#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/43/4314391.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_4314391
loop_
_publ_author_name
'Henrik Braband'
'Theresa I. Zahn'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Synthesis and Structural Characterization of Cationic Rhenium(V) and
 Technetium(V) Dioxo Complexes Containing Four N-Heterocyclic Carbene
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6160
_journal_page_last               6162
_journal_paper_doi               10.1021/ic0348345
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C54 H100 N8 O8.5 Tc2'
_chemical_formula_weight         1193.42
_chemical_name_systematic
;
Tetrakis(1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene)dioxotechnetium(V) 
pertechnetate
;
_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                100.134(5)
_cell_angle_beta                 98.187(5)
_cell_angle_gamma                106.092(5)
_cell_formula_units_Z            2
_cell_length_a                   12.302(5)
_cell_length_b                   16.386(5)
_cell_length_c                   16.688(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3116.1(18)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32131
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  10sec/frame
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         14919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.396
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0945P)²+2.8722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                10796
_reflns_number_total             14919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348345si20030716_125321_2.cif
_cod_data_source_block           tcocarb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C54 H100 N8 O8.50 Tc2'
_cod_database_code               4314391
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
Tc1 Tc 0.76888(2) 0.185367(18) 0.749629(18) 0.01729(9) Uani 1 1 d . . .
O1 O 0.6469(2) 0.14243(15) 0.66747(15) 0.0206(5) Uani 1 1 d . . .
O2 O 0.8902(2) 0.22789(16) 0.83182(16) 0.0249(5) Uani 1 1 d . . .
C1 C 0.6939(3) 0.0823(2) 0.8149(2) 0.0235(7) Uani 1 1 d . . .
N2 N 0.5797(3) 0.04581(19) 0.81657(19) 0.0238(6) Uani 1 1 d . . .
C3 C 0.5667(4) -0.0149(3) 0.8661(3) 0.0319(9) Uani 1 1 d . . .
C4 C 0.6732(4) -0.0162(3) 0.8970(3) 0.0345(9) Uani 1 1 d . . .
N5 N 0.7506(3) 0.0430(2) 0.8642(2) 0.0270(7) Uani 1 1 d . . .
C6 C 0.4530(4) -0.0670(3) 0.8811(3) 0.0499(12) Uani 1 1 d . . .
H6A H 0.3901 -0.0518 0.8504 0.075 Uiso 1 1 calc R . .
H6B H 0.4526 -0.0537 0.9407 0.075 Uiso 1 1 calc R . .
H6C H 0.4421 -0.1294 0.8621 0.075 Uiso 1 1 calc R . .
C7 C 0.7068(5) -0.0655(4) 0.9582(4) 0.0598(15) Uani 1 1 d . . .
H7A H 0.7908 -0.0533 0.9690 0.090 Uiso 1 1 calc R . .
H7B H 0.6691 -0.1281 0.9357 0.090 Uiso 1 1 calc R . .
H7C H 0.6827 -0.0475 1.0102 0.090 Uiso 1 1 calc R . .
C8 C 0.4849(3) 0.0703(2) 0.7715(2) 0.0263(8) Uani 1 1 d . . .
H8 H 0.5226 0.1201 0.7475 0.032 Uiso 1 1 calc R . .
C9 C 0.4103(4) -0.0020(3) 0.6988(3) 0.0405(10) Uani 1 1 d . . .
H9A H 0.4595 -0.0211 0.6630 0.061 Uiso 1 1 calc R . .
H9B H 0.3555 0.0195 0.6668 0.061 Uiso 1 1 calc R . .
H9C H 0.3678 -0.0513 0.7195 0.061 Uiso 1 1 calc R . .
C10 C 0.4137(4) 0.1039(3) 0.8294(3) 0.0399(10) Uani 1 1 d . . .
H10A H 0.4653 0.1507 0.8752 0.060 Uiso 1 1 calc R . .
H10B H 0.3709 0.0562 0.8518 0.060 Uiso 1 1 calc R . .
