#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:30:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179793 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008975.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_7008975
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         'C42 H98 Mo4 Nb2 O22'
_chemical_formula_sum            'C42 H98 Mo4 Nb2 O22'
_chemical_formula_weight         1524.78
_chemical_name_systematic
tetramolybdenumdiniobiumoctaoxotetradecaisopropoxide
_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                94.154(2)
_cell_angle_beta                 93.941(2)
_cell_angle_gamma                107.329(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0293(12)
_cell_length_b                   10.9976(13)
_cell_length_c                   15.7176(18)
_cell_measurement_reflns_used    '999 with I>10sigma(I) '
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.30
_cell_volume                     1643.1(3)
_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 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Bruker SMART CCD 1K '
_diffrn_measurement_method       'Bruker SMART '
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9739
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.8477
_exptl_absorpt_correction_T_min  0.5247
_exptl_absorpt_correction_type   'Bruker SADABS '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00031(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          3.448
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                3116
_reflns_number_total             7114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907720k.txt
_cod_data_source_block           monb1m
_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               7008975
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
Mo1 Mo 0.60143(6) 0.07418(5) 0.25818(4) 0.05436(18) Uani 1 1 d . . .
Mo2 Mo 0.50958(5) -0.02770(5) 0.39417(3) 0.05347(18) Uani 1 1 d . . .
Nb1 Nb 0.76065(6) 0.35386(5) 0.21162(4) 0.05946(19) Uani 1 1 d . . .
O1 O 0.4418(4) 0.0748(4) 0.3195(2) 0.0573(11) Uani 1 1 d . . .
O2 O 0.5665(4) 0.2058(3) 0.1769(2) 0.0554(10) Uani 1 1 d . . .
O3 O 0.6946(4) 0.0302(4) 0.3575(2) 0.0571(11) Uani 1 1 d . . .
O4 O 0.7936(4) 0.1709(4) 0.2165(2) 0.0598(11) Uani 1 1 d . . .
O5 O 0.6053(4) -0.0291(4) 0.5157(2) 0.0601(11) Uani 1 1 d . . .
O6 O 0.8011(5) 0.3415(4) 0.0977(3) 0.0728(13) Uani 1 1 d . . .
O7 O 0.6804(5) 0.4829(4) 0.2044(3) 0.0834(14) Uani 1 1 d . . .
O8 O 0.4310(4) -0.1823(4) 0.3617(3) 0.0756(13) Uani 1 1 d . . .
O9 O 0.9393(5) 0.4485(4) 0.2563(3) 0.0808(13) Uani 1 1 d . . .
O10 O 0.5547(5) -0.0546(4) 0.1872(3) 0.0730(13) Uani 1 1 d . . .
O11 O 0.6948(4) 0.2958(4) 0.3226(3) 0.0665(12) Uani 1 1 d . . .
C1 C 0.4400(7) 0.2148(7) 0.1306(4) 0.074(2) Uani 1 1 d . . .
H1A H 0.4680 0.2821 0.0920 0.088 Uiso 1 1 calc R . .
C2 C 0.9253(7) 0.1452(7) 0.2193(5) 0.086(2) Uani 1 1 d . . .
H2A H 0.9869 0.2055 0.1853 0.103 Uiso 1 1 calc R . .
C3 C 0.7351(7) -0.0613(8) 0.5353(5) 0.082(2) Uani 1 1 d . . .
H3A H 0.7198 -0.0950 0.5911 0.098 Uiso 1 1 calc R . .
C4 C 0.7928(9) 0.2640(8) 0.0214(5) 0.092(2) Uani 1 1 d . . .
H4A H 0.7485 0.1749 0.0320 0.111 Uiso 1 1 calc R . .
C5 C 0.9948(8) 0.1643(10) 0.3086(6) 0.150(5) Uani 1 1 d . . .
H5A H 1.0092 0.2507 0.3321 0.225 Uiso 1 1 calc R . .
H5B H 1.0837 0.1481 0.3077 0.225 Uiso 1 1 calc R . .
H5C H 0.9362 0.1062 0.3433 0.225 Uiso 1 1 calc R . .
C6 C 0.3493(8) 0.2539(9) 0.1920(5) 0.117(3) Uani 1 1 d . . .
H6A H 0.4016 0.3331 0.2245 0.176 Uiso 1 1 calc R . .
H6B H 0.3193 0.1888 0.2302 0.176 Uiso 1 1 calc R . .
