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_4304349
_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         'C34 H41 Br Cl2 N O P '
_chemical_formula_sum            'C34 H41 Br Cl2 N O P'
_chemical_formula_weight         661.492
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           maXus
_cell_angle_alpha                79.6019(11)
_cell_angle_beta                 83.6492(11)
_cell_angle_gamma                88.124(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8565(3)
_cell_length_b                   11.3286(3)
_cell_length_c                   15.5802(5)
_cell_measurement_reflns_used    14208
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     1700.47(9)
_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)'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.03262
_diffrn_orient_matrix_UB_12      -0.02626
_diffrn_orient_matrix_UB_13      0.09311
_diffrn_orient_matrix_UB_21      -0.00994
_diffrn_orient_matrix_UB_22      0.08525
_diffrn_orient_matrix_UB_23      0.02624
_diffrn_orient_matrix_UB_31      -0.06141
_diffrn_orient_matrix_UB_32      -0.02183
_diffrn_orient_matrix_UB_33      0.00769
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11881
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  0.465
_exptl_absorpt_correction_T_min  0.385
_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    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_refine_diff_density_max         1.493
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.232
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.232
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.1146
_refine_ls_shift/su_max          0.744
_refine_ls_shift/su_mean         0.031
_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          0.3181
_refine_ls_wR_factor_ref         0.3463
_reflns_number_gt                4121
_reflns_number_total             5940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701836j-file003_1.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C34 H41 Br Cl2 N O P '
_cod_database_code               4304349