#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:18:23 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/96/7049670.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_7049670
loop_
_publ_author_name
'Arumugam, Ramar'
'Shankar, Bhaskaran'
'Soumya, K. R.'
'Sathiyendiran, Malaichamy'
_publ_section_title
;
 fac-Re(CO)₃-based neutral heteroleptic tetrahedrons.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7425
_journal_page_last               7431
_journal_paper_doi               10.1039/c8dt05065a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C156 H116 N16 O28 Re4'
_chemical_formula_sum            'C156 H116 N16 O28 Re4'
_chemical_formula_weight         3407.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-06 deposited with the CCDC.    2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.942(2)
_cell_length_b                   23.014(2)
_cell_length_c                   34.149(3)
_cell_measurement_reflns_used    9620
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.35
_cell_volume                     16458(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1776
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            120616
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.219
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Greenish yellow'
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       Block
_exptl_crystal_F_000             6752
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.560
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         15593
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0547P)²+120.9868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10085
_reflns_number_total             15593
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt05065a2.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
'Adding full bibliography for 7049668--7049673.cif.'
_cod_database_code               7049670
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.817
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
C1 C 0.4936(5) 0.5979(4) 0.5672(3) 0.039(3) Uani 1 1 d . . . . .
C2 C 0.5572(5) 0.5844(5) 0.5712(3) 0.045(3) Uani 1 1 d . . . . .
H2 H 0.570613 0.546000 0.569699 0.054 Uiso 1 1 calc R U . . .
C3 C 0.6011(5) 0.6284(4) 0.5776(3) 0.041(3) Uani 1 1 d . . . . .
H3 H 0.644046 0.619585 0.581207 0.049 Uiso 1 1 calc R U . . .
C4 C 0.5808(5) 0.6850(4) 0.5786(3) 0.037(2) Uani 1 1 d . . . . .
C5 C 0.5169(5) 0.6984(5) 0.5718(3) 0.041(3) Uani 1 1 d . . . . .
H5 H 0.503929 0.737054 0.570822 0.049 Uiso 1 1 calc R U . . .
C6 C 0.4726(5) 0.6547(4) 0.5664(3) 0.038(3) Uani 1 1 d . . . . .
H6 H 0.429750 0.663311 0.562291 0.046 Uiso 1 1 calc R U . . .
C7 C 0.4100(5) 0.5410(5) 0.5308(3) 0.038(2) Uani 1 1 d . . . . .
C8 C 0.4039(6) 0.5730(5) 0.4966(3) 0.054(3) Uani 1 1 d . . . . .
H8 H 0.427003 0.606846 0.492240 0.065 Uiso 1 1 calc R U . . .
C9 C 0.3614(7) 0.5513(6) 0.4696(4) 0.062(4) Uani 1 1 d . . . . .
H9 H 0.355100 0.571473 0.446308 0.075 Uiso 1 1 calc R U . . .
C10 C 0.3276(6) 0.5000(6) 0.4759(3) 0.059(3) Uani 1 1 d . . . . .
H10 H 0.298690 0.487406 0.457042 0.071 Uiso 1 1 calc R U . . .
C11 C 0.3359(5) 0.4676(5) 0.5094(3) 0.049(3) Uani 1 1 d . . . . .
H11 H 0.313817 0.433059 0.513414 0.059 Uiso 1 1 calc R U . . .
C12 C 0.3784(5) 0.4887(5) 0.5368(3) 0.040(3) Uani 1 1 d . . . . .
C13 C 0.4380(4) 0.5047(4) 0.5891(3) 0.032(2) Uani 1 1 d . . . . .
C14 C 0.4678(5) 0.5000(4) 0.6271(3) 0.036(2) Uani 1 1 d . . . . .
C15 C 0.4816(5) 0.5496(5) 0.6497(3) 0.041(3) Uani 1 1 d . . . . .
H15 H 0.469187 0.585940 0.640640 0.049 Uiso 1 1 calc R U . . .
C16 C 0.5129(5) 0.5454(6) 0.6847(3) 0.052(3) Uani 1 1 d . . . . .
H16 H 0.521866 0.578556 0.699220 0.062 Uiso 1 1 calc R U . . .
C17 C 0.5312(6) 0.4909(6) 0.6984(4) 0.064(4) Uani 1 1 d . . . . .
H17 H 0.553679 0.487740 0.721742 0.077 Uiso 1 1 calc R U . . .
C18 C 0.5165(5) 0.4430(5) 0.6780(3) 0.051(3) Uani 1 1 d . . . . .
H18 H 0.529113 0.407086 0.687714 0.062 Uiso 1 1 calc R U . . .
C19 C 0.4827(5) 0.4449(5) 0.6425(3) 0.041(3) Uani 1 1 d . . . . .
C20 C 0.2974(7) 0.3649(5) 0.5749(4) 0.061(4) Uani 1 1 d . . . . .
C21 C 0.4186(6) 0.3454(5) 0.5507(3) 0.054(3) Uani 1 1 d . . . . .
