#------------------------------------------------------------------------------
#$Date: 2023-10-06 03:30:12 +0300 (Fri, 06 Oct 2023) $
#$Revision: 286765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/26/7062663.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_7062663
loop_
_publ_author_name
'Pohorenec, Ryan A.'
'Brennessel, William W.'
'Jones, William D.'
_publ_section_title
;
 Synthesis, characterization, and structure determination of
 bis-oxazolidine complexes of rhenium
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16872
_journal_page_last               16878
_journal_paper_doi               10.1039/D3NJ02181E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C19 H17 N3 O6 Re, Br'
_chemical_formula_sum            'C19 H17 Br N3 O6 Re'
_chemical_formula_weight         649.46
_chemical_name_common            jonrap04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-28
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2317(2)
_cell_length_b                   10.72530(10)
_cell_length_c                   20.2888(2)
_cell_measurement_reflns_used    37721
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.1530
_cell_measurement_theta_min      2.8770
_cell_volume                     4092.40(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     27.00 120.00   0.50    0.12    --   47.27  72.00 176.00  186
  2  ω     35.00 120.00   0.50    0.12    --   47.27  38.00  90.00  170
  3  ω     32.00 118.00   0.50    0.12    --   47.27  57.00 -90.00  172
  4  ω     42.00 106.00   0.50    0.47    --  113.25 -94.00   0.00  128
  5  ω     42.00 111.00   0.50    0.47    --  113.25-125.00  60.00  138
  6  ω     42.00 111.00   0.50    0.47    --  113.25-125.00-150.00  138
  7  ω     42.00  80.00   0.50    0.47    --  113.25 -61.00-180.00   76
  8  ω     42.00  80.00   0.50    0.47    --  113.25 -61.00-120.00   76
  9  ω     42.00  80.00   0.50    0.47    --  113.25 -61.00 -90.00   76
 10  ω     42.00  80.00   0.50    0.47    --  113.25 -61.00 -60.00   76
 11  ω    -24.00  68.00   0.50    0.12    --   47.27 -72.00  46.00  184
 12  ω     42.00 134.00   0.50    0.47    --  113.25 -72.00  46.00  184
 13  ω     42.00  80.00   0.50    0.47    --  113.25 -61.00  60.00   76
 14  ω     42.00  80.00   0.50    0.47    --  113.25 -61.00  90.00   76
 15  ω     95.00 178.00   0.50    0.47    --  113.25 125.00 120.00  166
 16  ω    100.00 172.00   0.50    0.47    --  113.25  15.00  90.00  144
 17  ω     93.00 178.00   0.50    0.47    --  113.25  72.00 176.00  170
 18  ω     97.00 178.00   0.50    0.47    --  113.25  61.00 120.00  162
 19  ω    100.00 172.00   0.50    0.47    --  113.25  15.00 120.00  144
 20  ω     91.00 178.00   0.50    0.47    --  113.25  77.00 -90.00  174
 21  ω    100.00 172.00   0.50    0.47    --  113.25  15.00 -30.00  144
 22  ω    -68.00  25.00   0.50    0.12    --  -47.27  72.00 176.00  186
 23  ω   -112.00 -19.00   0.50    0.47    --  -91.75  72.00 176.00  186
 24  ω     -3.00  28.00   0.50    0.12    --  -47.27  19.00 -60.00   62
 25  ω    -73.00 -19.00   0.50    0.47    --  -91.75  61.00   0.00  108
 26  ω   -120.00 -27.00   0.50    0.12    --  -47.27 -72.00  46.00  186
 27  ω   -163.00 -71.00   0.50    0.47    --  -91.75 -72.00  46.00  184
 28  ω   -120.00 -73.00   0.50    0.12    --  -47.27-125.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0742625000
_diffrn_orient_matrix_UB_12      -0.0428953000
_diffrn_orient_matrix_UB_13      -0.0373152000
_diffrn_orient_matrix_UB_21      -0.0024610000
_diffrn_orient_matrix_UB_22      0.1076681000
_diffrn_orient_matrix_UB_23      -0.0507475000
_diffrn_orient_matrix_UB_31      0.0344772000
_diffrn_orient_matrix_UB_32      -0.0848047000
_diffrn_orient_matrix_UB_33      -0.0454304000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.217
_diffrn_reflns_theta_min         2.880
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
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    2.108
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethyl ether'
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0286
_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)+(0.0299P)²+18.7825P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8381
_reflns_number_total             8801
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj02181e2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7062663--7062665.cif.'
