#------------------------------------------------------------------------------
#$Date: 2020-04-05 13:46:33 +0300 (Sun, 05 Apr 2020) $
#$Revision: 250280 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/35/7703562.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_7703562
loop_
_publ_author_name
'Srivastava, Ravi'
'Quadrelli, Elsje Alessandra'
'Camp, Clément'
_publ_section_title
;
 Lability of Ta-NHC adducts as a synthetic route towards heterobimetallic
 Ta/Rh complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3120
_journal_page_last               3128
_journal_paper_doi               10.1039/d0dt00344a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H81 N2 O5 Si Ta, C12 H28 O4 Si'
_chemical_formula_sum            'C55 H111 N2 O9 Si2 Ta'
_chemical_formula_weight         1181.58
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-30 deposited with the CCDC.	2020-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                95.525(3)
_cell_angle_beta                 102.339(3)
_cell_angle_gamma                93.414(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7495(4)
_cell_length_b                   16.7483(7)
_cell_length_c                   21.3697(8)
_cell_measurement_reflns_used    31353
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.8360
_cell_measurement_theta_min      3.8700
_cell_volume                     3381.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00  65.00   1.00    4.24    --  -10.87  77.00 -30.00  108
  2  ω    -39.00  62.00   1.00    4.24    --  -10.87  57.00 120.00  101
  3  ω    -35.00  64.00   1.00    4.24    --  -10.87  37.00 -90.00   99
  4  ω    -85.00  13.00   1.00    4.24    --  -10.87 -37.00-150.00   98
  5  ω    -80.00 -10.00   1.00    4.24    --  -10.87 146.00  20.64   70
  6  ω     -4.00  53.00   1.00    4.24    --   11.65 -99.00-180.00   57
  7  ω    -45.00   2.00   1.00    4.24    --   11.65 126.00  92.00   47
  8  ω    -84.00  17.00   1.00    4.24    --  -10.87 -57.00 120.00  101
  9  ω    -85.00  13.00   1.00    4.24    --  -10.87 -37.00 -60.00   98
 10  ω    -68.00   2.00   1.00    4.24    --  -10.87 126.00-131.95   70
 11  ω    -67.00   3.00   1.00    4.24    --  -10.87 125.00 -26.68   70
 12  ω     -4.00  53.00   1.00    4.24    --   11.65 -99.00 -90.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0552715000
_diffrn_orient_matrix_UB_12      -0.0176392000
_diffrn_orient_matrix_UB_13      0.0198581000
_diffrn_orient_matrix_UB_21      -0.0232626000
_diffrn_orient_matrix_UB_22      0.0152973000
_diffrn_orient_matrix_UB_23      0.0277204000
_diffrn_orient_matrix_UB_31      -0.0445866000
_diffrn_orient_matrix_UB_32      -0.0357432000
_diffrn_orient_matrix_UB_33      -0.0025010000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            90751
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.014
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.788
_refine_diff_density_min         -2.688
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00287(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         17805
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0187P)²+20.3888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15596
_reflns_number_total             17805
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00344a2.cif
_cod_data_source_block           rs273
_cod_depositor_comments
'Adding full bibliography for 7703559--7703562.cif.'
_cod_database_code               7703562
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C55 H109 N2 O9 Si2 Ta'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C5) = Uanis(C4)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C11(H11A,H11B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C36(H36), C38(H38)
3.c Idealised Me refined as rotating group:
 C01O(H01A,H01B,H01C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_olex2_date_sample_data_collection 2019-05-23
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id RS2773
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.850
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.40565(2) 0.73656(2) 0.47552(2) 0.01303(6) Uani 1 1 d . . . . .
Si1 Si 0.40845(12) 0.73390(6) 0.31008(5) 0.0165(2) Uani 1 1 d . . . . .
O1 O 0.4080(3) 0.73270(17) 0.38561(13) 0.0174(5) Uani 1 1 d . . . . .
O2 O 0.5313(3) 0.79897(19) 0.30334(16) 0.0285(7) Uani 1 1 d . . . . .
O3 O 0.4330(4) 0.64532(19) 0.27930(17) 0.0303(7) Uani 1 1 d . . . . .
O4 O 0.2572(3) 0.75914(19) 0.27334(15) 0.0276(7) Uani 1 1 d . . . . .
