POCOP-Ligated Nickel Siloxide Complexes: Syntheses, Characterization, and Reactivities
Hao, Jingjun; Vabre, Boris; Zargarian, Davit; Organometallics 33 (2014) 6568–; doi:10.1021/om500916d

data_4084775
_publ_section_title
;
 POCOP-Ligated Nickel Siloxide Complexes: Syntheses, Characterization, and
 Reactivities
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6568
_journal_paper_doi               10.1021/om500916d
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C27 H42 Ni O3 P2'
_chemical_formula_sum            'C27 H42 Ni O3 P2'
_chemical_formula_weight         535.25
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8783(9)
_cell_length_b                   11.9099(5)
_cell_length_c                   11.3431(5)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    250
_cell_measurement_theta_max      69.18
_cell_measurement_theta_min      4.27
_cell_volume                     2820.6(2)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, )'
_computing_data_collection       'APEX2  (Bruker AXS, 0)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, )'
_computing_molecular_graphics    'SHELXTL  (Bruker AXS, 2003)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      250
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            75224
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.736
_diffrn_reflns_theta_min         4.235
_exptl_absorpt_coefficient_mu    2.253
_exptl_absorpt_correction_T_max  0.8165
_exptl_absorpt_correction_T_min  0.7076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 2413 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.428(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5252
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1562P)^2^+1.0832P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.1924
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                5207
_reflns_number_total             5252
_cod_data_source_file            om500916d_si_002.cif
_cod_data_source_block           BOR131
_cod_depositor_comments
'Adding full bibliography for 4084774--4084780.cif.'
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4084775
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.823