4,4'-(1,2-Diazaniumylethane-1,2-diyl)dibenzoate trihydrate
Numata, Takashi; Ikenomoto, Shun; Akitsu, Takashiro; IUCrData 1 (2016) x160252–; doi:10.1107/S2414314616002522

data_1542542
_publ_section_title
;
 4,4'-(1,2-Diazaniumylethane-1,2-diyl)dibenzoate trihydrate
;
_journal_coeditor_code           RZ4001
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x160252
_journal_paper_doi               10.1107/S2414314616002522
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C16 H16 N2 O4, 3H2 O'
_chemical_formula_moiety         'C16 H16 N2 O4, 3(H2 O)'
_chemical_formula_sum            'C16 H22 N2 O7'
_chemical_formula_weight         354.35
_chemical_name_systematic
;
4,4'-(1,2-Diazaniumylethane-1,2-diyl)dibenzoate trihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                109.182(6)
_cell_angle_beta                 93.369(6)
_cell_angle_gamma                98.437(6)
_cell_formula_units_Z            1
_cell_length_a                   6.778(3)
_cell_length_b                   6.953(3)
_cell_length_c                   9.458(4)
_cell_measurement_reflns_used    2325
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.29
_cell_volume                     413.7(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2325
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             188
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.214
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 217 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_coef       0.061(11)
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+0.1469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                1969
_reflns_number_total             2030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz4001sup1.cif
_cod_data_source_block           I
_cod_database_code               1542542
_cod_database_fobs_code          1542542
_shelx_hkl_checksum              42731
_shelx_res_checksum              9268