O5 O 0.4051(3) 0.73872(15) 0.56372(12) 0.0143(5) Uani 1 1 d . . . . .
N1 N 0.4336(3) 0.8291(2) 0.73057(16) 0.0179(7) Uani 1 1 d . . . . .
N2 N 0.4679(3) 0.8264(2) 0.83181(16) 0.0182(7) Uani 1 1 d . . . . .
C1 C 0.6128(4) 0.6942(2) 0.49313(18) 0.0133(7) Uani 1 1 d . . . . .
H1A H 0.619038 0.661905 0.528811 0.016 Uiso 1 1 calc R . . . .
H1B H 0.616961 0.657726 0.455585 0.016 Uiso 1 1 calc R . . . .
C01O C 0.0846(6) 0.6453(4) 0.2594(3) 0.0533(17) Uani 1 1 d . . . . .
H01A H 0.157736 0.608990 0.264826 0.080 Uiso 1 1 calc GR . . . .
H01B H 0.001283 0.618703 0.230944 0.080 Uiso 1 1 calc GR . . . .
H01C H 0.064265 0.661850 0.300477 0.080 Uiso 1 1 calc GR . . . .
C2 C 0.7492(4) 0.7521(2) 0.5083(2) 0.0187(8) Uani 1 1 d . . . . .
C3 C 0.7471(4) 0.8063(3) 0.4546(2) 0.0211(8) Uani 1 1 d . . . . .
H3A H 0.741048 0.773656 0.414430 0.032 Uiso 1 1 calc GR . . . .
H3B H 0.831862 0.841613 0.464281 0.032 Uiso 1 1 calc GR . . . .
H3C H 0.667002 0.837548 0.451240 0.032 Uiso 1 1 calc GR . . . .
C4 C 0.8771(4) 0.7026(2) 0.5126(2) 0.0184(5) Uani 1 1 d . . . . .
H4A H 0.881790 0.669886 0.547408 0.028 Uiso 1 1 calc GR . . . .
H4B H 0.961291 0.738210 0.520358 0.028 Uiso 1 1 calc GR . . . .
H4C H 0.868419 0.668723 0.472899 0.028 Uiso 1 1 calc GR . . . .
C5 C 0.7681(4) 0.8005(2) 0.57277(19) 0.0184(5) Uani 1 1 d . U . . .
H5A H 0.690929 0.833602 0.572401 0.028 Uiso 1 1 calc GR . . . .
H5B H 0.854886 0.833980 0.581694 0.028 Uiso 1 1 calc GR . . . .
H5C H 0.770442 0.764816 0.605507 0.028 Uiso 1 1 calc GR . . . .
C6 C 0.3809(4) 0.8644(2) 0.4787(2) 0.0177(7) Uani 1 1 d . . . . .
H6A H 0.435104 0.888437 0.520496 0.021 Uiso 1 1 calc R . . . .
H6B H 0.428318 0.883986 0.446959 0.021 Uiso 1 1 calc R . . . .
C7 C 0.2372(4) 0.9020(2) 0.46868(19) 0.0168(7) Uani 1 1 d . . . . .
C8 C 0.2582(5) 0.9903(3) 0.4575(2) 0.0273(9) Uani 1 1 d . . . . .
H8A H 0.326275 1.018484 0.493122 0.041 Uiso 1 1 calc GR . . . .
H8B H 0.170216 1.014340 0.453710 0.041 Uiso 1 1 calc GR . . . .
H8C H 0.291201 0.993547 0.418474 0.041 Uiso 1 1 calc GR . . . .
C9 C 0.1741(5) 0.8977(3) 0.5280(2) 0.0269(9) Uani 1 1 d . . . . .
H9A H 0.164836 0.842713 0.536762 0.040 Uiso 1 1 calc GR . . . .
H9B H 0.083066 0.918437 0.520044 0.040 Uiso 1 1 calc GR . . . .
H9C H 0.234877 0.929179 0.564409 0.040 Uiso 1 1 calc GR . . . .
C10 C 0.1349(4) 0.8569(2) 0.4097(2) 0.0232(9) Uani 1 1 d . . . . .
H10A H 0.178316 0.854648 0.373367 0.035 Uiso 1 1 calc GR . . . .
