#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:30:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179793 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008976.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_7008976
loop_
_publ_author_name
'Johansson, Anders'
'Roman, Magnus'
'Seisenbaeva, Gulaim A.'
'Kloo, Lars'
'Szabo, Zoltan'
'Kessler, Vadim G.'
_publ_section_title
;
 The solution thermolysis approach to molybdenum(V) alkoxides:
 synthesis, solid state and solution structures of the bimetallic
 alkoxides of molybdenum(V) and niobium(V), tantalum(V) and
 tungsten(VI)
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              387
_journal_paper_doi               10.1039/a907720k
_journal_year                    2000
_chemical_formula_moiety         'C21 H49 Mo2 O11 Ta'
_chemical_formula_sum            'C42 H98 Mo4 O22 Ta2'
_chemical_formula_weight         1700.86
_chemical_name_common            ' Molybdenum-tantalum oxoisopropoxide '
_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                94.159(5)
_cell_angle_beta                 94.091(7)
_cell_angle_gamma                107.143(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0444(17)
_cell_length_b                   11.0070(19)
_cell_length_c                   15.769(3)
_cell_measurement_reflns_used    '998 with I > 10 sigma(I) '
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.30
_cell_volume                     1653.7(5)
_computing_cell_refinement       ' Bruker SMART '
_computing_data_collection       ' Bruker SMART '
_computing_data_reduction        ' Bruker SAINTPLUS'
_computing_molecular_graphics    ' Bruker SHELXTL 5.3  '
_computing_publication_material  ' Bruker SHELXTL 5.3  '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  ' SMART CCD'
_diffrn_measurement_method       'CCD area Detector'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9792
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    4.091
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.1927
_exptl_absorpt_correction_type   'Bruker SADABS '
_exptl_absorpt_process_details   ' Bruker SADABS '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          '0.60 mm '
_exptl_crystal_size_mid          '0.50 mm '
_exptl_crystal_size_min          '0.20 mm '
_refine_diff_density_max         0.899
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.737
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         7141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0444P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3909
_reflns_number_total             7141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907720k.txt
_cod_data_source_block           tamopr2t
_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               7008976
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
Ta1 Ta 0.74049(3) 0.64895(3) 0.28884(2) 0.05114(12) Uani 1 1 d . . .
Mo1 Mo 0.89938(6) 0.92647(6) 0.24102(4) 0.04569(18) Uani 1 1 d . . .
Mo2 Mo 0.99063(6) 1.02793(6) 0.10552(4) 0.04544(18) Uani 1 1 d . . .
O1 O 0.7087(4) 0.8319(4) 0.2837(3) 0.0471(12) Uani 1 1 d . . .
O2 O 0.9340(4) 0.7954(4) 0.3237(3) 0.0499(13) Uani 1 1 d . . .
O3 O 1.0596(4) 0.9257(4) 0.1813(3) 0.0472(12) Uani 1 1 d . . .
O4 O 1.1058(5) 0.9706(5) 0.0158(3) 0.0539(13) Uani 1 1 d . . .
O5 O 0.8073(4) 0.9710(5) 0.1422(3) 0.0494(13) Uani 1 1 d . . .
O6 O 0.8047(5) 0.7058(5) 0.1769(3) 0.0583(14) Uani 1 1 d . . .
O7 O 0.9477(5) 1.0553(5) 0.3132(3) 0.0629(14) Uani 1 1 d . . .
O8 O 1.0685(5) 1.1826(5) 0.1376(3) 0.0649(15) Uani 1 1 d . . .
O9 O 0.6991(5) 0.6560(5) 0.4027(3) 0.0633(15) Uani 1 1 d . . .
O10 O 0.8191(6) 0.5163(5) 0.2958(4) 0.0800(18) Uani 1 1 d . . .
O11 O 0.5618(6) 0.5558(6) 0.2433(4) 0.0789(18) Uani 1 1 d . . .
C1 C 1.0598(9) 0.7860(10) 0.3699(6) 0.077(3) Uani 1 1 d . . .
H1A H 1.0321 0.7173 0.4072 0.092 Uiso 1 1 calc R . .
C2 C 0.5774(8) 0.8620(9) 0.2833(6) 0.079(3) Uani 1 1 d . . .
H2A H 0.5164 0.8014 0.3170 0.095 Uiso 1 1 calc R . .
C3 C 1.2373(8) 0.9413(10) 0.0381(6) 0.078(3) Uani 1 1 d . . .
H3A H 1.2229 0.9078 0.0937 0.093 Uiso 1 1 calc R . .
C4 C 0.7063(11) 0.7345(10) 0.4796(6) 0.087(3) Uani 1 1 d . . .
