#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:34:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179754 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/50/7005031.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_7005031
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 H11 N O6 W'
_chemical_formula_sum            'C11 H11 N O6 W'
_chemical_formula_weight         437.06
_chemical_name_common            'Complex 2b'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.036(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5753(5)
_cell_length_b                   6.8567(3)
_cell_length_c                   18.7407(9)
_cell_measurement_reflns_used    5358
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.2026
_cell_measurement_theta_min      2.8309
_cell_volume                     1357.01(11)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8020
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.533
_exptl_absorpt_correction_T_max  0.4245
_exptl_absorpt_correction_T_min  0.3762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0166P)²+1.6326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0402
_reflns_number_gt                2917
_reflns_number_total             3119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615079a.txt
_cod_data_source_block           Complex_2b
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7005031
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
W1 W 0.795441(9) 0.580278(15) 0.087830(5) 0.01115(4) Uani 1 1 d . . .
O1 O 0.8106(2) 0.6599(3) 0.26075(10) 0.0191(4) Uani 1 1 d . . .
O2 O 0.9307(2) 0.1637(3) 0.08627(14) 0.0309(5) Uani 1 1 d . . .
O3 O 0.7941(2) 0.6469(3) -0.07911(11) 0.0235(5) Uani 1 1 d . . .
O4 O 1.0701(2) 0.7713(3) 0.09412(12) 0.0277(5) Uani 1 1 d . . .
O5 O 0.6571(2) 0.9862(3) 0.10704(12) 0.0239(5) Uani 1 1 d . . .
O6 O 0.52890(19) 0.3676(3) 0.06195(11) 0.0199(4) Uani 1 1 d . . .
N1 N 0.6880(2) 0.4522(4) 0.35470(12) 0.0183(5) Uani 1 1 d . . .
H1 H 0.7266 0.5633 0.3468 0.022 Uiso 1 1 calc R . .
C1 C 0.7757(3) 0.5369(4) 0.20601(15) 0.0145(5) Uani 1 1 d . . .
C2 C 0.7090(3) 0.3764(4) 0.23028(14) 0.0157(6) Uani 1 1 d . . .
H2 H 0.6876 0.2805 0.1951 0.019 Uiso 1 1 calc R . .
C3 C 0.6683(3) 0.3350(4) 0.29945(15) 0.0153(5) Uani 1 1 d . . .
C4 C 0.6524(3) 0.4158(5) 0.42757(16) 0.0234(7) Uani 1 1 d . . .
H4A H 0.6013 0.2966 0.4287 0.035 Uiso 1 1 calc R . .
H4B H 0.6029 0.5262 0.4441 0.035 Uiso 1 1 calc R . .
H4C H 0.7289 0.4000 0.4589 0.035 Uiso 1 1 calc R . .
C5 C 0.5954(3) 0.1506(5) 0.30939(17) 0.0252(7) Uani 1 1 d . . .
H5A H 0.6388 0.0712 0.3467 0.038 Uiso 1 1 calc R . .
H5B H 0.5899 0.0774 0.2644 0.038 Uiso 1 1 calc R . .
H5C H 0.5100 0.1824 0.3236 0.038 Uiso 1 1 calc R . .
C6 C 0.8918(3) 0.8241(5) 0.24950(15) 0.0236(7) Uani 1 1 d . . .
H6A H 0.9759 0.7775 0.2379 0.035 Uiso 1 1 calc R . .
H6B H 0.8991 0.9034 0.2930 0.035 Uiso 1 1 calc R . .
H6C H 0.8558 0.9032 0.2099 0.035 Uiso 1 1 calc R . .
C7 C 0.8827(3) 0.3129(4) 0.08589(15) 0.0178(6) Uani 1 1 d . . .
C8 C 0.7957(3) 0.6193(4) -0.01787(15) 0.0163(6) Uani 1 1 d . . .