H10C H 0.3592 0.1265 0.7984 0.060 Uiso 1 1 calc R . .
C11 C 0.8774(3) 0.0598(3) 0.8790(3) 0.0316(9) Uani 1 1 d . . .
H11 H 0.9081 0.1042 0.8470 0.038 Uiso 1 1 calc R . .
C12 C 0.9345(4) 0.1011(4) 0.9698(3) 0.0501(12) Uani 1 1 d . . .
H12A H 0.9104 0.1522 0.9886 0.075 Uiso 1 1 calc R . .
H12B H 1.0186 0.1190 0.9756 0.075 Uiso 1 1 calc R . .
H12C H 0.9112 0.0586 1.0037 0.075 Uiso 1 1 calc R . .
C13 C 0.9106(4) -0.0204(3) 0.8442(3) 0.0456(11) Uani 1 1 d . . .
H13A H 0.8720 -0.0437 0.7857 0.068 Uiso 1 1 calc R . .
H13B H 0.8866 -0.0649 0.8759 0.068 Uiso 1 1 calc R . .
H13C H 0.9945 -0.0041 0.8486 0.068 Uiso 1 1 calc R . .
C21 C 0.6815(3) 0.2718(2) 0.8149(2) 0.0212(7) Uani 1 1 d . . .
N22 N 0.6077(3) 0.3109(2) 0.7800(2) 0.0269(7) Uani 1 1 d . . .
C23 C 0.5692(4) 0.3590(3) 0.8419(3) 0.0364(10) Uani 1 1 d . . .
C24 C 0.6212(4) 0.3513(3) 0.9155(3) 0.0357(9) Uani 1 1 d . . .
N25 N 0.6883(3) 0.2967(2) 0.8983(2) 0.0266(7) Uani 1 1 d . . .
C26 C 0.4843(5) 0.4085(4) 0.8261(4) 0.0598(15) Uani 1 1 d . . .
H26A H 0.4609 0.4022 0.7661 0.090 Uiso 1 1 calc R . .
H26B H 0.5208 0.4704 0.8530 0.090 Uiso 1 1 calc R . .
H26C H 0.4161 0.3851 0.8490 0.090 Uiso 1 1 calc R . .
C27 C 0.6106(5) 0.3936(4) 1.0011(3) 0.0567(14) Uani 1 1 d . . .
H27A H 0.6581 0.3766 1.0434 0.085 Uiso 1 1 calc R . .
H27B H 0.5297 0.3746 1.0065 0.085 Uiso 1 1 calc R . .
H27C H 0.6372 0.4572 1.0087 0.085 Uiso 1 1 calc R . .
C28 C 0.5751(3) 0.3031(3) 0.6898(3) 0.0312(8) Uani 1 1 d . . .
H28 H 0.6182 0.2661 0.6630 0.037 Uiso 1 1 calc R . .
C29 C 0.4478(4) 0.2548(3) 0.6552(3) 0.0494(12) Uani 1 1 d . . .
H29A H 0.4269 0.1993 0.6725 0.074 Uiso 1 1 calc R . .
H29B H 0.4330 0.2435 0.5944 0.074 Uiso 1 1 calc R . .
H29C H 0.4013 0.2903 0.6764 0.074 Uiso 1 1 calc R . .
C30 C 0.6158(5) 0.3905(3) 0.6661(3) 0.0450(11) Uani 1 1 d . . .
H30A H 0.6984 0.4181 0.6897 0.068 Uiso 1 1 calc R . .
H30B H 0.5724 0.4283 0.6878 0.068 Uiso 1 1 calc R . .
H30C H 0.6029 0.3812 0.6054 0.068 Uiso 1 1 calc R . .
C31 C 0.7593(3) 0.2688(2) 0.9612(2) 0.0271(8) Uani 1 1 d . . .
H31 H 0.7957 0.2296 0.9294 0.033 Uiso 1 1 calc R . .
