#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:06:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180123 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/21/7102124.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_7102124
loop_
_publ_author_name
'Barybin, Mikhail V'
'Chisholm, Malcolm H'
'Patmore, Nathan J'
'Robinson, Randall E'
'Singh, Namrata'
_publ_section_title
;
 Concerning the molecular and electronic structure of a
 tungsten-tungsten quadruply bonded complex supported by two
 6-carboethoxy-2-carboxylatoazulene ligands.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3652
_journal_page_last               3654
_journal_paper_doi               10.1039/b708746b
_journal_year                    2007
_chemical_formula_moiety         'C60 H68 O12 W2, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H84 O14 W2'
_chemical_formula_weight         1493.05
_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                106.775(10)
_cell_angle_beta                 93.233(10)
_cell_angle_gamma                114.97(2)
_cell_formula_units_Z            1
_cell_length_a                   10.358(3)
_cell_length_b                   10.563(3)
_cell_length_c                   17.222(7)
_cell_measurement_temperature    150(2)
_cell_volume                     1600.6(10)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_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  0.086
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14874
_diffrn_reflns_theta_full        23.04
_diffrn_reflns_theta_max         23.04
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    3.654
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular Plate'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.828
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4440
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0475
_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)+(0.0430P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                3244
_reflns_number_total             4440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708746b.txt
_cod_data_source_block           trans-W2(TiPB)2(Azu-2)2
_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_database_code               7102124
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
W1 W 0.40312(4) 0.51539(4) 0.51213(3) 0.03864(19) Uani 1 1 d . . .
O1 O 0.2695(5) 0.3098(6) 0.4290(4) 0.0402(16) Uani 1 1 d . . .
O2 O 0.5327(6) 0.7224(6) 0.5960(4) 0.0376(15) Uani 1 1 d . . .
O3 O 0.4130(5) 0.6071(6) 0.4204(4) 0.0390(16) Uani 1 1 d . . .
O4 O 0.3899(5) 0.4246(5) 0.6049(4) 0.0354(15) Uani 1 1 d . . .
O5 O -0.1078(7) -0.6916(7) 0.0380(4) 0.0573(19) Uani 1 1 d . . .
O6 O -0.3048(8) -0.6571(8) 0.0369(5) 0.092(3) Uani 1 1 d . . .
O7 O 0.1858(6) 0.5331(6) 0.5719(4) 0.0469(18) Uani 1 1 d . . .
C1 C 0.2860(9) -0.0265(9) 0.2976(6) 0.043(2) Uani 1 1 d . . .
H1 H 0.3852 -0.0063 0.3024 0.051 Uiso 1 1 calc R . .
C2 C 0.2360(8) 0.0756(9) 0.3358(6) 0.039(2) Uani 1 1 d . . .
C3 C 0.0821(9) 0.0053(10) 0.3127(6) 0.044(3) Uani 1 1 d . . .
H3 H 0.0213 0.0501 0.3303 0.053 Uiso 1 1 calc R . .
C4 C -0.1089(10) -0.2486(10) 0.2246(7) 0.051(3) Uani 1 1 d . . .
H4 H -0.1817 -0.2216 0.2425 0.061 Uiso 1 1 calc R . .
C5 C -0.1582(10) -0.3878(10) 0.1679(7) 0.058(3) Uani 1 1 d . . .
H5 H -0.2611 -0.4426 0.1508 0.069 Uiso 1 1 calc R . .
C6 C -0.0823(10) -0.4631(10) 0.1309(6) 0.051(3) Uani 1 1 d . . .
C7 C 0.0638(10) -0.4203(10) 0.1481(6) 0.051(3) Uani 1 1 d . . .
H7 H 0.0938 -0.4909 0.1187 0.061 Uiso 1 1 calc R . .
C8 C 0.1745(10) -0.2861(10) 0.2032(6) 0.049(3) Uani 1 1 d . . .
H8 H 0.2688 -0.2804 0.2079 0.059 Uiso 1 1 calc R . .
C9 C 0.1681(9) -0.1614(9) 0.2516(6) 0.040(2) Uani 1 1 d . . .
