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#$Date: 2021-01-05 09:41:00 +0200 (Tue, 05 Jan 2021) $
#$Revision: 260524 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/62/7706299.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7706299
loop_
_publ_author_name
'Lamprecht, Zandria'
'Malan, Frederick P.'
'Fernández, Israel'
'Lotz, Simon'
'Bezuidenhout, Daniela I.'
_publ_section_title
;
 Chelated Fischer carbene complexes of annulated thiophenes: synthesis,
 structure and electrochemistry.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15339
_journal_page_last               15354
_journal_paper_doi               10.1039/d0dt03298k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C26 H20 Cr2 O12 S2'
_chemical_formula_weight         692.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-12 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                92.975(3)
_cell_angle_beta                 96.209(3)
_cell_angle_gamma                103.001(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1185(6)
_cell_length_b                   9.6691(8)
_cell_length_c                   10.7876(9)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.17
_cell_volume                     717.00(10)
_computing_cell_refinement       'SAINT-2016/2 (Bruker AXS, 2016)'
_computing_data_collection       'APEX III (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT-2016/2 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'Bruker SHELXTL'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23044
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.168
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.9001.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       blade
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0278
_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/[σ²(Fo²)+(0.0287P)²+0.2152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2243
_reflns_number_total             2926
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03298k2.cif
_cod_data_source_block           mo_ZL315F3_0m_a
_cod_database_code               7706299
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.946
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.20896(5) 0.28576(3) 0.23832(3) 0.01558(10) Uani 1 1 d . . . . .
S1 S 0.36488(7) 0.00112(5) 0.66330(5) 0.01751(13) Uani 1 1 d . . . . .
O1 O 0.5125(2) 0.54745(17) 0.35870(17) 0.0455(5) Uani 1 1 d . . . . .
O2 O -0.1412(2) 0.41167(15) 0.26027(15) 0.0276(4) Uani 1 1 d . . . . .
O3 O 0.1763(2) 0.41807(17) -0.00946(15) 0.0335(4) Uani 1 1 d . . . . .
O4 O -0.0455(2) -0.00357(15) 0.13440(14) 0.0294(4) Uani 1 1 d . . . . .
O5 O 0.53679(19) 0.16828(14) 0.12484(13) 0.0187(3) Uani 1 1 d . . . . .
O6 O 0.14756(19) 0.20179(13) 0.51180(12) 0.0179(3) Uani 1 1 d . . . . .
C1 C 0.3991(3) 0.4510(2) 0.3138(2) 0.0249(5) Uani 1 1 d . . . . .
C2 C -0.0079(3) 0.3639(2) 0.25832(19) 0.0195(5) Uani 1 1 d . . . . .
C3 C 0.1948(3) 0.3651(2) 0.0823(2) 0.0213(5) Uani 1 1 d . . . . .
C4 C 0.0449(3) 0.1056(2) 0.17225(18) 0.0183(5) Uani 1 1 d . . . . .
C5 C 0.6792(3) 0.2144(2) -0.0624(2) 0.0263(5) Uani 1 1 d . . . . .
H5A H 0.663885 0.111666 -0.079357 0.039 Uiso 1 1 calc R U . . .
H5B H 0.806013 0.255258 -0.013944 0.039 Uiso 1 1 calc R U . . .
H5C H 0.670844 0.259067 -0.141705 0.039 Uiso 1 1 calc R U . . .
C6 C 0.5217(3) 0.2407(2) 0.01048(19) 0.0212(5) Uani 1 1 d . . . . .
H6A H 0.538038 0.344150 0.030631 0.025 Uiso 1 1 calc R U . . .
H6B H 0.392886 0.202927 -0.038707 0.025 Uiso 1 1 calc R U . . .
C7 C 0.4279(3) 0.1869(2) 0.21352(18) 0.0161(4) Uani 1 1 d . . . . .
C8 C 0.4712(3) 0.1073(2) 0.31790(19) 0.0167(4) Uani 1 1 d . . . . .
C9 C 0.3708(3) 0.1162(2) 0.41959(18) 0.0160(4) Uani 1 1 d . . . . .
C10 C 0.2289(3) 0.2028(2) 0.40696(18) 0.0163(4) Uani 1 1 d . . . . .
C11 C 0.0069(3) 0.2867(2) 0.52957(19) 0.0202(5) Uani 1 1 d . . . . .
H11A H -0.105318 0.258747 0.463398 0.024 Uiso 1 1 calc R U . . .
H11B H 0.066940 0.389047 0.526011 0.024 Uiso 1 1 calc R U . . .
C12 C -0.0579(3) 0.2596(2) 0.6558(2) 0.0280(5) Uani 1 1 d . . . . .
H12A H -0.156474 0.312849 0.670256 0.042 Uiso 1 1 calc R U . . .
H12B H 0.053759 0.290624 0.720516 0.042 Uiso 1 1 calc R U . . .
H12C H -0.113148 0.157595 0.658870 0.042 Uiso 1 1 calc R U . . .