C32 C 0.6867(4) 0.2143(3) 1.0108(3) 0.0377(10) Uani 1 1 d . . .
H32A H 0.6248 0.1661 0.9726 0.056 Uiso 1 1 calc R . .
H32B H 0.6528 0.2508 1.0459 0.056 Uiso 1 1 calc R . .
H32C H 0.7356 0.1907 1.0459 0.056 Uiso 1 1 calc R . .
C33 C 0.8589(4) 0.3454(3) 1.0161(3) 0.0449(11) Uani 1 1 d . . .
H33A H 0.9027 0.3780 0.9809 0.067 Uiso 1 1 calc R . .
H33B H 0.9099 0.3234 1.0510 0.067 Uiso 1 1 calc R . .
H33C H 0.8279 0.3840 1.0514 0.067 Uiso 1 1 calc R . .
C41 C 0.8464(3) 0.2895(2) 0.6863(2) 0.0220(7) Uani 1 1 d . . .
N42 N 0.8384(3) 0.28454(19) 0.60322(19) 0.0241(6) Uani 1 1 d . . .
C43 C 0.9032(4) 0.3627(3) 0.5878(3) 0.0320(9) Uani 1 1 d . . .
C44 C 0.9525(4) 0.4175(3) 0.6621(3) 0.0357(9) Uani 1 1 d . . .
N45 N 0.9171(3) 0.3723(2) 0.7225(2) 0.0271(7) Uani 1 1 d . . .
C46 C 0.9108(5) 0.3802(3) 0.5033(3) 0.0464(12) Uani 1 1 d . . .
H46A H 0.8654 0.3278 0.4607 0.070 Uiso 1 1 calc R . .
H46B H 0.9916 0.3959 0.4974 0.070 Uiso 1 1 calc R . .
H46C H 0.8803 0.4284 0.4964 0.070 Uiso 1 1 calc R . .
C47 C 1.0335(5) 0.5096(3) 0.6795(3) 0.0574(15) Uani 1 1 d . . .
H47A H 1.0558 0.5335 0.7397 0.086 Uiso 1 1 calc R . .
H47B H 0.9945 0.5457 0.6533 0.086 Uiso 1 1 calc R . .
H47C H 1.1026 0.5092 0.6568 0.086 Uiso 1 1 calc R . .
C48 C 0.7711(3) 0.2051(2) 0.5386(2) 0.0256(8) Uani 1 1 d . . .
H48 H 0.7300 0.1619 0.5683 0.031 Uiso 1 1 calc R . .
C49 C 0.6780(4) 0.2220(3) 0.4791(3) 0.0384(10) Uani 1 1 d . . .
H49A H 0.6306 0.2486 0.5109 0.058 Uiso 1 1 calc R . .
H49B H 0.6290 0.1668 0.4420 0.058 Uiso 1 1 calc R . .
H49C H 0.7144 0.2616 0.4460 0.058 Uiso 1 1 calc R . .
C50 C 0.8478(4) 0.1631(3) 0.4931(3) 0.0357(9) Uani 1 1 d . . .
H50A H 0.9058 0.1531 0.5336 0.054 Uiso 1 1 calc R . .
H50B H 0.8866 0.2018 0.4602 0.054 Uiso 1 1 calc R . .
H50C H 0.8004 0.1073 0.4561 0.054 Uiso 1 1 calc R . .
C51 C 0.9476(4) 0.4092(3) 0.8131(3) 0.0334(9) Uani 1 1 d . . .
H51 H 0.9065 0.3623 0.8392 0.040 Uiso 1 1 calc R . .
C52 C 0.9042(4) 0.4861(3) 0.8386(3) 0.0448(11) Uani 1 1 d . . .
H52A H 0.8213 0.4697 0.8155 0.067 Uiso 1 1 calc R . .
H52B H 0.9457 0.5354 0.8175 0.067 Uiso 1 1 calc R . .
H52C H 0.9176 0.5029 0.8994 0.067 Uiso 1 1 calc R . .