C22 C 0.3710(7) 0.3035(6) 0.6179(4) 0.074(4) Uani 1 1 d . . . . .
C23 C 0.5773(5) 0.7745(4) 0.6469(3) 0.041(3) Uani 1 1 d . . . . .
C24 C 0.5492(5) 0.7230(5) 0.6607(3) 0.047(3) Uani 1 1 d . . . . .
H24 H 0.563486 0.687368 0.651240 0.056 Uiso 1 1 calc R U . . .
C25 C 0.5007(6) 0.7244(6) 0.6879(4) 0.064(4) Uani 1 1 d . . . . .
H25 H 0.481872 0.690044 0.696395 0.076 Uiso 1 1 calc R U . . .
C26 C 0.4797(6) 0.7776(6) 0.7028(4) 0.064(4) Uani 1 1 d . . . . .
H26 H 0.446183 0.779083 0.720659 0.077 Uiso 1 1 calc R U . . .
C27 C 0.5090(6) 0.8269(6) 0.6910(4) 0.060(3) Uani 1 1 d . . . . .
H27 H 0.495437 0.861922 0.701753 0.072 Uiso 1 1 calc R U . . .
C28 C 0.5585(5) 0.8285(5) 0.6634(3) 0.037(2) Uani 1 1 d . . . . .
C29 C 0.6229(5) 0.7734(4) 0.6147(3) 0.035(2) Uani 1 1 d . . . . .
C30 C 0.7043(5) 0.7944(5) 0.5765(3) 0.041(3) Uani 1 1 d . . . . .
C31 C 0.6769(5) 0.7429(5) 0.5623(3) 0.043(3) Uani 1 1 d . . . . .
C32 C 0.7019(6) 0.7142(5) 0.5302(3) 0.059(3) Uani 1 1 d . . . . .
H32 H 0.683572 0.680039 0.521006 0.070 Uiso 1 1 calc R U . . .
C33 C 0.7548(7) 0.7380(6) 0.5124(4) 0.076(4) Uani 1 1 d . . . . .
H33 H 0.773562 0.719018 0.491268 0.092 Uiso 1 1 calc R U . . .
C34 C 0.7804(7) 0.7903(6) 0.5257(4) 0.078(5) Uani 1 1 d . . . . .
H34 H 0.814977 0.806476 0.512594 0.093 Uiso 1 1 calc R U . . .
C35 C 0.7559(6) 0.8186(5) 0.5578(3) 0.060(4) Uani 1 1 d . . . . .
H35 H 0.773678 0.853274 0.566577 0.072 Uiso 1 1 calc R U . . .
C36 C 0.7721(6) 0.9070(5) 0.6335(3) 0.049(3) Uani 1 1 d . . . . .
C37 C 0.6659(7) 0.9380(5) 0.5941(4) 0.071(4) Uani 1 1 d . . . . .
C38 C 0.6838(6) 0.9657(5) 0.6700(3) 0.049(3) Uani 1 1 d . . . . .
C39 C 0.3678(7) 0.9080(6) 0.7158(5) 0.073(4) Uani 1 1 d . . . . .
H39 H 0.394034 0.937652 0.706572 0.087 Uiso 1 1 calc R U . . .
C40 C 0.3367(8) 0.8717(7) 0.6891(4) 0.080(5) Uani 1 1 d . . . . .
H40 H 0.341583 0.878895 0.662446 0.096 Uiso 1 1 calc R U . . .
C41 C 0.2995(7) 0.8263(6) 0.7004(4) 0.071(4) Uani 1 1 d . . . . .
H41 H 0.280324 0.801465 0.682458 0.085 Uiso 1 1 calc R U . . .
C42 C 0.2920(5) 0.8193(5) 0.7414(3) 0.043(3) Uani 1 1 d . . . . .
C43 C 0.3199(5) 0.8564(5) 0.7680(3) 0.041(3) Uani 1 1 d . . . . .
C44 C 0.3603(6) 0.9005(5) 0.7552(3) 0.050(3) Uani 1 1 d . . . . .
H44 H 0.381500 0.924218 0.773045 0.061 Uiso 1 1 calc R U . . .
C45 C 0.2664(5) 0.7920(4) 0.8009(3) 0.037(2) Uani 1 1 d . . . . .
C46 C 0.2373(5) 0.7530(4) 0.8316(3) 0.039(3) Uani 1 1 d . . . . .
C47 C 0.1821(6) 0.7682(5) 0.8508(3) 0.055(3) Uani 1 1 d . . . . .
H47 H 0.162952 0.804119 0.846568 0.065 Uiso 1 1 calc R U . . .
C48 C 0.2658(5) 0.6989(4) 0.8369(3) 0.044(3) Uani 1 1 d . . . . .
H48 H 0.302849 0.689306 0.823321 0.053 Uiso 1 1 calc R U . . .
C49 C 0.2387(5) 0.6600(5) 0.8624(3) 0.048(3) Uani 1 1 d . . . . .
C50 C 0.1825(6) 0.6746(5) 0.8823(4) 0.063(4) Uani 1 1 d . . . . .
