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_4085904
_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         'C37 H28 Cl2 Ni O P2, C H2 Cl2'
_chemical_formula_sum            'C38 H30 Cl4 Ni O P2'
_chemical_formula_weight         765.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.62126(17)
_cell_length_b                   18.4902(4)
_cell_length_c                   20.0628(5)
_cell_measurement_reflns_used    78249
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.03
_cell_volume                     3569.15(13)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            87198
_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         27.499
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.9468
_exptl_absorpt_correction_T_min  0.7309
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 3401 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0498P)^2^+2.4769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.792
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                7863
_reflns_number_total             8203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00264_si_002.cif
_cod_data_source_block           l0707a
_cod_depositor_comments
'Adding full bibliography for 4085904--4085907.cif.'
_cod_original_cell_volume        3569.16(13)
_cod_database_code               4085904
_shelxl_version_number           2014/6
_shelx_res_checksum              60383
_shelx_hkl_checksum              63876