C53 C 1.0766(4) 0.4294(3) 0.8475(3) 0.0455(11) Uani 1 1 d . . .
H53A H 1.1001 0.3777 0.8299 0.068 Uiso 1 1 calc R . .
H53B H 1.0916 0.4457 0.9084 0.068 Uiso 1 1 calc R . .
H53C H 1.1208 0.4777 0.8265 0.068 Uiso 1 1 calc R . .
C61 C 0.8567(3) 0.0993(2) 0.6860(2) 0.0210(7) Uani 1 1 d . . .
N62 N 0.9729(3) 0.1163(2) 0.6886(2) 0.0260(7) Uani 1 1 d . . .
C63 C 0.9968(4) 0.0444(3) 0.6440(3) 0.0331(9) Uani 1 1 d . . .
C64 C 0.8946(4) -0.0177(3) 0.6130(3) 0.0310(8) Uani 1 1 d . . .
N65 N 0.8092(3) 0.0159(2) 0.63912(19) 0.0241(6) Uani 1 1 d . . .
C66 C 1.1136(4) 0.0355(4) 0.6405(4) 0.0512(13) Uani 1 1 d . . .
H66A H 1.1728 0.0911 0.6679 0.077 Uiso 1 1 calc R . .
H66B H 1.1199 0.0196 0.5823 0.077 Uiso 1 1 calc R . .
H66C H 1.1247 -0.0100 0.6688 0.077 Uiso 1 1 calc R . .
C67 C 0.8739(4) -0.1087(3) 0.5635(3) 0.0456(11) Uani 1 1 d . . .
H67A H 0.7908 -0.1396 0.5490 0.068 Uiso 1 1 calc R . .
H67B H 0.9131 -0.1398 0.5967 0.068 Uiso 1 1 calc R . .
H67C H 0.9043 -0.1058 0.5126 0.068 Uiso 1 1 calc R . .
C68 C 1.0598(3) 0.2011(3) 0.7295(3) 0.0319(9) Uani 1 1 d . . .
H68 H 1.0162 0.2391 0.7540 0.038 Uiso 1 1 calc R . .
C69 C 1.1447(4) 0.1945(4) 0.8022(3) 0.0482(12) Uani 1 1 d . . .
H69A H 1.1018 0.1649 0.8396 0.072 Uiso 1 1 calc R . .
H69B H 1.1931 0.2531 0.8326 0.072 Uiso 1 1 calc R . .
H69C H 1.1937 0.1611 0.7812 0.072 Uiso 1 1 calc R . .
C70 C 1.1194(4) 0.2471(3) 0.6678(3) 0.0453(11) Uani 1 1 d . . .
H70A H 1.0609 0.2497 0.6227 0.068 Uiso 1 1 calc R . .
H70B H 1.1681 0.2146 0.6447 0.068 Uiso 1 1 calc R . .
H70C H 1.1674 0.3064 0.6965 0.068 Uiso 1 1 calc R . .
C71 C 0.6836(3) -0.0308(2) 0.6192(2) 0.0259(8) Uani 1 1 d . . .
H71 H 0.6466 0.0085 0.6500 0.031 Uiso 1 1 calc R . .
C72 C 0.6529(4) -0.1148(3) 0.6500(3) 0.0401(10) Uani 1 1 d . . .
H72A H 0.6869 -0.1024 0.7094 0.060 Uiso 1 1 calc R . .
H72B H 0.6835 -0.1570 0.6191 0.060 Uiso 1 1 calc R . .
H72C H 0.5688 -0.1391 0.6415 0.060 Uiso 1 1 calc R . .
C73 C 0.6337(4) -0.0439(3) 0.5267(3) 0.0393(10) Uani 1 1 d . . .
H73A H 0.6560 0.0121 0.5105 0.059 Uiso 1 1 calc R . .
H73B H 0.5493 -0.0671 0.5166 0.059 Uiso 1 1 calc R . .
