Preparation and Dehydration Kinetics of Complex Sulfadiazine Calcium Hydrate with Both Channel-Type and Coordinated Water
Sun, Jia; Xie, Chuang; Zhang, Xia; Bao, Ying; Hou, Baohong; Wang, Zhao; Gong, Junbo; Hao, Hongxun; Wang, Yongli; Wang, Jingkang; Yin, Qiuxiang; Organic Process Research & Development 20 (2016) 780–; doi:10.1021/acs.oprd.6b00027

data_1542985
_publ_section_title
;
 Preparation and Dehydration Kinetics of Complex Sulfadiazine Calcium
 Hydrate with Both Channel-Type and Coordinated Water
;
_journal_issue                   4
_journal_name_full               'Organic Process Research &amp; Development'
_journal_page_first              780
_journal_paper_doi               10.1021/acs.oprd.6b00027
_journal_volume                  20
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_sum            'C40 H68 Ca2 N16 O24 S4'
_chemical_formula_weight         1365.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.850(3)
_cell_length_b                   15.604(3)
_cell_length_c                   14.083(3)
_cell_measurement_reflns_used    21647
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     3043.5(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29926
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.997
_exptl_absorpt_coefficient_mu    0.414
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.32(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         13668
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.5451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                10377
_reflns_number_total             13668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op6b00027_si_002.cif
_cod_data_source_block           b
_cod_depositor_comments          'Adding full bibliography for 1542985.cif.'
_cod_database_code               1542985
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              91305
_shelx_hkl_checksum              44699