Bis[1,2-bis(diphenylphosphino)ethene]nickel(II) diperchlorate
Li, Yi-Zhi; Liu, Jia-Cheng; Qu, Jian-Qiang; Wang, Liu-Fang; Xia, Chun-Gu; Niu, Jian-Zhong; Acta Crystallographica Section E 58 (2002) m237–m238; doi:10.1107/S1600536802007213

data_2201054
_publ_section_title
;
 Bis[1,2-bis(diphenylphosphino)ethene]nickel(II) diperchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m237
_journal_page_last               m238
_journal_paper_doi               10.1107/S1600536802007213
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ni (C26 H22 P2)2] (Cl O4)2'
_chemical_formula_moiety         'C52 H44 Ni P4 2+, 2Cl O4 1-'
_chemical_formula_sum            'C52 H44 Cl2 Ni O8 P4'
_chemical_formula_weight         1050.34
_chemical_name_systematic
;
 Bis[1,2-bis(diphenylphosphino)ethene)]nickel(II) diperchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8450(10)
_cell_length_b                   16.1980(10)
_cell_length_c                   13.1980(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.89
_cell_measurement_theta_min      9.19
_cell_volume                     2308.7(3)
_computing_cell_refinement       CAD-4/PC
_computing_data_collection       'CAD-4/PC (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.434
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.03P)^2^+0.65P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                3195
_reflns_number_total             4029
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6161.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2201054
_cod_database_fobs_code          2201054