Bis(benzyltrimethylammonium) tetrachloronickelate(II) <i>N</i>-methylpyrrolidin-2-one solvate
Kooijman, Huub; Keegstra, Menno A.; Brandsma, Lambert; Spek, Anthony L.; Acta Crystallographica Section E 60 (2004) m1513–m1515; doi:10.1107/S1600536804023487

data_2204279
_publ_section_title
;
 Bis(benzyltrimethylammonium) tetrachloronickelate(II)
 <i>N</i>-methylpyrrolidin-2-one solvate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1513
_journal_page_last               m1515
_journal_paper_doi               10.1107/S1600536804023487
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C10 H16 N1)2 [Ni Cl4], C5 H9 N O'
_chemical_formula_moiety         '2C10 H16 N +, Ni Cl4 2-, C5 H9 N O'
_chemical_formula_sum            'C25 H41 Cl4 N3 Ni O'
_chemical_formula_weight         600.10
_chemical_name_systematic
;
Bis(benzyltrimethylammonium) tetrachloronickel(II)
N-methylpyrrolidin-2-one solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 93.112(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5787(10)
_cell_length_b                   9.4933(15)
_cell_length_c                   17.3172(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.65
_cell_measurement_theta_min      5.89
_cell_volume                     3049.8(6)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection
'locally modified CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method
'\w/2\q scans with \D\w = 0.81 + 0.35 tan\q (\%)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.1430
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4986
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        24.24
_diffrn_reflns_theta_max         24.24
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          1.25
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4812
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o~^2^)+(0.0815P)^2^] where P = (F~o~^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                2302
_reflns_number_total             4812
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6526.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2204279
_cod_database_fobs_code          2204279