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_7036873
_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
'0.38(C22 H12 Cr2 O12 S2), 0.62(C22 H12 Cr O12 S2 W)'
_chemical_formula_sum            'C22 H12 Cr1.38 O12 S2 W0.62'
_chemical_formula_weight         717.85
_chemical_name_systematic
'Thienyl[2,3-b]thiophenene-2,5-di[(ethoxycarbene)pentacarbonylchromium(0)], Thienyl[2,3-b]thiophenene-2-[(ethoxycarbene)pentacarbonylchromium(0)]-5-[(ethoxycarbene)pentacarbonyltungsten(0)] co-crystal'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic-phasing
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3950(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0556(8)
_cell_length_b                   14.5145(10)
_cell_length_c                   13.8325(9)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.357
_cell_measurement_theta_min      2.485
_cell_volume                     2609.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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  Bruker
_computing_structure_solution    'Bruker SHELXTS (Sheldrick, 2014)'
_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 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Focusing Montel optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            98242
_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         28.363
_diffrn_reflns_theta_min         2.485
_diffrn_source                   ' I\mS  micro focus'
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+4.0832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                5789
_reflns_number_total             6523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03555d1.cif
_cod_data_source_block           mo_ZL220F22_0m_a
_cod_depositor_comments
'Adding full bibliography for 7036872--7036876.cif.'
_cod_database_code               7036873
_shelxl_version_number           2013-4
_shelx_res_checksum              73229