H73C H 0.6639 -0.0851 0.4939 0.059 Uiso 1 1 calc R . .
Tc2 Tc 0.90609(5) 0.19688(3) 1.23927(3) 0.05963(15) Uani 1 1 d . . .
O3 O 0.8402(4) 0.1006(4) 1.1716(4) 0.107(2) Uani 1 1 d . . .
O4 O 0.9286(5) 0.2768(4) 1.1887(4) 0.1070(19) Uani 1 1 d . . .
O5 O 1.0307(8) 0.1952(5) 1.2907(7) 0.222(6) Uani 1 1 d . . .
O6 O 0.8142(9) 0.2126(5) 1.3020(5) 0.173(4) Uani 1 1 d . . .
O81 O 0.3484(13) 0.3607(8) 0.4746(9) 0.131(5) Uani 0.50 1 d P . .
C82 C 0.245(3) 0.3594(12) 0.5154(11) 0.170(13) Uani 0.50 1 d P . .
H82A H 0.2657 0.3645 0.5760 0.204 Uiso 0.50 1 calc PR . .
H82B H 0.1800 0.3051 0.4908 0.204 Uiso 0.50 1 calc PR . .
C83 C 0.2127(14) 0.4402(12) 0.4969(14) 0.114(7) Uani 0.50 1 d P . .
H83A H 0.1381 0.4432 0.5109 0.136 Uiso 0.50 1 calc PR . .
H83B H 0.2747 0.4961 0.5213 0.136 Uiso 0.50 1 calc PR . .
C84 C 0.2067(13) 0.4121(11) 0.4212(12) 0.086(5) Uani 0.50 1 d P . .
H84A H 0.2076 0.4610 0.3935 0.103 Uiso 0.50 1 calc PR . .
H84B H 0.1303 0.3675 0.3992 0.103 Uiso 0.50 1 calc PR . .
C85 C 0.2932(12) 0.3743(10) 0.3946(8) 0.075(4) Uani 0.50 1 d P . .
H85A H 0.3493 0.4149 0.3715 0.090 Uiso 0.50 1 calc PR . .
H85B H 0.2572 0.3185 0.3529 0.090 Uiso 0.50 1 calc PR . .
O91 O 0.6376(9) 0.4241(8) 1.2384(9) 0.202(4) Uani 1 1 d . . .
C92 C 0.6387(15) 0.3360(9) 1.2179(9) 0.179(7) Uani 1 1 d . B .
H92A H 0.5935 0.3073 1.1609 0.215 Uiso 1 1 calc R . .
H92B H 0.7190 0.3348 1.2196 0.215 Uiso 1 1 calc R . .
C93 C 0.593(3) 0.2935(17) 1.2721(14) 0.288(19) Uani 1 1 d . . .
H93A H 0.6437 0.2616 1.2939 0.346 Uiso 1 1 calc R A 1
H93B H 0.5164 0.2509 1.2450 0.346 Uiso 1 1 calc R A 1
C94 C 0.581(5) 0.357(3) 1.3383(17) 0.23(2) Uani 0.62(4) 1 d P B 1
H94A H 0.6463 0.3725 1.3862 0.274 Uiso 0.62(4) 1 calc PR B 1
H94B H 0.5079 0.3349 1.3570 0.274 Uiso 0.62(4) 1 calc PR B 1
C95 C 0.582(2) 0.4371(16) 1.3010(10) 0.099(8) Uani 0.62(4) 1 d P B 1
H95A H 0.5021 0.4371 1.2801 0.119 Uiso 0.62(4) 1 calc PR B 1
H95B H 0.6238 0.4925 1.3421 0.119 Uiso 0.62(4) 1 calc PR B 1
C94A C 0.542(4) 0.308(3) 1.296(2) 0.16(3) Uani 0.38(4) 1 d P B 2
H94C H 0.5352 0.2831 1.3455 0.189 Uiso 0.38(4) 1 calc PR B 2
H94D H 0.4657 0.2851 1.2573 0.189 Uiso 0.38(4) 1 calc PR B 2
C95A C 0.575(6) 0.4047(19) 1.321(4) 0.18(3) Uani 0.38(4) 1 d P B 2
H95C H 0.6307 0.4288 1.3749 0.217 Uiso 0.38(4) 1 calc PR B 2
H95D H 0.5074 0.4261 1.3227 0.217 Uiso 0.38(4) 1 calc PR B 2
O101 O 0.3014(10) 0.3260(14) 0.0175(7) 0.313(10) Uani 1 1 d . . .
