Redox-state dependent activation of silanes and ammonia with reverse polarity (PC<sub>carbene</sub>P)Ni complexes: electrophilic vs. nucleophilic carbenes.
LaPierre, Etienne A.; Piers, Warren E.; Gendy, Chris; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16789–16797; doi:10.1039/c8dt04409k

data_7048009
_publ_section_title
;
 Redox-state dependent activation of silanes and ammonia with reverse
 polarity (PC<sub>carbene</sub>P)Ni complexes: electrophilic vs.
 nucleophilic carbenes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16789
_journal_page_last               16797
_journal_paper_doi               10.1039/c8dt04409k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C31 H49 Br Ni P3, F6 Sb [+ solvent]'
_chemical_formula_sum            'C31 H49 Br F6 Ni P3 Sb'
_chemical_formula_weight         888.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-22 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   38.776(8)
_cell_length_b                   51.519(10)
_cell_length_c                   9.2266(18)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.56
_cell_volume                     18432(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
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_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            32766
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.594
_exptl_absorpt_coefficient_mu    2.007
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6296
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_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             7168
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.010(16)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         7965
_refine_ls_number_restraints     400
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_refine_ls_R_factor_all          0.0552
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_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^)+(0.0428P)^2^+0.7997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6611
_reflns_number_total             7965
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           new_a
_cod_depositor_comments
'Adding full bibliography for 7048006--7048012.cif.'
_cod_database_code               7048009
_shelx_shelxl_version_number     2014/7
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