Resolving alternative structure determinations of indapamide using 13C solid-state NMR
Evans, Caitlin L.; Evans, Ivana Radosavlijević; Hodgkinson, Paul; Chemical Communications  (2022) –; doi:10.1039/D1CC06256E

data_7129900
_publ_section_title
;
 Resolving alternative structure determinations of indapamide using 13C
 solid-state NMR
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06256E
_journal_year                    2022
_chemical_formula_moiety         'C16 H16 Cl N3 O3 S, 0.5(H2 O)'
_chemical_formula_sum            'C16 H17 Cl N3 O3.5 S'
_chemical_formula_weight         374.83
_chemical_name_common            Indapamide
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-04-23
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.1401(10)
_cell_length_b                   9.6025(4)
_cell_length_c                   23.4611(8)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.49
_cell_measurement_theta_min      2.29
_cell_volume                     6783.2(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker PHOTON III C14 MM CPAD'
_diffrn_detector_area_resol_mean 54.4
_diffrn_detector_type            'CPA sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            143804
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0 microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.4942
_exptl_absorpt_correction_T_min  0.3491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0925 after correction.
The Ratio of minimum to maximum transmission is 0.7064.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       prism
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         18001
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+24.9465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12598
_reflns_number_total             18001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06256e2.cif
_cod_data_source_block           21srv209_WOCPEM_New
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C16 H17 Cl N3 O3.50 S'
_cod_database_code               7129900
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.884
_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O2W-H2WB
 0.95 with sigma of 0.02
 H1WB-H1WA
 1.6 with sigma of 0.04
 H2WB-H2WA
 1.6 with sigma of 0.04
 N2C-H2C \\sim N2B-H2BA \\sim N2A-H2AA \\sim N2-H2
 with sigma of 0.005
 N3B-H3BB \\sim N3B-H3BA \\sim N3C-H3CB \\sim N3C-H3CA \\sim N3A-H3AB \\sim
N3-H3A
 with sigma of 0.002
 N3-H3B \\sim N3-H3A \\sim N3A-H3AA \\sim N3A-H3AB \\sim N3C-H3CA \\sim
N3C-H3CB \\sim N3B-H3BA \\sim N3B-
 H3BB
 with sigma of 0.005
 O1W-H1WA \\sim O1W-H1WB \\sim O2W-H2WA \\sim O2W-H2WB
 with sigma of 0.005
3. Others
 Fixed Uiso: H3A(0.05) H3B(0.05) H3AA(0.05) H3AB(0.05) H3BA(0.05) H3BB(0.05)
 H1WA(0.08) H1WB(0.08) H2WA(0.08) H2WB(0.08)
4.a Riding coordinates:
 N3A(H3AA,H3AB)
4.b Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C1B(H1B), C1C(H1C)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AB,H2AC), C2B(H2BB,H2BC), C2C(H2CA,H2CB)
4.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C14(H14), C15(H15), C5A(H5A),
 C6A(H6A), C7A(H7A), C8A(H8A), C11A(H11A), C14A(H14A), C15A(H15A), C5B(H5B),
 C6B(H6B), C7B(H7B), C8B(H8B), C11B(H11B), C14B(H14B), C15B(H15B), C5C(H5C),
 C6C(H6C), C7C(H7C), C8C(H8C), C11C(H11C), C14C(H14C), C15C(H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'