Organic NMR crystallography: enabling progress for applications to pharmaceuticals and plant cell walls.
Rehman, Zainab; Lubay, Jairah; Franks, W. Trent; Bartók, Albert P; Corlett, Emily K.; Nguyen, Bao; Scrivens, Garry; Samas, Brian M.; Frericks-Schmidt, Heather; Brown, Steven P.; Faraday discussions 255 (2025) 222–243; doi:10.1039/d4fd00088a

data_1571675
_publ_section_title
;
 Organic NMR crystallography: enabling progress for applications to
 pharmaceuticals and plant cell walls.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              222
_journal_page_last               243
_journal_paper_doi               10.1039/d4fd00088a
_journal_volume                  255
_journal_year                    2025
_chemical_formula_sum            'C22 H27 N5 O4 S'
_chemical_formula_weight         457.55
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2024-04-29 deposited with the CCDC.	2024-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.013(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1890(4)
_cell_length_b                   12.6757(6)
_cell_length_c                   10.9694(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      44.59
_cell_measurement_theta_min      4.41
_cell_volume                     1167.10(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15363
_diffrn_reflns_theta_full        44.59
_diffrn_reflns_theta_max         44.59
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    1.550
_exptl_absorpt_correction_T_max  0.9406
_exptl_absorpt_correction_T_min  0.8358
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.106
_refine_diff_density_min         -0.098
_refine_diff_density_rms         0.024
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         1846
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                1798
_reflns_number_total             1846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4fd00088a2.cif
_cod_data_source_block           z501
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1571675.cif.
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1571675