#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:32:15 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178786 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/40/4104042.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_4104042
loop_
_publ_author_name
'Takahito Watanabe'
'Yutaka Ishida'
'Tsukasa Matsuo'
'Hiroyuki Kawaguchi'
_publ_contact_author_email       hkawa@chem.titech.ac.jp
_publ_contact_author_name        'Hioryuki Kawaguchi'
_publ_section_title
;
 Reductive Coupling of Six Carbon Monoxides by a Ditantalum Hydride
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3474
_journal_page_last               3475
_journal_paper_doi               10.1021/ja9007276
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C158 H204 O22 Ta4''C4 H8 O''C4 H8 O'
_chemical_formula_sum            'C166 H220 O24 Ta4'
_chemical_formula_weight         3323.22
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.639(3)
_cell_angle_beta                 106.946(4)
_cell_angle_gamma                97.7005(16)
_cell_formula_units_Z            1
_cell_length_a                   13.695(5)
_cell_length_b                   18.865(7)
_cell_length_c                   19.053(8)
_cell_measurement_reflns_used    10838
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0957
_cell_volume                     4047(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32107
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.8095
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         7.671
_refine_diff_density_min         -2.677
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    calcd
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         17740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0754
_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)+(0.1196P)²+30.3638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2089
_reflns_number_gt                13766
_reflns_number_total             17740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9007276_si_002.cif
_cod_data_source_block
'[(tBu-L)Ta(THF)]4[OC=C(O)C(O)=C(O)C(O)=CO](THF)2'
_cod_database_code               4104042
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 0.12389(3) 0.289793(18) 0.10698(2) 0.02183(11) Uani 1 1 d . . .
Ta2 Ta 0.15493(2) 0.076327(18) 0.198797(19) 0.02040(11) Uani 1 1 d . . .
O1 O 0.1589(4) 0.2328(3) 0.1715(3) 0.0215(11) Uani 1 1 d . . .
O2 O 0.0421(4) 0.1712(3) 0.0222(3) 0.0218(11) Uani 1 1 d . . .
O3 O -0.0884(4) 0.0121(3) -0.0827(3) 0.0206(11) Uani 1 1 d . . .
O4 O 0.2398(5) 0.2944(4) 0.0734(4) 0.0300(13) Uani 1 1 d . . .
O5 O 0.0295(5) 0.3084(3) 0.0213(4) 0.0266(12) Uani 1 1 d . . .
O6 O 0.1701(5) 0.3985(3) 0.2016(4) 0.0256(12) Uani 1 1 d . . .
O7 O -0.0264(5) 0.2816(4) 0.1323(4) 0.0313(14) Uani 1 1 d . A .
O8 O 0.3003(5) 0.0961(4) 0.2149(4) 0.0263(12) Uani 1 1 d . . .
O9 O 0.1677(5) 0.1773(3) 0.2966(4) 0.0274(13) Uani 1 1 d . . .
O10 O 0.1554(5) 0.0143(4) 0.2584(4) 0.0253(12) Uani 1 1 d . . .
O11 O -0.0196(4) 0.0478(3) 0.1805(4) 0.0241(12) Uani 1 1 d . C .
O12 O 0.7543(19) -0.0027(15) 0.4097(16) 0.179(8) Uiso 1 1 d . . .
C1 C 0.1162(6) 0.1478(5) 0.1347(5) 0.0210(15) Uani 1 1 d . . .
C2 C 0.0510(6) 0.1173(5) 0.0520(5) 0.0227(16) Uani 1 1 d . . .
C3 C -0.0094(7) 0.0309(5) -0.0076(5) 0.0240(16) Uani 1 1 d . . .
C4 C 0.2928(8) 0.2716(5) 0.0196(7) 0.033(2) Uani 1 1 d . . .
C5 C 0.4024(8) 0.2758(6) 0.0497(7) 0.035(2) Uani 1 1 d . . .
C6 C 0.4466(8) 0.2465(6) -0.0103(7) 0.040(2) Uani 1 1 d . . .
H1 H 0.5186 0.2457 0.0084 0.048 Uiso 1 1 calc R . .
C7 C 0.3929(10) 0.2182(7) -0.0956(8) 0.044(3) Uani 1 1 d . . .
C8 C 0.2893(8) 0.2207(6) -0.1214(6) 0.034(2) Uani 1 1 d . . .
H2 H 0.2516 0.2034 -0.1793 0.041 Uiso 1 1 calc R . .
C9 C 0.2365(8) 0.2476(5) -0.0658(6) 0.0314(19) Uani 1 1 d . . .
C10 C 0.1278(7) 0.2563(5) -0.0960(5) 0.0285(18) Uani 1 1 d . . .
H3 H 0.0770 0.2208 -0.0880 0.034 Uiso 1 1 calc R . .
H4 H 0.1028 0.2378 -0.1572 0.034 Uiso 1 1 calc R . .
C11 C 0.0837(7) 0.3685(5) 0.0117(5) 0.0252(17) Uani 1 1 d . . .
C12 C 0.1302(7) 0.3460(5) -0.0472(5) 0.0271(18) Uani 1 1 d . . .
C13 C 0.1907(7) 0.4070(6) -0.0528(6) 0.0320(19) Uani 1 1 d . . .
