Ni(II) Phosphine and Phosphide Complexes Supported by a PNP-Pyrrole Pincer Ligand
Kessler, Julie A.; Iluc, Vlad M.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02784B

data_7044051
_publ_section_title
;
 Ni(II) Phosphine and Phosphide Complexes Supported by a PNP-Pyrrole
 Pincer Ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02784B
_journal_year                    2017
_chemical_formula_sum            'C21 H43 F6 N Ni O3 P4'
_chemical_formula_weight         654.15
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-07-28 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                109.950(2)
_cell_angle_beta                 107.078(2)
_cell_angle_gamma                107.074(2)
_cell_formula_units_Z            4
_cell_length_a                   14.4915(6)
_cell_length_b                   15.0549(6)
_cell_length_c                   16.2395(6)
_cell_measurement_reflns_used    7855
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.24
_cell_volume                     2861.4(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71121
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.484
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7500
_reflns_number_total             10079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02784b2.cif
_cod_data_source_block           JK4_165_0m
_cod_database_code               7044051
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2013-4
_shelx_res_checksum              77969