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_4084401
_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_sum            'C31 H40 Br2 Cl2 N Ni P'
_chemical_formula_weight         747.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.135(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.067(3)
_cell_length_b                   15.738(3)
_cell_length_c                   21.280(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3318.9(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26648
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    3.222
_exptl_absorpt_correction_T_max  0.9095
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0570
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                4548
_reflns_number_total             7577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500685x_si_001.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
'Adding full bibliography for 4084401--4084405.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4084401