C51 C 0.1556(6) 0.7283(6) 0.8769(4) 0.068(4) Uani 1 1 d . . . . .
C52 C 0.0699(8) 0.7932(7) 0.8929(6) 0.127(8) Uani 1 1 d . . . . .
H52A H 0.032685 0.794915 0.909287 0.191 Uiso 1 1 calc R U . . .
H52B H 0.098548 0.824104 0.899848 0.191 Uiso 1 1 calc R U . . .
H52C H 0.057374 0.797435 0.865982 0.191 Uiso 1 1 calc R U . . .
C56 C 0.3093(6) 0.5828(5) 0.8421(4) 0.062(4) Uani 1 1 d . . . . .
H56A H 0.322379 0.544588 0.850058 0.094 Uiso 1 1 calc R U . . .
H56B H 0.290589 0.580829 0.816430 0.094 Uiso 1 1 calc R U . . .
H56C H 0.345746 0.608037 0.841472 0.094 Uiso 1 1 calc R U . . .
C57 C 0.2236(6) 0.7283(5) 0.7460(3) 0.054(3) Uani 1 1 d . . . . .
H57A H 0.203664 0.739276 0.721490 0.065 Uiso 1 1 calc R U . . .
H57B H 0.190158 0.716725 0.764047 0.065 Uiso 1 1 calc R U . . .
C58 C 0.2676(5) 0.6776(4) 0.7391(3) 0.039(3) Uani 1 1 d . . . . .
C59 C 0.2405(5) 0.6256(5) 0.7273(3) 0.046(3) Uani 1 1 d . . . . .
H59 H 0.196468 0.623323 0.724201 0.056 Uiso 1 1 calc R U . . .
C60 C 0.2784(5) 0.5760(5) 0.7200(3) 0.042(3) Uani 1 1 d . . . . .
C61 C 0.3434(6) 0.5779(5) 0.7257(3) 0.044(3) Uani 1 1 d . . . . .
H61 H 0.368319 0.545033 0.721407 0.052 Uiso 1 1 calc R U . . .
C62 C 0.3712(6) 0.6297(5) 0.7379(3) 0.049(3) Uani 1 1 d . . . . .
H62 H 0.415173 0.631528 0.741364 0.059 Uiso 1 1 calc R U . . .
C63 C 0.3346(5) 0.6785(5) 0.7449(3) 0.047(3) Uani 1 1 d . . . . .
H63 H 0.354163 0.712371 0.753617 0.056 Uiso 1 1 calc R U . . .
C64 C 0.2430(6) 0.5210(5) 0.7069(4) 0.055(3) Uani 1 1 d . . . . .
H64A H 0.219621 0.505226 0.729057 0.066 Uiso 1 1 calc R U . . .
H64B H 0.212200 0.531219 0.686869 0.066 Uiso 1 1 calc R U . . .
C65 C 0.3190(6) 0.4258(6) 0.7544(3) 0.061(4) Uani 1 1 d . . . . .
H65 H 0.295609 0.448303 0.771923 0.073 Uiso 1 1 calc R U . . .
C66 C 0.3581(7) 0.3804(7) 0.7671(4) 0.071(4) Uani 1 1 d . . . . .
H66 H 0.361689 0.373047 0.793803 0.085 Uiso 1 1 calc R U . . .
C67 C 0.3911(7) 0.3468(6) 0.7415(4) 0.071(4) Uani 1 1 d . . . . .
H67 H 0.415591 0.316236 0.751110 0.086 Uiso 1 1 calc R U . . .
C69 C 0.3895(6) 0.3566(5) 0.7014(3) 0.054(3) Uani 1 1 d . . . . .
H69 H 0.413669 0.333917 0.684398 0.065 Uiso 1 1 calc R U . . .
C70 C 0.3508(5) 0.4013(4) 0.6872(3) 0.041(3) Uani 1 1 d . . . . .
C71 C 0.3166(5) 0.4356(5) 0.7140(3) 0.046(3) Uani 1 1 d . . . . .
C72 C 0.3012(5) 0.4671(5) 0.6535(3) 0.037(3) Uani 1 1 d . . . . .
C73 C 0.2785(5) 0.5073(4) 0.6226(3) 0.042(3) Uani 1 1 d . . . . .
C75 C 0.2316(6) 0.4927(6) 0.5957(4) 0.062(3) Uani 1 1 d . . . . .
H75 H 0.212969 0.456023 0.596037 0.075 Uiso 1 1 calc R U . . .
C76 C 0.2136(7) 0.5328(7) 0.5688(4) 0.074(4) Uani 1 1 d . . . . .
C77 C 0.2390(8) 0.5893(6) 0.5690(4) 0.073(4) Uani 1 1 d . . . . .
C78 C 0.2851(6) 0.6045(5) 0.5961(4) 0.059(3) Uani 1 1 d . . . . .
C79 C 0.3040(5) 0.5622(5) 0.6230(3) 0.046(3) Uani 1 1 d . . . . .
