#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:34:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179754 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/50/7005032.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_7005032
loop_
_publ_author_name
'Stander, Elzet'
'Cronje, Stephanie'
'Raubenheimer, Helgard G.'
_publ_section_title
;
 Preparing alpha,beta-unsaturated Fischer-type carbene complexes via an
 unforeseen route.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              424
_journal_page_last               429
_journal_paper_doi               10.1039/b615079a
_journal_year                    2007
_chemical_formula_moiety         'C11 H13 Cr N O5 S'
_chemical_formula_sum            'C11 H13 Cr N O5 S'
_chemical_formula_weight         323.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.563(1)
_cell_angle_beta                 85.909(1)
_cell_angle_gamma                81.968(1)
_cell_formula_units_Z            2
_cell_length_a                   6.8048(5)
_cell_length_b                   8.7412(6)
_cell_length_c                   12.1146(9)
_cell_measurement_reflns_used    4085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2265
_cell_measurement_theta_min      2.475
_cell_volume                     676.63(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
X-Seed (Barbour, 2001; Atwood and Barbour, 2003)
;
_computing_publication_material
;
X-Seed
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7516
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_correction_T_min  0.8880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            'Orange red'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0357P)²+0.4274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                2763
_reflns_number_total             3070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615079a.txt
_cod_data_source_block           Complex_3a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005032
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.57334(4) 0.36728(3) 0.72951(2) 0.01169(9) Uani 1 1 d . . .
S1 S 0.57698(6) 0.65789(5) 0.62049(4) 0.01370(11) Uani 1 1 d . . .
O1 O 0.30673(18) 0.50072(14) 0.91269(11) 0.0147(3) Uani 1 1 d . . .
O2 O 0.9094(2) 0.32629(18) 0.89098(13) 0.0265(3) Uani 1 1 d . . .
O3 O 0.5346(2) 0.02263(16) 0.86927(13) 0.0247(3) Uani 1 1 d . . .
O4 O 0.8192(2) 0.22043(18) 0.56090(13) 0.0235(3) Uani 1 1 d . . .
O5 O 0.1775(2) 0.37737(17) 0.62266(13) 0.0229(3) Uani 1 1 d . . .
N1 N 0.1797(2) 0.82517(18) 0.83124(14) 0.0159(3) Uani 1 1 d . . .
H1 H 0.1753 0.7338 0.8886 0.019 Uiso 1 1 calc R . .
C1 C 0.4138(2) 0.5153(2) 0.81338(15) 0.0127(3) Uani 1 1 d . . .
C2 C 0.4136(3) 0.6753(2) 0.73811(15) 0.0134(3) Uani 1 1 d . . .
C3 C 0.2979(3) 0.8207(2) 0.74019(16) 0.0137(3) Uani 1 1 d . . .
C4 C 0.0561(3) 0.9698(2) 0.84390(18) 0.0230(4) Uani 1 1 d . . .
H4A H 0.1411 1.0507 0.8457 0.035 Uiso 1 1 calc R . .
H4B H -0.0233 0.9402 0.9166 0.035 Uiso 1 1 calc R . .
H4C H -0.0324 1.0156 0.7780 0.035 Uiso 1 1 calc R . .
C5 C 0.3031(3) 0.9724(2) 0.63915(17) 0.0191(4) Uani 1 1 d . . .
H5A H 0.1682 1.0291 0.6244 0.029 Uiso 1 1 calc R . .
H5B H 0.3572 0.9442 0.5699 0.029 Uiso 1 1 calc R . .
H5C H 0.3873 1.0433 0.6569 0.029 Uiso 1 1 calc R . .
C6 C 0.3131(3) 0.3391(2) 0.99528(16) 0.0175(4) Uani 1 1 d . . .
H6A H 0.2745 0.2647 0.9571 0.026 Uiso 1 1 calc R . .
H6B H 0.2209 0.3413 1.0609 0.026 Uiso 1 1 calc R . .
