#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:18:23 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/96/7049671.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_7049671
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         'C148 H92 N16 O24 Re4'
_chemical_formula_sum            'C148 H92 N16 O24 Re4'
_chemical_formula_weight         3223.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c 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                   18.7918(6)
_cell_length_b                   23.7918(7)
_cell_length_c                   35.3639(11)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.46
_cell_volume                     15810.9(8)
_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 0.997
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            75563
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.694
_diffrn_reflns_theta_min         2.168
_exptl_absorpt_coefficient_mu    3.118
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       Block
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.691
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         14987
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0261P)²+67.3488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12436
_reflns_number_total             14987
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt05065a2.cif
_cod_data_source_block           Complex5
_cod_depositor_comments
'Adding full bibliography for 7049668--7049673.cif.'
_cod_database_code               7049671
_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   0.706
_shelx_estimated_absorpt_t_max   0.789
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
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 0.3715(2) 0.63626(19) 0.36273(12) 0.0248(10) Uani 1 1 d . . . . .
H1 H 0.330297 0.621565 0.352088 0.030 Uiso 1 1 calc R U . . .
C2 C 0.3711(2) 0.68927(19) 0.37917(12) 0.0260(10) Uani 1 1 d . . . . .
H2 H 0.329044 0.709914 0.379647 0.031 Uiso 1 1 calc R U . . .
C3 C 0.4320(2) 0.71174(19) 0.39482(12) 0.0257(10) Uani 1 1 d . . . . .
H3 H 0.430540 0.746969 0.406184 0.031 Uiso 1 1 calc R U . . .
C4 C 0.4959(2) 0.68180(19) 0.39366(12) 0.0244(9) Uani 1 1 d . . . . .
C5 C 0.4954(2) 0.62867(19) 0.37767(11) 0.0246(10) Uani 1 1 d . . . . .
H5 H 0.537414 0.608027 0.377231 0.029 Uiso 1 1 calc R U . . .
C6 C 0.4346(2) 0.60529(19) 0.36235(11) 0.0261(10) Uani 1 1 d . . . . .
C7 C 0.4398(3) 0.5465(2) 0.34571(13) 0.0285(10) Uani 1 1 d . . . . .
H7A H 0.472320 0.547244 0.324426 0.034 Uiso 1 1 calc R U . . .
H7B H 0.459651 0.521436 0.364611 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5659(3) 0.7045(2) 0.40861(14) 0.0323(11) Uani 1 1 d . . . . .
H8A H 0.582042 0.680655 0.429157 0.039 Uiso 1 1 calc R U . . .
H8B H 0.601252 0.702690 0.388666 0.039 Uiso 1 1 calc R U . . .
C9 C 0.5639(3) 0.7809(2) 0.45882(13) 0.0304(11) Uani 1 1 d . . . . .
C10 C 0.5546(2) 0.8086(2) 0.39894(13) 0.0278(10) Uani 1 1 d . . . . .
C11 C 0.5507(3) 0.8127(2) 0.35970(13) 0.0335(11) Uani 1 1 d . . . . .
H11 H 0.552493 0.781266 0.344089 0.040 Uiso 1 1 calc R U . . .
C12 C 0.5440(3) 0.8665(2) 0.34554(13) 0.0336(11) Uani 1 1 d . . . . .
H12 H 0.542316 0.871627 0.319483 0.040 Uiso 1 1 calc R U . . .
C13 C 0.5395(3) 0.9136(2) 0.36913(13) 0.0330(11) Uani 1 1 d . . . . .
H13 H 0.533714 0.948951 0.358395 0.040 Uiso 1 1 calc R U . . .
C14 C 0.5436(3) 0.9087(2) 0.40810(13) 0.0298(11) Uani 1 1 d . . . . .
H14 H 0.540529 0.940090 0.423677 0.036 Uiso 1 1 calc R U . . .
C15 C 0.5525(2) 0.8554(2) 0.42294(12) 0.0282(10) Uani 1 1 d . . . . .
