The crystal structure of 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium tetrachloridozincate(II) monohydrate, C10H18Cl4ZnN2O
Reiss, Guido J.; Sergeeva, Alena; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 851–854; doi:10.1515/ncrs-2020-0054

data_8105307
_publ_section_title
;
 The crystal structure of
 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
 tetrachloridozincate(II) monohydrate, C10H18Cl4ZnN2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              851
_journal_page_last               854
_journal_paper_doi               10.1515/ncrs-2020-0054
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H16 N2, Cl4 Zn, H2 O'
_chemical_formula_sum            'C10 H18 Cl4 N2 O Zn'
_chemical_formula_weight         389.43
_chemical_melting_point          489
_chemical_name_common
;
Nicotin-1,1'-diium tetrachloridozincate(II) monohydrate
;
_chemical_name_systematic
;
3-((1<i>R</i>,2<i>S</i>)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
tetrachloridozincate(II) monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.07520(10)
_cell_length_b                   7.50850(10)
_cell_length_c                   29.3383(5)
_cell_measurement_reflns_used    22078
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      31.7250
_cell_measurement_theta_min      2.9620
_cell_volume                     1558.57(4)
_computing_cell_refinement       'CrysAlis^Pro^, Ver. 38.43 [1]'
_computing_data_collection       'CrysAlis^Pro^, Ver. 38.43 [1]'
_computing_data_reduction        'CrysAlis^Pro^, Ver. 38.43 [1]'
_computing_molecular_graphics    'Diamond 4.0 [4]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT  [2]'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            27747
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        27.999
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         4.168
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.35 
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.8024
_exptl_crystal_size_mid          0.5406
_exptl_crystal_size_min          0.1315
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3750
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0152P)^2^+2.3631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3604
_reflns_number_total             3750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0054_suppl.cif
_cod_data_source_block           exp_1094_rt
_cod_database_code               8105307