H5 H 0.2234 0.3912 -0.0926 0.038 Uiso 1 1 calc R . .
C14 C 0.2055(7) 0.4910(6) -0.0021(6) 0.0309(19) Uani 1 1 d . . .
C15 C 0.1567(7) 0.5119(5) 0.0575(6) 0.0293(19) Uani 1 1 d . . .
H6 H 0.1665 0.5684 0.0939 0.035 Uiso 1 1 calc R . .
C16 C 0.0947(7) 0.4519(5) 0.0640(5) 0.0254(17) Uani 1 1 d . . .
C17 C 0.0403(8) 0.4737(6) 0.1246(6) 0.034(2) Uani 1 1 d . . .
H7 H -0.0111 0.4223 0.1099 0.041 Uiso 1 1 calc R . .
H8 H -0.0018 0.5099 0.1155 0.041 Uiso 1 1 calc R . .
C18 C 0.1725(7) 0.4778(5) 0.2552(6) 0.0283(18) Uani 1 1 d . . .
C19 C 0.2328(7) 0.5158(5) 0.3429(6) 0.0307(19) Uani 1 1 d . . .
C20 C 0.2301(10) 0.5950(6) 0.3916(6) 0.044(3) Uani 1 1 d . . .
H9 H 0.2731 0.6241 0.4505 0.053 Uiso 1 1 calc R . .
C21 C 0.1649(9) 0.6351(7) 0.3566(7) 0.044(2) Uani 1 1 d . . .
C22 C 0.1118(9) 0.5958(6) 0.2725(6) 0.037(2) Uani 1 1 d . . .
H10 H 0.0729 0.6234 0.2485 0.045 Uiso 1 1 calc R . .
C23 C 0.1105(8) 0.5159(5) 0.2178(6) 0.0315(19) Uani 1 1 d . . .
C24 C 0.4698(7) 0.3166(7) 0.1431(7) 0.036(2) Uani 1 1 d . . .
C25 C 0.4262(8) 0.2763(7) 0.1881(7) 0.040(2) Uani 1 1 d . . .
H11 H 0.3540 0.2803 0.1822 0.060 Uiso 1 1 calc R . .
H12 H 0.4734 0.3051 0.2483 0.060 Uiso 1 1 calc R . .
H13 H 0.4239 0.2182 0.1623 0.060 Uiso 1 1 calc R . .
C26 C 0.5844(9) 0.3134(10) 0.1628(9) 0.059(4) Uani 1 1 d . . .
H14 H 0.5848 0.2561 0.1429 0.088 Uiso 1 1 calc R . .
H15 H 0.6257 0.3463 0.2240 0.088 Uiso 1 1 calc R . .
H16 H 0.6166 0.3359 0.1342 0.088 Uiso 1 1 calc R . .
C27 C 0.4741(8) 0.4087(7) 0.1853(7) 0.042(2) Uani 1 1 d . . .
H17 H 0.5037 0.4352 0.1585 0.063 Uiso 1 1 calc R . .
H18 H 0.5196 0.4364 0.2457 0.063 Uiso 1 1 calc R . .
H19 H 0.4016 0.4128 0.1783 0.063 Uiso 1 1 calc R . .
C28 C 0.4469(11) 0.1887(8) -0.1559(9) 0.058(3) Uani 1 1 d . . .
H20 H 0.4730 0.2332 -0.1656 0.087 Uiso 1 1 calc R . .
H21 H 0.3957 0.1414 -0.2097 0.087 Uiso 1 1 calc R . .
H22 H 0.5073 0.1722 -0.1320 0.087 Uiso 1 1 calc R . .
C29 C 0.2825(9) 0.5561(7) -0.0034(8) 0.044(3) Uani 1 1 d . . .
C30 C 0.3962(9) 0.5588(9) 0.0372(12) 0.075(5) Uani 1 1 d . . .
H23 H 0.4452 0.6009 0.0361 0.113 Uiso 1 1 calc R . .
H24 H 0.4054 0.5049 0.0060 0.113 Uiso 1 1 calc R . .
H25 H 0.4119 0.5725 0.0960 0.113 Uiso 1 1 calc R . .
C31 C 0.2565(13) 0.5342(8) -0.0965(10) 0.068(4) Uani 1 1 d . . .
H26 H 0.1824 0.5326 -0.1225 0.102 Uiso 1 1 calc R . .
H27 H 0.2653 0.4801 -0.1278 0.102 Uiso 1 1 calc R . .
H28 H 0.3052 0.5760 -0.0981 0.102 Uiso 1 1 calc R . .
C32 C 0.2675(11) 0.6413(7) 0.0421(10) 0.060(3) Uani 1 1 d . . .
H29 H 0.1932 0.6386 0.0150 0.090 Uiso 1 1 calc R . .
H30 H 0.3159 0.6818 0.0387 0.090 Uiso 1 1 calc R . .
H31 H 0.2837 0.6577 0.1016 0.090 Uiso 1 1 calc R . .
C33 C 0.2973(8) 0.4748(6) 0.3846(6) 0.037(2) Uani 1 1 d . . .
C34 C 0.2233(8) 0.3951(5) 0.3701(6) 0.032(2) Uani 1 1 d . . .
H32 H 0.2650 0.3736 0.4031 0.048 Uiso 1 1 calc R . .