H10B H 0.050691 0.884557 0.400371 0.035 Uiso 1 1 calc GR . . . .
H10C H 0.111571 0.803229 0.418517 0.035 Uiso 1 1 calc GR . . . .
C11 C 0.2212(4) 0.6518(2) 0.45075(19) 0.0172(7) Uani 1 1 d . . . . .
H11A H 0.166004 0.664615 0.482609 0.021 Uiso 1 1 calc R . . . .
H11B H 0.166585 0.664803 0.409997 0.021 Uiso 1 1 calc R . . . .
C12 C 0.2254(4) 0.5593(2) 0.4441(2) 0.0185(8) Uani 1 1 d . . . . .
C13 C 0.3159(5) 0.5321(2) 0.3972(2) 0.0227(8) Uani 1 1 d . . . . .
H13A H 0.281080 0.551313 0.356297 0.034 Uiso 1 1 calc GR . . . .
H13B H 0.311926 0.474410 0.391681 0.034 Uiso 1 1 calc GR . . . .
H13C H 0.411642 0.553583 0.414022 0.034 Uiso 1 1 calc GR . . . .
C14 C 0.0747(5) 0.5209(2) 0.4187(2) 0.0243(9) Uani 1 1 d . . . . .
H14A H 0.016938 0.538457 0.447656 0.036 Uiso 1 1 calc GR . . . .
H14B H 0.075150 0.463404 0.415571 0.036 Uiso 1 1 calc GR . . . .
H14C H 0.037671 0.536950 0.376810 0.036 Uiso 1 1 calc GR . . . .
C15 C 0.2852(5) 0.5305(3) 0.5092(2) 0.0249(9) Uani 1 1 d . . . . .
H15A H 0.379152 0.555031 0.525871 0.037 Uiso 1 1 calc GR . . . .
H15B H 0.287128 0.473068 0.504129 0.037 Uiso 1 1 calc GR . . . .
H15C H 0.226962 0.545434 0.538740 0.037 Uiso 1 1 calc GR . . . .
C16 C 0.1326(5) 0.7182(3) 0.2309(2) 0.0295(10) Uani 1 1 d . . . . .
C17 C 0.1620(8) 0.6942(5) 0.1656(3) 0.063(2) Uani 1 1 d . . . . .
H17A H 0.195869 0.741011 0.148985 0.095 Uiso 1 1 calc GR . . . .
H17B H 0.076807 0.670514 0.136770 0.095 Uiso 1 1 calc GR . . . .
H17C H 0.231877 0.655930 0.169387 0.095 Uiso 1 1 calc GR . . . .
C18 C 0.0233(7) 0.7786(4) 0.2276(4) 0.066(2) Uani 1 1 d . . . . .
H18A H 0.007734 0.792937 0.269955 0.100 Uiso 1 1 calc GR . . . .
H18B H -0.063280 0.755393 0.199578 0.100 Uiso 1 1 calc GR . . . .
H18C H 0.055768 0.825812 0.211119 0.100 Uiso 1 1 calc GR . . . .
C19 C 0.5491(5) 0.6055(3) 0.2617(2) 0.0281(10) Uani 1 1 d . . . . .
C20 C 0.5919(7) 0.6432(4) 0.2068(3) 0.0496(16) Uani 1 1 d . . . . .
H20A H 0.510734 0.643757 0.172360 0.074 Uiso 1 1 calc GR . . . .
H20B H 0.660691 0.612453 0.191651 0.074 Uiso 1 1 calc GR . . . .
H20C H 0.631555 0.697320 0.221450 0.074 Uiso 1 1 calc GR . . . .
C21 C 0.6690(7) 0.6090(4) 0.3196(3) 0.0526(16) Uani 1 1 d . . . . .
H21A H 0.701317 0.664122 0.334823 0.079 Uiso 1 1 calc GR . . . .
H21B H 0.744809 0.581231 0.307951 0.079 Uiso 1 1 calc GR . . . .
H21C H 0.637450 0.583754 0.353106 0.079 Uiso 1 1 calc GR . . . .
C22 C 0.4898(6) 0.5184(3) 0.2400(3) 0.0428(13) Uani 1 1 d . . . . .