C102 C 0.3577(10) 0.3294(15) 0.0898(9) 0.255(12) Uani 1 1 d . . .
H10A H 0.4240 0.3837 0.1072 0.306 Uiso 1 1 calc R . .
H10B H 0.3887 0.2795 0.0866 0.306 Uiso 1 1 calc R . .
C103 C 0.2881(14) 0.327(2) 0.1489(12) 0.36(2) Uani 1 1 d . . .
H10C H 0.2956 0.2814 0.1789 0.428 Uiso 1 1 calc R . .
H10D H 0.3163 0.3838 0.1900 0.428 Uiso 1 1 calc R . .
C104 C 0.1897(14) 0.3134(13) 0.1201(11) 0.204(8) Uani 1 1 d . . .
H10E H 0.1524 0.3466 0.1566 0.245 Uiso 1 1 calc R . .
H10F H 0.1460 0.2505 0.1074 0.245 Uiso 1 1 calc R . .
C105 C 0.2037(16) 0.3471(15) 0.0415(9) 0.249(11) Uani 1 1 d . . .
H10G H 0.1337 0.3183 -0.0028 0.298 Uiso 1 1 calc R . .
H10H H 0.2176 0.4109 0.0528 0.298 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'
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'
Tc Tc -1.4390 0.7593 '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'
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
O2 Tc1 O1 179.75(13) . . ?
O2 Tc1 C61 89.53(12) . . ?
O1 Tc1 C61 90.52(12) . . ?
O2 Tc1 C41 89.58(13) . . ?
O1 Tc1 C41 90.67(12) . . ?
C61 Tc1 C41 90.33(13) . . ?
O2 Tc1 C1 89.41(13) . . ?
O1 Tc1 C1 90.35(12) . . ?
C61 Tc1 C1 89.77(13) . . ?
C41 Tc1 C1 178.98(14) . . ?
O2 Tc1 C21 89.99(13) . . ?
O1 Tc1 C21 89.96(12) . . ?
C61 Tc1 C21 179.41(13) . . ?
C41 Tc1 C21 90.00(13) . . ?
C1 Tc1 C21 89.89(13) . . ?
N5 C1 N2 104.1(3) . . ?
N5 C1 Tc1 128.1(3) . . ?
N2 C1 Tc1 127.7(3) . . ?
C1 N2 C3 111.1(3) . . ?
C1 N2 C8 123.1(3) . . ?
C3 N2 C8 125.8(3) . . ?
C4 C3 N2 107.1(3) . . ?
C4 C3 C6 128.1(4) . . ?
N2 C3 C6 124.9(4) . . ?
C3 C4 N5 106.5(3) . . ?
C3 C4 C7 128.2(4) . . ?
N5 C4 C7 125.2(4) . . ?
C1 N5 C4 111.1(3) . . ?
C1 N5 C11 123.8(3) . . ?
C4 N5 C11 125.1(3) . . ?
N2 C8 C9 112.3(3) . . ?
N2 C8 C10 112.4(3) . . ?
C9 C8 C10 112.3(3) . . ?
N5 C11 C12 112.0(4) . . ?
N5 C11 C13 112.6(4) . . ?
C12 C11 C13 113.2(4) . . ?
N25 C21 N22 104.4(3) . . ?
N25 C21 Tc1 127.8(3) . . ?
N22 C21 Tc1 127.8(3) . . ?
C21 N22 C23 110.6(3) . . ?