C16 C 0.5812(15) 0.7462(15) 0.4893(11) 0.034(3) Uani 0.339(7) 1 d . U P A 1
C17 C 0.5298(12) 0.7058(13) 0.4972(8) 0.037(3) Uani 0.339(7) 1 d . U P A 1
H17 H 0.488655 0.704925 0.482633 0.045 Uiso 0.339(7) 1 calc R U P A 1
C18 C 0.5376(12) 0.6667(12) 0.5261(8) 0.040(4) Uani 0.339(7) 1 d . U P A 1
H18 H 0.502845 0.640065 0.531460 0.049 Uiso 0.339(7) 1 calc R U P A 1
C21 C 0.6435(11) 0.7499(8) 0.5101(7) 0.027(3) Uani 0.339(7) 1 d . U P A 1
H21 H 0.679944 0.774878 0.504301 0.033 Uiso 0.339(7) 1 calc R U P A 1
C16A C 0.5664(7) 0.7389(7) 0.4911(4) 0.035(2) Uani 0.661(7) 1 d . U P A 2
C17A C 0.5066(6) 0.7045(5) 0.4991(3) 0.038(2) Uani 0.661(7) 1 d . U P A 2
H17' H 0.465135 0.707353 0.484800 0.046 Uiso 0.661(7) 1 calc R U P A 2
C18A C 0.5117(7) 0.6661(6) 0.5291(5) 0.049(2) Uani 0.661(7) 1 d . U P A 2
C19A C 0.5737(7) 0.6617(5) 0.5496(3) 0.057(2) Uani 0.661(7) 1 d . U P A 2
C20A C 0.6313(7) 0.6925(6) 0.5415(3) 0.060(2) Uani 0.661(7) 1 d . U P A 2
H20' H 0.673261 0.687677 0.555041 0.072 Uiso 0.661(7) 1 calc R U P A 2
C21A C 0.6274(7) 0.7319(7) 0.5124(4) 0.053(3) Uani 0.661(7) 1 d . U P A 2
H21' H 0.666941 0.754023 0.507108 0.064 Uiso 0.661(7) 1 calc R U P A 2
C23 C 0.4418(3) 0.77307(19) 0.57944(13) 0.0321(11) Uani 1 1 d . . . . .
C24 C 0.4361(3) 0.7408(2) 0.61193(13) 0.0417(13) Uani 1 1 d . . . . .
H24 H 0.394309 0.721955 0.618069 0.050 Uiso 1 1 calc R U . . .
C25 C 0.4956(4) 0.7381(2) 0.63468(15) 0.0490(16) Uani 1 1 d . . . . .
H25 H 0.494210 0.716947 0.656769 0.059 Uiso 1 1 calc R U . . .
C27 C 0.5581(4) 0.7668(3) 0.62505(15) 0.0527(17) Uani 1 1 d . . . . .
H27 H 0.597825 0.762953 0.640501 0.063 Uiso 1 1 calc R U . . .
C28 C 0.5627(3) 0.8008(2) 0.59313(14) 0.0416(13) Uani 1 1 d . . . . .
H28 H 0.603786 0.820951 0.587455 0.050 Uiso 1 1 calc R U . . .
C29 C 0.5022(3) 0.8032(2) 0.57001(12) 0.0310(11) Uani 1 1 d . . . . .
C30 C 0.4257(2) 0.81864(17) 0.52427(12) 0.0228(9) Uani 1 1 d . . . . .
C31 C 0.3908(2) 0.83573(19) 0.48927(12) 0.0241(9) Uani 1 1 d . . . . .
C32 C 0.3380(3) 0.80269(19) 0.47188(12) 0.0284(10) Uani 1 1 d . . . . .
H32 H 0.328620 0.766952 0.481298 0.034 Uiso 1 1 calc R U . . .
C33 C 0.3000(3) 0.8219(2) 0.44141(12) 0.0292(10) Uani 1 1 d . . . . .
H33 H 0.265751 0.799157 0.430154 0.035 Uiso 1 1 calc R U . . .
C34 C 0.3131(3) 0.8756(2) 0.42743(13) 0.0293(10) Uani 1 1 d . . . . .
H34 H 0.285696 0.889479 0.407628 0.035 Uiso 1 1 calc R U . . .
C35 C 0.3658(3) 0.9080(2) 0.44258(13) 0.0286(10) Uani 1 1 d . . . . .
H35 H 0.374069 0.943583 0.432625 0.034 Uiso 1 1 calc R U . . .
C36 C 0.4085(2) 0.88869(19) 0.47328(12) 0.0238(9) Uani 1 1 d . . . . .
C37 C 0.6088(3) 0.9559(3) 0.48604(14) 0.0386(13) Uani 1 1 d . . . . .
C38 C 0.5415(2) 0.9420(2) 0.55295(14) 0.0288(10) Uani 1 1 d . . . . .
C39 C 0.6478(3) 0.8729(3) 0.52776(15) 0.0432(14) Uani 1 1 d . . . . .
C40 C 0.3181(3) 0.50370(19) 0.35678(13) 0.0292(11) Uani 1 1 d . . . . .
C41 C 0.3146(3) 0.5012(2) 0.39643(14) 0.0424(14) Uani 1 1 d . . . . .
H41 H 0.351192 0.514246 0.411790 0.051 Uiso 1 1 calc R U . . .
C42 C 0.2533(4) 0.4783(3) 0.41098(16) 0.0533(17) Uani 1 1 d . . . . .
H42 H 0.248352 0.474908 0.437043 0.064 Uiso 1 1 calc R U . . .
C43 C 0.1985(4) 0.4601(3) 0.38746(18) 0.0568(18) Uani 1 1 d . . . . .
H43 H 0.157690 0.445286 0.398549 0.068 Uiso 1 1 calc R U . . .