H22A H 0.460314 0.495615 0.274985 0.064 Uiso 1 1 calc GR . . . .
H22B H 0.561235 0.487794 0.226998 0.064 Uiso 1 1 calc GR . . . .
H22C H 0.410550 0.516889 0.204258 0.064 Uiso 1 1 calc GR . . . .
C23 C 0.5400(5) 0.8767(3) 0.2798(2) 0.0287(10) Uani 1 1 d . . . . .
C24 C 0.4726(7) 0.8694(4) 0.2086(3) 0.0448(14) Uani 1 1 d . . . . .
H24A H 0.513180 0.827868 0.186132 0.067 Uiso 1 1 calc GR . . . .
H24B H 0.488627 0.919686 0.192163 0.067 Uiso 1 1 calc GR . . . .
H24C H 0.373061 0.856100 0.202350 0.067 Uiso 1 1 calc GR . . . .
C25 C 0.4697(7) 0.9359(3) 0.3180(3) 0.0424(13) Uani 1 1 d . . . . .
H25A H 0.372091 0.917828 0.312511 0.064 Uiso 1 1 calc GR . . . .
H25B H 0.477054 0.987826 0.302880 0.064 Uiso 1 1 calc GR . . . .
H25C H 0.515160 0.939727 0.362801 0.064 Uiso 1 1 calc GR . . . .
C26 C 0.6968(6) 0.9007(4) 0.2913(3) 0.0484(15) Uani 1 1 d . . . . .
H26A H 0.738166 0.903943 0.336577 0.073 Uiso 1 1 calc GR . . . .
H26B H 0.711006 0.952088 0.276327 0.073 Uiso 1 1 calc GR . . . .
H26C H 0.740440 0.861083 0.268318 0.073 Uiso 1 1 calc GR . . . .
C27 C 0.3994(4) 0.7345(2) 0.63003(18) 0.0147(7) Uani 1 1 d . . . . .
C28 C 0.2482(5) 0.7098(3) 0.6319(2) 0.0240(9) Uani 1 1 d . . . . .
H28A H 0.188755 0.750361 0.615817 0.036 Uiso 1 1 calc GR . . . .
H28B H 0.242161 0.703906 0.675481 0.036 Uiso 1 1 calc GR . . . .
H28C H 0.217914 0.659523 0.605520 0.036 Uiso 1 1 calc GR . . . .
C29 C 0.4968(5) 0.6721(3) 0.6563(2) 0.0250(9) Uani 1 1 d . . . . .
H29A H 0.461407 0.619894 0.634209 0.037 Uiso 1 1 calc GR . . . .
H29B H 0.500967 0.671794 0.701557 0.037 Uiso 1 1 calc GR . . . .
H29C H 0.589461 0.685260 0.649687 0.037 Uiso 1 1 calc GR . . . .
C30 C 0.4501(4) 0.8189(2) 0.66423(19) 0.0182(8) Uani 1 1 d . . . . .
H30A H 0.548763 0.829853 0.663894 0.022 Uiso 1 1 calc R . . . .
H30B H 0.397675 0.857985 0.640446 0.022 Uiso 1 1 calc R . . . .
C31 C 0.3084(4) 0.8467(3) 0.7483(2) 0.0220(8) Uani 1 1 d . . . . .
H31 H 0.225575 0.857946 0.720976 0.026 Uiso 1 1 calc R . . . .
C32 C 0.3300(4) 0.8445(3) 0.8119(2) 0.0224(8) Uani 1 1 d . . . . .
H32 H 0.265305 0.853276 0.837602 0.027 Uiso 1 1 calc R . . . .
C33 C 0.5346(4) 0.8164(2) 0.78228(19) 0.0182(8) Uani 1 1 d . . . . .
C34 C 0.5325(4) 0.8174(3) 0.89787(19) 0.0181(8) Uani 1 1 d . . . . .
C35 C 0.5454(4) 0.7402(3) 0.9159(2) 0.0220(8) Uani 1 1 d . . . . .
C36 C 0.6056(5) 0.7330(3) 0.9802(2) 0.0265(9) Uani 1 1 d . . . . .
H36 H 0.614047 0.681998 0.993634 0.032 Uiso 1 1 calc R . . . .
C37 C 0.6532(5) 0.7998(3) 1.0247(2) 0.0284(10) Uani 1 1 d . . . . .
