Influence of the d-Electron Count on CO Binding by Three-Coordinate [(tBu2PCH2SiMe2)2N]Fe, -Co, and -Ni
Michael J. Ingleson; Benjamin C. Fullmer; Drew T. Buschhorn; Hongjun Fan; Maren Pink; John C. Huffman; Kenneth G. Caulton; Inorganic Chemistry 47 (2008) 407–409; doi:10.1021/ic7023764

data_4304795
_publ_section_title
;
Influence of the d-Electron Count on CO Binding by Three-Coordinate
[(tBu2PCH2SiMe2)2N]Fe, -Co, and -Ni
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              407
_journal_page_last               409
_journal_paper_doi               10.1021/ic7023764
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C22 H52 N Ni P2 Si2'
_chemical_formula_sum            'C22 H52 N Ni P2 Si2'
_chemical_formula_weight         507.48
_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                   17.206(2)
_cell_length_b                   11.5897(14)
_cell_length_c                   29.700(4)
_cell_measurement_reflns_used    8977
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.2
_cell_volume                     5922.5(13)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003), XTEL (loc. libr.)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'0.30 degree frames measured for 10 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            149268
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  707
_diffrn_standards_number         370
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.7839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0281P)^2^+2.9198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                5934
_reflns_number_total             6824
_reflns_threshold_expression     &gt;2sigma(I)
_cod_data_source_file            ic7023764-file004.cif
_cod_data_source_block           05180
_cod_original_cell_volume        5922.6(12)
_cod_database_code               4304795