Mono-, di- and tetrarhenium Fischer carbene complexes with thienothiophene substituents
Lamprecht, Zandria; Radhakrishnan, Shankara; Hildebrandt, Alexander; Lang, Heinrich; Liles, David Charles; Weststrate, Nora-ann; Lotz, Simon; Bezuidenhout, Daniela Ina; Dalton Trans.  (2017) –; doi:10.1039/C7DT02969A

data_7044239
_publ_section_title
;
 Mono-, di- and tetrarhenium Fischer carbene complexes with
 thienothiophene substituents
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02969A
_journal_year                    2017
_chemical_formula_moiety         'C13 H8 Br O5 Re S2'
_chemical_formula_sum            'C13 H8 Br O5 Re S2'
_chemical_formula_weight         574.42
_chemical_name_systematic
Bromo-(ethoxy-(thieno[3,2-b]thiophen-2-yl)-carbene)-tetracarbonyl-rhenium
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic-phasing
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3951(4)
_cell_length_b                   14.2116(10)
_cell_length_c                   15.5998(11)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.272
_cell_measurement_theta_min      2.612
_cell_volume                     1639.48(19)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'APEX2 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_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 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            78470
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_min         2.611
_diffrn_source                   ' I\mS  micro focus'
_exptl_absorpt_coefficient_mu    10.121
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.984
_refine_diff_density_min         -2.154
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.406(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0220P)^2^+4.5301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3946
_reflns_number_total             4087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02969a2.cif
_cod_data_source_block           mo_Zl303F3_0m
_cod_database_code               7044239
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.114
_shelx_estimated_absorpt_t_max   0.214
_shelx_res_checksum              17350