H4A H 0.7495 0.8236 0.4692 0.105 Uiso 1 1 calc R . .
C5 C 1.1541(9) 0.7526(12) 0.3114(7) 0.116(4) Uani 1 1 d . . .
H5A H 1.1059 0.6733 0.2779 0.174 Uiso 1 1 calc R . .
H5B H 1.2348 0.7437 0.3438 0.174 Uiso 1 1 calc R . .
H5C H 1.1833 0.8188 0.2742 0.174 Uiso 1 1 calc R . .
C6 C 0.5062(10) 0.8397(13) 0.1921(7) 0.144(6) Uani 1 1 d . . .
H6A H 0.4941 0.7534 0.1694 0.217 Uiso 1 1 calc R . .
H6B H 0.5633 0.8978 0.1572 0.217 Uiso 1 1 calc R . .
H6C H 0.4164 0.8540 0.1926 0.217 Uiso 1 1 calc R . .
C7 C 1.3508(9) 1.0528(11) 0.0581(7) 0.117(4) Uani 1 1 d . . .
H7B H 1.4341 1.0301 0.0731 0.176 Uiso 1 1 calc R . .
H7C H 1.3322 1.1033 0.1054 0.176 Uiso 1 1 calc R . .
H7D H 1.3637 1.1013 0.0095 0.176 Uiso 1 1 calc R . .
C8 C 1.2435(11) 0.8305(11) -0.0163(8) 0.131(5) Uani 1 1 d . . .
H8B H 1.3288 0.8116 -0.0005 0.197 Uiso 1 1 calc R . .
H8C H 1.2410 0.8487 -0.0749 0.197 Uiso 1 1 calc R . .
H8D H 1.1650 0.7584 -0.0092 0.197 Uiso 1 1 calc R . .
C9 C 0.8081(14) 0.6542(13) 0.0933(8) 0.115(4) Uani 1 1 d . . .
H9A H 0.8548 0.7324 0.0678 0.138 Uiso 1 1 calc R . .
C10 C 0.5635(12) 0.7213(13) 0.5037(7) 0.132(5) Uani 1 1 d . . .
H10A H 0.5104 0.7457 0.4586 0.198 Uiso 1 1 calc R . .
H10B H 0.5688 0.7755 0.5551 0.198 Uiso 1 1 calc R . .
H10C H 0.5186 0.6341 0.5131 0.198 Uiso 1 1 calc R . .
C11 C 1.1303(12) 0.9064(11) 0.4248(8) 0.131(5) Uani 1 1 d . . .
H11A H 1.0660 0.9248 0.4623 0.197 Uiso 1 1 calc R . .
H11B H 1.1605 0.9751 0.3896 0.197 Uiso 1 1 calc R . .
H11C H 1.2100 0.8972 0.4581 0.197 Uiso 1 1 calc R . .
C12 C 0.7953(11) 0.7020(12) 0.5457(7) 0.126(5) Uani 1 1 d . . .
H12A H 0.8873 0.7152 0.5275 0.189 Uiso 1 1 calc R . .
H12B H 0.7562 0.6141 0.5555 0.189 Uiso 1 1 calc R . .
H12C H 0.8011 0.7555 0.5976 0.189 Uiso 1 1 calc R . .
C13 C 0.8181(14) 0.3732(11) 0.3994(9) 0.147(5) Uani 1 1 d . . .
H13A H 0.8548 0.3059 0.4154 0.220 Uiso 1 1 calc R . .
H13B H 0.7177 0.3422 0.3926 0.220 Uiso 1 1 calc R . .
H13C H 0.8482 0.4436 0.4431 0.220 Uiso 1 1 calc R . .
C14 C 0.8675(16) 0.4140(12) 0.3218(10) 0.139(5) Uani 1 1 d . . .
H14A H 0.9659 0.4597 0.3406 0.167 Uiso 1 1 calc R . .
C15 C 0.6017(11) 0.9919(10) 0.3269(10) 0.157(6) Uani 1 1 d . . .
H15A H 0.6456 0.9966 0.3837 0.235 Uiso 1 1 calc R . .
H15B H 0.5137 1.0092 0.3298 0.235 Uiso 1 1 calc R . .
H15C H 0.6613 1.0539 0.2954 0.235 Uiso 1 1 calc R . .
C16 C 0.4344(14) 0.3371(13) 0.2353(11) 0.182(7) Uani 1 1 d . . .
H16A H 0.3401 0.2818 0.2333 0.272 Uiso 1 1 calc R . .
H16B H 0.4884 0.3247 0.2848 0.272 Uiso 1 1 calc R . .
H16C H 0.4752 0.3175 0.1848 0.272 Uiso 1 1 calc R . .