H33 H 0.1934 0.3536 0.3099 0.048 Uiso 1 1 calc R . .
H34 H 0.1649 0.4082 0.3883 0.048 Uiso 1 1 calc R . .
C35 C 0.3833(8) 0.4548(6) 0.3489(7) 0.042(2) Uani 1 1 d . . .
H35 H 0.4304 0.5059 0.3604 0.063 Uiso 1 1 calc R . .
H36 H 0.3489 0.4171 0.2877 0.063 Uiso 1 1 calc R . .
H37 H 0.4256 0.4288 0.3759 0.063 Uiso 1 1 calc R . .
C36 C 0.3567(10) 0.5302(7) 0.4788(7) 0.055(3) Uani 1 1 d . . .
H38 H 0.4056 0.5804 0.4901 0.082 Uiso 1 1 calc R . .
H39 H 0.3978 0.5014 0.5023 0.082 Uiso 1 1 calc R . .
H40 H 0.3053 0.5449 0.5051 0.082 Uiso 1 1 calc R . .
C37 C 0.1701(16) 0.7218(8) 0.4171(8) 0.081(5) Uani 1 1 d . . .
H41 H 0.2250 0.7618 0.4182 0.122 Uiso 1 1 calc R . .
H42 H 0.1882 0.7291 0.4740 0.122 Uiso 1 1 calc R . .
H43 H 0.1004 0.7305 0.3982 0.122 Uiso 1 1 calc R . .
C38 C -0.0359(8) 0.3203(7) 0.2144(6) 0.039(2) Uani 1 1 d . . .
H44 H -0.0157 0.3810 0.2400 0.047 Uiso 0.44(4) 1 calc PR A 1
H45 H 0.0103 0.3061 0.2540 0.047 Uiso 0.44(4) 1 calc PR A 1
H46 H 0.0145 0.3768 0.2517 0.047 Uiso 0.56(4) 1 calc PR A 2
H47 H -0.0208 0.2875 0.2430 0.047 Uiso 0.56(4) 1 calc PR A 2
C39 C -0.157(2) 0.284(2) 0.1933(17) 0.046(8) Uiso 0.44(4) 1 d P A 1
H48 H -0.1687 0.2331 0.1975 0.056 Uiso 0.44(4) 1 calc PR A 1
H49 H -0.1814 0.3243 0.2325 0.056 Uiso 0.44(4) 1 calc PR A 1
C40 C -0.216(2) 0.264(2) 0.1014(16) 0.041(7) Uiso 0.44(4) 1 d P A 1
H50 H -0.2282 0.3139 0.0990 0.049 Uiso 0.44(4) 1 calc PR A 1
H51 H -0.2856 0.2203 0.0726 0.049 Uiso 0.44(4) 1 calc PR A 1
C41 C -0.1506(16) 0.3221(16) 0.1940(12) 0.042(6) Uiso 0.56(4) 1 d P A 2
H52 H -0.1598 0.3701 0.1869 0.050 Uiso 0.56(4) 1 calc PR A 2
H53 H -0.1757 0.3228 0.2379 0.050 Uiso 0.56(4) 1 calc PR A 2
C42 C -0.2084(13) 0.2399(12) 0.1093(10) 0.027(4) Uiso 0.56(4) 1 d P A 2
H54 H -0.2201 0.1927 0.1193 0.032 Uiso 0.56(4) 1 calc PR A 2
H55 H -0.2784 0.2408 0.0760 0.032 Uiso 0.56(4) 1 calc PR A 2
C43 C -0.1325(7) 0.2345(6) 0.0643(6) 0.0319(19) Uani 1 1 d . . .
H56 H -0.1447 0.1748 0.0436 0.038 Uiso 0.44(4) 1 calc PR A 1
H57 H -0.1386 0.2443 0.0163 0.038 Uiso 0.44(4) 1 calc PR A 1
H58 H -0.1360 0.1765 0.0295 0.038 Uiso 0.56(4) 1 calc PR A 2
H59 H -0.1501 0.2590 0.0272 0.038 Uiso 0.56(4) 1 calc PR A 2
C44 C 0.4091(6) 0.1295(5) 0.2465(5) 0.0238(16) Uani 1 1 d . . .
C45 C 0.4717(7) 0.0894(6) 0.2053(6) 0.0305(19) Uani 1 1 d . . .
C46 C 0.5810(8) 0.1283(7) 0.2425(7) 0.039(2) Uani 1 1 d . . .
H60 H 0.6242 0.1012 0.2158 0.046 Uiso 1 1 calc R . .
C47 C 0.6312(8) 0.2032(7) 0.3151(7) 0.040(2) Uani 1 1 d . . .
C48 C 0.5665(7) 0.2418(6) 0.3530(6) 0.034(2) Uani 1 1 d . . .
H61 H 0.5996 0.2935 0.4038 0.041 Uiso 1 1 calc R . .
C49 C 0.4549(7) 0.2086(6) 0.3204(6) 0.0278(18) Uani 1 1 d . . .
C50 C 0.3886(7) 0.2579(5) 0.3549(6) 0.032(2) Uani 1 1 d . . .
H62 H 0.3290 0.2530 0.3070 0.038 Uiso 1 1 calc R . .
H63 H 0.4328 0.3165 0.3899 0.038 Uiso 1 1 calc R . .
