#------------------------------------------------------------------------------
#$Date: 2020-09-10 04:16:19 +0300 (Thu, 10 Sep 2020) $
#$Revision: 256286 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/90/1559028.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_1559028
loop_
_publ_author_name
'Donnelly, Liam J.'
'Parsons, Simon'
'Morrison, Carole A.'
'Thomas, Stephen P.'
'Love, Jason B.'
_publ_section_title
;
 Synthesis and structures of anionic rhenium polyhydride complexes of
 boron--hydride ligands and their application in catalysis
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03458D
_journal_year                    2020
_chemical_formula_moiety         'C32 H64 B4 Re, C16 H34.03 K O8'
_chemical_formula_sum            'C48 H98.03 B4 K O8 Re'
_chemical_formula_weight         1071.83
_chemical_name_systematic        '[ReH8BBN4][K(18c6)(DME)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)

_shelx_SHELXL_version_number      2018/3

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

_publ_contact_author_address      'University of Edinburgh, Joseph Black Building, David Brewster Road, Edinburgh, EH9 3FJ' 
_publ_contact_author_email        'jason.love@ed.ac.uk, Stephen.Thomas@ed.ac.uk'
_publ_contact_author_name         'Liam J. Donnelly, Simon Parsons, Gary S. Nichol, Stephen P. Thomas* and Jason B. Love*'
_publ_contact_author_fax          ?
_publ_contact_author_phone        ?
_publ_requested_journal           ?
_publ_section_title               'Synthesis and Structures of Anionic Rhenium Boryl Polyhydrides and their Catalysis'
_publ_section_abstract            'The anionic rhenium boryl hydride complex, [ReH7(Bpin)3]-, has been synthesized by exhaustive deoxygenation of perrhenate (ReO4-) with HBpin. X-ray diffraction, NMR and IR spectroscopy analysis supports its structure as a polyhydridic Re centre with trigonal planar geometry with respect to the boryl ligands. This complex was applied in the catalytic hydroboration N-heteroaromatic substrates using [NR4][ReO4] as a precatalyst and in the stoichiometric C-H borylation of arenes. The reactivity of  [ReH7(Bpin)3]- was further explored through reactions with 9-BBN or PPh3 to produce the corresponding derivatized complexes. This work represent the first example for the synthesis of Re compounds bearing boron-centred ligands in the Re(III), Re(V) and Re(VII) oxidation states.'

;
_audit_update_record
;
2020-01-21 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                96.7140(10)
_cell_angle_beta                 91.2900(10)
_cell_angle_gamma                102.351(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2627(2)
_cell_length_b                   15.9727(3)
_cell_length_c                   16.0123(2)
_cell_measurement_reflns_used    39271
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      30.3910
_cell_measurement_theta_min      3.6110
_cell_volume                     2791.22(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      220.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -39.00   1.00   15.00    --  -24.15-178.00 -90.00   65
  2  ω      2.00  96.00   1.00   15.00    --   25.71  57.00 -90.00   94
  3  ω     -7.00  39.00   1.00   15.00    --   25.71  77.00 120.00   46
  4  ω     -7.00  39.00   1.00   15.00    --   25.71  77.00   0.00   46
  5  ω    -41.00 101.00   1.00   15.00    --   25.71  19.00  90.00  142
  6  ω    -20.00  71.00   1.00   15.00    --   25.71 -99.00-120.00   91
  7  ω    -45.00  49.00   1.00   15.00    --   25.71 -57.00 120.00   94
  8  ω    -39.00   9.00   1.00   15.00    --  -24.15 -77.00  30.00   48
  9  ω    -57.00  39.00   1.00   15.00    --  -24.15  77.00  30.00   96
 10  ω     35.00 108.00   1.00   15.00    --   25.71-178.00 150.00   73
 11  ω    -45.00  49.00   1.00   15.00    --   25.71 -57.00 -90.00   94
 12  ω     -7.00  39.00   1.00   15.00    --   25.71  77.00-120.00   46
 13  ω      2.00  96.00   1.00   15.00    --   25.71  57.00-180.00   94
 14  ω     -7.00  39.00   1.00   15.00    --   25.71  77.00  30.00   46
 15  ω     -7.00  39.00   1.00   15.00    --   25.71  77.00 -60.00   46
 16  ω    -20.00  15.00   1.00   15.00    --   25.71 -99.00  90.00   35
 17  ω      2.00  96.00   1.00   15.00    --   25.71  57.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0468719000
_diffrn_orient_matrix_UB_12      -0.0372368000
_diffrn_orient_matrix_UB_13      0.0016483000
_diffrn_orient_matrix_UB_21      0.0434967000
_diffrn_orient_matrix_UB_22      -0.0262642000
_diffrn_orient_matrix_UB_23      -0.0039702000
_diffrn_orient_matrix_UB_31      0.0087993000
_diffrn_orient_matrix_UB_32      0.0047725000
_diffrn_orient_matrix_UB_33      0.0444494000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73081
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.525
_diffrn_reflns_theta_min         3.326
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Clear Red'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       Block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         15734
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0181P)²+0.7134P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14293
_reflns_number_total             15734
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03458d2.cif
_cod_data_source_block           j19010_refinalised
_cod_database_code               1559028
_chemical_oxdiff_formula         'Re1 B4 C100 K1 O10 H100'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.865
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.43424(2) 0.72546(2) 0.25407(2) 0.02168(2) Uani 1 1 d . . . . .
