Two and Three-Dimensional Halogen-Bonded Frameworks: Self-assembly Influenced by Crystallization Solvents
Liu, Chuan-Zhi; Wang, Jingjing; Yang, Bo; Li, Zhongyi; Yan, Meng; Liu, Xinming; Hu, Zhiyuan; Liu, Lantao; Li, Zhan-Ting; Chemical Communications  (2023) –; doi:10.1039/D3CC02981F

data_7132096
_publ_section_title
;
 Two and Three-Dimensional Halogen-Bonded Frameworks: Self-assembly
 Influenced by Crystallization Solvents
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02981F
_journal_year                    2023
_chemical_formula_moiety         'C6 F4 I2, 2(C H Cl3), C53 H48 N4'
_chemical_formula_sum            'C61 H50 Cl6 F4 I2 N4'
_chemical_formula_weight         1381.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2fwws0
_audit_creation_date             2023-04-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-06 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.661(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.043(3)
_cell_length_b                   14.0514(12)
_cell_length_c                   20.8239(17)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.58
_cell_volume                     6147.9(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      297.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1871
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75711
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.584
_diffrn_source_current           35.0
_diffrn_source_power             1.225
_diffrn_source_voltage           35.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4580
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2153 before and 0.0864 after correction.
The Ratio of minimum to maximum transmission is 0.6143.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.1065
_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^)+(0.0923P)^2^+121.6085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2425
_refine_ls_wR_factor_ref         0.2587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3854
_reflns_number_total             5405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02981f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        6147.9(9)
_cod_database_code               7132096
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C6(H6), C7(H7), C4(H4), C3(H3), C10(H10), C20(H20), C19(H19),
 C24(H24), C23(H23), C17(H17), C16(H16)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              20522
_shelx_hkl_checksum              21240
_olex2_submission_special_instructions 'No special instructions were received'