Bimetallic nickel complexes supported by 2,5-bis(phosphine)-1,4-hydroquinonate ligands. Structural, electrochemical and theoretical investigations
Louis R. Pignotti; Rudy L. Luck; Nihal Deligonul; John D. Protasiewicz; Kevin E. Johnson; Lillian P. Nguyen; Eugenijus Urnezius; Inorganica Chimica Acta 424 (2015) 275–285; doi:

data_1518929
_publ_section_title
;
 Bimetallic nickel complexes supported by
 2,5-bis(phosphine)-1,4-hydroquinonate ligands. Structural,
 electrochemical and theoretical investigations
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              275
_journal_page_last               285
_journal_volume                  424
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H40 F2 N2 Ni2 O2 P2 S2, 2(C4 H8 O)'
_chemical_formula_sum            'C38 H56 F2 N2 Ni2 O4 P2 S2'
_chemical_formula_weight         886.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.76(2)
_cell_angle_beta                 82.07(2)
_cell_angle_gamma                68.31(2)
_cell_formula_units_Z            2
_cell_length_a                   11.663(3)
_cell_length_b                   11.840(2)
_cell_length_c                   17.266(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     2144.4(9)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled \w/2\t scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.087603
_diffrn_orient_matrix_UB_12      0.019265
_diffrn_orient_matrix_UB_13      -0.011823
_diffrn_orient_matrix_UB_21      0.026889
_diffrn_orient_matrix_UB_22      -0.072915
_diffrn_orient_matrix_UB_23      -0.026145
_diffrn_orient_matrix_UB_31      -0.011831
_diffrn_orient_matrix_UB_32      -0.054435
_diffrn_orient_matrix_UB_33      0.052508
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0097
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5923
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         1.22
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  0.7966
_exptl_absorpt_correction_T_min  0.7206
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   9
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         5591
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+2.3904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                4851
_reflns_number_total             5591
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2015-424-274-285-6.cif
_cod_data_source_block           6
_cod_original_cell_volume        2144.4(8)
_cod_database_code               1518929