Synthesis and Structures of Nickel Complexes with a PN-Chelate Phosphaalkene Ligand
Takeuchi, Katsuhiko; Minami, Ataru; Nakajima, Yumiko; Ozawa, Fumiyuki; Organometallics 33 (2014) 5365–; doi:10.1021/om500685x

data_4084402
_publ_section_title
;
 Synthesis and Structures of Nickel Complexes with a PN-Chelate
 Phosphaalkene Ligand
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5365
_journal_paper_doi               10.1021/om500685x
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C60 H72 Br2 N2 Ni2 P2, 0.46(C4 H10 O)'
_chemical_formula_sum            'C61.84 H76.61 Br2 N2 Ni2 O0.46 P2'
_chemical_formula_weight         1194.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.421(3)
_cell_length_b                   21.212(4)
_cell_length_c                   34.351(6)
_cell_measurement_temperature    173(2)
_cell_volume                     12694(4)
_computing_cell_refinement       'CrystalClear (rigaku/MSC inc., 2006)'
_computing_data_collection       'CrystalClear (rigaku/MSC inc., 2006)'
_computing_data_reduction        'CrystalClear (rigaku/MSC inc., 2006)'
_computing_molecular_graphics    'Mercury 3.1.1'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  ' CCD area detector '
_diffrn_measurement_method       ' phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            96304
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  0.8601
_exptl_absorpt_correction_T_min  0.7463
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.445
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         14503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2166
_reflns_number_gt                8714
_reflns_number_total             14503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500685x_si_001.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
'Adding full bibliography for 4084401--4084405.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4084402