The crystal structure of 3,5-dicarboxybenzenaminium perchlorate monohydrate, C8H8ClNO9
Cai, Bin; Li, Shu-Jing; Zhu, Meng-En; Li, Meng-Qi; Meng, Yuning; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 1–2; doi:10.1515/ncrs-2019-0358

data_8104995
_publ_section_title
;
 The crystal structure of 3,5-dicarboxybenzenaminium perchlorate
 monohydrate, C8H8ClNO9
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1
_journal_page_last               2
_journal_paper_doi               10.1515/ncrs-2019-0358
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C8 H8 N O4, Cl O4, H2 O'
_chemical_formula_sum            'C8 H10 Cl N O9'
_chemical_formula_weight         299.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.760(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1284(3)
_cell_length_b                   8.5538(5)
_cell_length_c                   18.7089(10)
_cell_measurement_reflns_used    9563
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.334
_cell_measurement_theta_min      3.249
_cell_volume                     1124.26(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015) [1]'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009 [4])'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009 [4])'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015) [3]'
_computing_structure_solution    'ShelXS (Sheldrick, 2008) [2]'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_diffrn_measurement_device       'Bruker APEX-II diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17482
_diffrn_reflns_theta_full        25.1999
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0667 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.9489.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.7700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             617.0809
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.8660
_refine_diff_density_min         -0.5685
_refine_diff_density_rms         0.0771
_refine_ls_d_res_high            0.8346
_refine_ls_d_res_low             9.2191
_refine_ls_goodness_of_fit_ref   1.0672
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0672
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0523P)^2^+1.5467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -6
_reflns_number_gt                1827
_reflns_number_total             2024
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2019-0358_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8104995
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 N1(H1a,H1b,H1c), O1W(H1Wa,H1Wb)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;