H1A H 0.5146(18) 0.6549(13) 0.2944(12) 0.038(5) Uiso 1 1 d . . . . .
H1B H 0.5738(18) 0.7248(13) 0.2108(12) 0.037(5) Uiso 1 1 d . . . . .
H2A H 0.4506(18) 0.7508(13) 0.3628(12) 0.037(5) Uiso 1 1 d . . . . .
H2B H 0.3011(18) 0.7303(14) 0.3026(13) 0.044(6) Uiso 1 1 d . . . . .
H3A H 0.5167(19) 0.8330(14) 0.2708(13) 0.046(6) Uiso 1 1 d . . . . .
H3B H 0.3646(18) 0.7995(14) 0.2108(12) 0.041(6) Uiso 1 1 d . . . . .
H4A H 0.4123(17) 0.6924(13) 0.1476(11) 0.033(5) Uiso 1 1 d . . . . .
H4B H 0.3467(19) 0.6264(14) 0.2350(13) 0.048(6) Uiso 1 1 d . . . . .
C11 C 0.71674(17) 0.74149(13) 0.33287(11) 0.0352(4) Uani 1 1 d . . . . .
H11 H 0.680376 0.786176 0.364244 0.042 Uiso 1 1 calc R . . . .
C12 C 0.8262(2) 0.78671(15) 0.28676(16) 0.0514(6) Uani 1 1 d . . . . .
H12A H 0.801224 0.831499 0.257963 0.062 Uiso 1 1 calc R . . . .
H12B H 0.890782 0.815703 0.328913 0.062 Uiso 1 1 calc R . . . .
C13 C 0.8791(2) 0.72826(17) 0.22229(17) 0.0591(7) Uani 1 1 d . . . . .
H13A H 0.930458 0.764319 0.185713 0.071 Uiso 1 1 calc R . . . .
H13B H 0.931350 0.698523 0.252173 0.071 Uiso 1 1 calc R . . . .
C14 C 0.7842(2) 0.66125(17) 0.16782(14) 0.0514(6) Uani 1 1 d . . . . .
H14A H 0.824724 0.618659 0.138390 0.062 Uiso 1 1 calc R . . . .
H14B H 0.750394 0.689886 0.125014 0.062 Uiso 1 1 calc R . . . .
C15 C 0.67832(17) 0.61297(13) 0.21505(11) 0.0338(4) Uani 1 1 d . . . . .
H15 H 0.617449 0.575903 0.173324 0.041 Uiso 1 1 calc R . . . .
C16 C 0.7187(2) 0.55637(14) 0.27642(15) 0.0483(5) Uani 1 1 d . . . . .
H16A H 0.645945 0.518217 0.294081 0.058 Uiso 1 1 calc R . . . .
H16B H 0.767177 0.519657 0.246027 0.058 Uiso 1 1 calc R . . . .
C17 C 0.7926(2) 0.60417(17) 0.35492(15) 0.0561(6) Uani 1 1 d . . . . .
H17A H 0.791395 0.563798 0.396664 0.067 Uiso 1 1 calc R . . . .
H17B H 0.877286 0.623363 0.340317 0.067 Uiso 1 1 calc R . . . .
C18 C 0.7479(2) 0.68182(17) 0.39467(13) 0.0499(6) Uani 1 1 d . . . . .
H18A H 0.810527 0.715792 0.435925 0.060 Uiso 1 1 calc R . . . .
H18B H 0.675140 0.661255 0.425343 0.060 Uiso 1 1 calc R . . . .
C21 C 0.31230(18) 0.82669(13) 0.43305(11) 0.0358(4) Uani 1 1 d . . . . .
H21 H 0.347173 0.878024 0.405257 0.043 Uiso 1 1 calc R . . . .
C22 C 0.3764(2) 0.83637(16) 0.52084(13) 0.0542(6) Uani 1 1 d . . . . .
H22A H 0.464447 0.851971 0.514495 0.065 Uiso 1 1 calc R . . . .
