Active control of molecular stacking types in a congeneric library of dihalogenated salicylideneaniline crystals and their solid solutions
Yoshikawa, Isao; Zhang, Zaixiang; Suzuki, Masahiro; Ikedo, Hana; Yin, Qiuxiang; Houjou, Hirohiko; CrystEngComm 25 (2023) 5109–5117; doi:10.1039/D3CE00601H

data_7247231
_publ_section_title
;
 Active control of molecular stacking types in a congeneric library of
 dihalogenated salicylideneaniline crystals and their solid solutions
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5109
_journal_page_last               5117
_journal_paper_doi               10.1039/D3CE00601H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C13 H9 Br2 N O'
_chemical_formula_sum            'C13 H9 Br2 N O'
_chemical_formula_weight         355.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-08-02 deposited with the CCDC.	2023-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.05690(10)
_cell_length_b                   6.93300(10)
_cell_length_c                   28.5038(3)
_cell_measurement_reflns_used    10439
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      70.7840
_cell_measurement_theta_min      4.6480
_cell_volume                     1196.95(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10509
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.133
_diffrn_reflns_theta_min         3.101
_diffrn_source                   'rotating anode X-ray generator'
_exptl_absorpt_coefficient_mu    8.437
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane and dichloromethane'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2120
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0527P)^2^+1.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.844
_reflns_Friedel_fraction_max     0.827
_reflns_number_gt                2119
_reflns_number_total             2120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00601h2.cif
_cod_data_source_block           o1-4BB
_cod_depositor_comments
'Adding full bibliography for 7247230--7247235.cif.'
_cod_database_code               7247231
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.209
_shelx_estimated_absorpt_t_max   0.312
_shelx_res_checksum              20291