Supramolecular synthesis and thermochemical investigations of pharmaceutical inorganic isoniazid salts
de Melo, Cristiane C.; de Sousa Carvalho, Paulo; Diniz, Luan F.; D'Vries, Richard F.; Ayala, Alejandro P.; Ellena, Javier; CrystEngComm 18 (2016) 6378–; doi:10.1039/C6CE00969G

data_7225824
_publ_section_title
;
 Supramolecular synthesis and thermochemical investigations of
 pharmaceutical inorganic isoniazid salts
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6378
_journal_paper_doi               10.1039/C6CE00969G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C6 H9 N3 O, O4 S, 0.5(H2 O)'
_chemical_formula_sum            'C6 H10 N3 O5.5 S'
_chemical_formula_weight         244.23
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-19 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4175(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.9562(3)
_cell_length_b                   19.7321(8)
_cell_length_c                   13.4459(6)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      3.04
_cell_volume                     1842.31(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.9865
_diffrn_measured_fraction_theta_max 0.9793
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10216
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.367
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.7609
_exptl_crystal_description       prism
_exptl_crystal_F_000             1017.6278
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4715
_refine_diff_density_min         -0.6114
_refine_diff_density_rms         0.0989
_refine_ls_d_res_high            0.7906
_refine_ls_d_res_low             7.9495
_refine_ls_goodness_of_fit_ref   1.0594
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0594
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+1.4319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.0
_reflns_number_gt                3282
_reflns_number_total             3830
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6ce00969g2.cif
_cod_data_source_block           NHSO4
_cod_depositor_comments
'Adding full bibliography for 7225824--7225827.cif.'
_cod_database_code               7225824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 N1'(H1',H3'a,H3'b,H3'c,H2',H3a,H2,H3b,H1,H3c)
2.b Free rotating group:
 OW1(HW1a,HW1b)
2.c Aromatic/amide H refined with riding coordinates:
 C6'(H6'), C6(H6), C3'(H3'), C5(H5), C4(H4), C3(H3), C5'(H5'), C4'(H4')
;
_olex2_submission_special_instructions 'No special instructions were received'