#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/12/7021205.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_7021205
loop_
_publ_author_name
'van der Westhuizen, Belinda'
'Swarts, Pieter J'
'Strydom, Ian'
'Liles, David C'
'Fernández, Israel'
'Swarts, Jannie C'
'Bezuidenhout, Daniela I'
_publ_section_title
;
 Electrochemical illumination of thienyl and ferrocenyl chromium(0)
 Fischer carbene complexes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5367
_journal_page_last               5378
_journal_paper_doi               10.1039/c3dt32913e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C12 H8 Cr1 O6 S1'
_chemical_formula_sum            'C12 H8 Cr O6 S'
_chemical_formula_weight         332.25
_chemical_name_systematic
;
Pentacarbonyl(ethoxy-thiophenyl-methylidene)chromium
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.737(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5803(6)
_cell_length_b                   7.6532(5)
_cell_length_c                   9.6551(6)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.046
_cell_measurement_theta_min      2.790
_cell_volume                     699.70(8)
_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 et al., 2008)
;
_computing_publication_material
'SHELXL-97, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20399
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal-prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0878P)²+3.5878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2371
_reflns_number_gt                1330
_reflns_number_total             1497
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt32913e.txt
_cod_data_source_block           mo_bvdwcrthoet_0m
_cod_depositor_comments          'Adding full bibliography for 7021205.cif.'
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C12 H8 Cr1 O6 S1'
_cod_database_code               7021205
#BEGIN Tags that were not found in dictionaries:
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cr1 Cr 0.28935(14) 0.2500 0.29276(14) 0.0370(5) Uani 1 2 d S 1
C1 C 0.4424(9) 0.2500 0.4455(10) 0.049(2) Uani 1 2 d S 1
O1 O 0.5269(9) 0.2500 0.5290(9) 0.091(3) Uani 1 2 d S 1
C2 C 0.2046(7) 0.4261(9) 0.3884(7) 0.0495(15) Uani 1 1 d . 1
O2 O 0.1625(6) 0.5345(8) 0.4540(7) 0.0800(18) Uani 1 1 d . 1
C3 C 0.3841(7) 0.4298(9) 0.2069(6) 0.0492(15) Uani 1 1 d . 1
O3 O 0.4458(7) 0.5359(8) 0.1619(7) 0.0846(19) Uani 1 1 d . 1
C4 C 0.1217(9) 0.2500 0.1287(9) 0.0425(19) Uani 1 2 d S 1
O4 O -0.0169(7) 0.2500 0.1321(7) 0.0545(17) Uani 1 2 d S 1
S1 S -0.0085(4) 0.2500 -0.1454(4) 0.0434(14) Uani 0.526(8) 2 d SP 1
C5 C 0.1360(8) 0.2500 -0.0163(8) 0.0326(16) Uani 1 2 d S 1
C6 C 0.2616(10) 0.2500 -0.0784(9) 0.049(2) Uani 1 2 d S 1
H6 H 0.3528 0.2500 -0.0290 0.059 Uiso 1 2 calc SR 1
C7 C 0.2268(15) 0.2500 -0.2277(11) 0.068(3) Uani 1 2 d S 1
H7 H 0.2945 0.2500 -0.2872 0.082 Uiso 1 2 calc SR 1
C8 C 0.0973(19) 0.2500 -0.2708(16) 0.046(4) Uani 0.526(8) 2 d SP 1
H8 H 0.0612 0.2500 -0.3658 0.055 Uiso 1 2 calc SR 1
C9 C -0.0790(10) 0.2500 0.2561(11) 0.052(2) Uani 1 2 d S 1
H9A H -0.0498 0.3529 0.3117 0.063 Uiso 0.50 1 calc PR 1
H9B H -0.0498 0.1471 0.3117 0.063 Uiso 0.50 1 calc PR 1
C10 C -0.2358(11) 0.2500 0.2136(15) 0.068(3) Uani 1 2 d S 1
H10A H -0.2809 0.2500 0.2958 0.102 Uiso 1 2 calc SR 1
H10B H -0.2635 0.1476 0.1589 0.102 Uiso 0.50 1 calc PR 1
H10C H -0.2635 0.3524 0.1589 0.102 Uiso 0.50 1 calc PR 1
S1A S -0.1462(7) 0.2500 -0.0095(8) 0.078(2) Uani 0.474(8) 2 d SP 2
C8A C -0.275(3) 0.2500 0.090(3) 0.084(9) Uani 0.474(8) 2 d SP 2
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'
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'
Cr Cr 0.3209 0.6236 '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
C2 Cr1 C2 91.2(4) 4_565 .
