Using CS2 to Probe the Mechanistic Details of Decarboxylation of Bis(phosphinite)-Ligated Nickel Pincer Formate Complexes
Ma, Qiang-Qiang; Liu, Ting; Adhikary, Anubendu; Zhang, Jie; Krause, Jeanette A.; Guan, Hairong; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00759

data_4086807
_publ_section_title
;
 Using CS2 to Probe the Mechanistic Details of Decarboxylation of
 Bis(phosphinite)-Ligated Nickel Pincer Formate Complexes
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00759
_journal_year                    2016
_chemical_formula_moiety         'C23 H40 Ni O2 P2 S2'
_chemical_formula_sum            'C23 H40 Ni O2 P2 S2'
_chemical_formula_weight         533.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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           SHELXL-2014/7
_cell_angle_alpha                99.6750(10)
_cell_angle_beta                 100.6600(10)
_cell_angle_gamma                103.8270(10)
_cell_formula_units_Z            2
_cell_length_a                   8.51600(10)
_cell_length_b                   11.9625(2)
_cell_length_c                   14.0994(3)
_cell_measurement_reflns_used    3333
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.48
_cell_measurement_theta_min      3.27
_cell_volume                     1336.31(4)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker SMART v5.634'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART6000 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11415
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.969
_diffrn_reflns_theta_min         3.271
_exptl_absorpt_coefficient_mu    3.766
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick)'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_transmission_factor_max   0.806
_exptl_transmission_factor_min   0.728
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0590P)^2^+0.2428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4064
_reflns_number_total             4623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00759_si_002.cif
_cod_data_source_block           3
_cod_database_code               4086807
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.728
_shelx_estimated_absorpt_t_max   0.806
_shelx_res_checksum              51842
_shelx_hkl_checksum              32131