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_7121308
_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_sum            'C30 H50 Ni P2 S'
_chemical_formula_weight         563.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1nb1mn
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-01-23 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(11)
_cell_angle_beta                 92.402(10)
_cell_angle_gamma                90.000(8)
_cell_formula_units_Z            4
_cell_length_a                   9.9110(16)
_cell_length_b                   16.711(3)
_cell_length_c                   18.048(2)
_cell_measurement_reflns_used    3005
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      3.20
_cell_volume                     2986.5(8)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.998
_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  0.2229
_diffrn_reflns_av_unetI/netI     0.1653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25694
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.190
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5244
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1856
_refine_ls_R_factor_gt           0.0950
_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^)+(0.0476P)^2^+8.5137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2728
_reflns_number_total             5244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00705e2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '__diffrn_measurement_method' replaced with
'_diffrn_measurement_method'.

Automatic conversion script
Id: cif_correct_tags 4968 2017-02-21 14:55:21Z antanas 

 Adding full bibliography for 7121308--7121314.cif.
;
_cod_original_cell_volume        2986.6(8)
_cod_database_code               7121308
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              3895