C44 C 0.2017(3) 0.4629(2) 0.34827(16) 0.0437(14) Uani 1 1 d . . . . .
H44 H 0.164199 0.451111 0.333054 0.052 Uiso 1 1 calc R U . . .
C45 C 0.2643(3) 0.4844(2) 0.33313(13) 0.0300(11) Uani 1 1 d . . . . .
C46 C 0.3497(2) 0.51471(18) 0.29689(12) 0.0232(9) Uani 1 1 d . . . . .
C47 C 0.3969(2) 0.5276(2) 0.26460(12) 0.0260(10) Uani 1 1 d . . . . .
C48 C 0.4081(2) 0.5832(2) 0.25347(13) 0.0305(10) Uani 1 1 d . . . . .
H48 H 0.386544 0.613242 0.265783 0.037 Uiso 1 1 calc R U . . .
C49 C 0.4534(3) 0.5909(2) 0.22285(14) 0.0369(12) Uani 1 1 d . . . . .
C50 C 0.4878(3) 0.5466(2) 0.20636(14) 0.0383(13) Uani 1 1 d . . . . .
C51 C 0.4795(3) 0.4930(2) 0.21769(15) 0.0392(13) Uani 1 1 d . . . . .
H51 H 0.504823 0.463712 0.206588 0.047 Uiso 1 1 calc R U . . .
C52 C 0.4316(3) 0.4835(2) 0.24660(14) 0.0322(11) Uani 1 1 d . . . . .
H52 H 0.422367 0.446809 0.254210 0.039 Uiso 1 1 calc R U . . .
C53 C 0.5129(3) 0.6237(3) 0.17371(18) 0.061(2) Uani 1 1 d . . . . .
H53A H 0.485379 0.629181 0.150812 0.073 Uiso 1 1 calc R U . . .
H53B H 0.555729 0.646301 0.171954 0.073 Uiso 1 1 calc R U . . .
C54 C 0.1907(2) 0.71479(19) 0.20112(12) 0.0239(9) Uani 1 1 d . . . . .
H54 H 0.151643 0.690846 0.200160 0.029 Uiso 1 1 calc R U . . .
C55 C 0.2593(2) 0.69298(18) 0.20213(11) 0.0220(9) Uani 1 1 d . . . . .
C56 C 0.3189(3) 0.72725(18) 0.20156(12) 0.0255(10) Uani 1 1 d . . . . .
H56 H 0.364427 0.711834 0.201464 0.031 Uiso 1 1 calc R U . . .
C57 C 0.2297(2) 0.6635(2) 0.28325(12) 0.0267(10) Uani 1 1 d . . . . .
H57 H 0.263493 0.686820 0.272190 0.032 Uiso 1 1 calc R U . . .
C58 C 0.1956(3) 0.6805(2) 0.31584(12) 0.0301(11) Uani 1 1 d . . . . .
H58 H 0.205414 0.715535 0.326252 0.036 Uiso 1 1 calc R U . . .
C59 C 0.1467(3) 0.6450(2) 0.33306(13) 0.0346(12) Uani 1 1 d . . . . .
H59 H 0.123224 0.656809 0.354800 0.041 Uiso 1 1 calc R U . . .
C60 C 0.1327(2) 0.5930(2) 0.31847(13) 0.0308(11) Uani 1 1 d . . . . .
H60 H 0.100875 0.569542 0.330946 0.037 Uiso 1 1 calc R U . . .
C61 C 0.1658(2) 0.5739(2) 0.28464(13) 0.0270(10) Uani 1 1 d . . . . .
C62 C 0.2137(2) 0.6109(2) 0.26638(12) 0.0249(9) Uani 1 1 d . . . . .
C63 C 0.2448(2) 0.59496(18) 0.22996(12) 0.0218(9) Uani 1 1 d . . . . .
C64 C 0.2960(2) 0.60276(19) 0.17306(12) 0.0257(10) Uani 1 1 d . . . . .
C65 C 0.3264(3) 0.6209(2) 0.13901(13) 0.0344(12) Uani 1 1 d . . . . .
H65 H 0.332345 0.658864 0.133495 0.041 Uiso 1 1 calc R U . . .
C66 C 0.3470(3) 0.5791(2) 0.11404(13) 0.0400(13) Uani 1 1 d . . . . .
H66 H 0.367975 0.589118 0.091191 0.048 Uiso 1 1 calc R U . . .
C67 C 0.3369(3) 0.5224(2) 0.12244(13) 0.0394(13) Uani 1 1 d . . . . .
H67 H 0.350377 0.495413 0.104791 0.047 Uiso 1 1 calc R U . . .
C68 C 0.3072(3) 0.5051(2) 0.15638(13) 0.0350(12) Uani 1 1 d . . . . .
H68 H 0.301354 0.467148 0.161873 0.042 Uiso 1 1 calc R U . . .
C69 C 0.2864(2) 0.54648(19) 0.18203(12) 0.0270(10) Uani 1 1 d . . . . .