C10 C 0.0347(9) -0.1406(9) 0.2598(6) 0.044(3) Uani 1 1 d . . .
C11 C 0.3268(8) 0.2265(9) 0.3904(6) 0.036(2) Uani 1 1 d . . .
C12 C -0.1765(11) -0.6141(11) 0.0647(7) 0.058(3) Uani 1 1 d . . .
C13 C -0.1886(11) -0.8305(10) -0.0286(7) 0.063(3) Uani 1 1 d . . .
H13A H -0.2343 -0.8156 -0.0751 0.075 Uiso 1 1 calc R . .
H13B H -0.2663 -0.9017 -0.0097 0.075 Uiso 1 1 calc R . .
C14 C -0.0840(13) -0.8893(11) -0.0562(8) 0.079(4) Uani 1 1 d . . .
H14A H -0.1358 -0.9842 -0.1022 0.118 Uiso 1 1 calc R . .
H14B H -0.0404 -0.9047 -0.0099 0.118 Uiso 1 1 calc R . .
H14C H -0.0072 -0.8177 -0.0744 0.118 Uiso 1 1 calc R . .
C15 C 0.5178(9) 0.6217(8) 0.3802(5) 0.031(2) Uani 1 1 d . . .
C16 C 0.5324(8) 0.6894(9) 0.3159(6) 0.037(2) Uani 1 1 d . . .
C17 C 0.4794(9) 0.5978(10) 0.2315(7) 0.046(3) Uani 1 1 d . . .
C18 C 0.5022(9) 0.6708(10) 0.1737(6) 0.044(3) Uani 1 1 d . . .
H18 H 0.4660 0.6117 0.1167 0.053 Uiso 1 1 calc R . .
C19 C 0.5745(10) 0.8239(11) 0.1946(6) 0.044(2) Uani 1 1 d . B .
C20 C 0.6222(9) 0.9097(10) 0.2782(6) 0.037(2) Uani 1 1 d . . .
H20 H 0.6704 1.0150 0.2940 0.044 Uiso 1 1 calc R . .
C21 C 0.6007(8) 0.8440(9) 0.3403(6) 0.036(2) Uani 1 1 d . . .
C22 C 0.6624(8) 0.9394(9) 0.4311(6) 0.038(2) Uani 1 1 d . . .
H22 H 0.5999 0.8819 0.4633 0.046 Uiso 1 1 calc R . .
C23 C 0.6568(9) 1.0877(9) 0.4549(6) 0.048(3) Uani 1 1 d . . .
H23A H 0.5571 1.0698 0.4372 0.072 Uiso 1 1 calc R . .
H23B H 0.7222 1.1509 0.4276 0.072 Uiso 1 1 calc R . .
H23C H 0.6875 1.1376 0.5151 0.072 Uiso 1 1 calc R . .
C24 C 0.8148(9) 0.9640(10) 0.4587(6) 0.051(3) Uani 1 1 d . . .
H24A H 0.8502 1.0250 0.5176 0.077 Uiso 1 1 calc R . .
H24B H 0.8792 1.0151 0.4262 0.077 Uiso 1 1 calc R . .
H24C H 0.8140 0.8678 0.4501 0.077 Uiso 1 1 calc R . .
C25 C 0.4010(10) 0.4297(9) 0.2064(7) 0.055(3) Uani 1 1 d . . .
H25 H 0.4538 0.4020 0.2436 0.066 Uiso 1 1 calc R . .
C26 C 0.3990(15) 0.3456(13) 0.1179(9) 0.123(6) Uani 1 1 d . . .
H26A H 0.4988 0.3794 0.1088 0.185 Uiso 1 1 calc R . .
H26B H 0.3422 0.3646 0.0792 0.185 Uiso 1 1 calc R . .
H26C H 0.3546 0.2388 0.1086 0.185 Uiso 1 1 calc R . .
C27 C 0.2473(11) 0.3743(11) 0.2196(8) 0.080(4) Uani 1 1 d . . .
H27A H 0.2006 0.2656 0.2027 0.120 Uiso 1 1 calc R . .
H27B H 0.1931 0.4041 0.1863 0.120 Uiso 1 1 calc R . .