H79 H 0.334797 0.571464 0.641577 0.055 Uiso 1 1 calc R U . . .
C80 C 0.3302(11) 0.6845(7) 0.6282(5) 0.136(8) Uani 1 1 d . . . . .
H80A H 0.345719 0.722903 0.622872 0.204 Uiso 1 1 calc R U . . .
H80B H 0.295564 0.686650 0.646631 0.204 Uiso 1 1 calc R U . . .
H80C H 0.363993 0.661392 0.639103 0.204 Uiso 1 1 calc R U . . .
C81 C 0.1714(12) 0.6637(12) 0.5491(9) 0.213(15) Uani 1 1 d . . . . .
H81A H 0.163223 0.689838 0.527798 0.319 Uiso 1 1 calc R U . . .
H81B H 0.134457 0.639915 0.553572 0.319 Uiso 1 1 calc R U . . .
H81C H 0.180687 0.685677 0.572350 0.319 Uiso 1 1 calc R U . . .
C82 C 0.1401(10) 0.4711(9) 0.5361(6) 0.139(8) Uani 1 1 d . . . . .
H82A H 0.109798 0.472308 0.515058 0.208 Uiso 1 1 calc R U . . .
H82B H 0.172220 0.442512 0.530514 0.208 Uiso 1 1 calc R U . . .
H82C H 0.118589 0.461030 0.560009 0.208 Uiso 1 1 calc R U . . .
N1 N 0.3972(4) 0.4667(3) 0.5733(2) 0.035(2) Uani 1 1 d . . . . .
N2 N 0.4482(4) 0.5507(4) 0.5638(2) 0.036(2) Uani 1 1 d . . . . .
N3 N 0.6257(4) 0.7301(3) 0.5866(2) 0.037(2) Uani 1 1 d . . . . .
N4 N 0.6692(4) 0.8121(3) 0.6092(2) 0.038(2) Uani 1 1 d . . . . .
N5 N 0.3021(4) 0.8388(3) 0.8057(2) 0.035(2) Uani 1 1 d . . . . .
N6 N 0.2579(5) 0.7785(4) 0.7622(3) 0.047(2) Uani 1 1 d . . . . .
N7 N 0.2861(5) 0.4762(4) 0.6916(3) 0.047(2) Uani 1 1 d . . . . .
N8 N 0.3399(4) 0.4211(4) 0.6498(2) 0.037(2) Uani 1 1 d . . . . .
O1 O 0.6854(5) 1.0094(4) 0.6861(3) 0.082(3) Uani 1 1 d . . . . .
O2 O 0.8247(4) 0.9175(4) 0.6301(2) 0.068(3) Uani 1 1 d . . . . .
O3 O 0.6572(7) 0.9655(5) 0.5671(3) 0.111(4) Uani 1 1 d . . . . .
O4 O 0.5841(3) 0.8788(3) 0.6546(2) 0.0483(19) Uani 1 1 d . . . . .
O5 O 0.2473(5) 0.3542(5) 0.5624(3) 0.094(4) Uani 1 1 d . . . . .
O6 O 0.4427(5) 0.3253(5) 0.5242(3) 0.090(3) Uani 1 1 d . . . . .
O7 O 0.3624(8) 0.2556(4) 0.6293(4) 0.136(5) Uani 1 1 d . . . . .
O8 O 0.4676(3) 0.3955(3) 0.6250(2) 0.0450(18) Uani 1 1 d . . . . .
O9 O 0.1010(5) 0.7388(5) 0.8981(3) 0.100(4) Uani 1 1 d . . . . .
C55 C 0.1710(15) 0.6179(17) 0.9347(8) 0.093(8) Uani 0.54(2) 1 d D U P A 1
H55A H 0.143698 0.588549 0.945657 0.139 Uiso 0.54(2) 1 calc R U P A 1
H55B H 0.213325 0.602507 0.931666 0.139 Uiso 0.54(2) 1 calc R U P A 1
H55C H 0.172247 0.650815 0.951987 0.139 Uiso 0.54(2) 1 calc R U P A 1
O10 O 0.1497(15) 0.6333(12) 0.9018(8) 0.083(7) Uani 0.54(2) 1 d D U P A 1
C55' C 0.1281(19) 0.6057(18) 0.8988(11) 0.101(10) Uani 0.46(2) 1 d D U P A 2
H55D H 0.108867 0.580240 0.917626 0.152 Uiso 0.46(2) 1 calc R U P A 2
H55E H 0.095299 0.624085 0.883492 0.152 Uiso 0.46(2) 1 calc R U P A 2
H55F H 0.155560 0.583748 0.881822 0.152 Uiso 0.46(2) 1 calc R U P A 2
O10' O 0.1602(15) 0.6438(10) 0.9162(9) 0.076(7) Uani 0.46(2) 1 d D U P A 2
O11 O 0.2635(4) 0.6048(3) 0.8691(2) 0.062(2) Uani 1 1 d . . . . .
