Hydroboration of CO2 catalyzed by bis(phosphinite) pincer ligated nickel thiolate complexes.
Liu, Ting; Meng, Wenjuan; Ma, Qiang-Qiang; Zhang, Jie; Li, Huizhen; Li, Shujun; Zhao, Qianyi; Chen, Xuenian; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4504–4509; doi:10.1039/c7dt00490g

data_7042440
_publ_section_title
;
 Hydroboration of CO2 catalyzed by bis(phosphinite) pincer ligated nickel
 thiolate complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4504
_journal_page_last               4509
_journal_paper_doi               10.1039/c7dt00490g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C29 H46 Ni O3 P2 S'
_chemical_formula_sum            'C29 H46 Ni O3 P2 S'
_chemical_formula_weight         595.37
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-10-25 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                100.6840(10)
_cell_angle_beta                 100.6810(10)
_cell_angle_gamma                103.9190(10)
_cell_formula_units_Z            6
_cell_length_a                   11.3208(8)
_cell_length_b                   16.0967(11)
_cell_length_c                   27.9299(19)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.27
_cell_volume                     4711.3(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33145
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.76
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.8543
_exptl_absorpt_correction_T_min  0.8543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         16577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.5625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                11903
_reflns_number_total             16577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00490g2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7042438--7042444.cif.'
_cod_database_code               7042440
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5), C33(H33), C32(H32), C34(H34), C62(H62), C61(H61),
 C63(H63), C82(H82), C85(H85), C84(H84), C83(H83), C26(H26), C24(H24), C25(H25),
  C27(H27), C56(H56), C55(H55), C54(H54), C53(H53)
2.b Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C8(H8A,H8B,H8C), C75(H75A,H75B,H75C), C41(H41A,H41B,
 H41C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C78(H78A,H78B,H78C), C42(H42A,
 H42B,H42C), C16(H16A,H16B,H16C), C71(H71A,H71B,H71C), C74(H74A,H74B,H74C),
 C72(H72A,H72B,H72C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C51(H51A,H51B,
 H51C), C43(H43A,H43B,H43C), C18(H18A,H18B,H18C), C87(H87A,H87B,H87C), C37(H37A,
 H37B,H37C), C10(H10A,H10B,H10C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C),
 C70(H70A,H70B,H70C), C80(H80A,H80B,H80C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C),
  C29(H29A,H29B,H29C), C47(H47A,H47B,H47C), C39(H39A,H39B,H39C), C46(H46A,H46B,
 H46C), C76(H76A,H76B,H76C), C22(H22A,H22B,H22C), C45(H45A,H45B,H45C), C38(H38A,
 H38B,H38C), C58(H58A,H58B,H58C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C),
 C79(H79A,H79B,H79C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'