C51 C 0.2337(7) 0.1939(5) 0.3761(5) 0.0241(16) Uani 1 1 d . . .
C52 C 0.3413(8) 0.2354(5) 0.4081(5) 0.031(2) Uani 1 1 d . . .
C53 C 0.4048(8) 0.2570(5) 0.4902(6) 0.0316(19) Uani 1 1 d . . .
H64 H 0.4785 0.2865 0.5123 0.038 Uiso 1 1 calc R . .
C54 C 0.3664(10) 0.2380(6) 0.5414(7) 0.044(3) Uani 1 1 d . B .
C55 C 0.2589(8) 0.1922(6) 0.5050(6) 0.035(2) Uani 1 1 d . . .
H65 H 0.2299 0.1761 0.5374 0.042 Uiso 1 1 calc R . .
C56 C 0.1921(8) 0.1689(5) 0.4226(5) 0.0305(19) Uani 1 1 d . . .
C57 C 0.0747(8) 0.1149(5) 0.3823(6) 0.032(2) Uani 1 1 d . . .
H66 H 0.0415 0.1344 0.4241 0.039 Uiso 1 1 calc R . .
H67 H 0.0345 0.1203 0.3334 0.039 Uiso 1 1 calc R . .
C58 C 0.1159(7) -0.0186(5) 0.2999(5) 0.0270(17) Uani 1 1 d . . .
C59 C 0.1255(8) -0.0970(6) 0.2871(6) 0.033(2) Uani 1 1 d . . .
C60 C 0.0651(9) -0.1340(6) 0.3175(7) 0.044(3) Uani 1 1 d . . .
H68 H 0.0659 -0.1878 0.3074 0.052 Uiso 1 1 calc R . .
C61 C 0.0050(10) -0.0973(7) 0.3610(6) 0.049(3) Uani 1 1 d . . .
C62 C 0.0089(9) -0.0172(7) 0.3808(7) 0.045(3) Uani 1 1 d . . .
H69 H -0.0285 0.0103 0.4138 0.055 Uiso 1 1 calc R . .
C63 C 0.0675(7) 0.0242(5) 0.3528(5) 0.0295(18) Uani 1 1 d . . .
C64 C 0.4214(8) 0.0073(6) 0.1208(6) 0.037(2) Uani 1 1 d . . .
C65 C 0.3412(9) 0.0177(8) 0.0538(7) 0.051(3) Uani 1 1 d . . .
H70 H 0.2841 0.0340 0.0722 0.076 Uiso 1 1 calc R . .
H71 H 0.3102 -0.0346 0.0002 0.076 Uiso 1 1 calc R . .
H72 H 0.3778 0.0604 0.0460 0.076 Uiso 1 1 calc R . .
C66 C 0.3610(10) -0.0606(7) 0.1306(9) 0.056(3) Uani 1 1 d . . .
H73 H 0.4109 -0.0688 0.1731 0.084 Uiso 1 1 calc R . .
H74 H 0.3299 -0.1122 0.0763 0.084 Uiso 1 1 calc R . .
H75 H 0.3038 -0.0440 0.1487 0.084 Uiso 1 1 calc R . .
C67 C 0.5050(9) -0.0245(8) 0.0871(8) 0.055(3) Uani 1 1 d . . .
H76 H 0.5470 0.0179 0.0819 0.082 Uiso 1 1 calc R . .
H77 H 0.4686 -0.0745 0.0315 0.082 Uiso 1 1 calc R . .
H78 H 0.5528 -0.0374 0.1264 0.082 Uiso 1 1 calc R . .
C68 C 0.7495(8) 0.2409(8) 0.3499(8) 0.053(3) Uani 1 1 d . . .
H79 H 0.7855 0.2152 0.3806 0.079 Uiso 1 1 calc R . .
H80 H 0.7682 0.3002 0.3886 0.079 Uiso 1 1 calc R . .
H81 H 0.7725 0.2321 0.3035 0.079 Uiso 1 1 calc R . .
C69 C 0.4368(9) 0.2645(7) 0.6331(6) 0.043(2) Uani 1 1 d . . .
