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_7133761
_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_moiety         'C9 H9 Br O, 4(C6 H11 O3 S), 4(C H6 N3)'
_chemical_formula_sum            'C37 H77 Br N12 O13 S4'
_chemical_formula_weight         1106.25
_chemical_name_systematic
'guanidinium cyclohexanemonosulfonate 2-bromopropiophenone'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-09-13 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.365(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4620(7)
_cell_length_b                   8.6851(3)
_cell_length_c                   19.0810(7)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    130.(2)
_cell_measurement_theta_max      74.45
_cell_measurement_theta_min      4.70
_cell_volume                     2855.24(18)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_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      130.(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON III detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            64513
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         74.80
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5125
_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    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol, ethanol'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.316
_refine_diff_density_min         -1.497
_refine_ls_abs_structure_details
;

Flack x determined using 3586 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.588
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         11250
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.593
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.1263
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3445
_refine_ls_wR_factor_ref         0.3666
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                9625
_reflns_number_total             11250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03430a2.cif
_cod_data_source_block           23mdw94d_Hunter
_cod_depositor_comments
'Adding full bibliography for 7133757--7133764.cif.'
_cod_database_code               7133761
_shelx_res_checksum              18292