_cod_database_code               7062663
_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_max   0.783
_shelx_estimated_absorpt_t_min   0.277
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6), C23(H23), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C20(H20A,H20B), C22(H22A,H22B),
 C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35)
;
_olex2_submission_original_sample_id jonrap04
_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 1.223
_oxdiff_exptl_absorpt_empirical_full_min 0.869
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Re1 Re 0.23175(2) 0.74937(2) 0.53447(2) 0.01087(5) Uani 1 1 d . . . . .
O1 O 0.28354(18) 1.1741(3) 0.47677(16) 0.0226(6) Uani 1 1 d . . . . .
H1 H 0.253(4) 1.214(7) 0.495(4) 0.05(2) Uiso 1 1 d . . . . .
O2 O 0.40607(17) 0.8862(3) 0.48657(15) 0.0193(6) Uani 1 1 d . . . . .
O3 O 0.31779(15) 0.9773(3) 0.65545(14) 0.0158(6) Uani 1 1 d . . . . .
O4 O 0.09887(15) 0.5848(3) 0.50426(15) 0.0178(6) Uani 1 1 d . . . . .
O5 O 0.14050(15) 0.9344(3) 0.59581(15) 0.0180(6) Uani 1 1 d . . . . .
O6 O 0.17963(17) 0.8327(3) 0.38744(15) 0.0236(7) Uani 1 1 d . . . . .
N1 N 0.33183(17) 0.8622(3) 0.56312(16) 0.0113(6) Uani 1 1 d . . . . .
N2 N 0.30914(18) 0.6273(3) 0.50360(16) 0.0134(6) Uani 1 1 d . . . . .
N3 N 0.27631(18) 0.6843(3) 0.63572(16) 0.0122(6) Uani 1 1 d . . . . .
C1 C 0.2749(2) 1.0451(4) 0.4876(2) 0.0182(8) Uani 1 1 d . . . . .
H1A H 0.275357 0.998143 0.445704 0.022 Uiso 1 1 calc R U . . .
H1B H 0.228718 1.030105 0.500540 0.022 Uiso 1 1 calc R U . . .
C2 C 0.3361(2) 1.0010(4) 0.5442(2) 0.0167(8) Uani 1 1 d . . . . .
C3 C 0.4055(2) 1.0047(4) 0.5188(2) 0.0210(9) Uani 1 1 d . . . . .
H3A H 0.405449 1.073815 0.486493 0.025 Uiso 1 1 calc R U . . .
H3B H 0.447065 1.013901 0.556636 0.025 Uiso 1 1 calc R U . . .
C4 C 0.3911(2) 0.8023(4) 0.5351(2) 0.0135(7) Uani 1 1 d . . . . .
H4 H 0.434169 0.793498 0.572154 0.016 Uiso 1 1 calc R U . . .
C5 C 0.3357(2) 1.0700(4) 0.6103(2) 0.0164(8) Uani 1 1 d . . . . .
H5A H 0.383094 1.106340 0.628988 0.020 Uiso 1 1 calc R U . . .
H5B H 0.300060 1.137849 0.602969 0.020 Uiso 1 1 calc R U . . .
C6 C 0.3507(2) 0.8682(4) 0.63941(19) 0.0131(7) Uani 1 1 d . . . . .
H6 H 0.403434 0.876005 0.654878 0.016 Uiso 1 1 calc R U . . .
C7 C 0.3730(2) 0.6776(4) 0.50233(18) 0.0120(7) Uani 1 1 d . . . . .
C8 C 0.4239(2) 0.6147(4) 0.4757(2) 0.0152(8) Uani 1 1 d . . . . .
H8 H 0.468339 0.652800 0.475226 0.018 Uiso 1 1 calc R U . . .
C9 C 0.4093(2) 0.4958(4) 0.4497(2) 0.0179(8) Uani 1 1 d . . . . .
H9 H 0.442585 0.452557 0.429509 0.021 Uiso 1 1 calc R U . . .
C10 C 0.3444(2) 0.4408(4) 0.4539(2) 0.0184(8) Uani 1 1 d . . . . .
H10 H 0.333728 0.357894 0.438608 0.022 Uiso 1 1 calc R U . . .
C11 C 0.2959(2) 0.5095(4) 0.4807(2) 0.0168(8) Uani 1 1 d . . . . .
H11 H 0.251587 0.472433 0.483064 0.020 Uiso 1 1 calc R U . . .
