Nickel(II) Complexes Containing Bidentate Amido Phosphine Ligands Derived from α-Iminophosphorus Ylides: Synthesis and Structural Characterization
Pei-Ying Lee; Lan-Chang Liang; Inorganic Chemistry 47 (2008) 749–758; doi:10.1021/ic701836j

data_4304354
_publ_section_title
;
Nickel(II) Complexes Containing Bidentate Amido Phosphine Ligands Derived
from \a-Iminophosphorus Ylides: Synthesis and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              749
_journal_page_last               758
_journal_paper_doi               10.1021/ic701836j
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C44 H54 N2 O2 P2 '
_chemical_formula_sum            'C44 H54 N2 O2 P2'
_chemical_formula_weight         704.876
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3792(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3747(3)
_cell_length_b                   16.4104(4)
_cell_length_c                   21.9760(7)
_cell_measurement_reflns_used    28470
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     4006.74(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.04592
_diffrn_orient_matrix_UB_12      0.01627
_diffrn_orient_matrix_UB_13      -0.07568
_diffrn_orient_matrix_UB_21      -0.05197
_diffrn_orient_matrix_UB_22      -0.00117
_diffrn_orient_matrix_UB_23      -0.03179
_diffrn_orient_matrix_UB_31      0.00007
_diffrn_orient_matrix_UB_32      0.04655
_diffrn_orient_matrix_UB_33      -0.00183
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33766
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.114
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.004
_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          0.1597
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                4360
_reflns_number_total             7078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701836j-file003_6.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4006.7(2)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C44 H54 N2 O2 P2 '
_cod_database_code               4304354