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_4038969
_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            'C38 H16 O18 S6 W3'
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_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                94.7090(10)
_cell_angle_beta                 99.6690(10)
_cell_angle_gamma                90.3600(10)
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_cell_length_a                   7.64250(10)
_cell_length_b                   9.4015(2)
_cell_length_c                   16.0890(3)
_cell_measurement_reflns_used    12673
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.1940
_cell_measurement_theta_min      2.7890
_cell_volume                     1135.50(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
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_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23090
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
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_diffrn_reflns_theta_min         2.796
_diffrn_source                   'Rotating-anode X-ray tube'
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_exptl_absorpt_correction_T_max  1.0000
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.431
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_refine_diff_density_max         2.685
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_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)'
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     297
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0846P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3867
_reflns_number_total             4461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1111115.cif
_cod_data_source_block           PCOD1111115
_cod_depositor_comments
;

2025-07-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         752.21
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C19 H8 O9 S3 W1.50'
_cod_database_code               4038969
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              8799
_shelx_hkl_checksum              82485