C12 C 0.3246(2) 0.7592(4) 0.67393(19) 0.0135(8) Uani 1 1 d . . . . .
C13 C 0.3469(2) 0.7426(4) 0.7429(2) 0.0170(8) Uani 1 1 d . . . . .
H13 H 0.379557 0.799083 0.769064 0.020 Uiso 1 1 calc R U . . .
C14 C 0.3208(2) 0.6424(4) 0.7729(2) 0.0185(8) Uani 1 1 d . . . . .
H14 H 0.334231 0.630157 0.820204 0.022 Uiso 1 1 calc R U . . .
C15 C 0.2748(2) 0.5599(4) 0.7332(2) 0.0210(9) Uani 1 1 d . . . . .
H15 H 0.258185 0.488071 0.752566 0.025 Uiso 1 1 calc R U . . .
C16 C 0.2535(2) 0.5837(4) 0.6649(2) 0.0172(8) Uani 1 1 d . . . . .
H16 H 0.221765 0.527315 0.637762 0.021 Uiso 1 1 calc R U . . .
C17 C 0.1503(2) 0.6411(4) 0.5166(2) 0.0159(8) Uani 1 1 d . . . . .
C18 C 0.1738(2) 0.8662(4) 0.5717(2) 0.0152(8) Uani 1 1 d . . . . .
C19 C 0.1988(2) 0.8054(4) 0.4424(2) 0.0154(8) Uani 1 1 d . . . . .
Re2 Re 0.50438(2) 0.36649(2) 0.74455(2) 0.01174(5) Uani 1 1 d . . . . .
O7 O 0.50044(19) -0.0801(3) 0.78023(17) 0.0233(7) Uani 1 1 d . . . . .
H7 H 0.516(3) -0.115(5) 0.754(3) 0.018(14) Uiso 1 1 d . . . . .
O8 O 0.47493(15) 0.2342(3) 0.89435(14) 0.0152(6) Uani 1 1 d . . . . .
O9 O 0.66171(16) 0.1336(3) 0.82784(16) 0.0197(6) Uani 1 1 d . . . . .
O10 O 0.43372(17) 0.5553(3) 0.63833(16) 0.0253(7) Uani 1 1 d . . . . .
O11 O 0.5093(2) 0.2022(3) 0.62157(16) 0.0276(7) Uani 1 1 d . . . . .
O12 O 0.35305(17) 0.2771(3) 0.74706(18) 0.0255(7) Uani 1 1 d . . . . .
N4 N 0.56013(18) 0.2480(3) 0.83094(16) 0.0114(6) Uani 1 1 d . . . . .
N5 N 0.50966(17) 0.4883(3) 0.83037(16) 0.0136(6) Uani 1 1 d . . . . .
N6 N 0.61583(17) 0.4188(3) 0.75676(17) 0.0131(6) Uani 1 1 d . . . . .
C20 C 0.5098(2) 0.0489(4) 0.7684(2) 0.0191(8) Uani 1 1 d . . . . .
H20A H 0.463319 0.088564 0.750071 0.023 Uiso 1 1 calc R U . . .
H20B H 0.540722 0.059929 0.735485 0.023 Uiso 1 1 calc R U . . .
C21 C 0.5442(2) 0.1082(4) 0.8357(2) 0.0141(7) Uani 1 1 d . . . . .
C22 C 0.4936(2) 0.1053(4) 0.8858(2) 0.0175(8) Uani 1 1 d . . . . .
H22A H 0.450660 0.055429 0.867363 0.021 Uiso 1 1 calc R U . . .
H22B H 0.517786 0.068781 0.929379 0.021 Uiso 1 1 calc R U . . .
C23 C 0.5386(2) 0.2970(4) 0.89372(19) 0.0136(7) Uani 1 1 d . . . . .
H23 H 0.575144 0.272430 0.934302 0.016 Uiso 1 1 calc R U . . .
C24 C 0.6189(2) 0.0547(4) 0.8611(2) 0.0188(8) Uani 1 1 d . . . . .
H24A H 0.633605 0.061264 0.910763 0.023 Uiso 1 1 calc R U . . .
H24B H 0.621533 -0.033600 0.847626 0.023 Uiso 1 1 calc R U . . .
C25 C 0.6400(2) 0.2541(4) 0.8415(2) 0.0147(8) Uani 1 1 d . . . . .
H25 H 0.659827 0.273256 0.890020 0.018 Uiso 1 1 calc R U . . .
C26 C 0.5313(2) 0.4362(4) 0.89148(19) 0.0126(7) Uani 1 1 d . . . . .