H27C H 0.2481 0.4172 0.2783 0.120 Uiso 1 1 calc R . .
C28 C 0.6006(10) 0.8947(12) 0.1281(7) 0.055(3) Uani 1 1 d D . .
H28 H 0.5447 0.8203 0.0720 0.067 Uiso 1 1 calc R A 1
C29 C 0.773(2) 0.975(5) 0.131(2) 0.081(11) Uiso 0.48(5) 1 d PD B 1
H29A H 0.8091 0.9005 0.1200 0.122 Uiso 0.48(5) 1 calc PR B 1
H29B H 0.8236 1.0511 0.1852 0.122 Uiso 0.48(5) 1 calc PR B 1
H29C H 0.7909 1.0211 0.0879 0.122 Uiso 0.48(5) 1 calc PR B 1
C29A C 0.743(2) 0.894(4) 0.1007(17) 0.051(9) Uiso 0.52(5) 1 d PD B 2
H29D H 0.7383 0.7959 0.0925 0.076 Uiso 0.52(5) 1 calc PR B 2
H29E H 0.8283 0.9703 0.1438 0.076 Uiso 0.52(5) 1 calc PR B 2
H29F H 0.7515 0.9142 0.0487 0.076 Uiso 0.52(5) 1 calc PR B 2
C30 C 0.5795(12) 1.0302(12) 0.1459(7) 0.069(3) Uani 1 1 d . B .
H30A H 0.5966 1.0671 0.0994 0.103 Uiso 1 1 calc R . .
H30B H 0.6482 1.1071 0.1965 0.103 Uiso 1 1 calc R . .
H30C H 0.4797 1.0057 0.1534 0.103 Uiso 1 1 calc R . .
C31 C 0.0516(9) 0.4005(10) 0.5604(7) 0.061(3) Uani 1 1 d . . .
H31A H 0.0728 0.3226 0.5701 0.073 Uiso 1 1 calc R . .
H31B H -0.0051 0.3609 0.5032 0.073 Uiso 1 1 calc R . .
C32 C -0.0330(10) 0.4446(12) 0.6222(7) 0.074(4) Uani 1 1 d . . .
H32A H -0.0650 0.3764 0.6542 0.088 Uiso 1 1 calc R . .
H32B H -0.1197 0.4434 0.5939 0.088 Uiso 1 1 calc R . .
C33 C 0.0730(11) 0.6006(13) 0.6783(8) 0.081(4) Uani 1 1 d . . .
H33A H 0.0499 0.6753 0.6656 0.097 Uiso 1 1 calc R . .
H33B H 0.0719 0.6118 0.7373 0.097 Uiso 1 1 calc R . .
C34 C 0.2161(10) 0.6163(10) 0.6590(7) 0.055(3) Uani 1 1 d . . .
H34A H 0.2852 0.7222 0.6711 0.066 Uiso 1 1 calc R . .
H34B H 0.2584 0.5752 0.6921 0.066 Uiso 1 1 calc R . .
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'
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
O1 W1 O2 178.6(2) . .
O1 W1 O3 90.4(2) . .
O2 W1 O3 89.5(2) . .
O1 W1 O4 89.8(2) . .
O2 W1 O4 90.3(2) . .
O3 W1 O4 178.8(2) . .
O1 W1 W1 91.14(15) . 2_666
O2 W1 W1 90.30(15) . 2_666
O3 W1 W1 91.35(14) . 2_666
O4 W1 W1 89.84(14) . 2_666
C11 O1 W1 119.0(5) . .
C11 O2 W1 119.7(5) 2_666 .
C15 O3 W1 118.2(5) . .
C15 O4 W1 119.6(5) 2_666 .
C12 O5 C13 116.9(8) . .
C34 O7 C31 103.4(7) . .
C9 C1 C2 109.3(7) . .
C1 C2 C3 108.7(8) . .
C1 C2 C11 125.3(7) . .
C3 C2 C11 126.0(8) . .
C10 C3 C2 108.7(8) . .
C5 C4 C10 128.4(9) . .
C4 C5 C6 130.6(9) . .