H6C H 0.2687 0.2648 0.1607 0.176 Uiso 1 1 calc R . .
C7 C 0.8502(8) 0.0528(8) 0.5581(6) 0.129(3) Uani 1 1 d . . .
H7A H 0.9344 0.0303 0.5710 0.193 Uiso 1 1 calc R . .
H7B H 0.8315 0.0994 0.6075 0.193 Uiso 1 1 calc R . .
H7C H 0.8620 0.1050 0.5111 0.193 Uiso 1 1 calc R . .
C8 C 0.6284(12) 0.5847(10) 0.1774(8) 0.142(4) Uani 1 1 d . . .
H8B H 0.5290 0.5403 0.1602 0.170 Uiso 1 1 calc R . .
C9 C 0.7447(9) -0.1704(8) 0.4843(6) 0.134(4) Uani 1 1 d . . .
H9A H 0.8316 -0.1860 0.5009 0.201 Uiso 1 1 calc R . .
H9B H 0.7412 -0.1549 0.4250 0.201 Uiso 1 1 calc R . .
H9C H 0.6677 -0.2437 0.4927 0.201 Uiso 1 1 calc R . .
C10 C 0.7017(9) 0.2972(9) -0.0472(5) 0.138(4) Uani 1 1 d . . .
H10B H 0.6104 0.2873 -0.0282 0.206 Uiso 1 1 calc R . .
H10C H 0.6931 0.2412 -0.0984 0.206 Uiso 1 1 calc R . .
H10D H 0.7432 0.3842 -0.0588 0.206 Uiso 1 1 calc R . .
C11 C 0.6812(13) 0.6257(9) 0.0983(7) 0.171(5) Uani 1 1 d . . .
H11A H 0.6454 0.6931 0.0816 0.256 Uiso 1 1 calc R . .
H11B H 0.6516 0.5550 0.0547 0.256 Uiso 1 1 calc R . .
H11C H 0.7818 0.6565 0.1059 0.256 Uiso 1 1 calc R . .
C12 C 0.3659(9) 0.0935(8) 0.0776(6) 0.144(4) Uani 1 1 d . . .
H12A H 0.4279 0.0730 0.0390 0.217 Uiso 1 1 calc R . .
H12B H 0.2853 0.1028 0.0453 0.217 Uiso 1 1 calc R . .
H12C H 0.3363 0.0260 0.1141 0.217 Uiso 1 1 calc R . .
C13 C 0.9377(10) 0.2757(10) -0.0040(5) 0.148(4) Uani 1 1 d . . .
H13A H 0.9915 0.2531 0.0417 0.222 Uiso 1 1 calc R . .
H13B H 0.9828 0.3622 -0.0153 0.222 Uiso 1 1 calc R . .
H13C H 0.9311 0.2191 -0.0547 0.222 Uiso 1 1 calc R . .
C14 C 0.8994(9) 0.0103(8) 0.1758(7) 0.161(5) Uani 1 1 d . . .
H14A H 0.8550 0.0041 0.1189 0.242 Uiso 1 1 calc R . .
H14B H 0.8397 -0.0508 0.2082 0.242 Uiso 1 1 calc R . .
H14C H 0.9873 -0.0073 0.1729 0.242 Uiso 1 1 calc R . .
C15 C 0.6890(11) 0.3454(10) 0.4071(7) 0.127(3) Uani 1 1 d . . .
H15A H 0.6457 0.2675 0.4342 0.152 Uiso 1 1 calc R . .
C16 C 1.0638(11) 0.6682(10) 0.2612(8) 0.174(5) Uani 1 1 d . . .
H16A H 1.1569 0.7273 0.2677 0.261 Uiso 1 1 calc R . .
H16B H 1.0116 0.6891 0.3060 0.261 Uiso 1 1 calc R . .
H16C H 1.0179 0.6735 0.2066 0.261 Uiso 1 1 calc R . .
C17 C 1.0709(11) 0.5420(11) 0.2663(10) 0.190(6) Uani 1 1 d . . .
H17 H 1.0693 0.5504 0.3287 0.228 Uiso 1 1 calc R . .
C18 C 1.1857(11) 0.5071(10) 0.2733(10) 0.232(8) Uani 1 1 d . . .
H18A H 1.1606 0.4157 0.2733 0.348 Uiso 1 1 calc R . .
H18B H 1.2409 0.5470 0.3258 0.348 Uiso 1 1 calc R . .