C70 C 0.1570(3) 0.4488(3) 0.2051(2) 0.0545(17) Uani 1 1 d . . . . .
C71 C 0.1815(4) 0.4009(3) 0.2706(2) 0.066(2) Uani 1 1 d . . . . .
C73 C 0.2855(3) 0.4149(2) 0.22517(14) 0.0320(11) Uani 1 1 d . . . . .
C74 C 0.3203(3) 0.76662(19) 0.55221(12) 0.0285(11) Uani 1 1 d . . . . .
C75 C 0.3034(3) 0.70945(19) 0.55270(12) 0.0306(11) Uani 1 1 d . . . . .
H75 H 0.339421 0.682614 0.552849 0.037 Uiso 1 1 calc R U . . .
C76 C 0.2672(3) 0.80701(19) 0.55297(12) 0.0297(11) Uani 1 1 d . . . . .
H76 H 0.278914 0.844968 0.553666 0.036 Uiso 1 1 calc R U . . .
N1 N 0.4909(2) 0.83148(16) 0.53573(10) 0.0252(8) Uani 1 1 d . . . . .
N2 N 0.3935(2) 0.78300(16) 0.55044(10) 0.0280(9) Uani 1 1 d . . . . .
N3 N 0.5591(2) 0.83675(17) 0.46041(10) 0.0281(9) Uani 1 1 d . . . . .
N4 N 0.5608(2) 0.76247(17) 0.42222(11) 0.0300(9) Uani 1 1 d . . . . .
N5 N 0.3718(2) 0.52383(15) 0.33308(10) 0.0248(8) Uani 1 1 d . . . . .
N6 N 0.2858(2) 0.49149(15) 0.29520(10) 0.0250(8) Uani 1 1 d . . . . .
N7 N 0.2692(2) 0.63296(15) 0.20349(10) 0.0243(8) Uani 1 1 d . . . . .
N8 N 0.2549(2) 0.54274(15) 0.21781(10) 0.0236(8) Uani 1 1 d . . . . .
O1 O 0.52879(19) 0.96774(15) 0.57962(9) 0.0355(8) Uani 1 1 d . . . . .
O2 O 0.6413(2) 0.99215(18) 0.47271(11) 0.0494(10) Uani 1 1 d . . . . .
O3 O 0.7051(2) 0.8623(2) 0.53769(13) 0.0711(15) Uani 1 1 d . . . . .
O4 O 0.45997(16) 0.92091(13) 0.48533(8) 0.0264(7) Uani 1 1 d . . . . .
O7 O 0.14883(17) 0.52355(14) 0.27217(10) 0.0331(8) Uani 1 1 d . . . . .
O8 O 0.1609(4) 0.3592(2) 0.2832(2) 0.131(3) Uani 1 1 d . . . . .
O9 O 0.1193(3) 0.4378(2) 0.18041(17) 0.0910(19) Uani 1 1 d . . . . .
O10 O 0.3247(2) 0.38189(14) 0.21295(10) 0.0380(8) Uani 1 1 d . . . . .
O11 O 0.4719(2) 0.64063(18) 0.20606(12) 0.0555(11) Uani 1 1 d . . . . .
O12 O 0.5312(2) 0.5664(2) 0.17752(11) 0.0607(13) Uani 1 1 d . . . . .
Re1 Re 0.55733(2) 0.89541(2) 0.50956(2) 0.02679(6) Uani 1 1 d . . . . .
Re2 Re 0.21880(2) 0.46637(2) 0.24599(2) 0.02957(6) Uani 1 1 d . . . . .
C19 C 0.5952(9) 0.6698(7) 0.5448(5) 0.060(4) Uani 0.339(7) 1 d G U P A 1
C20 C 0.6467(8) 0.7130(6) 0.5402(4) 0.051(3) Uani 0.339(7) 1 d G U P A 1
O6 O 0.6964(6) 0.7085(5) 0.5703(3) 0.065(3) Uani 0.339(7) 1 d G U P A 1
C22 C 0.6757(9) 0.6626(6) 0.5934(4) 0.111(6) Uani 0.339(7) 1 d G U P A 1
H22A H 0.666473 0.675397 0.618981 0.134 Uiso 0.339(7) 1 calc R U P A 1
H22B H 0.713457 0.634746 0.594301 0.134 Uiso 0.339(7) 1 calc R U P A 1
O5 O 0.6132(9) 0.6386(6) 0.5777(5) 0.085(4) Uani 0.339(7) 1 d G U P A 1
O5A O 0.5692(7) 0.6216(5) 0.5765(3) 0.097(3) Uani 0.661(7) 1 d . U P A 2
C22A C 0.4942(10) 0.6023(6) 0.5743(4) 0.106(4) Uani 0.661(7) 1 d . U P A 2
H22C H 0.492002 0.562009 0.570174 0.127 Uiso 0.661(7) 1 calc R U P A 2
H22D H 0.468848 0.611215 0.597411 0.127 Uiso 0.661(7) 1 calc R U P A 2
O6A O 0.4634(6) 0.6325(3) 0.5422(2) 0.096(3) Uani 0.661(7) 1 d . U P A 2
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_1
_geom_angle_site_symmetry_3
C2 C1 C6 119.3(4) . .
