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_4086717
_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         'C38 H56 Ni O P2 Si'
_chemical_formula_sum            'C38 H56 Ni O P2 Si'
_chemical_formula_weight         677.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   shelxt
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.026(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1646(9)
_cell_length_b                   14.9580(13)
_cell_length_c                   19.3421(17)
_cell_measurement_reflns_used    13777
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      3.1
_cell_volume                     3600.7(6)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 2.0 r15 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 2.0 r15 
;
_computing_data_reduction
; 
Rigaku CrystalClear-SM Expert 2.0 r15 
;
_computing_molecular_graphics
;
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type
; 
 'Rigaku SCX Mini, Rigaku Mercury275R CCD'
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15326
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.178
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       Block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+2.0714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4880
_reflns_number_total             6175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00514_si_003.cif
_cod_data_source_block           '_(CyPSiP)NiH(CO)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        3600.7(5)
_cod_database_code               4086717
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.934
_exptl_absorpt_special_details   'Jacobson, R. (1998) Private Communication'
_shelx_res_checksum              84692
_shelx_hkl_checksum              30059