C38 C 0.6385(5) 0.8757(3) 1.0046(2) 0.0276(10) Uani 1 1 d . . . . .
H38 H 0.670468 0.920758 1.034293 0.033 Uiso 1 1 calc R . . . .
C39 C 0.5774(4) 0.8864(3) 0.9412(2) 0.0225(8) Uani 1 1 d . . . . .
C40 C 0.4990(6) 0.6671(3) 0.8680(2) 0.0334(11) Uani 1 1 d . . . . .
H40A H 0.403540 0.670389 0.845386 0.050 Uiso 1 1 calc GR . . . .
H40B H 0.504484 0.619740 0.890180 0.050 Uiso 1 1 calc GR . . . .
H40C H 0.559123 0.664216 0.837838 0.050 Uiso 1 1 calc GR . . . .
C41 C 0.7256(6) 0.7898(4) 1.0928(2) 0.0434(13) Uani 1 1 d . . . . .
H41A H 0.824865 0.787508 1.095489 0.065 Uiso 1 1 calc GR . . . .
H41B H 0.687891 0.740870 1.105018 0.065 Uiso 1 1 calc GR . . . .
H41C H 0.710409 0.834654 1.121317 0.065 Uiso 1 1 calc GR . . . .
C42 C 0.5624(5) 0.9687(3) 0.9201(2) 0.0312(10) Uani 1 1 d . . . . .
H42A H 0.609980 0.974286 0.885630 0.047 Uiso 1 1 calc GR . . . .
H42B H 0.603342 1.008392 0.955762 0.047 Uiso 1 1 calc GR . . . .
H42C H 0.464393 0.976240 0.905534 0.047 Uiso 1 1 calc GR . . . .
Si2 Si 0.96252(11) 0.79907(7) 0.83843(5) 0.0176(2) Uani 1 1 d . . . . .
O6 O 1.0407(3) 0.71876(17) 0.82228(13) 0.0186(6) Uani 1 1 d . . . . .
O7 O 0.9842(3) 0.86234(17) 0.78699(14) 0.0195(6) Uani 1 1 d . . . . .
O8 O 1.0507(3) 0.84195(18) 0.90791(15) 0.0251(6) Uani 1 1 d . . . . .
O9 O 0.8015(3) 0.7741(2) 0.83778(17) 0.0294(7) Uani 1 1 d . . . . .
H9 H 0.750292 0.795197 0.809469 0.044 Uiso 1 1 calc GR . . . .
C43 C 0.9604(4) 0.9468(2) 0.7882(2) 0.0205(8) Uani 1 1 d . . . . .
C44 C 1.0927(5) 0.9962(3) 0.8270(2) 0.0281(10) Uani 1 1 d . . . . .
H44A H 1.112156 0.982535 0.870448 0.042 Uiso 1 1 calc GR . . . .
H44B H 1.078493 1.052475 0.827224 0.042 Uiso 1 1 calc GR . . . .
H44C H 1.170856 0.984839 0.807776 0.042 Uiso 1 1 calc GR . . . .
C45 C 0.8357(5) 0.9654(3) 0.8177(3) 0.0300(10) Uani 1 1 d . . . . .
H45A H 0.752939 0.933499 0.793544 0.045 Uiso 1 1 calc GR . . . .
H45B H 0.820720 1.021481 0.816792 0.045 Uiso 1 1 calc GR . . . .
H45C H 0.854650 0.953100 0.861570 0.045 Uiso 1 1 calc GR . . . .
C46 C 1.0825(5) 0.8149(3) 0.9707(2) 0.0257(9) Uani 1 1 d . . . . .
C47 C 1.2361(5) 0.7982(4) 0.9845(3) 0.0401(12) Uani 1 1 d . . . . .
H47A H 1.250589 0.756062 0.953451 0.060 Uiso 1 1 calc GR . . . .
H47B H 1.262565 0.781941 1.027023 0.060 Uiso 1 1 calc GR . . . .
H47C H 1.292787 0.846150 0.981877 0.060 Uiso 1 1 calc GR . . . .
C48 C 1.0569(6) 0.8840(4) 1.0174(3) 0.0428(13) Uani 1 1 d . . . . .
