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_2019289
_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 I2 (C18 H40 P2)]'
_chemical_formula_moiety         'C18 H40 I2 Ni P2'
_chemical_formula_sum            'C18 H40 I2 Ni P2'
_chemical_formula_weight         630.95
_chemical_name_common            (dtbpe)NiI2
_chemical_name_systematic
'[1,2-Bis(di-<i>tert</i>-butylphosphanyl)ethane-\k^2^<i>P</i>,<i>P</i>']diiodidonickel(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                 110.9990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.4783(9)
_cell_length_b                   8.3037(4)
_cell_length_c                   14.9472(7)
_cell_measurement_reflns_used    8357
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.67
_cell_volume                     2372.90(19)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker APEXII Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'ImuS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12902
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    3.554
_exptl_absorpt_correction_T_max  0.8423
_exptl_absorpt_correction_T_min  0.6751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008<i>a</i>)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.482
_refine_ls_abs_structure_details 'Flack (1983), <b>???? Friedel pairs</b>'
_refine_ls_abs_structure_Flack   0.115(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4689
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.1993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0478
_reflns_number_gt                4404
_reflns_number_total             4689
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fa3325.cif
_cod_data_source_block           lw23
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               2019289
_shelx_res_checksum              35456