C2 C1 H1 120.4 . .
C6 C1 H1 120.4 . .
C3 C2 C1 120.9(4) . .
C3 C2 H2 119.5 . .
C1 C2 H2 119.5 . .
C2 C3 C4 120.3(4) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C5 C4 C3 118.1(4) . .
C5 C4 C8 118.3(4) . .
C3 C4 C8 123.6(4) . .
C6 C5 C4 122.3(4) . .
C6 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
C5 C6 C1 119.1(4) . .
C5 C6 C7 118.0(4) . .
C1 C6 C7 122.9(4) . .
N5 C7 C6 113.8(4) . .
N5 C7 H7A 108.8 . .
C6 C7 H7A 108.8 . .
N5 C7 H7B 108.8 . .
C6 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
N4 C8 C4 113.2(4) . .
N4 C8 H8A 108.9 . .
C4 C8 H8A 108.9 . .
N4 C8 H8B 108.9 . .
C4 C8 H8B 108.9 . .
H8A C8 H8B 107.8 . .
N3 C9 N4 110.9(4) . .
N3 C9 C16 124.9(17) . .
N4 C9 C16 123.5(18) . .
N3 C9 C16A 128.7(8) . .
N4 C9 C16A 120.2(8) . .
N4 C10 C11 131.0(4) . .
N4 C10 C15 105.9(4) . .
C11 C10 C15 123.1(5) . .
C12 C11 C10 115.5(4) . .
C12 C11 H11 122.2 . .
C10 C11 H11 122.2 . .
C11 C12 C13 122.1(4) . .
C11 C12 H12 119.0 . .
C13 C12 H12 118.9 . .
C14 C13 C12 121.5(5) . .
C14 C13 H13 119.2 . .
C12 C13 H13 119.2 . .
C15 C14 C13 117.5(4) . .
C15 C14 H14 121.3 . .
C13 C14 H14 121.3 . .
C14 C15 C10 120.2(4) . .
C14 C15 N3 131.3(4) . .
C10 C15 N3 108.5(4) . .
C21 C16 C17 122(2) . .
C21 C16 C9 124.7(18) . .
C17 C16 C9 114(2) . .
C16 C17 C18 123(2) . .
C16 C17 H17 118.7 . .
C18 C17 H17 118.7 . .
C19 C18 C17 116(2) . .
C19 C18 H18 122.1 . .
C17 C18 H18 122.1 . .
C16 C21 C20 113.9(17) . .
C16 C21 H21 123.0 . .
C20 C21 H21 123.0 . .
C21A C16A C17A 118.7(12) . .
C21A C16A C9 121.1(10) . .
C17A C16A C9 120.2(11) . .
C18A C17A C16A 118.1(11) . .
C18A C17A H17' 121.0 . .
C16A C17A H17' 121.0 . .
O6A C18A C19A 110.9(12) . .
O6A C18A C17A 128.6(13) . .
C19A C18A C17A 120.5(12) . .
C20A C19A C18A 121.9(10) . .
C20A C19A O5A 126.1(12) . .
C18A C19A O5A 111.9(12) . .
C19A C20A C21A 119.0(10) . .
C19A C20A H20' 120.5 . .
C21A C20A H20' 120.5 . .
C16A C21A C20A 121.8(11) . .
C16A C21A H21' 119.1 . .
C20A C21A H21' 119.1 . .
C29 C23 C24 123.4(5) . .
C29 C23 N2 105.7(4) . .
C24 C23 N2 130.9(5) . .
C25 C24 C23 116.5(6) . .
C25 C24 H24 121.7 . .
C23 C24 H24 121.7 . .
C24 C25 C27 121.0(5) . .
C24 C25 H25 119.5 . .
C27 C25 H25 119.5 . .
C28 C27 C25 122.2(5) . .
C28 C27 H27 118.9 . .
C25 C27 H27 118.9 . .
C27 C28 C29 116.4(6) . .
C27 C28 H28 121.8 . .
C29 C28 H28 121.8 . .
C23 C29 C28 120.3(5) . .
C23 C29 N1 109.4(4) . .
C28 C29 N1 130.3(5) . .
N1 C30 N2 109.8(4) . .
N1 C30 C31 127.6(4) . .
N2 C30 C31 122.5(4) . .
C32 C31 C36 119.1(4) . .
C32 C31 C30 122.2(4) . .
C36 C31 C30 118.6(4) . .
C33 C32 C31 121.7(4) . .
C33 C32 H32 119.2 . .
C31 C32 H32 119.2 . .
C32 C33 C34 119.5(4) . .
C32 C33 H33 120.2 . .
