Tris(tri-<i>o</i>-tolyl phosphite-κ<i>P</i>)nickel: a coordinatively unsaturated nickel(0) complex
Kampmann, Sven S.; Skelton, Brian W.; Wild, Duncan A.; Koutsantonis, George A.; Stewart, Scott G.; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615001680

data_2019866
_publ_section_title
;
 Tris(tri-<i>o</i>-tolyl phosphite-\k<i>P</i>)nickel: a coordinatively
 unsaturated nickel(0) complex
;
_journal_coeditor_code           FG3327
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615001680
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (C21 H21 O3 P)3]'
_chemical_formula_moiety         'C63 H63 Ni O9 P3'
_chemical_formula_sum            'C63 H63 Ni O9 P3'
_chemical_formula_weight         1115.75
_chemical_name_systematic
;
Tris(tri-<i>o</i>-tolylphosphite-\k<i>P</i>)nickel(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.129(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5898(9)
_cell_length_b                   12.3292(3)
_cell_length_c                   43.403(2)
_cell_measurement_reflns_used    15074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.067
_cell_measurement_theta_min      4.143
_cell_volume                     11203.7(8)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Gemini diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            56232
_diffrn_reflns_theta_full        67.355
_diffrn_reflns_theta_max         67.355
_diffrn_reflns_theta_min         4.161
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       needle
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.412
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9993
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0994
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1046P)^2^+70.9791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2586
_reflns_number_gt                8185
_reflns_number_total             9993
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3327sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        11203.8(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2019866
_cod_database_fobs_code          2019866
_shelx_hkl_checksum              81727
_shelx_res_checksum              42126