C27 C 0.5471(2) 0.5063(4) 0.9499(2) 0.0166(8) Uani 1 1 d . . . . .
H27 H 0.566467 0.467993 0.991921 0.020 Uiso 1 1 calc R U . . .
C28 C 0.5340(2) 0.6334(4) 0.9460(2) 0.0182(8) Uani 1 1 d . . . . .
H28 H 0.541538 0.682758 0.985739 0.022 Uiso 1 1 calc R U . . .
C29 C 0.5099(2) 0.6878(4) 0.8833(2) 0.0179(8) Uani 1 1 d . . . . .
H29 H 0.499625 0.774426 0.879340 0.022 Uiso 1 1 calc R U . . .
C30 C 0.5013(2) 0.6123(4) 0.8267(2) 0.0156(8) Uani 1 1 d . . . . .
H30 H 0.488904 0.650167 0.783488 0.019 Uiso 1 1 calc R U . . .
C31 C 0.6654(2) 0.3516(4) 0.7994(2) 0.0146(7) Uani 1 1 d . . . . .
C32 C 0.7379(2) 0.3765(4) 0.8085(2) 0.0174(8) Uani 1 1 d . . . . .
H32 H 0.771568 0.328101 0.838870 0.021 Uiso 1 1 calc R U . . .
C33 C 0.7599(2) 0.4730(4) 0.7724(2) 0.0216(9) Uani 1 1 d . . . . .
H33 H 0.809147 0.489818 0.776455 0.026 Uiso 1 1 calc R U . . .
C34 C 0.7091(2) 0.5449(4) 0.7303(2) 0.0228(9) Uani 1 1 d . . . . .
H34 H 0.722929 0.613467 0.706290 0.027 Uiso 1 1 calc R U . . .
C35 C 0.6381(2) 0.5148(4) 0.7239(2) 0.0182(8) Uani 1 1 d . . . . .
H35 H 0.603527 0.564134 0.695069 0.022 Uiso 1 1 calc R U . . .
C36 C 0.4614(2) 0.4869(4) 0.6781(2) 0.0159(8) Uani 1 1 d . . . . .
C37 C 0.5083(2) 0.2599(4) 0.6686(2) 0.0188(8) Uani 1 1 d . . . . .
C38 C 0.4087(2) 0.3106(4) 0.7459(2) 0.0165(8) Uani 1 1 d . . . . .
Br1 Br 0.16728(2) 1.28919(4) 0.55181(2) 0.02196(10) Uani 1 1 d . . . . .
Br2 Br 0.56354(2) -0.18844(4) 0.65744(2) 0.02283(10) 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 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
N2 Re1 N1 78.31(12) . . ?
N3 Re1 N1 77.33(12) . . ?
N3 Re1 N2 85.42(12) . . ?
C17 Re1 N1 174.35(15) . . ?
C17 Re1 N2 99.31(15) . . ?
C17 Re1 N3 97.44(15) . . ?
C17 Re1 C18 87.22(16) . . ?
C17 Re1 C19 85.15(17) . . ?
C18 Re1 N1 94.75(14) . . ?
C18 Re1 N2 171.94(15) . . ?
C18 Re1 N3 89.08(14) . . ?
C18 Re1 C19 94.41(17) . . ?
C19 Re1 N1 99.95(14) . . ?
C19 Re1 N2 90.86(15) . . ?
C19 Re1 N3 175.76(15) . . ?
C1 O1 H1 108(5) . . ?
C4 O2 C3 103.0(3) . . ?
C6 O3 C5 104.4(3) . . ?
C2 N1 Re1 122.9(2) . . ?
C4 N1 Re1 110.2(2) . . ?
C4 N1 C2 103.4(3) . . ?
C6 N1 Re1 107.3(2) . . ?
C6 N1 C2 101.5(3) . . ?
C6 N1 C4 111.2(3) . . ?
C7 N2 Re1 116.5(3) . . ?
C7 N2 C11 118.4(3) . . ?
C11 N2 Re1 124.8(3) . . ?
C12 N3 Re1 116.3(3) . . ?
C12 N3 C16 118.3(3) . . ?
C16 N3 Re1 125.0(3) . . ?
O1 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
O1 C1 C2 108.7(3) . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
C1 C2 N1 114.2(3) . . ?
C3 C2 N1 101.8(3) . . ?
C3 C2 C1 109.1(3) . . ?
C3 C2 C5 116.5(4) . . ?
