Structure, magnetism and colour in simple bis(phosphine)nickel(II) dihalide complexes: an experimental and theoretical investigation
Schultz, Madeleine; Plessow, Philipp-Nikolaus; Rominger, Frank; Weigel, Laura; Acta Crystallographica Section C 69 (2013) 1437–1447; doi:10.1107/S0108270113030692

data_2019288
_publ_section_title
;
 Structure, magnetism and colour in simple bis(phosphine)nickel(II)
 dihalide complexes: an experimental and theoretical investigation
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1437
_journal_page_last               1447
_journal_paper_doi               10.1107/S0108270113030692
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni Br2 (C18 H40 P2)]'
_chemical_formula_moiety         'C18 H40 Br2 Ni P2'
_chemical_formula_sum            'C18 H40 Br2 Ni P2'
_chemical_formula_weight         536.97
_chemical_name_common            (dtbpe)NiBr2
_chemical_name_systematic
'[1,2-Bis(di-<i>tert</i>-butylphosphanyl)ethane-\k^2^<i>P</i>,<i>P</i>']dibromidonickel(II)'
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.2720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3765(14)
_cell_length_b                   8.1817(6)
_cell_length_c                   14.7392(10)
_cell_measurement_reflns_used    2012
_cell_measurement_temperature    200(2)
_cell_volume                     2273.9(3)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3740
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    4.507
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008<i>a</i>)
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .12
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.503
_refine_ls_abs_structure_details 'Flack (1983), <b>???? Friedel pairs</b>'
_refine_ls_abs_structure_Flack   0.033(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3024
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                2676
_reflns_number_total             3024
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fa3325.cif
_cod_data_source_block           msc11
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2019288
_shelx_res_checksum              84239