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_7706301
_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            'C30.85 H22.85 Cr2 O12 S3'
_chemical_formula_weight         785.75
_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                101.964(4)
_cell_angle_beta                 99.888(4)
_cell_angle_gamma                103.629(4)
_cell_formula_units_Z            4
_cell_length_a                   10.7421(13)
_cell_length_b                   16.0557(18)
_cell_length_c                   21.988(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.25
_cell_volume                     3507.1(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-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108937
_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         2.246
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1320 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.8793.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.244
_refine_diff_density_max         1.557
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         14354
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0422P)^2^+22.9566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10935
_reflns_number_total             14354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03298k2.cif
_cod_data_source_block           mo_ZL334F4_0m_a
_cod_original_cell_volume        3507.1(7)
_cod_database_code               7706301
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              68511