Study of three solvates of sulfamethazine
Ahuja, Dipali; Bannigan, Pauric; Rasmuson, Ake; CrystEngComm  (2017) –; doi:10.1039/C7CE01610G

data_7229350
_publ_section_title
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 Study of three solvates of sulfamethazine
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01610G
_journal_year                    2017
_chemical_formula_moiety         'C12 H14 N4 O2 S, C4 H9 N O'
_chemical_formula_sum            'C16 H23 N5 O3 S'
_chemical_formula_weight         365.45
_chemical_name_common            SMT-DMA
_chemical_name_systematic        'Sulfamethazine -DMA Solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-03
_audit_creation_method
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Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
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_audit_update_record
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2017-08-24 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.336(4)
_cell_length_b                   8.0711(10)
_cell_length_c                   15.218(2)
_cell_measurement_reflns_used    2807
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.83
_cell_measurement_theta_min      2.84
_cell_volume                     3848.9(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13797
_diffrn_reflns_point_group_measured_fraction_full 0.827
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.600
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0286 after correction.
The Ratio of minimum to maximum transmission is 0.9486.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 980 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.15(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7337
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+1.7769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.607
_reflns_Friedel_fraction_full    0.646
_reflns_Friedel_fraction_max     0.651
_reflns_number_gt                3633
_reflns_number_total             7337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01610g1.cif
_cod_data_source_block           pbda02_1_0ma_a
_cod_original_cell_volume        3848.8(8)
_cod_database_code               7229350
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N2A(H2A)
2.b Rotating group:
 N1A(H1AA,H1AB), N1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C6A(H6A), C2A(H2AA), C5A(H5A), C9A(H9A), C5(H5), C2(H2), C3(H3),
 N2(H2B), C6(H6), C9(H9)
2.d Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C4B(H4BA,H4BB,H4BC), C4C(H4CA,H4CB,H4CC), C1C(H1CA,H1CB,
 H1CC), C11A(H11A,H11B,H11C), C12(H12D,H12E,H12F), C11(H11D,H11E,H11F),
 C1B(H1BA,H1BB,H1BC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC)
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_shelx_res_checksum              14262
_olex2_submission_special_instructions 'No special instructions were received'