C34 C33 H33 120.2 . .
C35 C34 C33 120.5(4) . .
C35 C34 H34 119.7 . .
C33 C34 H34 119.7 . .
C34 C35 C36 121.7(4) . .
C34 C35 H35 119.2 . .
C36 C35 H35 119.2 . .
O4 C36 C31 124.4(4) . .
O4 C36 C35 118.4(4) . .
C31 C36 C35 117.2(4) . .
O2 C37 Re1 177.9(5) . .
O1 C38 Re1 175.8(4) . .
O3 C39 Re1 175.3(6) . .
C45 C40 N5 106.1(4) . .
C45 C40 C41 123.5(5) . .
N5 C40 C41 130.4(5) . .
C42 C41 C40 115.5(6) . .
C42 C41 H41 122.3 . .
C40 C41 H41 122.3 . .
C41 C42 C43 121.3(5) . .
C41 C42 H42 119.3 . .
C43 C42 H42 119.3 . .
C44 C43 C42 123.2(6) . .
C44 C43 H43 118.4 . .
C42 C43 H43 118.4 . .
C43 C44 C45 116.1(6) . .
C43 C44 H44 122.0 . .
C45 C44 H44 122.0 . .
C44 C45 C40 120.3(5) . .
C44 C45 N6 130.7(5) . .
C40 C45 N6 109.0(4) . .
N6 C46 N5 112.7(4) . .
N6 C46 C47 126.6(4) . .
N5 C46 C47 120.7(4) . .
C52 C47 C48 121.0(4) . .
C52 C47 C46 118.5(4) . .
C48 C47 C46 120.4(4) . .
C49 C48 C47 116.0(5) . .
C49 C48 H48 122.0 . .
C47 C48 H48 122.0 . .
C50 C49 O11 111.3(5) . .
C50 C49 C48 121.3(5) . .
O11 C49 C48 127.4(5) . .
C51 C50 C49 123.3(5) . .
C51 C50 O12 127.5(5) . .
C49 C50 O12 109.2(5) . .
C50 C51 C52 116.8(5) . .
C50 C51 H51 121.6 . .
C52 C51 H51 121.6 . .
C51 C52 C47 121.5(5) . .
C51 C52 H52 119.3 . .
C47 C52 H52 119.3 . .
O12 C53 O11 109.0(4) . .
O12 C53 H53A 109.9 . .
O11 C53 H53A 109.9 . .
O12 C53 H53B 109.9 . .
O11 C53 H53B 109.9 . .
H53A C53 H53B 108.3 . .
C55 C54 C56 119.4(4) . 2_565
C55 C54 H54 120.3 . .
C56 C54 H54 120.3 2_565 .
C56 C55 C54 122.0(4) . .
C56 C55 N7 118.6(4) . .
C54 C55 N7 119.4(4) . .
C55 C56 C54 118.5(4) . 2_565
C55 C56 H56 120.7 . .
C54 C56 H56 120.7 2_565 .
C58 C57 C62 120.8(4) . .
C58 C57 H57 119.6 . .
C62 C57 H57 119.6 . .
C57 C58 C59 119.7(5) . .
C57 C58 H58 120.1 . .
C59 C58 H58 120.1 . .
C60 C59 C58 120.8(4) . .
C60 C59 H59 119.6 . .
C58 C59 H59 119.6 . .
C59 C60 C61 121.5(4) . .
C59 C60 H60 119.2 . .
C61 C60 H60 119.2 . .
O7 C61 C62 124.6(4) . .
O7 C61 C60 117.9(4) . .
C62 C61 C60 117.6(4) . .
C61 C62 C57 119.4(4) . .
C61 C62 C63 119.6(4) . .
C57 C62 C63 120.9(4) . .
N8 C63 N7 110.2(4) . .
N8 C63 C62 125.7(4) . .
N7 C63 C62 124.0(4) . .
C69 C64 N7 106.0(4) . .
C69 C64 C65 123.2(4) . .
N7 C64 C65 130.8(4) . .
C66 C65 C64 116.1(5) . .
C66 C65 H65 121.9 . .
C64 C65 H65 121.9 . .
C65 C66 C67 121.4(5) . .
C65 C66 H66 119.3 . .
C67 C66 H66 119.3 . .
C68 C67 C66 121.7(4) . .
C68 C67 H67 119.1 . .
C66 C67 H67 119.1 . .
C67 C68 C69 117.8(5) . .
C67 C68 H68 121.1 . .
C69 C68 H68 121.1 . .
C64 C69 C68 119.7(4) . .
C64 C69 N8 108.8(4) . .
C68 C69 N8 131.4(4) . .
O9 C70 Re2 179.5(8) . .
O8 C71 Re2 174.9(6) . .
O10 C73 Re2 177.6(4) . .
C76 C74 C75 120.7(5) . .
C76 C74 N2 120.3(4) . .
C75 C74 N2 119.0(5) . .
