The crystal structure of 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium tetrachloridocobaltate(II) monohydrate, C10H18Cl4CoN2O
Reiss, Guido J.; Sergeeva, Alena; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 159–161; doi:10.1515/ncrs-2016-0245

data_8106468
_publ_section_title
;
 The crystal structure of
 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
 tetrachloridocobaltate(II) monohydrate, C10H18Cl4CoN2O
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              159
_journal_page_last               161
_journal_paper_doi               10.1515/ncrs-2016-0245
_journal_volume                  232
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C10 H16 N2, Cl4 Co, H2 O'
_chemical_formula_sum            'C10 H18 Cl4 Co N2 O'
_chemical_formula_weight         382.99
_chemical_name_systematic
;
3-((1<i>R</i>,2<i>S</i>)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
tetrachloridocobaltate(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   difmap
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0057(3)
_cell_length_b                   7.4317(3)
_cell_length_c                   29.2510(13)
_cell_measurement_reflns_used    8263
_cell_measurement_temperature    110.0(1)
_cell_measurement_theta_max      31.6110
_cell_measurement_theta_min      2.9770
_cell_volume                     1522.93(11)
_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_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'SHELXL-2014/7 [3]'
_computing_structure_solution    'SHELXT  [2]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2711
_diffrn_detector_type            EOS
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            13791
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        28.998
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.785
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.35.
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'blue turquoise'
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       plate
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 1462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Crystallogr. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0356
_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^)+(0.015P)^2^+3.2P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.718
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3865
_reflns_number_total             4052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0245_suppl.cif
_cod_data_source_block           exp_1115
_cod_database_code               8106468
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              46638
_shelx_hkl_checksum              85954