C5 C2 N1 103.7(3) . . ?
C5 C2 C1 111.2(3) . . ?
O2 C3 C2 102.8(3) . . ?
O2 C3 H3A 111.2 . . ?
O2 C3 H3B 111.2 . . ?
C2 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
O2 C4 N1 105.7(3) . . ?
O2 C4 H4 109.1 . . ?
O2 C4 C7 108.8(3) . . ?
N1 C4 H4 109.1 . . ?
C7 C4 N1 114.8(3) . . ?
C7 C4 H4 109.1 . . ?
O3 C5 C2 105.6(3) . . ?
O3 C5 H5A 110.6 . . ?
O3 C5 H5B 110.6 . . ?
C2 C5 H5A 110.6 . . ?
C2 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
O3 C6 N1 104.4(3) . . ?
O3 C6 H6 109.6 . . ?
O3 C6 C12 109.3(3) . . ?
N1 C6 H6 109.6 . . ?
C12 C6 N1 114.3(3) . . ?
C12 C6 H6 109.6 . . ?
N2 C7 C4 118.5(3) . . ?
N2 C7 C8 122.2(4) . . ?
C8 C7 C4 119.3(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 120.8 . . ?
C8 C9 C10 118.5(4) . . ?
C10 C9 H9 120.8 . . ?
C9 C10 H10 120.6 . . ?
C11 C10 C9 118.8(4) . . ?
C11 C10 H10 120.6 . . ?
N2 C11 C10 122.5(4) . . ?
N2 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
N3 C12 C6 117.0(3) . . ?
N3 C12 C13 122.4(4) . . ?
C13 C12 C6 120.5(4) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.6(4) . . ?
C14 C13 H13 120.7 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.3(4) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 118.9(4) . . ?
C16 C15 H15 120.5 . . ?
N3 C16 C15 122.2(4) . . ?
N3 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
O4 C17 Re1 174.7(4) . . ?
O5 C18 Re1 177.9(4) . . ?
O6 C19 Re1 176.9(4) . . ?
N5 Re2 N4 77.25(12) . . ?
N5 Re2 N6 82.74(12) . . ?
N6 Re2 N4 76.08(12) . . ?
C36 Re2 N4 172.29(15) . . ?
C36 Re2 N5 95.72(15) . . ?
C36 Re2 N6 100.09(15) . . ?
C36 Re2 C37 85.47(18) . . ?
C36 Re2 C38 87.00(17) . . ?
C37 Re2 N4 101.27(15) . . ?
C37 Re2 N5 175.10(15) . . ?
C37 Re2 N6 92.38(16) . . ?
C37 Re2 C38 91.37(18) . . ?
C38 Re2 N4 96.50(14) . . ?
C38 Re2 N5 93.44(15) . . ?
C38 Re2 N6 172.21(15) . . ?
C20 O7 H7 106(4) . . ?
C23 O8 C22 102.6(3) . . ?
C25 O9 C24 103.0(3) . . ?
C21 N4 Re2 122.1(2) . . ?
C23 N4 Re2 106.8(2) . . ?
C23 N4 C21 101.1(3) . . ?
C25 N4 Re2 113.1(2) . . ?
C25 N4 C21 104.2(3) . . ?
C25 N4 C23 108.4(3) . . ?
C26 N5 Re2 116.4(3) . . ?
C30 N5 Re2 124.8(3) . . ?
C30 N5 C26 118.3(3) . . ?
C31 N6 Re2 118.7(3) . . ?
C35 N6 Re2 123.3(3) . . ?
C35 N6 C31 118.0(3) . . ?
O7 C20 H20A 110.2 . . ?
O7 C20 H20B 110.2 . . ?
O7 C20 C21 107.5(3) . . ?
H20A C20 H20B 108.5 . . ?
C21 C20 H20A 110.2 . . ?
C21 C20 H20B 110.2 . . ?
N4 C21 C22 102.8(3) . . ?
C20 C21 N4 113.8(3) . . ?
C20 C21 C22 111.4(3) . . ?
C20 C21 C24 110.2(3) . . ?
C24 C21 N4 101.6(3) . . ?
C24 C21 C22 116.5(3) . . ?
O8 C22 C21 105.4(3) . . ?
O8 C22 H22A 110.7 . . ?
O8 C22 H22B 110.7 . . ?
C21 C22 H22A 110.7 . . ?
C21 C22 H22B 110.7 . . ?
H22A C22 H22B 108.8 . . ?
O8 C23 N4 103.6(3) . . ?
