Synthesis and Reactivity of NHC-Supported Ni2(μ(2)-η(2),η(2)-S2)-Bridging Disulfide and Ni2(μ-S)2-Bridging Sulfide Complexes.
Olechnowicz, Frank; Hillhouse, Gregory L.; Jordan, Richard F.; Inorganic chemistry 54 (2015) 2705–2712; doi:10.1021/ic502892r

data_4342643
_publ_section_title
;
 Synthesis and Reactivity of NHC-Supported
 Ni2(\m(2)-\h(2),\h(2)-S2)-Bridging Disulfide and Ni2(\m-S)2-Bridging
 Sulfide Complexes.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2705
_journal_page_last               2712
_journal_paper_doi               10.1021/ic502892r
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C38 H51 N3 Ni S2, C4 H8 O'
_chemical_formula_sum            'C42 H59 N3 Ni O S2'
_chemical_formula_weight         744.75
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                90
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_cell_length_b                   15.7096(7)
_cell_length_c                   18.9277(8)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1051
_cell_measurement_theta_min      2.5125
_cell_volume                     4456.3(3)
_computing_cell_refinement       'APEX2 v2013.10-0 (Bruker AXS)'
_computing_data_collection       ShelXtl
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Mercury v3.3.1 (CCDC, 2014)'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
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_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            100626
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.220
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'Incoatec I\mS micro-focus tube'
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6236
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 3035 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.048(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9877
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0577P)^2^+4.3263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7922
_reflns_number_total             9877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502892r_si_002.cif
_cod_data_source_block           FDO02
_cod_depositor_comments
'Adding full bibliography for 4342642--4342646.cif.'
_cod_database_code               4342643
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.927
_shelxl_version_number           2014/6
_shelx_res_checksum              72930
_shelx_hkl_checksum              43144
_shelx_fab_checksum              52815