Hydrogen-bonded frameworks for conformational analysis of reactive substrates.
Dillon, Alexandra M.; Shtukenberg, Alexander G.; Demkiw, Krystyna M.; Woerpel, K. A.; Ward, Michael D.; Chemical communications (Cambridge, England) 60 (2024) 11770–11773; doi:10.1039/d4cc03430a

data_7133763
_publ_section_title
;
 Hydrogen-bonded frameworks for conformational analysis of reactive
 substrates.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11770
_journal_page_last               11773
_journal_paper_doi               10.1039/d4cc03430a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C23 H33 Br N6 O9 S2'
_chemical_formula_weight         681.58
_chemical_name_systematic
'guanidinium 4,4?-biphenyldisulfonate 2-bromopropiophenone'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.032(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.674(3)
_cell_length_b                   11.6225(12)
_cell_length_c                   8.2592(8)
_cell_measurement_reflns_used    3017
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      22.83
_cell_measurement_theta_min      2.62
_cell_volume                     2984.3(5)
_computing_cell_refinement       'Bruker APEX4'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker APEX4'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1380)'
_computing_publication_material  'Bruker APEX4'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 SMART APEXII'
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.1323
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21396
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.87
_diffrn_source                   Incoatec
_diffrn_source_type              'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.576
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol ethanol'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.059
_refine_diff_density_min         -1.169
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7077
_refine_ls_number_restraints     661
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+15.6818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.875
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                4459
_reflns_number_total             7077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03430a2.cif
_cod_data_source_block           23mdw67d
_cod_depositor_comments
'Adding full bibliography for 7133757--7133764.cif.'
_cod_database_code               7133763
_shelx_res_checksum              11000