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_7037112
_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         'C14 H8 O6 S2 W'
_chemical_formula_sum            'C14 H8 O6 S2 W'
_chemical_formula_weight         520.17
_chemical_name_systematic
;
 Pentacarbonyl-(ethoxy-thieno[2,3-b]thiophen-2-yl-methylidene)-tungsten
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic-phasing
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3613(7)
_cell_length_b                   26.0082(11)
_cell_length_c                   7.5595(3)
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.557
_cell_measurement_theta_min      2.489
_cell_volume                     3216.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae <i>et al</i>., 2008)
;
_computing_publication_material  'SHELXL-2013, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL, SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_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_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0076
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            128826
_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         27.482
_diffrn_reflns_theta_min         2.490
_exptl_absorpt_coefficient_mu    7.467
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane, DCM'
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.351
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3678
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.348
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+4.6338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                3594
_reflns_number_total             3678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03555d1.cif
_cod_data_source_block           mo_ZL215F1_0ma_a
_cod_database_code               7037112
_shelxl_version_number           2013-4
_shelx_res_checksum              69540
_shelx_hkl_checksum              11361