C17 C 0.881(2) 0.3369(12) 0.2556(10) 0.214(9) Uani 1 1 d . . .
H17A H 0.9147 0.2703 0.2764 0.321 Uiso 1 1 calc R . .
H17B H 0.9468 0.3852 0.2200 0.321 Uiso 1 1 calc R . .
H17C H 0.7920 0.2997 0.2230 0.321 Uiso 1 1 calc R . .
C18 C 0.4337(14) 0.4598(13) 0.2393(15) 0.204(10) Uani 1 1 d . . .
C19 C 0.910(2) 0.5885(17) 0.0870(9) 0.228(10) Uani 1 1 d . . .
H19A H 0.9104 0.5577 0.0285 0.342 Uiso 1 1 calc R . .
H19B H 0.8886 0.5176 0.1211 0.342 Uiso 1 1 calc R . .
H19C H 1.0012 0.6459 0.1072 0.342 Uiso 1 1 calc R . .
C20 C 0.3196(13) 0.4916(13) 0.2279(12) 0.204(9) Uani 1 1 d . . .
H20A H 0.2401 0.4172 0.2274 0.305 Uiso 1 1 calc R . .
H20B H 0.3170 0.5274 0.1743 0.305 Uiso 1 1 calc R . .
H20C H 0.3175 0.5536 0.2734 0.305 Uiso 1 1 calc R . .
C21 C 0.6840(19) 0.619(2) 0.0466(10) 0.280(14) Uani 1 1 d . . .
H21A H 0.6340 0.6789 0.0608 0.421 Uiso 1 1 calc R . .
H21B H 0.6308 0.5354 0.0584 0.421 Uiso 1 1 calc R . .
H21C H 0.6982 0.6186 -0.0130 0.421 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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
O11 Ta1 O10 99.1(3) . . ?
O11 Ta1 O9 96.0(2) . . ?
O10 Ta1 O9 95.8(2) . . ?
O11 Ta1 O6 94.6(2) . . ?
O10 Ta1 O6 98.7(2) . . ?
O9 Ta1 O6 160.4(2) . . ?
O11 Ta1 O2 164.7(2) . . ?
O10 Ta1 O2 94.3(2) . . ?
O9 Ta1 O2 89.8(2) . . ?
O6 Ta1 O2 76.0(2) . . ?
O11 Ta1 O1 95.7(2) . . ?
O10 Ta1 O1 164.4(2) . . ?
O9 Ta1 O1 87.5(2) . . ?
O6 Ta1 O1 75.13(18) . . ?
O2 Ta1 O1 70.35(17) . . ?
O11 Ta1 Mo1 123.87(18) . . ?
O10 Ta1 Mo1 124.95(18) . . ?
O9 Ta1 Mo1 110.29(16) . . ?
O6 Ta1 Mo1 50.31(15) . . ?
O2 Ta1 Mo1 40.98(12) . . ?
O1 Ta1 Mo1 40.43(11) . . ?
O7 Mo1 O5 107.3(2) . . ?
O7 Mo1 O3 107.6(2) . . ?
O5 Mo1 O3 91.72(18) . . ?
O7 Mo1 O1 98.9(2) . . ?
O5 Mo1 O1 91.50(18) . . ?
O3 Mo1 O1 151.0(2) . . ?
O7 Mo1 O2 96.8(2) . . ?
O5 Mo1 O2 152.8(2) . . ?
O3 Mo1 O2 92.77(17) . . ?
O1 Mo1 O2 72.16(17) . . ?
O7 Mo1 O6 161.5(2) . . ?
O5 Mo1 O6 86.02(19) . . ?
O3 Mo1 O6 84.15(19) . . ?
O1 Mo1 O6 67.34(18) . . ?
O2 Mo1 O6 67.80(18) . . ?
O7 Mo1 Mo2 100.89(18) . . ?
O5 Mo1 Mo2 47.38(13) . . ?
O3 Mo1 Mo2 47.89(12) . . ?
O1 Mo1 Mo2 138.13(13) . . ?
O2 Mo1 Mo2 140.16(13) . . ?
O6 Mo1 Mo2 97.54(12) . . ?
O7 Mo1 Ta1 122.48(18) . . ?
O5 Mo1 Ta1 112.12(14) . . ?
O3 Mo1 Ta1 111.21(14) . . ?
O1 Mo1 Ta1 41.81(12) . . ?
O2 Mo1 Ta1 41.81(12) . . ?
O6 Mo1 Ta1 39.08(12) . . ?
Mo2 Mo1 Ta1 136.62(3) . . ?
O8 Mo2 O5 111.3(2) . . ?