H48A H 1.112565 0.931658 1.013193 0.064 Uiso 1 1 calc GR . . . .
H48B H 1.083063 0.870367 1.060703 0.064 Uiso 1 1 calc GR . . . .
H48C H 0.958946 0.893703 1.007652 0.064 Uiso 1 1 calc GR . . . .
C49 C 0.9901(5) 0.7401(3) 0.9743(2) 0.0334(11) Uani 1 1 d . . . . .
H49A H 0.892848 0.750843 0.962791 0.050 Uiso 1 1 calc GR . . . .
H49B H 1.011177 0.725299 1.017455 0.050 Uiso 1 1 calc GR . . . .
H49C H 1.007872 0.696782 0.945053 0.050 Uiso 1 1 calc GR . . . .
C50 C 0.9875(5) 0.6496(3) 0.7761(2) 0.0229(8) Uani 1 1 d . . . . .
C51 C 1.1144(5) 0.6034(3) 0.7703(2) 0.0311(10) Uani 1 1 d . . . . .
H51A H 1.182153 0.637237 0.756220 0.047 Uiso 1 1 calc GR . . . .
H51B H 1.085084 0.556598 0.739587 0.047 Uiso 1 1 calc GR . . . .
H51C H 1.156271 0.587156 0.811533 0.047 Uiso 1 1 calc GR . . . .
C52 C 0.9196(5) 0.6766(3) 0.7118(2) 0.0323(11) Uani 1 1 d . . . . .
H52A H 0.839199 0.705213 0.716349 0.048 Uiso 1 1 calc GR . . . .
H52B H 0.890254 0.630420 0.680457 0.048 Uiso 1 1 calc GR . . . .
H52C H 0.986414 0.711361 0.697916 0.048 Uiso 1 1 calc GR . . . .
C53 C 0.8835(6) 0.5971(3) 0.8016(3) 0.0399(12) Uani 1 1 d . . . . .
H53A H 0.929281 0.581294 0.842362 0.060 Uiso 1 1 calc GR . . . .
H53B H 0.850881 0.549992 0.771488 0.060 Uiso 1 1 calc GR . . . .
H53C H 0.804893 0.626887 0.806876 0.060 Uiso 1 1 calc GR . . . .
C54 C 0.9323(6) 0.9641(3) 0.7182(2) 0.0339(11) Uani 1 1 d . . . . .
H54A H 1.009605 0.948851 0.699630 0.051 Uiso 1 1 calc GR . . . .
H54B H 0.922290 1.020511 0.716112 0.051 Uiso 1 1 calc GR . . . .
H54C H 0.847165 0.933804 0.694590 0.051 Uiso 1 1 calc GR . . . .
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'
Si Si 0.0817 0.0704 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 24 -2 0.1762
2 -24 2 0.1762
-14 1 4 0.1768
14 -1 -4 0.1768
0 3 29 0.0617
0 -3 -29 0.0617
7 18 -15 0.2301
-7 -18 15 0.2301
6 18 7 0.1574
-6 -18 -7 0.1574
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
O1 Ta1 C1 88.95(13) . . ?
O1 Ta1 C6 89.76(14) . . ?
O1 Ta1 C11 89.15(13) . . ?
O5 Ta1 O1 179.01(11) . . ?
O5 Ta1 C1 90.26(13) . . ?
O5 Ta1 C6 91.15(13) . . ?
O5 Ta1 C11 90.74(13) . . ?
C1 Ta1 C6 120.05(14) . . ?
C1 Ta1 C11 120.26(14) . . ?
C11 Ta1 C6 119.64(15) . . ?
O2 Si1 O1 108.85(17) . . ?
O2 Si1 O3 110.71(18) . . ?
O2 Si1 O4 109.83(17) . . ?
O3 Si1 O1 109.85(17) . . ?
O4 Si1 O1 108.52(16) . . ?
O4 Si1 O3 109.05(18) . . ?
Si1 O1 Ta1 177.29(18) . . ?
C23 O2 Si1 136.8(3) . . ?
C19 O3 Si1 136.6(3) . . ?
C16 O4 Si1 136.1(3) . . ?
C27 O5 Ta1 175.8(2) . . ?
C31 N1 C30 124.0(3) . . ?
C33 N1 C30 124.2(3) . . ?