O12 O 0.3089(5) 0.6593(4) 0.5939(3) 0.082(3) Uani 1 1 d . . . . .
O13 O 0.2223(6) 0.6293(5) 0.5402(3) 0.108(4) Uani 1 1 d . . . . .
O14 O 0.1676(7) 0.5232(6) 0.5401(4) 0.125(5) Uani 1 1 d . . . . .
Re1 Re 0.68172(2) 0.89352(2) 0.64134(2) 0.04130(14) Uani 1 1 d . . . . .
Re2 Re 0.37949(2) 0.37920(2) 0.59652(2) 0.04156(14) Uani 1 1 d . . . . .
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'
Re Re -1.0185 7.2310 '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_3
C2 C1 C6 121.6(9) .
C2 C1 N2 118.4(10) .
C6 C1 N2 120.0(9) .
C1 C2 C3 119.7(10) .
C1 C2 H2 120.2 .
C3 C2 H2 120.2 .
C4 C3 C2 119.5(10) .
C4 C3 H3 120.3 .
C2 C3 H3 120.3 .
C3 C4 C5 120.3(9) .
C3 C4 N3 119.4(10) .
C5 C4 N3 120.3(9) .
C6 C5 C4 120.4(10) .
C6 C5 H5 119.8 .
C4 C5 H5 119.8 .
C1 C6 C5 118.3(9) .
C1 C6 H6 120.8 .
C5 C6 H6 120.8 .
C8 C7 C12 122.8(10) .
C8 C7 N2 130.3(10) .
C12 C7 N2 106.8(9) .
C9 C8 C7 115.6(11) .
C9 C8 H8 122.2 .
C7 C8 H8 122.2 .
C8 C9 C10 122.1(11) .
C8 C9 H9 118.9 .
C10 C9 H9 118.9 .
C11 C10 C9 121.5(11) .
C11 C10 H10 119.2 .
C9 C10 H10 119.2 .
C10 C11 C12 117.1(11) .
C10 C11 H11 121.5 .
C12 C11 H11 121.5 .
C11 C12 C7 120.7(10) .
C11 C12 N1 131.1(10) .
C7 C12 N1 108.1(9) .
N1 C13 N2 110.3(8) .
N1 C13 C14 126.1(9) .
N2 C13 C14 123.6(8) .
C15 C14 C19 118.7(9) .
C15 C14 C13 121.4(9) .
C19 C14 C13 119.9(9) .
C16 C15 C14 121.4(11) .
C16 C15 H15 119.3 .
C14 C15 H15 119.3 .
C15 C16 C17 119.3(11) .
C15 C16 H16 120.4 .
C17 C16 H16 120.4 .
C18 C17 C16 120.2(11) .
C18 C17 H17 119.9 .
C16 C17 H17 119.9 .
C17 C18 C19 122.6(12) .
C17 C18 H18 118.7 .
C19 C18 H18 118.7 .
O8 C19 C18 118.9(10) .
O8 C19 C14 123.6(9) .
C18 C19 C14 117.4(10) .
O5 C20 Re2 177.5(13) .
O6 C21 Re2 178.6(11) .
O7 C22 Re2 175.2(14) .
C24 C23 C28 119.3(9) .
C24 C23 C29 120.8(9) .
C28 C23 C29 119.8(9) .
C25 C24 C23 120.9(11) .
C25 C24 H24 119.5 .
C23 C24 H24 119.5 .
C24 C25 C26 120.0(12) .
C24 C25 H25 120.0 .
C26 C25 H25 120.0 .
C27 C26 C25 119.0(12) .
C27 C26 H26 120.5 .
C25 C26 H26 120.5 .
C26 C27 C28 124.0(11) .
C26 C27 H27 118.0 .
C28 C27 H27 118.0 .
O4 C28 C27 118.7(10) .
O4 C28 C23 124.5(9) .
C27 C28 C23 116.7(10) .
N4 C29 N3 110.5(8) .
N4 C29 C23 124.9(9) .
N3 C29 C23 124.4(9) .
C35 C30 N4 131.9(10) .
C35 C30 C31 120.4(10) .
N4 C30 C31 107.7(8) .
C32 C31 N3 131.6(10) .
C32 C31 C30 121.4(10) .
N3 C31 C30 106.9(9) .
C33 C32 C31 117.7(11) .
C33 C32 H32 121.1 .
C31 C32 H32 121.1 .
C32 C33 C34 120.5(11) .
C32 C33 H33 119.8 .
C34 C33 H33 119.8 .
C35 C34 C33 121.8(11) .
C35 C34 H34 119.1 .
C33 C34 H34 119.1 .
C30 C35 C34 118.2(11) .
C30 C35 H35 120.9 .
C34 C35 H35 120.9 .
O2 C36 Re1 176.4(11) .
O3 C37 Re1 177.9(12) .
O1 C38 Re1 178.0(10) .
C44 C39 C40 120.8(13) .
C44 C39 H39 119.6 .
C40 C39 H39 119.6 .
C41 C40 C39 122.7(13) .
C41 C40 H40 118.6 .