C2 Cr1 C3 176.2(3) 4_565 .
C2 Cr1 C3 88.1(3) . .
C2 Cr1 C3 88.1(3) 4_565 4_565
C2 Cr1 C3 176.2(3) . 4_565
C3 Cr1 C3 92.4(4) . 4_565
C2 Cr1 C1 87.7(3) 4_565 .
C2 Cr1 C1 87.7(3) . .
C3 Cr1 C1 88.6(3) . .
C3 Cr1 C1 88.6(3) 4_565 .
C2 Cr1 C4 91.9(3) 4_565 .
C2 Cr1 C4 91.9(3) . .
C3 Cr1 C4 91.9(3) . .
C3 Cr1 C4 91.9(3) 4_565 .
C1 Cr1 C4 179.3(4) . .
O1 C1 Cr1 179.7(10) . .
O2 C2 Cr1 174.7(6) . .
O3 C3 Cr1 176.4(7) . .
O4 C4 C5 105.6(7) . .
O4 C4 Cr1 129.7(6) . .
C5 C4 Cr1 124.7(6) . .
C4 O4 C9 124.7(8) . .
C8 S1 C5 90.8(7) . .
C4 C5 C6 128.8(8) . .
C4 C5 S1 121.7(6) . .
C6 C5 S1 109.5(6) . .
C7 C6 C5 110.0(9) . .
C7 C6 H6 125.0 . .
C5 C6 H6 125.0 . .
C8 C7 C6 113.8(11) . .
C8 C7 H7 123.1 . .
C6 C7 H7 123.1 . .
C7 C8 S1 115.8(12) . .
C7 C8 H8 122.1 . .
S1 C8 H8 122.1 . .
O4 C9 C10 107.6(9) . .
O4 C9 H9A 110.2 . .
C10 C9 H9A 110.2 . .
O4 C9 H9B 110.2 . .
C10 C9 H9B 110.2 . .
H9A C9 H9B 108.5 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C2 1.886(7) 4_565
Cr1 C2 1.886(7) .
Cr1 C3 1.907(7) .
Cr1 C3 1.907(7) 4_565
Cr1 C1 1.915(9) .
Cr1 C4 2.077(9) .
C1 O1 1.052(11) .
C2 O2 1.153(8) .
C3 O3 1.129(8) .
C4 O4 1.333(11) .
C4 C5 1.428(11) .
O4 C9 1.415(11) .
S1 C8 1.693(16) .
S1 C5 1.716(8) .
C5 C6 1.423(12) .
C6 C7 1.429(14) .
C6 H6 0.9300 .
C7 C8 1.25(2) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 C10 1.495(14) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
S1A C8A 1.68(4) .
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
C2 Cr1 C4 O4 45.6(2) 4_565
C2 Cr1 C4 O4 -45.6(2) .
C3 Cr1 C4 O4 -133.8(2) .
C3 Cr1 C4 O4 133.8(2) 4_565
C2 Cr1 C4 C5 -134.4(2) 4_565
C2 Cr1 C4 C5 134.4(2) .
C3 Cr1 C4 C5 46.2(2) .
C3 Cr1 C4 C5 -46.2(2) 4_565
C5 C4 O4 C9 180.0 .
O4 C4 C5 C6 180.0 .
Cr1 C4 C5 C6 0.0 .
O4 C4 C5 S1 0.0 .
Cr1 C4 C5 S1 180.0 .
C8 S1 C5 C4 180.0 .
C8 S1 C5 C6 0.0 .
C4 C5 C6 C7 180.0 .
S1 C5 C6 C7 0.0 .
C5 C6 C7 C8 0.0 .
C6 C7 C8 S1 0.0 .
C5 S1 C8 C7 0.00 .
C4 O4 C9 C10 180.0 .