C33 N1 C31 111.6(3) . . ?
C32 N2 C34 123.5(3) . . ?
C33 N2 C32 112.6(3) . . ?
C33 N2 C34 123.9(3) . . ?
C2 C1 Ta1 122.6(2) . . ?
C3 C2 C1 110.1(3) . . ?
C3 C2 C4 108.7(3) . . ?
C4 C2 C1 109.3(3) . . ?
C5 C2 C1 111.2(3) . . ?
C5 C2 C3 111.5(3) . . ?
C5 C2 C4 106.0(3) . . ?
C7 C6 Ta1 124.6(3) . . ?
C8 C7 C6 109.5(3) . . ?
C8 C7 C10 108.8(3) . . ?
C9 C7 C6 110.6(3) . . ?
C9 C7 C8 108.7(3) . . ?
C9 C7 C10 109.3(3) . . ?
C10 C7 C6 109.8(3) . . ?
C12 C11 Ta1 124.4(3) . . ?
C13 C12 C11 111.0(3) . . ?
C13 C12 C14 109.1(3) . . ?
C14 C12 C11 108.4(3) . . ?
C15 C12 C11 110.7(3) . . ?
C15 C12 C13 108.7(3) . . ?
C15 C12 C14 108.9(4) . . ?
O4 C16 C01O 110.1(4) . . ?
O4 C16 C17 110.0(5) . . ?
O4 C16 C18 104.8(4) . . ?
C17 C16 C01O 110.6(5) . . ?
C17 C16 C18 111.6(5) . . ?
C18 C16 C01O 109.6(6) . . ?
O3 C19 C20 109.7(4) . . ?
O3 C19 C21 109.8(4) . . ?
O3 C19 C22 104.5(4) . . ?
C20 C19 C22 110.3(4) . . ?
C21 C19 C20 112.3(5) . . ?
C21 C19 C22 110.0(5) . . ?
O2 C23 C24 109.9(4) . . ?
O2 C23 C25 109.5(4) . . ?
O2 C23 C26 104.7(4) . . ?
C24 C23 C26 110.6(5) . . ?
C25 C23 C24 111.3(5) . . ?
C25 C23 C26 110.6(5) . . ?
O5 C27 C28 107.7(3) . . ?
O5 C27 C29 108.2(3) . . ?
O5 C27 C30 105.4(3) . . ?
C28 C27 C29 110.8(3) . . ?
C28 C27 C30 112.8(3) . . ?
C29 C27 C30 111.6(3) . . ?
N1 C30 C27 113.2(3) . . ?
C32 C31 N1 106.9(4) . . ?
C31 C32 N2 106.1(4) . . ?
N1 C33 N2 102.9(3) . . ?
C35 C34 N2 118.6(4) . . ?
C35 C34 C39 122.7(4) . . ?
C39 C34 N2 118.8(4) . . ?
C34 C35 C36 117.5(4) . . ?
C34 C35 C40 121.6(4) . . ?
C36 C35 C40 121.0(4) . . ?
C37 C36 C35 121.8(4) . . ?
C36 C37 C38 118.8(4) . . ?
C36 C37 C41 120.3(5) . . ?
C38 C37 C41 120.8(5) . . ?
C37 C38 C39 121.8(4) . . ?
C34 C39 C42 121.3(4) . . ?
C38 C39 C34 117.4(4) . . ?
C38 C39 C42 121.3(4) . . ?
O6 Si2 O7 108.12(15) . . ?
O8 Si2 O6 106.44(16) . . ?
O8 Si2 O7 105.14(16) . . ?
O9 Si2 O6 109.44(17) . . ?
O9 Si2 O7 114.10(16) . . ?
O9 Si2 O8 113.19(18) . . ?
C50 O6 Si2 128.8(3) . . ?
C43 O7 Si2 129.7(3) . . ?
C46 O8 Si2 132.4(3) . . ?
O7 C43 C44 109.0(3) . . ?
O7 C43 C45 111.3(3) . . ?
O7 C43 C54 105.6(3) . . ?
C45 C43 C44 109.8(4) . . ?
C45 C43 C54 110.7(4) . . ?
C54 C43 C44 110.4(4) . . ?
O8 C46 C47 106.9(4) . . ?
