Base-Free Phosphine−Sulfonate Nickel Benzyl Complexes
Zhou, Xiaoyuan; Bontemps, Sébastien; Jordan, Richard F.; Organometallics 27 (2008) 4821–; doi:10.1021/om800741w

data_4072306
_publ_section_title
;
 Base-Free Phosphine&#x2212;Sulfonate Nickel Benzyl Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4821
_journal_paper_doi               10.1021/om800741w
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C59 H78 Ni2 O6 P2 S2'
_chemical_formula_weight         1126.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.493(5)
_cell_angle_beta                 85.024(5)
_cell_angle_gamma                81.311(5)
_cell_formula_units_Z            2
_cell_length_a                   10.524(3)
_cell_length_b                   14.941(4)
_cell_length_c                   17.791(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2753.6(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0627
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26770
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.8456
_exptl_absorpt_correction_T_min  0.7932
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         9780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                6263
_reflns_number_total             9780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800741w_si_004.cif
_cod_data_source_block           zhon07s
_cod_database_code               4072306