Synthesis and structure of annulated dithieno[2,3-b;3ʹ,2ʹ-d]thienyl- and ring-opened 3,3ʹ-bithienyl Fischer carbene complexes
Lamprecht, Zandria; Malan, Frederick P.; Liles, David C.; Lotz, Simon; Bezuidenhout, Daniela I.; Journal of Organometallic Chemistry 925 (2020) 121466–; doi:10.1016/j.jorganchem.2020.121466

data_4038965
_publ_section_title
;
 Synthesis and structure of annulated
 dithieno[2,3-b;3&#x02B9;,2&#x02B9;-d]thienyl- and ring-opened
 3,3&#x02B9;-bithienyl Fischer carbene complexes
;
_journal_name_full               'Journal of Organometallic Chemistry'
_journal_page_first              121466
_journal_paper_doi               10.1016/j.jorganchem.2020.121466
_journal_volume                  925
_journal_year                    2020
_chemical_formula_sum            'C20 H18 Cr O6 S3'
_chemical_formula_weight         502.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 114.7700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   52.4504(19)
_cell_length_b                   7.4685(3)
_cell_length_c                   25.3205(9)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.800
_cell_measurement_theta_min      2.266
_cell_volume                     9006.1(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            126740
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.267
_diffrn_source                   'I\ms micro focus'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       blade
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         7672
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+15.8847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6651
_reflns_number_total             7672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1111111.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4038965
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.914