Dinitrogen-Facilitated Reversible Formation of a Si‒H Bond in a Pincer-Supported Ni Complex
Charboneau, David J.; Balcells, David; Hazari, Nilay; Lant, Hannah M. C.; Mayer, James M.; Melvin, Patrick R.; Mercado, Brandon Q.; Morris, Wesley D.; Repisky, Michal; Suh, Hee-Won; Organometallics 35 (2016) 3154–; doi:10.1021/acs.organomet.6b00514

data_4086716
_publ_section_title
;
 Dinitrogen-Facilitated Reversible Formation of a Si--H Bond in a
 Pincer-Supported Ni Complex
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3154
_journal_paper_doi               10.1021/acs.organomet.6b00514
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C74 H112 N2 Ni2 P4 Si2'
_chemical_formula_sum            'C74 H112 N2 Ni2 P4 Si2'
_chemical_formula_weight         1327.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.697(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.107(3)
_cell_length_b                   14.1275(2)
_cell_length_c                   40.221(5)
_cell_measurement_reflns_used    106109
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.6
_cell_measurement_theta_min      1.9
_cell_volume                     19296(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
; 
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program 
(2009). J. Appl. Cryst., 42, 339-341. 
;
_computing_publication_material  'SHELXL-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            194936
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.580
_diffrn_reflns_theta_max         66.580
_diffrn_reflns_theta_min         2.271
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5712
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         16985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11259
_reflns_number_total             16985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00514_si_003.cif
_cod_data_source_block           '_(CyPSiHP)2Ni2(mu-N2)'
_cod_database_code               4086716
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.775
_shelx_res_checksum              97333
_shelx_hkl_checksum              72651
_shelx_fab_checksum              16080