C70 C 0.387(2) 0.3079(16) 0.6918(15) 0.057(6) Uiso 0.55(2) 1 d P B 1
H82 H 0.3148 0.2732 0.6729 0.085 Uiso 0.55(2) 1 calc PR B 1
H83 H 0.3841 0.3599 0.6926 0.085 Uiso 0.55(2) 1 calc PR B 1
H84 H 0.4304 0.3196 0.7488 0.085 Uiso 0.55(2) 1 calc PR B 1
C71 C 0.451(2) 0.1860(16) 0.6378(17) 0.063(7) Uiso 0.55(2) 1 d P B 1
H85 H 0.4941 0.1619 0.6059 0.094 Uiso 0.55(2) 1 calc PR B 1
H86 H 0.3809 0.1456 0.6136 0.094 Uiso 0.55(2) 1 calc PR B 1
H87 H 0.4879 0.2009 0.6971 0.094 Uiso 0.55(2) 1 calc PR B 1
C72 C 0.5571(18) 0.3174(15) 0.6640(15) 0.054(6) Uiso 0.55(2) 1 d P B 1
H88 H 0.6023 0.3173 0.7144 0.081 Uiso 0.55(2) 1 calc PR B 1
H89 H 0.5596 0.3741 0.6776 0.081 Uiso 0.55(2) 1 calc PR B 1
H90 H 0.5833 0.2931 0.6188 0.081 Uiso 0.55(2) 1 calc PR B 1
C73 C 0.494(3) 0.359(2) 0.678(2) 0.081(11) Uiso 0.45(2) 1 d P B 2
H91 H 0.5506 0.3765 0.7329 0.122 Uiso 0.45(2) 1 calc PR B 2
H92 H 0.4420 0.3893 0.6869 0.122 Uiso 0.45(2) 1 calc PR B 2
H93 H 0.5258 0.3707 0.6428 0.122 Uiso 0.45(2) 1 calc PR B 2
C74 C 0.363(3) 0.257(2) 0.683(2) 0.069(9) Uiso 0.45(2) 1 d P B 2
H94 H 0.3312 0.1988 0.6629 0.103 Uiso 0.45(2) 1 calc PR B 2
H95 H 0.3064 0.2821 0.6717 0.103 Uiso 0.45(2) 1 calc PR B 2
H96 H 0.4070 0.2859 0.7434 0.103 Uiso 0.45(2) 1 calc PR B 2
C75 C 0.523(4) 0.226(3) 0.635(3) 0.091(13) Uiso 0.45(2) 1 d P B 2
H97 H 0.5590 0.2352 0.6922 0.137 Uiso 0.45(2) 1 calc PR B 2
H98 H 0.5741 0.2496 0.6188 0.137 Uiso 0.45(2) 1 calc PR B 2
H99 H 0.4920 0.1663 0.5952 0.137 Uiso 0.45(2) 1 calc PR B 2
C76 C 0.2013(9) -0.1363(6) 0.2474(6) 0.037(2) Uani 1 1 d . . .
C77 C 0.1637(8) -0.1627(6) 0.1557(6) 0.036(2) Uani 1 1 d . . .
H100 H 0.0953 -0.2066 0.1248 0.053 Uiso 1 1 calc R . .
H101 H 0.2168 -0.1832 0.1341 0.053 Uiso 1 1 calc R . .
H102 H 0.1544 -0.1156 0.1480 0.053 Uiso 1 1 calc R . .
C78 C 0.3136(8) -0.0725(7) 0.3007(7) 0.044(2) Uani 1 1 d . . .
H103 H 0.3587 -0.0853 0.2680 0.066 Uiso 1 1 calc R . .
H104 H 0.3460 -0.0746 0.3526 0.066 Uiso 1 1 calc R . .
H105 H 0.3075 -0.0172 0.3153 0.066 Uiso 1 1 calc R . .
C79 C 0.2084(12) -0.2141(8) 0.2561(10) 0.068(4) Uani 1 1 d . . .
H106 H 0.1373 -0.2549 0.2258 0.102 Uiso 1 1 calc R . .
H107 H 0.2343 -0.1984 0.3161 0.102 Uiso 1 1 calc R . .
H108 H 0.2580 -0.2380 0.2320 0.102 Uiso 1 1 calc R . .
C80 C -0.0594(12) -0.1434(9) 0.3876(9) 0.063(3) Uiso 1 1 d . . .
H109 H -0.0148 -0.1349 0.4429 0.095 Uiso 1 1 calc R . .
H110 H -0.0848 -0.2023 0.3458 0.095 Uiso 1 1 calc R . .
H111 H -0.1209 -0.1232 0.3917 0.095 Uiso 1 1 calc R . .
C81 C -0.0839(8) 0.1030(6) 0.1812(7) 0.039(2) Uani 1 1 d . C .
H112 H -0.0965 0.1107 0.1315 0.047 Uiso 1 1 calc R . .
H113 H -0.0488 0.1575 0.2333 0.047 Uiso 1 1 calc R . .
C82 C -0.1878(9) 0.0598(8) 0.1782(9) 0.052(3) Uani 1 1 d . . .
H114 H -0.2483 0.0779 0.1558 0.062 Uiso 0.67(3) 1 calc PR C 1
H115 H -0.1817 0.0669 0.2341 0.062 Uiso 0.67(3) 1 calc PR C 1
H116 H -0.1959 0.0918 0.2321 0.062 Uiso 0.33(3) 1 calc PR C 2
H117 H -0.2491 0.0555 0.1318 0.062 Uiso 0.33(3) 1 calc PR C 2
C83 C -0.1975(13) -0.0339(10) 0.1121(12) 0.045(5) Uiso 0.67(3) 1 d P C 1
H118 H -0.2493 -0.0751 0.1131 0.054 Uiso 0.67(3) 1 calc PR C 1
H119 H -0.2185 -0.0436 0.0536 0.054 Uiso 0.67(3) 1 calc PR C 1
C84 C -0.1868(19) -0.0199(14) 0.1646(16) 0.020(7) Uiso 0.33(3) 1 d P C 2
H120 H -0.2532 -0.0617 0.1170 0.024 Uiso 0.33(3) 1 calc PR C 2
H121 H -0.1823 -0.0231 0.2160 0.024 Uiso 0.33(3) 1 calc PR C 2
C85 C -0.0917(8) -0.0356(6) 0.1448(7) 0.039(2) Uani 1 1 d . . .