O8 C23 H23 109.4 . . ?
O8 C23 C26 113.8(3) . . ?
N4 C23 H23 109.4 . . ?
C26 C23 N4 111.1(3) . . ?
C26 C23 H23 109.4 . . ?
O9 C24 C21 102.1(3) . . ?
O9 C24 H24A 111.3 . . ?
O9 C24 H24B 111.3 . . ?
C21 C24 H24A 111.3 . . ?
C21 C24 H24B 111.3 . . ?
H24A C24 H24B 109.2 . . ?
O9 C25 N4 105.5(3) . . ?
O9 C25 H25 108.4 . . ?
O9 C25 C31 112.7(3) . . ?
N4 C25 H25 108.4 . . ?
C31 C25 N4 113.2(3) . . ?
C31 C25 H25 108.4 . . ?
N5 C26 C23 116.8(3) . . ?
N5 C26 C27 122.4(4) . . ?
C27 C26 C23 120.9(4) . . ?
C26 C27 H27 120.6 . . ?
C26 C27 C28 118.8(4) . . ?
C28 C27 H27 120.6 . . ?
C27 C28 H28 120.4 . . ?
C27 C28 C29 119.2(4) . . ?
C29 C28 H28 120.4 . . ?
C28 C29 H29 120.9 . . ?
C30 C29 C28 118.2(4) . . ?
C30 C29 H29 120.9 . . ?
N5 C30 C29 122.7(4) . . ?
N5 C30 H30 118.6 . . ?
C29 C30 H30 118.6 . . ?
N6 C31 C25 117.9(3) . . ?
N6 C31 C32 122.2(4) . . ?
C32 C31 C25 119.7(4) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 C31 118.8(4) . . ?
C33 C32 H32 120.6 . . ?
C32 C33 H33 120.5 . . ?
C32 C33 C34 119.1(4) . . ?
C34 C33 H33 120.5 . . ?
C33 C34 H34 120.6 . . ?
C35 C34 C33 118.8(4) . . ?
C35 C34 H34 120.6 . . ?
N6 C35 C34 122.9(4) . . ?
N6 C35 H35 118.5 . . ?
C34 C35 H35 118.5 . . ?
O10 C36 Re2 177.4(4) . . ?
O11 C37 Re2 176.4(4) . . ?
O12 C38 Re2 179.4(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
Re1 N1 2.245(3) . ?
Re1 N2 2.171(3) . ?
Re1 N3 2.169(3) . ?
Re1 C17 1.923(4) . ?
Re1 C18 1.933(4) . ?
Re1 C19 1.938(4) . ?
O1 H1 0.86(8) . ?
O1 C1 1.416(5) . ?
O2 C3 1.430(5) . ?
O2 C4 1.407(5) . ?
O3 C5 1.441(5) . ?
O3 C6 1.401(5) . ?
O4 C17 1.141(5) . ?
O5 C18 1.146(5) . ?
O6 C19 1.137(5) . ?
N1 C2 1.544(5) . ?
N1 C4 1.518(5) . ?
N1 C6 1.516(5) . ?
N2 C7 1.346(5) . ?
N2 C11 1.351(5) . ?
N3 C12 1.344(5) . ?
N3 C16 1.347(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.537(6) . ?
C2 C3 1.528(6) . ?
C2 C5 1.534(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 1.0000 . ?
C4 C7 1.502(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6 1.0000 . ?
C6 C12 1.502(5) . ?
C7 C8 1.388(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.399(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(6) . ?
C16 H16 0.9500 . ?
Re2 N4 2.248(3) . ?
Re2 N5 2.162(3) . ?
Re2 N6 2.179(3) . ?
Re2 C36 1.924(4) . ?
Re2 C37 1.933(4) . ?
Re2 C38 1.941(4) . ?
O7 H7 0.77(6) . ?
O7 C20 1.422(5) . ?
O8 C22 1.448(5) . ?
O8 C23 1.399(5) . ?
O9 C24 1.444(5) . ?
O9 C25 1.403(5) . ?
O10 C36 1.137(5) . ?
O11 C37 1.141(6) . ?
O12 C38 1.133(5) . ?
N4 C21 1.538(5) . ?
N4 C23 1.514(5) . ?
N4 C25 1.508(5) . ?
N5 C26 1.344(5) . ?
N5 C30 1.341(5) . ?
N6 C31 1.353(5) . ?
N6 C35 1.344(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.526(6) . ?
C21 C22 1.546(5) . ?
