Bis(1,4,7-trithiacyclononane)nickel(II) bis(tetrafluoridoborate) nitromethane disolvate
Lee, John P.; Grant, Gregory J.; Noll, Bruce C.; Acta Crystallographica Section E 67 (2011) m1417–m1418; doi:10.1107/S1600536811037809

data_2231812
_publ_section_title
;
 Bis(1,4,7-trithiacyclononane)nickel(II) bis(tetrafluoridoborate)
 nitromethane disolvate
;
_journal_coeditor_code           BR2171
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1417
_journal_page_last               m1418
_journal_paper_doi               10.1107/S1600536811037809
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C6 H12 S3)2](BF4)2, 2C H3 N O2'
_chemical_formula_moiety         'C12 H24 Ni S6 2+, 2(B F4), 2(C H3 N O2)'
_chemical_formula_sum            'C14 H30 B2 F8 N2 Ni O4 S6'
_chemical_formula_weight         715.09
_chemical_name_systematic
;
Bis(1,4,7-trithiacyclononane)nickel(II) bis(tetrafluoridoborate)
nitromethane disolvate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1755(18)
_cell_length_b                   19.825(4)
_cell_length_c                   15.173(3)
_cell_measurement_reflns_used    241
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.1794
_cell_measurement_theta_min      2.8051
_cell_volume                     2759.7(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type
'Bruker SMART X2S benchtop crystallographic system'
_diffrn_measurement_method       'thin-slice \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25688
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.9407
_exptl_absorpt_correction_T_min  0.3709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+1.8397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                3855
_reflns_number_total             4889
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2171.cif
_cod_data_source_block           I
_cod_original_cell_volume        2759.6(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231812
_cod_database_fobs_code          2231812