H122 H -0.0752 -0.0765 0.0993 0.047 Uiso 0.67(3) 1 calc PR C 1
H123 H -0.0826 -0.0509 0.1893 0.047 Uiso 0.67(3) 1 calc PR C 1
H124 H -0.0575 -0.0654 0.1718 0.047 Uiso 0.33(3) 1 calc PR C 2
H125 H -0.1118 -0.0681 0.0830 0.047 Uiso 0.33(3) 1 calc PR C 2
C86 C 0.717(3) 0.035(2) 0.366(2) 0.167(12) Uiso 1 1 d . . .
H126 H 0.6981 -0.0001 0.3049 0.201 Uiso 1 1 calc R . .
H127 H 0.7689 0.0886 0.3873 0.201 Uiso 1 1 calc R . .
C87 C 0.611(2) 0.0476(16) 0.3861(16) 0.126(8) Uiso 1 1 d . . .
H128 H 0.6032 0.1021 0.3956 0.151 Uiso 1 1 calc R . .
H129 H 0.5456 0.0042 0.3382 0.151 Uiso 1 1 calc R . .
C88 C 0.6245(17) 0.0420(14) 0.4587(14) 0.102(6) Uiso 1 1 d . . .
H130 H 0.5650 -0.0025 0.4478 0.123 Uiso 1 1 calc R . .
H131 H 0.6278 0.0947 0.5054 0.123 Uiso 1 1 calc R . .
C89 C 0.725(3) 0.024(2) 0.479(2) 0.159(11) Uiso 1 1 d . . .
H132 H 0.7814 0.0740 0.5283 0.191 Uiso 1 1 calc R . .
H133 H 0.7177 -0.0196 0.4950 0.191 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'
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
O4 Ta1 O6 100.1(3) . .
O4 Ta1 O1 101.2(2) . .
O6 Ta1 O1 97.0(2) . .
O4 Ta1 O5 95.7(3) . .
O6 Ta1 O5 98.6(2) . .
O1 Ta1 O5 154.5(2) . .
O4 Ta1 O2 97.2(3) . .
O6 Ta1 O2 162.4(2) . .
O1 Ta1 O2 76.3(2) . .
O5 Ta1 O2 82.9(2) . .
O4 Ta1 O7 173.4(2) . .
O6 Ta1 O7 83.1(2) . .
O1 Ta1 O7 84.0(2) . .
O5 Ta1 O7 78.1(2) . .
O2 Ta1 O7 80.0(2) . .
O8 Ta2 O3 100.8(2) . 2
O8 Ta2 O9 98.5(3) . .
O3 Ta2 O9 155.3(2) 2 .
O8 Ta2 O10 97.1(2) . .
O3 Ta2 O10 100.7(2) 2 .
O9 Ta2 O10 92.1(2) . .
O8 Ta2 C1 96.7(3) . .
O3 Ta2 C1 80.2(3) 2 .
O9 Ta2 C1 82.3(3) . .
O10 Ta2 C1 165.7(3) . .
O8 Ta2 O11 177.5(2) . .
O3 Ta2 O11 78.8(2) 2 .
O9 Ta2 O11 82.6(2) . .
O10 Ta2 O11 80.6(2) . .
C1 Ta2 O11 85.7(3) . .
C1 O1 Ta1 121.7(5) . .
C2 O2 Ta1 115.8(5) . .
C3 O3 Ta2 138.9(5) . 2
C4 O4 Ta1 156.8(6) . .
C11 O5 Ta1 111.9(5) . .
C18 O6 Ta1 161.7(6) . .
C43 O7 C38 110.0(7) . .
C43 O7 Ta1 122.2(5) . .
C38 O7 Ta1 127.7(5) . .
C44 O8 Ta2 164.1(6) . .
C51 O9 Ta2 118.1(5) . .
C58 O10 Ta2 154.5(6) . .
C81 O11 C85 108.6(7) . .
C81 O11 Ta2 125.2(5) . .
C85 O11 Ta2 124.6(5) . .
C86 O12 C89 108(3) . .
C2 C1 O1 108.2(6) . .
C2 C1 Ta2 126.7(6) . .
O1 C1 Ta2 125.1(5) . .
O2 C2 C1 118.0(7) . .
O2 C2 C3 117.0(7) . .
C1 C2 C3 124.9(7) . .
C3 C3 O3 119.3(9) 2 .
C3 C3 C2 122.9(9) 2 .
O3 C3 C2 117.8(7) . .
O4 C4 C9 118.1(8) . .
O4 C4 C5 121.3(9) . .
C9 C4 C5 120.6(9) . .
C6 C5 C4 116.9(10) . .
C6 C5 C24 121.5(9) . .
C4 C5 C24 121.5(9) . .
C7 C6 C5 124.4(10) . .
C8 C7 C6 117.0(9) . .
C8 C7 C28 121.9(11) . .
C6 C7 C28 121.1(11) . .
C7 C8 C9 122.9(10) . .
C8 C9 C4 117.9(9) . .
C8 C9 C10 120.2(9) . .
C4 C9 C10 121.7(8) . .
C9 C10 C12 110.4(7) . .
O5 C11 C12 119.4(8) . .
O5 C11 C16 119.7(8) . .
C12 C11 C16 120.9(7) . .
C11 C12 C13 119.2(9) . .
C11 C12 C10 119.8(7) . .
C13 C12 C10 120.4(9) . .