C13 C 0.4295(3) 0.0346(2) 0.51565(18) 0.0158(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Cr1 C2 83.02(9) . . ?
C3 Cr1 C4 93.18(8) . . ?
C2 Cr1 C4 91.86(8) . . ?
C3 Cr1 C1 91.82(9) . . ?
C2 Cr1 C1 95.15(9) . . ?
C4 Cr1 C1 171.83(9) . . ?
C3 Cr1 C10 178.98(8) . . ?
C2 Cr1 C10 97.43(8) . . ?
C4 Cr1 C10 87.72(8) . . ?
C1 Cr1 C10 87.23(9) . . ?
C3 Cr1 C7 97.82(9) . . ?
C2 Cr1 C7 175.59(8) . . ?
C4 Cr1 C7 83.78(8) . . ?
C1 Cr1 C7 89.15(8) . . ?
C10 Cr1 C7 81.80(8) . . ?
C13 S1 C8 90.03(10) . 2_656 ?
C7 O5 C6 119.88(16) . . ?
C10 O6 C11 120.60(15) . . ?
O1 C1 Cr1 179.2(2) . . ?
O2 C2 Cr1 174.53(18) . . ?
O3 C3 Cr1 175.0(2) . . ?
O4 C4 Cr1 177.04(19) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O5 C6 C5 107.13(18) . . ?
O5 C6 H6A 110.3 . . ?
C5 C6 H6A 110.3 . . ?
O5 C6 H6B 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?
O5 C7 C8 109.70(18) . . ?
O5 C7 Cr1 137.83(15) . . ?
C8 C7 Cr1 112.34(14) . . ?
C9 C8 C7 117.13(19) . . ?
C9 C8 S1 113.47(16) . 2_656 ?
C7 C8 S1 129.40(16) . 2_656 ?
C8 C9 C13 111.13(18) . . ?
C8 C9 C10 115.45(18) . . ?
C13 C9 C10 133.41(18) . . ?
O6 C10 C9 108.04(16) . . ?
O6 C10 Cr1 138.84(15) . . ?
C9 C10 Cr1 113.11(14) . . ?
O6 C11 C12 106.92(17) . . ?
O6 C11 H11A 110.3 . . ?
C12 C11 H11A 110.3 . . ?
O6 C11 H11B 110.3 . . ?
C12 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C13 C9 112.8(2) 2_656 . ?
C13 C13 S1 112.5(2) 2_656 . ?
C9 C13 S1 134.64(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 C3 1.888(2) . ?
Cr1 C2 1.892(2) . ?
Cr1 C4 1.919(2) . ?
Cr1 C1 1.924(2) . ?
Cr1 C10 2.030(2) . ?
Cr1 C7 2.037(2) . ?
S1 C13 1.732(2) . ?
S1 C8 1.738(2) 2_656 ?
O1 C1 1.134(2) . ?
O2 C2 1.147(2) . ?
O3 C3 1.146(3) . ?
O4 C4 1.135(2) . ?
O5 C7 1.324(2) . ?
O5 C6 1.456(2) . ?
O6 C10 1.325(2) . ?
O6 C11 1.452(2) . ?
C5 C6 1.496(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.441(3) . ?
C8 C9 1.382(3) . ?
C9 C13 1.418(3) . ?
C9 C10 1.451(3) . ?
C11 C12 1.501(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C13 1.386(4) 2_656 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 O5 C6 C5 172.62(16) . . . . ?
C6 O5 C7 C8 -178.76(15) . . . . ?
C6 O5 C7 Cr1 5.7(3) . . . . ?
O5 C7 C8 C9 179.41(15) . . . . ?
Cr1 C7 C8 C9 -3.9(2) . . . . ?
O5 C7 C8 S1 -0.5(2) . . . 2_656 ?
Cr1 C7 C8 S1 176.25(11) . . . 2_656 ?
C7 C8 C9 C13 -179.23(16) . . . . ?
S1 C8 C9 C13 0.7(2) 2_656 . . . ?
C7 C8 C9 C10 1.5(3) . . . . ?
S1 C8 C9 C10 -178.56(13) 2_656 . . . ?
C11 O6 C10 C9 176.33(15) . . . . ?
C11 O6 C10 Cr1 -4.9(3) . . . . ?
C8 C9 C10 O6 -179.32(15) . . . . ?
C13 C9 C10 O6 1.7(3) . . . . ?
C8 C9 C10 Cr1 1.6(2) . . . . ?
C13 C9 C10 Cr1 -177.46(17) . . . . ?
C10 O6 C11 C12 179.15(16) . . . . ?
C8 C9 C13 C13 -0.5(3) . . . 2_656 ?
C10 C9 C13 C13 178.5(2) . . . 2_656 ?
C8 C9 C13 S1 179.66(16) . . . . ?
C10 C9 C13 S1 -1.3(4) . . . . ?
C8 S1 C13 C13 -0.2(2) 2_656 . . 2_656 ?
C8 S1 C13 C9 179.6(2) 2_656 . . . ?