H18C H 1.2392 0.5329 0.2258 0.348 Uiso 1 1 calc R . .
C19 C 0.5956(17) 0.4107(13) 0.4164(7) 0.245(9) Uani 1 1 d . . .
H19A H 0.6000 0.4416 0.4755 0.368 Uiso 1 1 calc R . .
H19B H 0.5029 0.3552 0.3979 0.368 Uiso 1 1 calc R . .
H19C H 0.6176 0.4818 0.3823 0.368 Uiso 1 1 calc R . .
C20 C 0.6238(16) 0.6674(11) 0.2446(8) 0.242(8) Uani 1 1 d . . .
H20A H 0.5895 0.7338 0.2242 0.363 Uiso 1 1 calc R . .
H20B H 0.7163 0.7047 0.2733 0.363 Uiso 1 1 calc R . .
H20C H 0.5623 0.6224 0.2839 0.363 Uiso 1 1 calc R . .
C21 C 0.8191(14) 0.3919(16) 0.4535(7) 0.292(11) Uani 1 1 d . . .
H21A H 0.8084 0.4248 0.5101 0.437 Uiso 1 1 calc R . .
H21B H 0.8787 0.4592 0.4253 0.437 Uiso 1 1 calc R . .
H21C H 0.8605 0.3240 0.4575 0.437 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'
Nb Nb -2.0727 0.6215 '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'
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
O10 Mo1 O1 108.15(19) . . ?
O10 Mo1 O3 106.71(18) . . ?
O1 Mo1 O3 91.30(15) . . ?
O10 Mo1 O4 99.52(19) . . ?
O1 Mo1 O4 150.31(16) . . ?
O3 Mo1 O4 90.88(15) . . ?
O10 Mo1 O2 98.09(17) . . ?
O1 Mo1 O2 92.67(15) . . ?
O3 Mo1 O2 152.24(16) . . ?
O4 Mo1 O2 72.59(14) . . ?
O10 Mo1 O11 162.11(17) . . ?
O1 Mo1 O11 83.53(15) . . ?
O3 Mo1 O11 86.01(15) . . ?
O4 Mo1 O11 67.09(15) . . ?
O2 Mo1 O11 67.19(14) . . ?
O10 Mo1 Mo2 100.47(15) . . ?
O1 Mo1 Mo2 47.39(10) . . ?
O3 Mo1 Mo2 47.61(11) . . ?
O4 Mo1 Mo2 137.67(11) . . ?
O2 Mo1 Mo2 139.57(10) . . ?
O11 Mo1 Mo2 97.40(10) . . ?
O10 Mo1 Nb1 123.40(15) . . ?
O1 Mo1 Nb1 110.85(11) . . ?
O3 Mo1 Nb1 111.65(11) . . ?
O4 Mo1 Nb1 41.85(10) . . ?
O2 Mo1 Nb1 41.85(10) . . ?
O11 Mo1 Nb1 38.73(10) . . ?
Mo2 Mo1 Nb1 136.13(3) . . ?
O8 Mo2 O1 109.23(18) . . ?
O8 Mo2 O3 111.52(19) . . ?
O1 Mo2 O3 92.15(15) . . ?
O8 Mo2 O5 108.24(19) . 2_656 ?
O1 Mo2 O5 86.38(15) . 2_656 ?
O3 Mo2 O5 138.27(16) . 2_656 ?
O8 Mo2 O5 104.17(18) . . ?
O1 Mo2 O5 144.28(16) . . ?
O3 Mo2 O5 87.08(15) . . ?
O5 Mo2 O5 71.26(16) 2_656 . ?
O8 Mo2 Mo1 104.99(15) . . ?
O1 Mo2 Mo1 47.92(11) . . ?
O3 Mo2 Mo1 48.00(11) . . ?
O5 Mo2 Mo1 130.42(10) 2_656 . ?
O5 Mo2 Mo1 133.02(11) . . ?
O7 Nb1 O9 99.6(2) . . ?
O7 Nb1 O6 97.23(19) . . ?
O9 Nb1 O6 96.4(2) . . ?
O7 Nb1 O11 98.54(18) . . ?
O9 Nb1 O11 95.60(18) . . ?
O6 Nb1 O11 158.28(18) . . ?
O7 Nb1 O2 93.64(18) . . ?
O9 Nb1 O2 165.01(17) . . ?
O6 Nb1 O2 88.79(17) . . ?
O11 Nb1 O2 75.41(16) . . ?
O7 Nb1 O4 163.80(18) . . ?