C12 C13 C14 122.6(9) . .
C13 C14 C15 116.8(8) . .
C13 C14 C29 120.8(9) . .
C15 C14 C29 122.0(9) . .
C16 C15 C14 121.9(8) . .
C15 C16 C11 118.6(8) . .
C15 C16 C17 121.9(8) . .
C11 C16 C17 119.5(8) . .
C16 C17 C23 117.3(8) . .
O6 C18 C19 119.9(8) . .
O6 C18 C23 117.0(8) . .
C19 C18 C23 123.1(8) . .
C20 C19 C18 115.9(9) . .
C20 C19 C33 120.3(9) . .
C18 C19 C33 123.8(8) . .
C19 C20 C21 122.9(9) . .
C22 C21 C20 117.6(9) . .
C22 C21 C37 124.9(10) . .
C20 C21 C37 117.3(10) . .
C21 C22 C23 123.5(9) . .
C22 C23 C18 116.8(8) . .
C22 C23 C17 119.7(8) . .
C18 C23 C17 123.4(8) . .
C5 C24 C26 113.7(10) . .
C5 C24 C25 113.2(8) . .
C26 C24 C25 104.7(8) . .
C5 C24 C27 108.6(8) . .
C26 C24 C27 107.5(9) . .
C25 C24 C27 108.8(9) . .
C30 C29 C14 110.0(9) . .
C30 C29 C32 110.4(11) . .
C14 C29 C32 110.9(9) . .
C30 C29 C31 109.9(12) . .
C14 C29 C31 108.7(9) . .
C32 C29 C31 106.9(10) . .
C36 C33 C19 112.7(9) . .
C36 C33 C35 105.9(9) . .
C19 C33 C35 109.0(8) . .
C36 C33 C34 107.3(9) . .
C19 C33 C34 111.0(8) . .
C35 C33 C34 110.8(8) . .
O7 C38 C41 105.0(10) . .
O7 C38 C39 104.3(12) . .
C41 C38 C39 26.7(11) . .
C40 C39 C38 105(2) . .
C39 C40 C43 99(2) . .
C38 C41 C42 100.6(15) . .
C43 C42 C41 104.0(13) . .
O7 C43 C42 104.7(9) . .
O7 C43 C40 107.3(12) . .
C42 C43 C40 20.8(11) . .
O8 C44 C45 121.6(8) . .
O8 C44 C49 116.8(7) . .
C45 C44 C49 121.5(8) . .
C46 C45 C44 117.1(9) . .
C46 C45 C64 121.0(9) . .
C44 C45 C64 121.9(8) . .
C47 C46 C45 124.7(10) . .
C46 C47 C48 116.7(9) . .
C46 C47 C68 120.9(10) . .
C48 C47 C68 122.4(10) . .
C47 C48 C49 123.5(9) . .
C48 C49 C44 116.4(8) . .
C48 C49 C50 121.1(8) . .
C44 C49 C50 122.0(7) . .
C49 C50 C52 116.4(7) . .
C52 C51 C56 120.5(8) . .
C52 C51 O9 119.3(7) . .
C56 C51 O9 120.2(8) . .
C51 C52 C53 118.6(8) . .
C51 C52 C50 120.6(8) . .
C53 C52 C50 120.8(8) . .
C54 C53 C52 123.4(9) . .
C53 C54 C55 116.1(9) . .
C53 C54 C69 122.8(10) . .
C55 C54 C69 121.1(9) . .
C54 C55 C56 122.4(9) . .
C51 C56 C55 118.8(8) . .
C51 C56 C57 119.8(8) . .
C55 C56 C57 121.5(8) . .
C63 C57 C56 111.1(8) . .
O10 C58 C63 120.2(7) . .
O10 C58 C59 118.4(8) . .
C63 C58 C59 121.3(8) . .
C60 C59 C58 115.0(9) . .
C60 C59 C76 122.5(8) . .
C58 C59 C76 122.4(8) . .
C61 C60 C59 124.4(10) . .
C60 C61 C62 118.3(9) . .
C60 C61 C80 119.9(11) . .
C62 C61 C80 121.7(11) . .
C61 C62 C63 120.8(10) . .
C58 C63 C62 119.0(9) . .
C58 C63 C57 123.0(8) . .
C62 C63 C57 118.0(8) . .
C65 C64 C67 108.2(9) . .
C65 C64 C66 107.8(9) . .
C67 C64 C66 107.0(9) . .
C65 C64 C45 110.0(9) . .
C67 C64 C45 112.8(8) . .
C66 C64 C45 110.8(8) . .
C75 C69 C70 137(2) . .
C75 C69 C54 110.3(19) . .
C70 C69 C54 111.2(13) . .
C75 C69 C71 45.7(18) . .
C70 C69 C71 109.4(16) . .
C54 C69 C71 108.5(13) . .
C75 C69 C73 106(2) . .
C70 C69 C73 72.0(18) . .
C54 C69 C73 106.7(17) . .
C71 C69 C73 140.9(19) . .
C75 C69 C72 60(2) . .
C70 C69 C72 111.0(15) . .
C54 C69 C72 113.8(12) . .
C71 C69 C72 102.4(15) . .
C73 C69 C72 46.8(16) . .
C75 C69 C74 119(2) . .
C70 C69 C74 33.4(14) . .