C21 C24 1.532(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23 1.0000 . ?
C23 C26 1.500(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25 1.0000 . ?
C25 C31 1.495(6) . ?
C26 C27 1.382(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.387(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.394(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.384(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.390(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.383(6) . ?
C35 H35 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 Br1 0.86(8) 2.35(8) 3.204(4) 170(7) . yes
O7 H7 Br2 0.77(6) 2.45(6) 3.208(4) 169(5) . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 N1 C2 C1 -17.2(4) . . . . ?
Re1 N1 C2 C3 -134.7(3) . . . . ?
Re1 N1 C2 C5 104.0(3) . . . . ?
Re1 N1 C4 O2 113.5(3) . . . . ?
Re1 N1 C4 C7 -6.4(4) . . . . ?
Re1 N1 C6 O3 -92.0(3) . . . . ?
Re1 N1 C6 C12 27.4(4) . . . . ?
Re1 N2 C7 C4 12.4(4) . . . . ?
Re1 N2 C7 C8 -171.8(3) . . . . ?
Re1 N2 C11 C10 171.9(3) . . . . ?
Re1 N3 C12 C6 -9.4(4) . . . . ?
Re1 N3 C12 C13 166.9(3) . . . . ?
Re1 N3 C16 C15 -167.8(3) . . . . ?
O1 C1 C2 N1 177.9(3) . . . . ?
O1 C1 C2 C3 -69.0(4) . . . . ?
O1 C1 C2 C5 60.9(4) . . . . ?
O2 C4 C7 N2 -121.7(4) . . . . ?
O2 C4 C7 C8 62.4(5) . . . . ?
O3 C6 C12 N3 103.2(4) . . . . ?
O3 C6 C12 C13 -73.2(5) . . . . ?
N1 C2 C3 O2 35.0(4) . . . . ?
N1 C2 C5 O3 -10.9(4) . . . . ?
N1 C4 C7 N2 -3.5(5) . . . . ?
N1 C4 C7 C8 -179.4(3) . . . . ?
N1 C6 C12 N3 -13.4(5) . . . . ?
N1 C6 C12 C13 170.2(3) . . . . ?
N2 C7 C8 C9 -0.4(6) . . . . ?
N3 C12 C13 C14 2.8(6) . . . . ?
C1 C2 C3 O2 -86.1(4) . . . . ?
C1 C2 C5 O3 112.3(4) . . . . ?
C2 N1 C4 O2 -19.5(4) . . . . ?
C2 N1 C4 C7 -139.4(3) . . . . ?
C2 N1 C6 O3 38.1(4) . . . . ?
C2 N1 C6 C12 157.4(3) . . . . ?
C3 O2 C4 N1 43.0(4) . . . . ?
C3 O2 C4 C7 166.8(3) . . . . ?
C3 C2 C5 O3 -121.8(4) . . . . ?
C4 O2 C3 C2 -49.0(4) . . . . ?
C4 N1 C2 C1 108.0(4) . . . . ?
C4 N1 C2 C3 -9.5(4) . . . . ?
C4 N1 C2 C5 -130.8(3) . . . . ?
C4 N1 C6 O3 147.5(3) . . . . ?
C4 N1 C6 C12 -93.2(4) . . . . ?
C4 C7 C8 C9 175.4(4) . . . . ?
C5 O3 C6 N1 -46.7(4) . . . . ?
C5 O3 C6 C12 -169.4(3) . . . . ?
C5 C2 C3 O2 147.0(4) . . . . ?
C6 O3 C5 C2 35.7(4) . . . . ?
C6 N1 C2 C1 -136.7(3) . . . . ?
C6 N1 C2 C3 105.9(3) . . . . ?
C6 N1 C2 C5 -15.5(4) . . . . ?
C6 N1 C4 O2 -127.7(3) . . . . ?
C6 N1 C4 C7 112.4(4) . . . . ?
C6 C12 C13 C14 179.0(4) . . . . ?
C7 N2 C11 C10 -2.4(6) . . . . ?
C7 C8 C9 C10 -2.7(6) . . . . ?
C8 C9 C10 C11 3.2(6) . . . . ?
C9 C10 C11 N2 -0.7(6) . . . . ?
C11 N2 C7 C4 -172.9(3) . . . . ?
C11 N2 C7 C8 2.9(6) . . . . ?
C12 N3 C16 C15 4.0(6) . . . . ?
C12 C13 C14 C15 1.7(6) . . . . ?
C13 C14 C15 C16 -3.2(6) . . . . ?