C21 N22 C28 123.9(3) . . ?
C23 N22 C28 125.6(3) . . ?
C24 C23 N22 107.0(3) . . ?
C24 C23 C26 127.9(4) . . ?
N22 C23 C26 125.1(4) . . ?
C23 C24 N25 106.9(3) . . ?
C23 C24 C27 127.2(4) . . ?
N25 C24 C27 126.0(4) . . ?
C21 N25 C24 111.2(3) . . ?
C21 N25 C31 123.4(3) . . ?
C24 N25 C31 125.5(3) . . ?
N22 C28 C29 112.7(4) . . ?
N22 C28 C30 112.2(4) . . ?
C29 C28 C30 113.3(4) . . ?
N25 C31 C32 112.5(3) . . ?
N25 C31 C33 112.1(3) . . ?
C32 C31 C33 113.1(3) . . ?
N42 C41 N45 104.2(3) . . ?
N42 C41 Tc1 128.2(2) . . ?
N45 C41 Tc1 127.6(3) . . ?
C41 N42 C43 111.3(3) . . ?
C41 N42 C48 123.6(3) . . ?
C43 N42 C48 125.2(3) . . ?
C44 C43 N42 106.8(3) . . ?
C44 C43 C46 128.1(4) . . ?
N42 C43 C46 125.1(4) . . ?
C43 C44 N45 106.9(3) . . ?
C43 C44 C47 127.7(4) . . ?
N45 C44 C47 125.4(4) . . ?
C41 N45 C44 110.8(3) . . ?
C41 N45 C51 123.9(3) . . ?
C44 N45 C51 125.2(3) . . ?
N42 C48 C50 112.6(3) . . ?
N42 C48 C49 111.8(3) . . ?
C50 C48 C49 112.3(3) . . ?
N45 C51 C52 112.9(4) . . ?
N45 C51 C53 111.9(4) . . ?
C52 C51 C53 112.7(3) . . ?
N65 C61 N62 103.9(3) . . ?
N65 C61 Tc1 128.5(2) . . ?
N62 C61 Tc1 127.5(3) . . ?
C61 N62 C63 111.3(3) . . ?
C61 N62 C68 123.7(3) . . ?
C63 N62 C68 124.9(3) . . ?
C64 C63 N62 106.4(3) . . ?
C64 C63 C66 126.9(4) . . ?
N62 C63 C66 126.4(4) . . ?
C63 C64 N65 107.3(3) . . ?
C63 C64 C67 127.2(4) . . ?
N65 C64 C67 125.4(4) . . ?
C61 N65 C64 111.0(3) . . ?
C61 N65 C71 123.4(3) . . ?
C64 N65 C71 125.6(3) . . ?
N62 C68 C69 112.3(4) . . ?
N62 C68 C70 112.6(3) . . ?
C69 C68 C70 113.1(4) . . ?
N65 C71 C72 112.9(3) . . ?
N65 C71 C73 111.1(3) . . ?
C72 C71 C73 113.1(3) . . ?
O5 Tc2 O4 110.0(4) . . ?
O5 Tc2 O3 109.4(4) . . ?
O4 Tc2 O3 109.9(3) . . ?
O5 Tc2 O6 112.9(6) . . ?
O4 Tc2 O6 107.6(4) . . ?
O3 Tc2 O6 107.0(4) . . ?
C85 O81 C82 94.5(13) . . ?
O81 C82 C83 103.5(11) . . ?
O81 C82 C84 79.7(8) . . ?
C83 C82 C84 39.1(9) . . ?
C84 C83 C82 89.5(12) . . ?
C83 C84 C85 119.8(15) . . ?
C83 C84 C82 51.4(11) . . ?
C85 C84 C82 78.7(11) . . ?
C84 C85 O81 101.2(12) . . ?
C95 O91 C92 111.6(13) . . ?
C95 O91 C95A 21.4(17) . . ?
C92 O91 C95A 90.9(14) . . ?
