#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/03/7000367.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_7000367
loop_
_publ_author_name
'Lotz, Simon'
'Crause, Chantelle'
'Olivier, Andrew J.'
'Liles, David C.'
'Görls, Helmar'
'Landman, Marilé'
'Bezuidenhout, Daniela I.'
_publ_section_title
;
 Synthesis and reactivity of metal carbene complexes with heterobiaryl
 spacer substituents
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              697
_journal_paper_doi               10.1039/b811762d
_journal_year                    2009
_chemical_formula_moiety         'C26 H20 N2 O12 W2'
_chemical_formula_sum            'C26 H20 N2 O12 W2'
_chemical_formula_weight         920.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7003(6)
_cell_length_b                   12.5957(4)
_cell_length_c                   13.4575(3)
_cell_measurement_reflns_used    18869
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.43
_cell_volume                     3000.32(15)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       phi-scan
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18869
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    7.725
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. R.H. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.643
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0313
_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)+(0.0343P)²+0.5780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                2779
_reflns_number_total             3431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811762d.txt
_cod_data_source_block           FO1045
_cod_original_sg_symbol_Hall     -P2ab2ac
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7000367
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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
W W 0.435193(9) 0.339562(12) 0.208198(12) 0.02706(8) Uani 1 1 d . . .
O1 O 0.32127(17) 0.4856(2) 0.33533(19) 0.0323(6) Uani 1 1 d . . .
N1 N 0.27595(19) 0.6298(3) 0.2028(2) 0.0263(7) Uani 1 1 d . . .
C1 C 0.3558(2) 0.4700(3) 0.2499(3) 0.0246(8) Uani 1 1 d . . .
C2 C 0.3326(2) 0.5554(3) 0.1829(3) 0.0238(8) Uani 1 1 d . . .
C3 C 0.3663(2) 0.5853(3) 0.0936(3) 0.0292(9) Uani 1 1 d . . .
H3A H 0.4061 0.5484 0.0612 0.035 Uiso 1 1 calc R . .
C4 C 0.3319(2) 0.6791(3) 0.0591(3) 0.0313(9) Uani 1 1 d . . .
H4A H 0.3444 0.7172 0.0004 0.038 Uiso 1 1 calc R . .
C5 C 0.2759(2) 0.7053(3) 0.1279(3) 0.0269(8) Uani 1 1 d . . .
C6 C 0.2160(3) 0.6232(4) 0.2775(3) 0.0395(11) Uani 1 1 d . . .
H6A H 0.1846 0.6872 0.2741 0.059 Uiso 1 1 calc R . .
H6B H 0.2386 0.6176 0.3437 0.059 Uiso 1 1 calc R . .
H6C H 0.1848 0.5605 0.2646 0.059 Uiso 1 1 calc R . .
C7 C 0.3271(3) 0.4153(4) 0.4204(3) 0.0462(12) Uani 1 1 d . . .
H7A H 0.2808 0.3714 0.4252 0.055 Uiso 1 1 calc R . .
H7B H 0.3707 0.3670 0.4113 0.055 Uiso 1 1 calc R . .
C8 C 0.3365(5) 0.4741(5) 0.5096(4) 0.097(3) Uani 1 1 d . . .
H8A H 0.3407 0.4251 0.5659 0.146 Uiso 1 1 calc R . .
H8B H 0.2929 0.5208 0.5194 0.146 Uiso 1 1 calc R . .
H8C H 0.3826 0.5170 0.5051 0.146 Uiso 1 1 calc R . .
O2 O 0.5559(2) 0.5119(4) 0.1380(4) 0.0752(13) Uani 1 1 d . . .
O3 O 0.5197(3) 0.3300(4) 0.4166(3) 0.0921(17) Uani 1 1 d . . .
O4 O 0.5504(3) 0.1592(4) 0.1440(3) 0.0920(19) Uani 1 1 d . . .
O5 O 0.3156(3) 0.1599(3) 0.2663(3) 0.0550(10) Uani 1 1 d . . .
O6 O 0.3605(3) 0.3272(3) -0.0065(3) 0.0571(10) Uani 1 1 d . . .
C9 C 0.5124(3) 0.4508(4) 0.1634(4) 0.0430(11) Uani 1 1 d . . .
C10 C 0.4875(3) 0.3353(4) 0.3437(4) 0.0504(13) Uani 1 1 d . . .
C11 C 0.5083(3) 0.2244(4) 0.1667(3) 0.0511(14) Uani 1 1 d . . .
C12 C 0.3585(3) 0.2257(4) 0.2488(3) 0.0348(10) Uani 1 1 d . . .
C13 C 0.3872(3) 0.3343(3) 0.0700(3) 0.0351(10) 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
C11 W C13 89.50(18) . . ?
C11 W C12 89.7(2) . . ?
C13 W C12 86.82(18) . . ?
C11 W C10 86.4(2) . . ?
C13 W C10 175.87(18) . . ?
C12 W C10 92.5(2) . . ?
C11 W C9 89.0(2) . . ?
C13 W C9 91.79(19) . . ?
C12 W C9 178.14(18) . . ?
C10 W C9 88.8(2) . . ?
C11 W C1 178.12(18) . . ?
C13 W C1 89.48(15) . . ?
C12 W C1 91.79(16) . . ?
C10 W C1 94.62(17) . . ?
C9 W C1 89.43(17) . . ?
C1 O1 C7 124.4(3) . . ?
C5 N1 C2 108.7(3) . . ?
C5 N1 C6 122.6(3) . . ?
C2 N1 C6 127.8(3) . . ?
O1 C1 C2 107.3(3) . . ?
O1 C1 W 128.4(3) . . ?
C2 C1 W 124.3(3) . . ?
N1 C2 C3 106.9(3) . . ?
N1 C2 C1 125.3(3) . . ?
C3 C2 C1 127.5(4) . . ?
C2 C3 C4 109.0(3) . . ?
C5 C4 C3 106.7(3) . . ?
N1 C5 C4 108.7(3) . . ?
N1 C5 C5 122.2(3) . 2_565 ?
C4 C5 C5 129.1(3) . 2_565 ?
C8 C7 O1 110.9(4) . . ?
O2 C9 W 179.2(5) . . ?
O3 C10 W 176.4(5) . . ?
O4 C11 W 179.2(5) . . ?
O5 C12 W 176.3(4) . . ?
O6 C13 W 177.3(4) . . ?
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
W C11 2.022(5) . ?
W C13 2.045(5) . ?
W C12 2.049(5) . ?
W C10 2.046(5) . ?
W C9 2.048(5) . ?
W C1 2.234(4) . ?
O1 C1 1.317(5) . ?
O1 C7 1.451(5) . ?
N1 C5 1.385(5) . ?
N1 C2 1.398(5) . ?
N1 C6 1.463(5) . ?
C1 C2 1.462(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.409(5) . ?
C4 C5 1.395(5) . ?
C5 C5 1.453(8) 2_565 ?
C7 C8 1.421(7) . ?
O2 C9 1.141(6) . ?
O3 C10 1.137(6) . ?
O4 C11 1.151(6) . ?
O5 C12 1.148(6) . ?
O6 C13 1.137(5) . ?