C14 C15 C16 N3 0.3(6) . . . . ?
C16 N3 C12 C6 178.1(3) . . . . ?
C16 N3 C12 C13 -5.6(6) . . . . ?
Re2 N4 C21 C20 20.8(4) . . . . ?
Re2 N4 C21 C22 -99.9(3) . . . . ?
Re2 N4 C21 C24 139.2(3) . . . . ?
Re2 N4 C23 O8 86.0(3) . . . . ?
Re2 N4 C23 C26 -36.5(3) . . . . ?
Re2 N4 C25 O9 -115.0(3) . . . . ?
Re2 N4 C25 C31 8.7(4) . . . . ?
Re2 N5 C26 C23 -9.0(4) . . . . ?
Re2 N5 C26 C27 170.3(3) . . . . ?
Re2 N5 C30 C29 -175.4(3) . . . . ?
Re2 N6 C31 C25 -6.6(5) . . . . ?
Re2 N6 C31 C32 178.0(3) . . . . ?
Re2 N6 C35 C34 -177.9(3) . . . . ?
O7 C20 C21 N4 178.1(3) . . . . ?
O7 C20 C21 C22 -66.1(4) . . . . ?
O7 C20 C21 C24 64.8(4) . . . . ?
O8 C23 C26 N5 -84.7(4) . . . . ?
O8 C23 C26 C27 96.0(4) . . . . ?
O9 C25 C31 N6 117.9(4) . . . . ?
O9 C25 C31 C32 -66.5(5) . . . . ?
N4 C21 C22 O8 10.4(4) . . . . ?
N4 C21 C24 O9 -35.0(4) . . . . ?
N4 C23 C26 N5 31.8(5) . . . . ?
N4 C23 C26 C27 -147.5(4) . . . . ?
N4 C25 C31 N6 -1.8(5) . . . . ?
N4 C25 C31 C32 173.8(4) . . . . ?
N5 C26 C27 C28 5.9(6) . . . . ?
N6 C31 C32 C33 -0.2(6) . . . . ?
C20 C21 C22 O8 -112.0(4) . . . . ?
C20 C21 C24 O9 86.0(4) . . . . ?
C21 N4 C23 O8 -42.7(3) . . . . ?
C21 N4 C23 C26 -165.2(3) . . . . ?
C21 N4 C25 O9 19.7(4) . . . . ?
C21 N4 C25 C31 143.4(3) . . . . ?
C22 O8 C23 N4 50.6(3) . . . . ?
C22 O8 C23 C26 171.3(3) . . . . ?
C22 C21 C24 O9 -145.8(4) . . . . ?
C23 O8 C22 C21 -37.6(4) . . . . ?
C23 N4 C21 C20 138.9(3) . . . . ?
C23 N4 C21 C22 18.2(4) . . . . ?
C23 N4 C21 C24 -102.7(3) . . . . ?
C23 N4 C25 O9 126.7(3) . . . . ?
C23 N4 C25 C31 -109.6(4) . . . . ?
C23 C26 C27 C28 -174.8(4) . . . . ?
C24 O9 C25 N4 -43.2(4) . . . . ?
C24 O9 C25 C31 -167.3(3) . . . . ?
C24 C21 C22 O8 120.4(4) . . . . ?
C25 O9 C24 C21 49.2(4) . . . . ?
C25 N4 C21 C20 -108.7(4) . . . . ?
C25 N4 C21 C22 130.6(3) . . . . ?
C25 N4 C21 C24 9.7(4) . . . . ?
C25 N4 C23 O8 -151.8(3) . . . . ?
C25 N4 C23 C26 85.6(4) . . . . ?
C25 C31 C32 C33 -175.6(4) . . . . ?
C26 N5 C30 C29 -3.9(6) . . . . ?
C26 C27 C28 C29 -4.1(6) . . . . ?
C27 C28 C29 C30 -1.4(6) . . . . ?
C28 C29 C30 N5 5.6(6) . . . . ?
C30 N5 C26 C23 178.7(3) . . . . ?
C30 N5 C26 C27 -2.0(6) . . . . ?
C31 N6 C35 C34 2.2(6) . . . . ?
C31 C32 C33 C34 2.4(7) . . . . ?
C32 C33 C34 C35 -2.3(7) . . . . ?
C33 C34 C35 N6 0.0(7) . . . . ?
C35 N6 C31 C25 173.4(4) . . . . ?
C35 N6 C31 C32 -2.1(6) . . . . ?