C93 C92 O91 109.2(12) . . ?
C94A C93 C92 121(4) . . ?
C94A C93 C94 39(3) . . ?
C92 C93 C94 107(2) . . ?
C93 C94 C95 105.1(16) . . ?
O91 C95 C94 101.1(15) . . ?
C93 C94A C95A 109(4) . . ?
C94A C95A O91 96(3) . . ?
C102 O101 C105 99.1(12) . . ?
O101 C102 C103 111.7(13) . . ?
C104 C103 C102 113.3(17) . . ?
C103 C104 C105 98.8(15) . . ?
O101 C105 C104 105.1(11) . . ?
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
Tc1 O2 1.760(3) . ?
Tc1 O1 1.765(2) . ?
Tc1 C61 2.220(3) . ?
Tc1 C41 2.226(4) . ?
Tc1 C1 2.227(4) . ?
Tc1 C21 2.232(3) . ?
C1 N5 1.360(5) . ?
C1 N2 1.372(5) . ?
N2 C3 1.391(5) . ?
N2 C8 1.484(5) . ?
C3 C4 1.346(6) . ?
C3 C6 1.504(6) . ?
C4 N5 1.404(5) . ?
C4 C7 1.490(6) . ?
N5 C11 1.484(5) . ?
C8 C9 1.514(6) . ?
C8 C10 1.524(5) . ?
C11 C12 1.523(6) . ?
C11 C13 1.526(6) . ?
C21 N25 1.363(5) . ?
C21 N22 1.370(5) . ?
N22 C23 1.405(5) . ?
N22 C28 1.475(5) . ?
C23 C24 1.345(6) . ?
C23 C26 1.512(6) . ?
C24 N25 1.398(5) . ?
C24 C27 1.514(6) . ?
N25 C31 1.484(5) . ?
C28 C29 1.519(6) . ?
C28 C30 1.522(6) . ?
C31 C32 1.520(6) . ?
C31 C33 1.529(6) . ?
C41 N42 1.362(5) . ?
C41 N45 1.368(5) . ?
N42 C43 1.397(5) . ?
N42 C48 1.482(5) . ?
C43 C44 1.343(6) . ?
C43 C46 1.498(6) . ?
C44 N45 1.401(5) . ?
C44 C47 1.511(6) . ?
N45 C51 1.477(5) . ?
C48 C50 1.524(5) . ?
C48 C49 1.526(5) . ?
C51 C52 1.519(6) . ?
C51 C53 1.530(6) . ?
C61 N65 1.368(5) . ?
C61 N62 1.372(4) . ?
N62 C63 1.405(5) . ?
N62 C68 1.475(5) . ?
C63 C64 1.343(6) . ?
C63 C66 1.492(6) . ?
C64 N65 1.401(5) . ?
C64 C67 1.506(6) . ?
N65 C71 1.481(5) . ?
C68 C69 1.524(6) . ?
C68 C70 1.533(6) . ?
C71 C72 1.523(5) . ?
C71 C73 1.531(6) . ?
Tc2 O5 1.657(6) . ?
Tc2 O4 1.661(5) . ?
Tc2 O3 1.680(5) . ?
Tc2 O6 1.687(7) . ?
O81 C85 1.492(17) . ?
O81 C82 1.53(3) . ?
C82 C83 1.55(3) . ?
C82 C84 1.98(3) . ?
C83 C84 1.25(2) . ?
C84 C85 1.454(19) . ?
O91 C95 1.35(2) . ?
O91 C92 1.429(14) . ?
O91 C95A 1.71(5) . ?
C92 C93 1.331(19) . ?
C93 C94A 0.86(7) . ?
C93 C94 1.43(3) . ?
C94 C95 1.55(3) . ?
C94A C95A 1.49(5) . ?
O101 C102 1.286(15) . ?
O101 C105 1.429(15) . ?
C102 C103 1.395(18) . ?
C103 C104 1.180(18) . ?
C104 C105 1.524(17) . ?