O8 Mo2 O3 109.1(2) . . ?
O5 Mo2 O3 92.07(18) . . ?
O8 Mo2 O4 108.3(2) . . ?
O5 Mo2 O4 138.5(2) . . ?
O3 Mo2 O4 86.48(18) . . ?
O8 Mo2 O4 103.9(2) . 2_775 ?
O5 Mo2 O4 87.15(18) . 2_775 ?
O3 Mo2 O4 144.8(2) . 2_775 ?
O4 Mo2 O4 71.54(18) . 2_775 ?
O8 Mo2 Mo1 105.13(18) . . ?
O5 Mo2 Mo1 47.83(13) . . ?
O3 Mo2 Mo1 47.80(13) . . ?
O4 Mo2 Mo1 130.29(13) . . ?
O4 Mo2 Mo1 132.91(13) 2_775 . ?
C2 O1 Mo1 131.7(4) . . ?
C2 O1 Ta1 127.8(5) . . ?
Mo1 O1 Ta1 97.76(17) . . ?
C1 O2 Mo1 132.1(5) . . ?
C1 O2 Ta1 128.4(5) . . ?
Mo1 O2 Ta1 97.20(18) . . ?
Mo1 O3 Mo2 84.31(17) . . ?
C3 O4 Mo2 123.4(5) . . ?
C3 O4 Mo2 128.1(5) . 2_775 ?
Mo2 O4 Mo2 108.46(18) . 2_775 ?
Mo2 O5 Mo1 84.79(17) . . ?
C9 O6 Ta1 139.8(7) . . ?
C9 O6 Mo1 129.5(7) . . ?
Ta1 O6 Mo1 90.61(19) . . ?
C4 O9 Ta1 146.7(6) . . ?
C14 O10 Ta1 165.8(7) . . ?
C18 O11 Ta1 155.9(10) . . ?
O2 C1 C5 111.4(8) . . ?
O2 C1 C11 110.1(8) . . ?
C5 C1 C11 111.8(9) . . ?
O1 C2 C15 109.8(8) . . ?
O1 C2 C6 109.7(8) . . ?
C15 C2 C6 115.4(9) . . ?
C7 C3 C8 123.7(8) . . ?
C7 C3 O4 111.8(8) . . ?
C8 C3 O4 110.3(8) . . ?
O9 C4 C12 109.2(9) . . ?
O9 C4 C10 109.8(8) . . ?
C12 C4 C10 113.1(9) . . ?
C21 C9 O6 113.9(12) . . ?
C21 C9 C19 124.3(15) . . ?
O6 C9 C19 112.9(11) . . ?
C17 C14 C13 124.9(13) . . ?
C17 C14 O10 112.7(13) . . ?
C13 C14 O10 112.0(11) . . ?
C20 C18 C16 122.7(14) . . ?
C20 C18 O11 118.3(13) . . ?
C16 C18 O11 118.3(12) . . ?
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
Ta1 O11 1.847(6) . ?
Ta1 O10 1.859(5) . ?
Ta1 O9 1.873(5) . ?
Ta1 O6 2.002(5) . ?
Ta1 O2 2.133(5) . ?
Ta1 O1 2.136(4) . ?
Ta1 Mo1 3.1746(8) . ?
Mo1 O7 1.680(5) . ?
Mo1 O5 1.923(4) . ?
Mo1 O3 1.923(4) . ?
Mo1 O1 2.078(4) . ?
Mo1 O2 2.099(4) . ?
Mo1 O6 2.443(5) . ?
Mo1 Mo2 2.5836(9) . ?
Mo2 O8 1.673(5) . ?
Mo2 O5 1.909(4) . ?
Mo2 O3 1.926(4) . ?
Mo2 O4 2.067(5) . ?
Mo2 O4 2.085(5) 2_775 ?
O1 C2 1.450(8) . ?
O2 C1 1.448(8) . ?
O4 C3 1.474(8) . ?
O4 Mo2 2.085(5) 2_775 ?
O6 C9 1.404(12) . ?
O9 C4 1.421(10) . ?
O10 C14 1.426(11) . ?
O11 C18 1.397(13) . ?
C1 C5 1.471(12) . ?
C1 C11 1.484(13) . ?
C2 C15 1.485(13) . ?
C2 C6 1.529(13) . ?
C3 C7 1.405(12) . ?
C3 C8 1.458(13) . ?
C4 C12 1.457(12) . ?
C4 C10 1.478(13) . ?
C9 C21 1.337(17) . ?
C9 C19 1.426(16) . ?
C13 C14 1.407(15) . ?
C14 C17 1.337(16) . ?
C16 C18 1.350(16) . ?
C18 C20 1.297(16) . ?
