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_4038971
_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_moiety         'C24 H14 N2 O10 S3 W2'
_chemical_formula_sum            'C24 H14 N2 O10 S3 W2'
_chemical_formula_weight         954.25
_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'
_atom_sites_solution_hydrogens   geom
_audit_contact_author_name
;
;
_audit_creation_date             2019-09-27
_cell_angle_alpha                90
_cell_angle_beta                 95.543(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5741(5)
_cell_length_b                   15.1714(10)
_cell_length_c                   32.440(2)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.76
_cell_measurement_theta_min      2.74
_cell_volume                     3220.4(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1304
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            130982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.118
_diffrn_reflns_theta_min         2.737
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.285
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1713 before and 0.0986 after correction.
The Ratio of minimum to maximum transmission is 0.6068.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_description       rod
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.081
_refine_diff_density_max         2.559
_refine_diff_density_min         -3.790
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0771P)^2^+38.7125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.2062
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4414
_reflns_number_total             6328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1111117.cif
_cod_data_source_block           7
_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_database_code               4038971
_shelxl_version_number           2013-3
_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C9 = C16-C17
 1.51 with sigma of 0.01
 C9-C10 = C15-C16
 1.34 with sigma of 0.01
 C10-C11 = C14-C15
 1.44 with sigma of 0.01
 C11-C12 = C13-C14
 1.39 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;