C76 C75 C74 119.6(5) 2_565 .
C76 C75 H75 120.2 2_565 .
C74 C75 H75 120.2 . .
C75 C76 C74 119.7(4) 2_565 .
C75 C76 H76 120.2 2_565 .
C74 C76 H76 120.2 . .
C30 N1 C29 107.1(4) . .
C30 N1 Re1 124.2(3) . .
C29 N1 Re1 128.0(3) . .
C23 N2 C30 108.0(4) . .
C23 N2 C74 123.3(4) . .
C30 N2 C74 127.8(4) . .
C9 N3 C15 106.4(4) . .
C9 N3 Re1 131.1(3) . .
C15 N3 Re1 122.5(3) . .
C9 N4 C10 108.3(4) . .
C9 N4 C8 127.6(4) . .
C10 N4 C8 124.0(4) . .
C46 N5 C40 106.8(4) . .
C46 N5 C7 127.9(4) . .
C40 N5 C7 125.2(4) . .
C46 N6 C45 105.4(4) . .
C46 N6 Re2 131.3(3) . .
C45 N6 Re2 123.3(3) . .
C63 N7 C64 107.9(4) . .
C63 N7 C55 129.0(4) . .
C64 N7 C55 122.3(4) . .
C63 N8 C69 107.1(4) . .
C63 N8 Re2 125.9(3) . .
C69 N8 Re2 126.7(3) . .
C36 O4 Re1 127.3(3) . .
C61 O7 Re2 125.8(3) . .
C49 O11 C53 103.8(5) . .
C50 O12 C53 104.8(4) . .
C39 Re1 C38 91.8(2) . .
C39 Re1 C37 84.7(3) . .
C38 Re1 C37 89.5(2) . .
C39 Re1 O4 175.81(19) . .
C38 Re1 O4 91.40(16) . .
C37 Re1 O4 92.58(18) . .
C39 Re1 N1 100.0(2) . .
C38 Re1 N1 88.56(17) . .
C37 Re1 N1 175.00(19) . .
O4 Re1 N1 82.87(13) . .
C39 Re1 N3 94.26(18) . .
C38 Re1 N3 171.44(17) . .
C37 Re1 N3 97.13(17) . .
O4 Re1 N3 82.89(13) . .
N1 Re1 N3 84.41(14) . .
C73 Re2 C70 88.0(2) . .
C73 Re2 C71 83.8(2) . .
C70 Re2 C71 86.8(3) . .
C73 Re2 O7 176.41(18) . .
C70 Re2 O7 95.5(2) . .
C71 Re2 O7 95.6(2) . .
C73 Re2 N8 98.92(17) . .
C70 Re2 N8 91.5(2) . .
C71 Re2 N8 176.7(2) . .
O7 Re2 N8 81.78(13) . .
C73 Re2 N6 95.92(18) . .
C70 Re2 N6 176.1(2) . .
C71 Re2 N6 94.0(3) . .
O7 Re2 N6 80.57(13) . .
N8 Re2 N6 87.56(13) . .
C18 C19 C20 124.2(16) . .
C18 C19 O5 126.8(16) . .
C20 C19 O5 108.0 . .
C21 C20 O6 130.8(12) . .
C21 C20 C19 121.2(12) . .
O6 C20 C19 108.0 . .
C20 O6 C22 108.0 . .
O6 C22 O5 108.0 . .
O6 C22 H22A 110.1 . .
O5 C22 H22A 110.1 . .
O6 C22 H22B 110.1 . .
O5 C22 H22B 110.1 . .
H22A C22 H22B 108.4 . .
C19 O5 C22 108.0 . .
C19A O5A C22A 103.9(10) . .
O6A C22A O5A 105.4(11) . .
O6A C22A H22C 110.7 . .
O5A C22A H22C 110.7 . .
O6A C22A H22D 110.7 . .
O5A C22A H22D 110.7 . .
H22C C22A H22D 108.8 . .
C18A O6A C22A 107.7(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.389(6) .
C1 C6 1.396(6) .
C1 H1 0.9300 .
C2 C3 1.380(7) .
C2 H2 0.9300 .
C3 C4 1.397(6) .
C3 H3 0.9300 .
C4 C5 1.385(6) .
C4 C8 1.516(6) .
C5 C6 1.381(7) .
C5 H5 0.9300 .
C6 C7 1.522(6) .
C7 N5 1.456(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 N4 1.464(6) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 N3 1.333(6) .
C9 N4 1.367(6) .
C9 C16 1.40(3) .
C9 C16A 1.518(15) .
C10 N4 1.377(6) .
C10 C11 1.393(6) .
C10 C15 1.402(6) .
C11 C12 1.381(7) .
C11 H11 0.9300 .
C12 C13 1.399(7) .
C12 H12 0.9300 .
C13 C14 1.385(7) .
C13 H13 0.9300 .
C14 C15 1.382(7) .
C14 H14 0.9300 .
C15 N3 1.403(6) .