C39 C40 H40 118.6 .
C40 C41 C42 115.6(14) .
C40 C41 H41 122.2 .
C42 C41 H41 122.2 .
C43 C42 N6 107.5(9) .
C43 C42 C41 122.3(12) .
N6 C42 C41 130.2(12) .
C42 C43 C44 120.3(10) .
C42 C43 N5 108.4(9) .
C44 C43 N5 131.3(11) .
C39 C44 C43 118.1(13) .
C39 C44 H44 121.0 .
C43 C44 H44 121.0 .
N5 C45 N6 112.2(9) .
N5 C45 C46 128.8(9) .
N6 C45 C46 119.0(9) .
C47 C46 C48 121.8(10) .
C47 C46 C45 121.4(9) .
C48 C46 C45 116.6(9) .
C46 C47 C51 118.2(11) .
C46 C47 H47 120.9 .
C51 C47 H47 120.9 .
C49 C48 C46 119.2(10) .
C49 C48 H48 120.4 .
C46 C48 H48 120.4 .
C48 C49 O11 123.1(10) .
C48 C49 C50 120.0(10) .
O11 C49 C50 116.9(10) .
O10 C50 C51 119.4(18) .
O10 C50 C49 120.1(17) .
C51 C50 C49 119.7(11) .
C51 C50 O10' 114.7(16) .
C49 C50 O10' 123.2(16) .
C50 C51 O9 115.5(11) .
C50 C51 C47 121.1(12) .
O9 C51 C47 123.4(12) .
O9 C52 H52A 109.5 .
O9 C52 H52B 109.5 .
H52A C52 H52B 109.5 .
O9 C52 H52C 109.5 .
H52A C52 H52C 109.5 .
H52B C52 H52C 109.5 .
O11 C56 H56A 109.5 .
O11 C56 H56B 109.5 .
H56A C56 H56B 109.5 .
O11 C56 H56C 109.5 .
H56A C56 H56C 109.5 .
H56B C56 H56C 109.5 .
N6 C57 C58 111.7(9) .
N6 C57 H57A 109.3 .
C58 C57 H57A 109.3 .
N6 C57 H57B 109.3 .
C58 C57 H57B 109.3 .
H57A C57 H57B 107.9 .
C59 C58 C63 117.3(10) .
C59 C58 C57 117.7(10) .
C63 C58 C57 125.0(10) .
C58 C59 C60 121.3(10) .
C58 C59 H59 119.3 .
C60 C59 H59 119.3 .
C61 C60 C59 120.3(10) .
C61 C60 C64 123.1(10) .
C59 C60 C64 116.5(10) .
C60 C61 C62 118.9(10) .
C60 C61 H61 120.5 .
C62 C61 H61 120.5 .
C63 C62 C61 121.1(11) .
C63 C62 H62 119.4 .
C61 C62 H62 119.4 .
C62 C63 C58 120.9(10) .
C62 C63 H63 119.5 .
C58 C63 H63 119.5 .
N7 C64 C60 112.7(9) .
N7 C64 H64A 109.1 .
C60 C64 H64A 109.1 .
N7 C64 H64B 109.1 .
C60 C64 H64B 109.1 .
H64A C64 H64B 107.8 .
C66 C65 C71 116.6(13) .
C66 C65 H65 121.7 .
C71 C65 H65 121.7 .
C67 C66 C65 121.7(13) .
C67 C66 H66 119.2 .
C65 C66 H66 119.2 .
C66 C67 C69 122.1(14) .
C66 C67 H67 119.0 .
C69 C67 H67 119.0 .
C67 C69 C70 118.4(12) .
C67 C69 H69 120.8 .
C70 C69 H69 120.8 .
N8 C70 C69 131.5(10) .
N8 C70 C71 109.5(9) .
C69 C70 C71 118.9(11) .
N7 C71 C65 132.8(12) .
N7 C71 C70 105.0(9) .
C65 C71 C70 122.3(12) .
N8 C72 N7 110.8(9) .
N8 C72 C73 128.4(9) .
N7 C72 C73 120.7(9) .
C79 C73 C75 120.3(11) .
C79 C73 C72 116.4(10) .
C75 C73 C72 123.2(10) .
C76 C75 C73 118.8(12) .
C76 C75 H75 120.6 .
C73 C75 H75 120.6 .
C75 C76 O14 124.3(14) .
C75 C76 C77 121.4(13) .
O14 C76 C77 114.3(14) .
C78 C77 O13 118.8(13) .
C78 C77 C76 120.2(12) .
O13 C77 C76 120.9(14) .
O12 C78 C77 117.0(12) .
O12 C78 C79 125.6(12) .
C77 C78 C79 117.5(12) .
C73 C79 C78 121.8(11) .
C73 C79 H79 119.1 .
C78 C79 H79 119.1 .
O12 C80 H80A 109.5 .
O12 C80 H80B 109.5 .
H80A C80 H80B 109.5 .
O12 C80 H80C 109.5 .
H80A C80 H80C 109.5 .