C54 C69 C74 110.0(15) . .
C71 C69 C74 78.9(17) . .
C73 C69 C74 104(2) . .
C72 C69 C74 132.8(17) . .
C77 C76 C59 112.2(8) . .
C77 C76 C78 113.5(8) . .
C59 C76 C78 106.5(9) . .
C77 C76 C79 107.6(10) . .
C59 C76 C79 109.9(8) . .
C78 C76 C79 107.1(9) . .
O11 C81 C82 104.0(8) . .
C84 C82 C81 109.1(13) . .
C84 C82 C83 32.6(11) . .
C81 C82 C83 97.9(10) . .
C85 C83 C82 101.0(12) . .
C82 C84 C85 107.8(16) . .
C83 C85 O11 107.4(10) . .
C83 C85 C84 35.1(11) . .
O11 C85 C84 103.7(11) . .
O12 C86 C87 101(2) . .
C88 C87 C86 106(2) . .
C87 C88 C89 105(2) . .
O12 C89 C88 110(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 O4 1.882(6) .
Ta1 O6 1.909(6) .
Ta1 O1 1.959(5) .
Ta1 O5 1.962(6) .
Ta1 O2 2.003(5) .
Ta1 O7 2.247(6) .
Ta2 O8 1.882(6) .
Ta2 O3 1.931(5) 2
Ta2 O9 1.945(6) .
Ta2 O10 1.950(5) .
Ta2 C1 2.198(8) .
Ta2 O11 2.265(6) .
O1 C1 1.393(9) .
O2 C2 1.365(9) .
O3 C3 1.379(9) .
O3 Ta2 1.931(5) 2
O4 C4 1.377(12) .
O5 C11 1.378(9) .
O6 C18 1.387(10) .
O7 C43 1.463(10) .
O7 C38 1.468(11) .
O8 C44 1.370(10) .
O9 C51 1.387(9) .
O10 C58 1.375(9) .
O11 C81 1.449(11) .
O11 C85 1.476(10) .
O12 C86 1.35(3) .
O12 C89 1.40(3) .
C1 C2 1.367(11) .
C2 C3 1.455(10) .
C3 C3 1.357(16) 2
C4 C9 1.409(14) .
C4 C5 1.420(14) .
C5 C6 1.388(14) .
C5 C24 1.510(15) .
C6 C7 1.383(16) .
C7 C8 1.374(15) .
C7 C28 1.493(14) .
C8 C9 1.408(13) .
C9 C10 1.490(13) .
C10 C12 1.529(12) .
C11 C12 1.387(13) .
C11 C16 1.409(12) .
C12 C13 1.387(11) .
C13 C14 1.399(13) .
C14 C15 1.421(14) .
C14 C29 1.522(12) .
C15 C16 1.394(11) .
C16 C17 1.493(13) .
C17 C23 1.513(13) .
C18 C19 1.410(12) .
C18 C23 1.415(12) .
C19 C20 1.390(13) .
C19 C33 1.522(13) .
C20 C21 1.443(15) .
C21 C22 1.340(14) .
C21 C37 1.516(15) .
C22 C23 1.408(13) .
C24 C26 1.519(13) .
C24 C25 1.551(12) .
C24 C27 1.552(15) .
C29 C30 1.506(16) .
C29 C32 1.537(16) .
C29 C31 1.551(18) .
C33 C36 1.507(14) .
C33 C35 1.535(15) .
C33 C34 1.559(14) .
C38 C41 1.51(2) .
C38 C39 1.56(3) .
C39 C40 1.55(4) .
C40 C43 1.56(3) .
C41 C42 1.55(3) .
C42 C43 1.518(19) .
C44 C45 1.406(13) .
C44 C49 1.421(12) .
C45 C46 1.385(13) .
C45 C64 1.541(13) .
C46 C47 1.369(15) .
C47 C48 1.390(15) .
C47 C68 1.493(13) .
C48 C49 1.403(12) .
C49 C50 1.472(13) .
C50 C52 1.519(12) .
C51 C52 1.382(12) .
C51 C56 1.385(11) .
C52 C53 1.389(12) .
C53 C54 1.382(13) .
C54 C55 1.393(15) .
C54 C69 1.537(14) .
C55 C56 1.398(13) .
C56 C57 1.541(13) .
C57 C63 1.531(12) .
C58 C63 1.392(13) .
C58 C59 1.422(12) .
C59 C60 1.407(13) .
C59 C76 1.542(15) .
C60 C61 1.377(17) .
C61 C62 1.379(16) .
C61 C80 1.493(16) .
C62 C63 1.408(13) .
C64 C65 1.528(16) .
C64 C67 1.537(14) .
C64 C66 1.540(14) .
C69 C75 1.47(4) .
C69 C70 1.48(3) .
C69 C71 1.56(3) .
C69 C73 1.56(4) .
C69 C72 1.59(3) .
C69 C74 1.60(4) .
C76 C77 1.489(13) .
C76 C78 1.543(14) .
C76 C79 1.560(13) .
C81 C82 1.514(14) .
C82 C84 1.41(2) .
C82 C83 1.63(2) .
C83 C85 1.412(19) .
C84 C85 1.49(3) .
C86 C87 1.63(3) .
C87 C88 1.39(3) .
C88 C89 1.45(3) .
