Synthesis and properties of mono- and dimetal Fischer multicarbene complexes derived from thiophene and thieno[2,3-b]thiophene.
Lamprecht, Zandria; van Jaarsveld, Nina A.; Bezuidenhout, Daniela I.; Liles, David C.; Lotz, Simon; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19218–19231; doi:10.1039/c5dt03555d

data_7036874
_publ_section_title
;
 Synthesis and properties of mono- and dimetal Fischer multicarbene
 complexes derived from thiophene and thieno[2,3-b]thiophene.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19218
_journal_page_last               19231
_journal_paper_doi               10.1039/c5dt03555d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H16 O12 S2 W2, 0.5(C1 H2 Cl2)'
_chemical_formula_sum            'C24.5 H17 Cl O12 S2 W2'
_chemical_formula_weight         970.65
_chemical_name_systematic
'2-(Ethoxy-(pentacarbonyl-tungsten)-carbene)-4,6-diethoxy-5,5,5,5-tetracarbonyl-5-tungsta-cyclopenta[b]thieno[3,2-d]thiophene hemidichloromethane'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic-phasing
_audit_creation_method           SHELXL-2014/5
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.7813(12)
_cell_length_b                   26.7813(12)
_cell_length_c                   17.3239(8)
_cell_measurement_reflns_used    9322
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.054
_cell_measurement_theta_min      2.567
_cell_volume                     12425.4(10)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae <i>et al</i>., 2008)
;
_computing_publication_material  'SHELXL-2014, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL, SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            270658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.240
_diffrn_reflns_theta_min         2.067
_exptl_absorpt_coefficient_mu    7.678
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7312
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         11904
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+19.9755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0446
_reflns_number_gt                10088
_reflns_number_total             11904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03555d1.cif
_cod_data_source_block           mo_ZL228F5_0m_a
_cod_depositor_comments
'Adding full bibliography for 7036872--7036876.cif.'
_cod_original_cell_volume        12425.4(13)
_cod_original_formula_sum        'C24.50 H17 Cl O12 S2 W2'
_cod_database_code               7036874
_shelx_estimated_absorpt_t_min   0.241
_shelx_estimated_absorpt_t_max   0.664
_shelxl_version_number           2014/5
_shelx_res_checksum              90597