H6C H 0.4481 0.3017 1.0239 0.026 Uiso 1 1 calc R . .
C7 C 0.8015(3) 0.7255(2) 0.65157(18) 0.0201(4) Uani 1 1 d . . .
H7A H 0.7798 0.8433 0.6373 0.030 Uiso 1 1 calc R . .
H7B H 0.9110 0.6990 0.6010 0.030 Uiso 1 1 calc R . .
H7C H 0.8348 0.6707 0.7332 0.030 Uiso 1 1 calc R . .
C8 C 0.7878(3) 0.3476(2) 0.82420(17) 0.0171(4) Uani 1 1 d . . .
C9 C 0.5445(3) 0.1591(2) 0.81789(16) 0.0161(4) Uani 1 1 d . . .
C10 C 0.7267(3) 0.2822(2) 0.62209(16) 0.0159(4) Uani 1 1 d . . .
C11 C 0.3289(3) 0.3760(2) 0.65854(16) 0.0149(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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C9 Cr1 C8 85.56(8) . . ?
C9 Cr1 C10 88.25(8) . . ?
C8 Cr1 C10 94.35(8) . . ?
C9 Cr1 C11 88.45(8) . . ?
C8 Cr1 C11 169.85(8) . . ?
C10 Cr1 C11 93.64(8) . . ?
C9 Cr1 C1 106.47(8) . . ?
C8 Cr1 C1 88.82(7) . . ?
C10 Cr1 C1 165.15(7) . . ?
C11 Cr1 C1 85.03(7) . . ?
C9 Cr1 S1 173.55(6) . . ?
C8 Cr1 S1 96.71(6) . . ?
C10 Cr1 S1 97.57(6) . . ?
C11 Cr1 S1 88.41(5) . . ?
C1 Cr1 S1 67.63(5) . . ?
C2 S1 C7 102.93(9) . . ?
C2 S1 Cr1 80.43(6) . . ?
C7 S1 Cr1 109.54(7) . . ?
C1 O1 C6 116.61(14) . . ?
C3 N1 C4 125.18(16) . . ?
C3 N1 H1 117.4 . . ?
C4 N1 H1 117.4 . . ?
O1 C1 C2 115.10(15) . . ?
O1 C1 Cr1 138.22(13) . . ?
C2 C1 Cr1 106.56(12) . . ?
C3 C2 C1 131.01(17) . . ?
C3 C2 S1 123.65(14) . . ?
C1 C2 S1 104.93(12) . . ?
N1 C3 C2 120.45(16) . . ?
N1 C3 C5 118.79(16) . . ?
C2 C3 C5 120.75(16) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S1 C7 H7A 109.5 . . ?
S1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
S1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 Cr1 173.46(18) . . ?
O3 C9 Cr1 175.52(17) . . ?
O4 C10 Cr1 175.68(16) . . ?
O5 C11 Cr1 175.82(17) . . ?
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 C9 1.8261(19) . ?
Cr1 C8 1.8760(19) . ?
Cr1 C10 1.8806(19) . ?
Cr1 C11 1.9074(19) . ?
Cr1 C1 2.0414(18) . ?
Cr1 S1 2.4676(5) . ?
S1 C2 1.7759(18) . ?
S1 C7 1.8170(19) . ?
O1 C1 1.341(2) . ?
O1 C6 1.447(2) . ?
O2 C8 1.154(2) . ?
O3 C9 1.167(2) . ?
O4 C10 1.153(2) . ?
O5 C11 1.144(2) . ?
N1 C3 1.325(2) . ?
N1 C4 1.462(2) . ?
N1 H1 0.8800 . ?
C1 C2 1.407(2) . ?
C2 C3 1.405(2) . ?
C3 C5 1.496(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.88 2.05 2.7259(19) 133.2 .
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
C2 C1 Cr1 S1 4.97(10) . . . . ?
