[NiIII(OMe)]-mediated reductive activation of CO2affording a Ni(κ1-OCO) complex
Chiou, Tzung-Wen; Tseng, Yen-Ming; Lu, Tsai-Te; Weng, Tsu-Chien; Sokaras, Dimosthenes; Ho, Wei-Chieh; Kuo, Ting-Shen; Jang, Ling-Yun; Lee, Jyh-Fu; Liaw, Wen-Feng; Chem. Sci. 7 (2016) 3640–; doi:10.1039/C5SC04652A

data_1542558
_publ_section_title
;
 [NiIII(OMe)]-mediated reductive activation of CO2affording a Ni(\k1-OCO)
 complex
;
_journal_issue                   6
_journal_name_full               'Chem. Sci.'
_journal_page_first              3640
_journal_paper_doi               10.1039/C5SC04652A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C68 H74 N Ni O3 P3 S3 Si3'
_chemical_formula_weight         1285.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccvcdq9
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-11-05 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.4702(8)
_cell_length_b                   17.1432(6)
_cell_length_c                   27.9778(8)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     13175.5(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker APEX2'
_computing_publication_material  'Bruker APEX2'
_computing_structure_refinement  'Shelxtl-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxtl-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            76294
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.517
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         13499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+24.4055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                9267
_reflns_number_total             13499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04652a2.cif
_cod_data_source_block           091120lt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1542558--1542560.cif.
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1542558