Non-stoichiometric carbamazepine cocrystal hydrates of 3,4-/3,5-dihydroxybenzoic acids: coformer-water exchange.
Rajbongshi, Trishna; Sarmah, Kashyap Kumar; Das, Susobhan; Deka, Poonam; Saha, Arijit; Saha, Binoy K.; Puschmann, Horst; Reddy, C. Malla; Thakuria, Ranjit; Chemical communications (Cambridge, England) 59 (2023) 3902–3905; doi:10.1039/d2cc06860e

data_7131384
_publ_section_title
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 Non-stoichiometric carbamazepine cocrystal hydrates of
 3,4-/3,5-dihydroxybenzoic acids: coformer-water exchange.
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_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3902
_journal_page_last               3905
_journal_paper_doi               10.1039/d2cc06860e
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C15 H12 N2 O, 0.25(C7 H5 O4), 0.5(H2 O)'
_chemical_formula_sum            'C16.75 H14.25 N2 O2.5'
_chemical_formula_weight         283.55
_chemical_name_systematic
'Carbamazapine-34dihydroxybenzoic acid hydrate cocrystal'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-10 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.1200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.0388(2)
_cell_length_b                   5.22610(10)
_cell_length_c                   26.3430(4)
_cell_measurement_reflns_used    13349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.275
_cell_measurement_theta_min      3.432
_cell_volume                     2831.87(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  Xcalibur
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13349
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.275
_diffrn_reflns_theta_min         3.432
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Xcalibur
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             1190
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.00098(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2582
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0428P)^2^+1.9001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2384
_reflns_number_total             2582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06860e2.cif
_cod_data_source_block           cbz_34dhba
_cod_depositor_comments
'Adding full bibliography for 7131382--7131385.cif.'
_cod_original_formula_sum        'C16.75 H14.25 N2 O2.50'
_cod_database_code               7131384
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   'Sheldrick,G.M.,2015,University of gottingen'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C006-C00F = C00F-C00J = C00J-C00E = C00E-C00A = C00A-C007 = C007-C006
 1.39 with sigma of 0.01
 C5-C8 = C8-C1 = C1-C4 = C4-C3 = C3-C10 = C10-C5
 1.39 with sigma of 0.01
 C009-C00D = C00D-C00H = C00H-C00I = C00I-C00G = C00G-C008 = C008-C009
 1.39 with sigma of 0.01
 C10-O7 \\sim O7-C4
 with sigma of 0.001
 C5-C1 \\sim C8-C4 \\sim C1-C3 \\sim C4-C10 \\sim C3-C5 \\sim C10-C8
 with sigma of 0.02
 C006-C00J \\sim C00F-C00E \\sim C00J-C00A \\sim C00E-C007 \\sim C00A-C006
\\sim C007-C00F
 with sigma of 0.02
 C009-C00H \\sim C00D-C00I \\sim C00H-C00G \\sim C00I-C008 \\sim C00G-C009
\\sim C008-C00D
 with sigma of 0.02
 C3-O2 \\sim O2-C1
 with sigma of 0.001
3. Restrained planarity
 C006, C00F, C00J, C00E, C00A, C007
 with sigma of 0.1
 C5, C8, C1, C4, C3, C10
 with sigma of 0.1
 C009, C00D, C00H, C00I, C00G, C008
 with sigma of 0.1
4. Rigid bond restraints
 C4, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Rigid body (RIGU) restrains
 C5, C2, O1, O8, C10, C8, C3, H10, C1, H8, C4, O7, H1, O2, H7, H2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C2(0.25) O1(0.25) C4(0.25) C5(0.25) O8(0.25) C3(0.25) C1(0.25)
 H1(0.25) O7(0.25) H7(0.25) C10(0.25) H10(0.25) C8(0.25) H8(0.25) O2(0.25)
 H2(0.25) O3(0.5) H3A(0.5) H3B(0.5)
7.a Free rotating group:
 O3(H3A,H3B)
7.b Aromatic/amide H refined with riding coordinates:
 C00A(H00C), C00B(H00D), C00C(H00E), C00D(H00F), C00E(H00G), C00F(H00H),
 C00G(H00I), C00H(H00J), C00I(H00K), C00J(H00L), C1(H1), C10(H10), C8(H8)
7.c X=CH2 refined with riding coordinates:
 N003(H00A,H00B)
7.d Idealised tetrahedral OH refined as rotating group:
 O7(H7), O2(H2)
;
_shelx_res_checksum              84781
_shelx_hkl_checksum              32726
_olex2_submission_special_instructions 'No special instructions were received'