C7 C6 C5 128.6(9) . .
C7 C6 C12 116.6(9) . .
C5 C6 C12 114.8(8) . .
C6 C7 C8 128.3(9) . .
C9 C8 C7 130.0(9) . .
C8 C9 C1 126.1(8) . .
C8 C9 C10 126.9(8) . .
C1 C9 C10 106.8(7) . .
C3 C10 C4 127.1(8) . .
C3 C10 C9 106.4(7) . .
C4 C10 C9 126.5(8) . .
O2 C11 O1 119.9(7) 2_666 .
O2 C11 C2 119.1(8) 2_666 .
O1 C11 C2 120.9(7) . .
O6 C12 O5 122.8(9) . .
O6 C12 C6 122.7(10) . .
O5 C12 C6 114.4(9) . .
O5 C13 C14 107.4(9) . .
O4 C15 O3 120.9(8) 2_666 .
O4 C15 C16 118.4(7) 2_666 .
O3 C15 C16 120.6(7) . .
C21 C16 C17 121.8(9) . .
C21 C16 C15 118.3(8) . .
C17 C16 C15 119.9(8) . .
C18 C17 C16 116.4(8) . .
C18 C17 C25 122.6(10) . .
C16 C17 C25 121.0(9) . .
C19 C18 C17 124.1(9) . .
C18 C19 C20 117.6(9) . .
C18 C19 C28 121.0(9) . .
C20 C19 C28 121.5(9) . .
C19 C20 C21 121.6(8) . .
C16 C21 C20 118.4(9) . .
C16 C21 C22 120.7(8) . .
C20 C21 C22 120.7(7) . .
C24 C22 C21 112.0(7) . .
C24 C22 C23 110.5(7) . .
C21 C22 C23 114.2(8) . .
C27 C25 C17 112.0(8) . .
C27 C25 C26 108.7(9) . .
C17 C25 C26 114.9(10) . .
C30 C28 C19 115.0(8) . .
C30 C28 C29A 121.1(13) . .
C19 C28 C29A 106.2(10) . .
C30 C28 C29 97.0(18) . .
C19 C28 C29 108.9(13) . .
C29A C28 C29 28.0(12) . .
O7 C31 C32 107.0(8) . .
C31 C32 C33 104.5(8) . .
C34 C33 C32 103.5(9) . .
O7 C34 C33 105.3(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 2.031(6) .
W1 O2 2.037(6) .
W1 O3 2.065(6) .
W1 O4 2.071(6) .
W1 W1 2.2081(7) 2_666
O1 C11 1.311(9) .
O2 C11 1.300(9) 2_666
O3 C15 1.298(9) .
O4 C15 1.288(9) 2_666
O5 C12 1.304(11) .
O5 C13 1.432(11) .
O6 C12 1.223(11) .
O7 C34 1.440(11) .
O7 C31 1.449(10) .
C1 C9 1.385(11) .
C1 C2 1.402(11) .
C2 C3 1.417(11) .
C2 C11 1.442(11) .
C3 C10 1.395(12) .
C4 C5 1.363(12) .
C4 C10 1.396(12) .
C5 C6 1.396(12) .
C6 C7 1.371(12) .
C6 C12 1.519(13) .
C7 C8 1.398(12) .
C8 C9 1.371(12) .
C9 C10 1.496(11) .
C11 O2 1.300(9) 2_666
C13 C14 1.498(13) .
C15 O4 1.288(9) 2_666
C15 C16 1.465(12) .
C16 C21 1.393(11) .
C16 C17 1.414(13) .
C17 C18 1.399(13) .
C17 C25 1.517(12) .
C18 C19 1.384(12) .
C19 C20 1.388(12) .
C19 C28 1.516(13) .
C20 C21 1.415(12) .
C21 C22 1.516(12) .
C22 C24 1.511(11) .
C22 C23 1.528(11) .
C25 C27 1.503(12) .
C25 C26 1.520(16) .
C28 C30 1.486(13) .
C28 C29A 1.579(15) .
C28 C29 1.612(18) .
C31 C32 1.512(13) .
C32 C33 1.512(14) .
C33 C34 1.488(12) .