O8 C46 C48 106.1(4) . . ?
O8 C46 C49 111.8(4) . . ?
C47 C46 C48 110.9(4) . . ?
C47 C46 C49 110.7(4) . . ?
C49 C46 C48 110.2(4) . . ?
O6 C50 C51 105.8(3) . . ?
O6 C50 C52 109.8(3) . . ?
O6 C50 C53 109.6(4) . . ?
C51 C50 C53 109.3(4) . . ?
C52 C50 C51 110.7(4) . . ?
C52 C50 C53 111.4(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
Ta1 O1 1.921(3) . ?
Ta1 O5 1.883(3) . ?
Ta1 C1 2.150(3) . ?
Ta1 C6 2.165(4) . ?
Ta1 C11 2.162(4) . ?
Si1 O1 1.617(3) . ?
Si1 O2 1.610(3) . ?
Si1 O3 1.616(3) . ?
Si1 O4 1.616(3) . ?
O2 C23 1.444(5) . ?
O3 C19 1.446(5) . ?
O4 C16 1.442(5) . ?
O5 C27 1.438(4) . ?
N1 C30 1.456(5) . ?
N1 C31 1.392(5) . ?
N1 C33 1.357(5) . ?
N2 C32 1.382(5) . ?
N2 C33 1.358(5) . ?
N2 C34 1.444(5) . ?
C1 C2 1.554(5) . ?
C01O C16 1.509(7) . ?
C2 C3 1.528(6) . ?
C2 C4 1.528(5) . ?
C2 C5 1.500(6) . ?
C6 C7 1.552(5) . ?
C7 C8 1.530(6) . ?
C7 C9 1.528(6) . ?
C7 C10 1.530(6) . ?
C11 C12 1.547(5) . ?
C12 C13 1.526(6) . ?
C12 C14 1.531(6) . ?
C12 C15 1.526(6) . ?
C16 C17 1.506(8) . ?
C16 C18 1.508(8) . ?
C19 C20 1.505(7) . ?
C19 C21 1.505(8) . ?
C19 C22 1.529(7) . ?
C23 C24 1.513(7) . ?
C23 C25 1.512(7) . ?
C23 C26 1.519(7) . ?
C27 C28 1.517(6) . ?
C27 C29 1.520(6) . ?
C27 C30 1.530(5) . ?
C31 C32 1.336(6) . ?
C34 C35 1.390(6) . ?
C34 C39 1.394(6) . ?
C35 C36 1.395(6) . ?
C35 C40 1.498(6) . ?
C36 C37 1.383(7) . ?
C37 C38 1.386(7) . ?
C37 C41 1.506(6) . ?
C38 C39 1.392(6) . ?
C39 C42 1.497(6) . ?
Si2 O6 1.629(3) . ?
Si2 O7 1.635(3) . ?
Si2 O8 1.623(3) . ?
Si2 O9 1.597(3) . ?
O6 C50 1.440(5) . ?
O7 C43 1.446(5) . ?
O8 C46 1.435(5) . ?
C43 C44 1.523(6) . ?
C43 C45 1.520(6) . ?
C43 C54 1.522(6) . ?
C46 C47 1.512(6) . ?
C46 C48 1.521(7) . ?
C46 C49 1.517(7) . ?
C50 C51 1.519(6) . ?
C50 C52 1.515(6) . ?
C50 C53 1.522(7) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9919 23.8441 -1.9992 -0.5704 0.3557 -0.7585
1.9919 -23.8441 1.9992 0.5704 -0.3557 0.7585
-13.9297 1.0042 3.9994 -0.7082 0.4503 0.5752
13.9297 -1.0042 -3.9994 0.7082 -0.4503 -0.5752
0.0177 2.8793 28.8935 0.5240 0.8446 -0.1760
-0.0177 -2.8793 -28.8935 -0.5240 -0.8446 0.1760
6.9567 17.9145 -14.9590 -0.2285 -0.3025 -0.9131
-6.9567 -17.9145 14.9590 0.2285 0.3025 0.9131
5.9750 17.8405 6.9620 0.1538 0.3269 -0.9215
-5.9750 -17.8405 -6.9620 -0.1538 -0.3269 0.9215
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.505 0.500 0.000 341.5 74.7 ?