H80B C80 H80C 109.5 .
O13 C81 H81A 109.5 .
O13 C81 H81B 109.5 .
H81A C81 H81B 109.5 .
O13 C81 H81C 109.5 .
H81A C81 H81C 109.5 .
H81B C81 H81C 109.5 .
O14 C82 H82A 109.5 .
O14 C82 H82B 109.5 .
H82A C82 H82B 109.5 .
O14 C82 H82C 109.5 .
H82A C82 H82C 109.5 .
H82B C82 H82C 109.5 .
C13 N1 C12 107.6(8) .
C13 N1 Re2 124.3(6) .
C12 N1 Re2 127.2(6) .
C13 N2 C7 107.2(8) .
C13 N2 C1 128.6(8) .
C7 N2 C1 123.9(8) .
C29 N3 C31 107.2(8) .
C29 N3 C4 128.7(8) .
C31 N3 C4 123.5(8) .
C29 N4 C30 107.7(8) .
C29 N4 Re1 126.1(7) .
C30 N4 Re1 125.9(6) .
C45 N5 C43 105.7(8) .
C45 N5 Re1 130.3(6) 3_656
C43 N5 Re1 122.9(7) 3_656
C45 N6 C42 106.1(9) .
C45 N6 C57 127.2(10) .
C42 N6 C57 126.5(9) .
C72 N7 C71 108.8(9) .
C72 N7 C64 126.6(10) .
C71 N7 C64 124.6(10) .
C72 N8 C70 105.9(8) .
C72 N8 Re2 130.3(7) .
C70 N8 Re2 123.8(7) .
C28 O4 Re1 125.8(6) .
C19 O8 Re2 124.5(6) .
C51 O9 C52 118.0(10) .
O10 C55 H55A 109.5 .
O10 C55 H55B 109.5 .
H55A C55 H55B 109.5 .
O10 C55 H55C 109.4 .
H55A C55 H55C 109.5 .
H55B C55 H55C 109.5 .
C55 O10 C50 117(3) .
O10' C55' H55D 109.3 .
O10' C55' H55E 109.5 .
H55D C55' H55E 109.5 .
O10' C55' H55F 109.5 .
H55D C55' H55F 109.5 .
H55E C55' H55F 109.5 .
C55' O10' C50 98(3) .
C49 O11 C56 118.0(9) .
C78 O12 C80 117.4(11) .
C81 O13 C77 115.0(15) .
C82 O14 C76 120.6(14) .
C38 Re1 C36 84.8(5) .
C38 Re1 C37 88.4(5) .
C36 Re1 C37 88.1(6) .
C38 Re1 O4 92.9(4) .
C36 Re1 O4 175.6(4) .
C37 Re1 O4 95.6(5) .
C38 Re1 N4 174.4(4) .
C36 Re1 N4 100.7(4) .
C37 Re1 N4 90.8(4) .
O4 Re1 N4 81.6(3) .
C38 Re1 N5 94.1(4) 3_656
C36 Re1 N5 93.1(4) 3_656
C37 Re1 N5 177.3(4) 3_656
O4 Re1 N5 83.3(3) 3_656
N4 Re1 N5 86.7(3) 3_656
C22 Re2 C20 84.6(6) .
C22 Re2 C21 88.9(6) .
C20 Re2 C21 89.9(5) .
C22 Re2 O8 93.9(5) .
C20 Re2 O8 175.5(4) .
C21 Re2 O8 94.2(4) .
C22 Re2 N1 175.4(5) .
C20 Re2 N1 99.9(4) .
C21 Re2 N1 90.3(4) .
O8 Re2 N1 81.7(3) .
C22 Re2 N8 92.8(5) .
C20 Re2 N8 93.2(4) .
C21 Re2 N8 176.5(4) .
O8 Re2 N8 82.7(3) .
N1 Re2 N8 87.7(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.374(15) .
C1 C6 1.379(14) .
C1 N2 1.450(12) .
C2 C3 1.385(14) .
C2 H2 0.9300 .
C3 C4 1.371(14) .
C3 H3 0.9300 .
C4 C5 1.394(14) .
C4 N3 1.427(12) .
C5 C6 1.380(13) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.384(15) .
C7 C12 1.390(14) .
C7 N2 1.400(12) .
C8 C9 1.376(16) .
C8 H8 0.9300 .
C9 C10 1.392(17) .
C9 H9 0.9300 .
C10 C11 1.378(16) .
C10 H10 0.9300 .
C11 C12 1.379(14) .
C11 H11 0.9300 .
C12 N1 1.403(12) .
C13 N1 1.337(11) .
C13 N2 1.383(12) .
C13 C14 1.444(13) .
C14 C15 1.407(13) .
C14 C19 1.408(14) .
C15 C16 1.366(14) .
C15 H15 0.9300 .
C16 C17 1.391(17) .
C16 H16 0.9300 .
C17 C18 1.340(16) .
C17 H17 0.9300 .
C18 C19 1.404(14) .
C18 H18 0.9300 .
C19 O8 1.323(12) .
