Chelated Fischer carbene complexes of annulated thiophenes: synthesis, structure and electrochemistry.
Lamprecht, Zandria; Malan, Frederick P.; Fernández, Israel; Lotz, Simon; Bezuidenhout, Daniela I.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15339–15354; doi:10.1039/d0dt03298k

data_7706298
_publ_section_title
;
 Chelated Fischer carbene complexes of annulated thiophenes: synthesis,
 structure and electrochemistry.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15339
_journal_page_last               15354
_journal_paper_doi               10.1039/d0dt03298k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C16 H12 Cr O6 S2'
_chemical_formula_weight         416.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-12 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                74.238(2)
_cell_angle_beta                 75.469(2)
_cell_angle_gamma                71.410(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4276(4)
_cell_length_b                   10.7016(6)
_cell_length_c                   12.2391(6)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.41
_cell_volume                     872.91(8)
_computing_cell_refinement       'SAINT-2016/2 (Bruker AXS, 2016)'
_computing_data_collection       'APEX III (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT-2016/2 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0809 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.9101.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.273
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0272P)^2^+0.4756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3149
_reflns_number_total             3567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03298k2.cif
_cod_data_source_block           mo_ZL315F2_0m_a
_cod_database_code               7706298
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              96955