Coordination of a Diphosphine–Ketone Ligand to Ni(0), Ni(I), and Ni(II): Reduction-Induced Coordination
Saes, Bartholomeus W. H.; Verhoeven, Dide G. A.; Lutz, Martin; Klein Gebbink, Robertus J. M.; Moret, Marc-Etienne; Organometallics 34 (2015) 2710–; doi:10.1021/acs.organomet.5b00264

data_4085907
_publ_section_title
;
 Coordination of a Diphosphine--Ketone Ligand to Ni(0), Ni(I), and Ni(II):
 Reduction-Induced Coordination
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2710
_journal_paper_doi               10.1021/acs.organomet.5b00264
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C55 H43 Ni O P3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C57 H48 Ni O1.5 P3'
_chemical_formula_weight         908.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 108.318(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5071(5)
_cell_length_b                   17.8465(6)
_cell_length_c                   19.8676(6)
_cell_measurement_reflns_used    33680
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.57
_cell_volume                     4546.5(3)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0374
_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       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54739
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         1.571
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10440
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0437P)^2^+1.9428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7831
_reflns_number_total             10440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00264_si_002.cif
_cod_data_source_block           l0682a
_cod_depositor_comments
'Adding full bibliography for 4085904--4085907.cif.'
_cod_original_formula_sum        'C57 H48 Ni O1.50 P3'
_cod_database_code               4085907
_shelxl_version_number           2014-3
_shelx_res_checksum              27513
_shelx_hkl_checksum              12000