C20 O5 1.157(15) .
C20 Re2 1.901(15) .
C21 O6 1.136(13) .
C21 Re2 1.930(12) .
C22 O7 1.183(16) .
C22 Re2 1.898(15) .
C23 C24 1.405(14) .
C23 C28 1.420(14) .
C23 C29 1.457(14) .
C24 C25 1.379(15) .
C24 H24 0.9300 .
C25 C26 1.395(17) .
C25 H25 0.9300 .
C26 C27 1.352(17) .
C26 H26 0.9300 .
C27 C28 1.399(15) .
C27 H27 0.9300 .
C28 O4 1.311(12) .
C29 N4 1.330(12) .
C29 N3 1.386(12) .
C30 C35 1.371(14) .
C30 N4 1.398(13) .
C30 C31 1.403(14) .
C31 C32 1.382(15) .
C31 N3 1.386(12) .
C32 C33 1.378(16) .
C32 H32 0.9300 .
C33 C34 1.395(17) .
C33 H33 0.9300 .
C34 C35 1.373(16) .
C34 H34 0.9300 .
C35 H35 0.9300 .
C36 O2 1.134(13) .
C36 Re1 1.936(13) .
C37 O3 1.132(15) .
C37 Re1 1.940(15) .
C38 O1 1.148(13) .
C38 Re1 1.928(12) .
C39 C44 1.368(17) .
C39 C40 1.40(2) .
C39 H39 0.9300 .
C40 C41 1.36(2) .
C40 H40 0.9300 .
C41 C42 1.416(16) .
C41 H41 0.9300 .
C42 C43 1.376(15) .
C42 N6 1.378(14) .
C43 C44 1.391(15) .
C43 N5 1.401(12) .
C44 H44 0.9300 .
C45 N5 1.323(12) .
C45 N6 1.368(13) .
C45 C46 1.509(14) .
C46 C47 1.375(15) .
C46 C48 1.392(14) .
C47 C51 1.394(16) .
C47 H47 0.9300 .
C48 C49 1.372(14) .
C48 H48 0.9300 .
C49 O11 1.393(13) .
C49 C50 1.400(16) .
C50 O10 1.35(3) .
C50 C51 1.371(17) .
C50 O10' 1.43(3) .
C51 O9 1.375(14) .
C52 O9 1.423(16) .
C52 H52A 0.9600 .
C52 H52B 0.9600 .
C52 H52C 0.9600 .
C56 O11 1.424(14) .
C56 H56A 0.9600 .
C56 H56B 0.9600 .
C56 H56C 0.9600 .
C57 N6 1.469(14) .
C57 C58 1.505(14) .
C57 H57A 0.9700 .
C57 H57B 0.9700 .
C58 C59 1.383(14) .
C58 C63 1.417(15) .
C59 C60 1.414(14) .
C59 H59 0.9300 .
C60 C61 1.374(15) .
C60 C64 1.533(14) .
C61 C62 1.392(15) .
C61 H61 0.9300 .
C62 C63 1.380(14) .
C62 H62 0.9300 .
C63 H63 0.9300 .
C64 N7 1.467(13) .
C64 H64A 0.9700 .
C64 H64B 0.9700 .
C65 C66 1.397(18) .
C65 C71 1.401(15) .
C65 H65 0.9300 .
C66 C67 1.357(19) .
C66 H66 0.9300 .
C67 C69 1.388(17) .
C67 H67 0.9300 .
C69 C70 1.398(15) .
C69 H69 0.9300 .
C70 N8 1.373(13) .
C70 C71 1.403(15) .
C71 N7 1.366(14) .
C72 N8 1.339(13) .
C72 N7 1.353(13) .
C72 C73 1.483(15) .
C73 C79 1.371(14) .
C73 C75 1.388(15) .
C75 C76 1.355(18) .
C75 H75 0.9300 .
C76 O14 1.391(16) .
C76 C77 1.405(19) .
C77 C78 1.385(19) .
C77 O13 1.392(16) .
C78 O12 1.357(14) .
C78 C79 1.394(16) .
C79 H79 0.9300 .
C80 O12 1.382(18) .
C80 H80A 0.9600 .
C80 H80B 0.9600 .
C80 H80C 0.9600 .
C81 O13 1.36(2) .
C81 H81A 0.9600 .
C81 H81B 0.9600 .
C81 H81C 0.9600 .
C82 O14 1.338(19) .
C82 H82A 0.9600 .
C82 H82B 0.9600 .
C82 H82C 0.9600 .
N1 Re2 2.195(8) .
N4 Re1 2.189(8) .
N5 Re1 2.229(8) 3_656
N8 Re2 2.221(8) .
O4 Re1 2.121(7) .
O8 Re2 2.119(7) .
C55 O10 1.26(3) .
C55 H55A 0.9600 .
C55 H55B 0.9600 .
C55 H55C 0.9600 .
C55' O10' 1.25(3) .
C55' H55D 0.9600 .
C55' H55E 0.9600 .
C55' H55F 0.9600 .
