Synthesis, crystal structure and reactivity of η<sup>2</sup>-thiophyne Ni complexes.
Terada, Misaki; Nishii, Yuji; Miura, Masahiro; Chemical communications (Cambridge, England) 54 (2018) 2918–2921; doi:10.1039/c8cc00705e

data_7121314
_publ_section_title
;
 Synthesis, crystal structure and reactivity of \h<sup>2</sup>-thiophyne
 Ni complexes.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2918
_journal_page_last               2921
_journal_paper_doi               10.1039/c8cc00705e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C35 H55 I Ni P2 S'
_chemical_formula_sum            'C35 H55 I Ni P2 S'
_chemical_formula_weight         755.40
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1nq2hy
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                75.82(2)
_cell_angle_beta                 88.78(3)
_cell_angle_gamma                78.187(16)
_cell_formula_units_Z            4
_cell_length_a                   12.354(9)
_cell_length_b                   16.268(11)
_cell_length_c                   20.938(14)
_cell_measurement_reflns_used    5262
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      3.00
_cell_volume                     3992(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1535
_diffrn_reflns_av_unetI/netI     0.2173
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35079
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.0882
_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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.2153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6623
_reflns_number_total             14039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00705e2.cif
_cod_data_source_block           shelxl_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7121308--7121314.cif.'
_cod_database_code               7121314
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.872
_shelxl_version_number           2013-4
_shelx_res_checksum              60451
_shelx_fab_checksum              80541