O9 Nb1 O4 95.88(18) . . ?
O6 Nb1 O4 85.63(16) . . ?
O11 Nb1 O4 75.16(16) . . ?
O2 Nb1 O4 70.42(14) . . ?
O7 Nb1 Mo1 124.43(15) . . ?
O9 Nb1 Mo1 124.54(14) . . ?
O6 Nb1 Mo1 108.09(13) . . ?
O11 Nb1 Mo1 50.35(12) . . ?
O2 Nb1 Mo1 40.63(9) . . ?
O4 Nb1 Mo1 40.43(10) . . ?
Mo2 O1 Mo1 84.69(14) . . ?
C1 O2 Mo1 132.1(4) . . ?
C1 O2 Nb1 128.2(4) . . ?
Mo1 O2 Nb1 97.51(15) . . ?
Mo2 O3 Mo1 84.38(14) . . ?
C2 O4 Mo1 132.2(4) . . ?
C2 O4 Nb1 126.7(4) . . ?
Mo1 O4 Nb1 97.72(15) . . ?
C3 O5 Mo2 124.9(4) . 2_656 ?
C3 O5 Mo2 126.3(4) . . ?
Mo2 O5 Mo2 108.74(16) 2_656 . ?
C4 O6 Nb1 148.3(4) . . ?
C8 O7 Nb1 165.7(5) . . ?
C17 O9 Nb1 160.8(6) . . ?
C15 O11 Nb1 140.4(5) . . ?
C15 O11 Mo1 128.6(5) . . ?
Nb1 O11 Mo1 90.91(16) . . ?
O2 C1 C12 110.8(6) . . ?
O2 C1 C6 109.9(5) . . ?
C12 C1 C6 112.6(7) . . ?
O4 C2 C5 111.9(6) . . ?
O4 C2 C14 107.6(6) . . ?
C5 C2 C14 113.4(7) . . ?
C9 C3 C7 123.9(7) . . ?
C9 C3 O5 114.2(6) . . ?
C7 C3 O5 110.3(7) . . ?
O6 C4 C10 110.0(7) . . ?
O6 C4 C13 110.1(7) . . ?
C10 C4 C13 112.7(7) . . ?
C20 C8 C11 123.0(10) . . ?
C20 C8 O7 111.9(10) . . ?
C11 C8 O7 110.8(8) . . ?
C19 C15 C21 118.6(11) . . ?
C19 C15 O11 115.4(10) . . ?
C21 C15 O11 113.4(9) . . ?
C18 C17 O9 119.6(11) . . ?
C18 C17 C16 126.6(11) . . ?
O9 C17 C16 113.6(9) . . ?
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
Mo1 O10 1.665(4) . ?
Mo1 O1 1.926(4) . ?
Mo1 O3 1.929(4) . ?
Mo1 O4 2.081(4) . ?
Mo1 O2 2.088(4) . ?
Mo1 O11 2.448(4) . ?
Mo1 Mo2 2.5836(8) . ?
Mo1 Nb1 3.1791(8) . ?
Mo2 O8 1.671(4) . ?
Mo2 O1 1.910(4) . ?
Mo2 O3 1.917(4) . ?
Mo2 O5 2.061(4) 2_656 ?
Mo2 O5 2.082(4) . ?
Nb1 O7 1.835(4) . ?
Nb1 O9 1.843(5) . ?
Nb1 O6 1.867(4) . ?
Nb1 O11 1.989(4) . ?
Nb1 O2 2.140(4) . ?
Nb1 O4 2.140(4) . ?
O2 C1 1.451(6) . ?
O4 C2 1.428(7) . ?
O5 C3 1.466(7) . ?
O5 Mo2 2.061(4) 2_656 ?
O6 C4 1.404(8) . ?
O7 C8 1.445(9) . ?
O9 C17 1.402(10) . ?
O11 C15 1.410(9) . ?
C1 C12 1.480(9) . ?
C1 C6 1.496(9) . ?
C2 C5 1.495(10) . ?
C2 C14 1.529(10) . ?
C3 C9 1.425(9) . ?
C3 C7 1.432(10) . ?
C4 C10 1.500(10) . ?
C4 C13 1.505(10) . ?
C8 C20 1.356(12) . ?
C8 C11 1.434(12) . ?
C15 C19 1.348(12) . ?
C15 C21 1.384(13) . ?
C16 C17 1.418(12) . ?
C17 C18 1.318(12) . ?
