C4 . 1.389(2) ?
C3 C2 . 1.510(2) ?
C13 C12 . 1.375(3) ?
C13 C14 . 1.375(2) ?
C12 C11 . 1.374(3) ?
C11 C10 . 1.375(2) ?
C4 C5 . 1.384(3) ?
C15 C16 . 1.550(8) ?
C8 C7 . 1.385(3) ?
C7 C6 . 1.374(3) ?
C5 C6 . 1.379(3) ?
C16A C15A . 1.51(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
N1 H1B Cl1 . 0.89(2) 2.30(2) 3.1417(14) 156.0(16) yes