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_7121311
_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            'C41 H66 B Br Cl2 Ni O2 P2 S'
_chemical_formula_weight         905.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2016-12-20 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.722(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.717(6)
_cell_length_b                   11.746(2)
_cell_length_c                   16.282(4)
_cell_measurement_reflns_used    2943
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      3.2
_cell_volume                     4366.1(17)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1486
_diffrn_reflns_av_unetI/netI     0.1413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50507
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         3.186
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.466
_refine_diff_density_min         -1.790
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         9974
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0307P)^2^+26.4541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5470
_reflns_number_total             9974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00705e2.cif
_cod_data_source_block           shelxl_CCDC3
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121308--7121314.cif.
;
_cod_database_code               7121311
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.754
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              548