C16 C21 1.39(3) .
C16 C17 1.39(3) .
C17 C18 1.39(3) .
C17 H17 0.9300 .
C18 C19 1.27(3) .
C18 H18 0.9300 .
C21 C20 1.381(19) .
C21 H21 0.9300 .
C16A C21A 1.380(17) .
C16A C17A 1.420(15) .
C17A C18A 1.404(17) .
C17A H17' 0.9300 .
C18A O6A 1.295(16) .
C18A C19A 1.38(2) .
C19A C20A 1.339(17) .
C19A O5A 1.349(12) .
C20A C21A 1.395(16) .
C20A H20' 0.9300 .
C21A H21' 0.9300 .
C23 C29 1.383(8) .
C23 C24 1.386(7) .
C23 N2 1.391(6) .
C24 C25 1.379(8) .
C24 H24 0.9300 .
C25 C27 1.399(9) .
C25 H25 0.9300 .
C27 C28 1.392(8) .
C27 H27 0.9300 .
C28 C29 1.402(7) .
C28 H28 0.9300 .
C29 N1 1.403(6) .
C30 N1 1.325(6) .
C30 N2 1.394(6) .
C30 C31 1.459(6) .
C31 C32 1.408(6) .
C31 C36 1.421(6) .
C32 C33 1.370(6) .
C32 H32 0.9300 .
C33 C34 1.392(7) .
C33 H33 0.9300 .
C34 C35 1.365(7) .
C34 H34 0.9300 .
C35 C36 1.426(6) .
C35 H35 0.9300 .
C36 O4 1.305(5) .
C37 O2 1.157(7) .
C37 Re1 1.924(6) .
C38 O1 1.149(6) .
C38 Re1 1.916(5) .
C39 O3 1.160(6) .
C39 Re1 1.895(5) .
C40 C45 1.390(7) .
C40 N5 1.396(6) .
C40 C41 1.405(7) .
C41 C42 1.373(9) .
C41 H41 0.9300 .
C42 C43 1.394(10) .
C42 H42 0.9300 .
C43 C44 1.389(8) .
C43 H43 0.9300 .
C44 C45 1.390(7) .
C44 H44 0.9300 .
C45 N6 1.411(6) .
C46 N6 1.324(6) .
C46 N5 1.363(6) .
C46 C47 1.477(6) .
C47 C52 1.391(7) .
C47 C48 1.395(7) .
C48 C49 1.390(7) .
C48 H48 0.9300 .
C49 C50 1.367(8) .
C49 O11 1.368(6) .
C50 C51 1.346(8) .
C50 O12 1.389(6) .
C51 C52 1.381(7) .
C51 H51 0.9300 .
C52 H52 0.9300 .
C53 O12 1.411(8) .
C53 O11 1.438(8) .
C53 H53A 0.9700 .
C53 H53B 0.9700 .
C54 C55 1.390(6) .
C54 C56 1.391(6) 2_565
C54 H54 0.9300 .
C55 C56 1.386(7) .
C55 N7 1.441(5) .
C56 H56 0.9300 .
C57 C58 1.379(6) .
C57 C62 1.419(6) .
C57 H57 0.9300 .
C58 C59 1.388(7) .
C58 H58 0.9300 .
C59 C60 1.366(7) .
C59 H59 0.9300 .
C60 C61 1.422(6) .
C60 H60 0.9300 .
C61 O7 1.315(6) .
C61 C62 1.415(7) .
C62 C63 1.464(6) .
C63 N8 1.328(5) .
C63 N7 1.380(6) .
C64 C69 1.388(6) .
C64 N7 1.388(5) .
C64 C65 1.401(7) .
C65 C66 1.385(7) .
C65 H65 0.9300 .
C66 C67 1.396(8) .
C66 H66 0.9300 .
C67 C68 1.386(7) .
C67 H67 0.9300 .
C68 C69 1.395(6) .
C68 H68 0.9300 .
C69 N8 1.400(6) .
C70 O9 1.153(7) .
C70 Re2 1.902(6) .
C71 O8 1.153(8) .
C71 Re2 1.918(6) .
C73 O10 1.159(6) .
C73 Re2 1.901(5) .
C74 C76 1.386(7) .
C74 C75 1.397(6) .
C74 N2 1.430(6) .
C75 C76 1.383(7) 2_565
C75 H75 0.9300 .
C76 H76 0.9300 .
N1 Re1 2.175(4) .
N3 Re1 2.229(4) .
N6 Re2 2.229(4) .
N8 Re2 2.181(4) .
O4 Re1 2.109(3) .
O7 Re2 2.106(3) .
C19 C20 1.4200 .
C19 O5 1.4200 .
C20 O6 1.4200 .
O6 C22 1.4200 .
C22 O5 1.4200 .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
O5A C22A 1.49(2) .
C22A O6A 1.462(13) .
C22A H22C 0.9700 .
C22A H22D 0.9700 .
