Amido Pincer Complexes of Nickel(II): Synthesis, Structure, and Reactivity
Liang, Lan-Chang; Chien, Pin-Shu; Lin, Jia-Ming; Huang, Mei-Hui; Huang, Yu-Lun; Liao, Ju-Hsiou; Organometallics 25 (2006) 1399–1411; doi:10.1021/om050943a

data_4074864
_publ_section_title
;
 Amido Pincer Complexes of Nickel(II): Synthesis, Structure, and Reactivity
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1399
_journal_page_last               1411
_journal_paper_doi               10.1021/om050943a
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C40 H39 N Ni P2 Si '
_chemical_formula_sum            'C40 H39 N Ni P2 Si'
_chemical_formula_weight         682.503
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           maXus
_cell_angle_alpha                96.604(2)
_cell_angle_beta                 94.5042(14)
_cell_angle_gamma                90.5390(8)
_cell_formula_units_Z            4
_cell_length_a                   10.9794(2)
_cell_length_b                   15.7917(4)
_cell_length_c                   20.8066(4)
_cell_measurement_reflns_used    39604
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     3571.90(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maXus(Mackay et al., 1999)'
_computing_structure_refinement  'maXus(Mackay et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01787
_diffrn_orient_matrix_UB_12      0.08957
_diffrn_orient_matrix_UB_13      0.00276
_diffrn_orient_matrix_UB_21      0.05398
_diffrn_orient_matrix_UB_22      -0.01055
_diffrn_orient_matrix_UB_23      0.03224
_diffrn_orient_matrix_UB_31      0.02952
_diffrn_orient_matrix_UB_32      -0.00074
_diffrn_orient_matrix_UB_33      -0.03852
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33801
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.69
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             1432
_refine_diff_density_max         0.82
_refine_diff_density_min         -1.14
_refine_diff_density_rms         0.22
_refine_ls_extinction_coef       42E4(8)
_refine_ls_extinction_expression
;
 equation(22) p292 'Crystallographic Computing' (1970)
 coefficient is multiplied by 10^4
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   2.854
_refine_ls_goodness_of_fit_gt    3.008
_refine_ls_goodness_of_fit_ref   2.962
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    78
_refine_ls_number_parameters     842
_refine_ls_number_reflns         6528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.150
_refine_ls_R_factor_gt           0.067
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details     ' w = 1 / ( s^2^(Fo^2^) + 0.10000 * Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.197
_refine_ls_wR_factor_gt          0.162
_refine_ls_wR_factor_ref         0.162
_reflns_d_resolution_high        0.65
_reflns_d_resolution_low         2.13
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              24
_reflns_limit_l_min              -24
_reflns_number_gt                6595
_reflns_number_total             14222
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            om050943asi20051115_045703.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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3571.89(13)
_cod_original_sg_symbol_H-M      'P -1          '
_cod_original_formula_sum        'C40 H39 N Ni P2 Si '
_cod_database_code               4074864