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_7133759
_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            'C21 H27 Cl N6 O7 S2'
_chemical_formula_weight         575.05
_chemical_name_systematic
'guanidinium 1,5-naphthalenedisulfonate 2-chloropropiophenone'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 90.117(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6588(5)
_cell_length_b                   20.9928(11)
_cell_length_c                   8.0310(5)
_cell_measurement_reflns_used    5853
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.72
_cell_volume                     1291.22(13)
_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 (Sheldrick 2015)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 SMART APEXII'
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12933
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              Incoatec
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.73
_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    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol ethanol'
_exptl_crystal_size_max          0.910
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.474
_refine_diff_density_min         -0.936
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3239
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1700
_refine_ls_R_factor_gt           0.1588
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1832P)^2^+6.9779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3972
_refine_ls_wR_factor_ref         0.4046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2767
_reflns_number_total             3239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03430a2.cif
_cod_data_source_block           24mdw38d
_cod_depositor_comments
'Adding full bibliography for 7133757--7133764.cif.'
_cod_database_code               7133759
_shelx_res_checksum              46704