Hydrogen bonding versus packing effects in the crystal structure of 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium tetraiodidozincate(II), C10H16I4ZnN2
Reiss, Guido J.; Sergeeva, Alena; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 959–962; doi:10.1515/ncrs-2020-0123

data_8105343
_publ_section_title
;
 Hydrogen bonding versus packing effects in the crystal structure of
 3-((1R,2S)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
 tetraiodidozincate(II), C10H16I4ZnN2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              959
_journal_page_last               962
_journal_paper_doi               10.1515/ncrs-2020-0123
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H16 N2, I4 Zn'
_chemical_formula_sum            'C10 H16 I4 N2 Zn'
_chemical_formula_weight         737.24
_chemical_melting_point          497
_chemical_name_common
;
Nicotin-1,1'-diium tetraiodidozincate(II) monohydrate
;
_chemical_name_systematic
;
3-((1<i>R</i>,2<i>S</i>)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
tetraiodidozincate(II) 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.919(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.33400(10)
_cell_length_b                   14.4781(3)
_cell_length_c                   8.6768(2)
_cell_measurement_reflns_used    45055
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      34.5798
_cell_measurement_theta_min      2.7826
_cell_volume                     917.93(3)
_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 4.6.2 [4]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT  [2]'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            57483
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         34.664
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.049
_exptl_absorpt_correction_T_max  0.373
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.667
_exptl_crystal_description       Block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.4722
_exptl_crystal_size_mid          0.2535
_exptl_crystal_size_min          0.1929
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 3488 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(12)
_refine_ls_extinction_coef       0.00118(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         7606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+0.28P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0397
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                7483
_reflns_number_total             7606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0123_suppl.cif
_cod_data_source_block           exp_1114_110
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '497 K' was changed to
'497' -- the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               8105343
_shelx_shelxl_version_number     2018/3