C9 C 0.9709(3) 0.7054(4) 0.09461(14) 0.0165(6) Uani 1 1 d . . .
C10 C 0.7087(3) 0.8409(4) 0.09905(14) 0.0145(5) Uani 1 1 d . . .
C11 C 0.6239(3) 0.4456(4) 0.07243(14) 0.0140(5) 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'
W W -0.8490 6.8722 '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
C8 W1 C10 90.53(11) . . ?
C8 W1 C9 87.50(11) . . ?
C10 W1 C9 92.16(11) . . ?
C8 W1 C11 88.19(11) . . ?
C10 W1 C11 90.58(11) . . ?
C9 W1 C11 174.92(10) . . ?
C8 W1 C7 94.46(11) . . ?
C10 W1 C7 175.01(11) . . ?
C9 W1 C7 88.20(11) . . ?
C11 W1 C7 89.45(11) . . ?
C8 W1 C1 174.79(10) . . ?
C10 W1 C1 87.05(10) . . ?
C9 W1 C1 97.2(1) . . ?
C11 W1 C1 87.22(10) . . ?
C7 W1 C1 87.97(11) . . ?
C1 O1 C6 120.9(2) . . ?
C3 N1 C4 126.4(3) . . ?
C3 N1 H1 116.8 . . ?
C4 N1 H1 116.8 . . ?
O1 C1 C2 111.3(2) . . ?
O1 C1 W1 128.5(2) . . ?
C2 C1 W1 119.9(2) . . ?
C1 C2 C3 129.7(3) . . ?
C1 C2 H2 115.1 . . ?
C3 C2 H2 115.1 . . ?
N1 C3 C2 123.6(3) . . ?
N1 C3 C5 118.6(3) . . ?
C2 C3 C5 117.8(3) . . ?
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 . . ?
O2 C7 W1 178.6(3) . . ?
O3 C8 W1 178.1(3) . . ?
O4 C9 W1 175.7(2) . . ?
O5 C10 W1 177.8(2) . . ?
O6 C11 W1 177.9(2) . . ?
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
W1 C8 1.999(3) . ?
W1 C10 2.024(3) . ?
W1 C9 2.042(3) . ?
W1 C11 2.043(3) . ?
W1 C7 2.053(3) . ?
W1 C1 2.255(3) . ?
O1 C1 1.364(3) . ?
O1 C6 1.438(3) . ?
O2 C7 1.142(4) . ?
O3 C8 1.162(3) . ?
O4 C9 1.143(3) . ?
O5 C10 1.150(4) . ?
O6 C11 1.146(3) . ?
N1 C3 1.319(4) . ?
N1 C4 1.457(4) . ?
N1 H1 0.8800 . ?
C1 C2 1.397(4) . ?
C2 C3 1.416(4) . ?
C2 H2 0.9500 . ?
C3 C5 1.498(4) . ?
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 . ?
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 2.00 2.655(3) 130.8 .
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
C10 W1 C1 O1 -51.6(2) . . . . ?
C9 W1 C1 O1 40.2(3) . . . . ?
C11 W1 C1 O1 -142.3(2) . . . . ?
C7 W1 C1 O1 128.2(2) . . . . ?
C10 W1 C1 C2 121.1(2) . . . . ?
C9 W1 C1 C2 -147.1(2) . . . . ?
C11 W1 C1 C2 30.4(2) . . . . ?
C7 W1 C1 C2 -59.1(2) . . . . ?
C2 C1 O1 C6 173.3(3) . . . . ?
W1 C1 O1 C6 -13.5(4) . . . . ?
O1 C1 C2 C3 4.5(4) . . . . ?
W1 C1 C2 C3 -169.4(2) . . . . ?
C1 C2 C3 N1 0.8(5) . . . . ?
C1 C2 C3 C5 178.9(3) . . . . ?
C2 C3 N1 C4 -177.9(3) . . . . ?
C5 C3 N1 C4 4.0(4) . . . . ?