H22B H 0.353883 0.884691 0.555669 0.065 Uiso 1 1 calc R . . . .
C23 C 0.3493(2) 0.75774(18) 0.56818(13) 0.0578(7) Uani 1 1 d . . . . .
H23A H 0.269089 0.753650 0.591950 0.069 Uiso 1 1 calc R . . . .
H23B H 0.409575 0.766050 0.615177 0.069 Uiso 1 1 calc R . . . .
C24 C 0.3506(2) 0.67274(17) 0.51391(13) 0.0526(6) Uani 1 1 d . . . . .
H24A H 0.311863 0.624960 0.544145 0.063 Uiso 1 1 calc R . . . .
H24B H 0.435373 0.668568 0.506751 0.063 Uiso 1 1 calc R . . . .
C25 C 0.28611(18) 0.66131(13) 0.42639(11) 0.0361(4) Uani 1 1 d . . . . .
H25 H 0.301959 0.608755 0.393405 0.043 Uiso 1 1 calc R . . . .
C26 C 0.14733(19) 0.65396(15) 0.42757(14) 0.0482(5) Uani 1 1 d . . . . .
H26A H 0.113203 0.637989 0.369625 0.058 Uiso 1 1 calc R . . . .
H26B H 0.112634 0.606640 0.459608 0.058 Uiso 1 1 calc R . . . .
C27 C 0.1060(2) 0.73437(17) 0.46462(16) 0.0555(6) Uani 1 1 d . . . . .
H27A H 0.115771 0.739808 0.526116 0.067 Uiso 1 1 calc R . . . .
H27B H 0.019080 0.727042 0.449945 0.067 Uiso 1 1 calc R . . . .
C28 C 0.1746(2) 0.81765(16) 0.43485(15) 0.0524(6) Uani 1 1 d . . . . .
H28A H 0.157871 0.866672 0.471943 0.063 Uiso 1 1 calc R . . . .
H28B H 0.142934 0.820906 0.378080 0.063 Uiso 1 1 calc R . . . .
C31 C 0.4090(2) 0.94689(13) 0.25212(12) 0.0399(5) Uani 1 1 d . . . . .
H31 H 0.367506 0.936952 0.305051 0.048 Uiso 1 1 calc R . . . .
C32 C 0.5209(3) 1.02200(15) 0.27144(15) 0.0600(7) Uani 1 1 d . . . . .
H32A H 0.492302 1.075214 0.287153 0.072 Uiso 1 1 calc R . . . .
H32B H 0.566734 1.011468 0.320448 0.072 Uiso 1 1 calc R . . . .
C33 C 0.6070(3) 1.03667(17) 0.20073(19) 0.0702(8) Uani 1 1 d . . . . .
H33A H 0.684853 1.072358 0.224625 0.084 Uiso 1 1 calc R . . . .
H33B H 0.573626 1.069641 0.161686 0.084 Uiso 1 1 calc R . . . .
C34 C 0.6312(2) 0.95579(15) 0.15102(16) 0.0514(6) Uani 1 1 d . . . . .
H34A H 0.693446 0.936008 0.182470 0.062 Uiso 1 1 calc R . . . .
H34B H 0.665187 0.971071 0.097619 0.062 Uiso 1 1 calc R . . . .
C35 C 0.52127(17) 0.88061(12) 0.13161(11) 0.0318(4) Uani 1 1 d . . . . .
H35 H 0.550582 0.828631 0.109179 0.038 Uiso 1 1 calc R . . . .
C36 C 0.4276(2) 0.89595(14) 0.06752(12) 0.0420(5) Uani 1 1 d . . . . .
H36A H 0.469243 0.910983 0.016475 0.050 Uiso 1 1 calc R . . . .
H36B H 0.367448 0.841773 0.052204 0.050 Uiso 1 1 calc R . . . .
C37 C 0.3612(2) 0.96601(15) 0.09733(13) 0.0480(5) Uani 1 1 d . . . . .
H37A H 0.290977 0.961434 0.058473 0.058 Uiso 1 1 calc R . . . .
H37B H 0.415600 1.022341 0.094775 0.058 Uiso 1 1 calc R . . . .
C38 C 0.3167(2) 0.96283(16) 0.18659(14) 0.0496(6) Uani 1 1 d . . . . .
H38A H 0.243043 0.916951 0.184858 0.060 Uiso 1 1 calc R . . . .
H38B H 0.294075 1.017647 0.205512 0.060 Uiso 1 1 calc R . . . .
C41 C 0.35832(17) 0.53741(12) 0.10218(11) 0.0326(4) Uani 1 1 d . . . . .
H41 H 0.439062 0.531047 0.122804 0.039 Uiso 1 1 calc R . . . .
C42 C 0.3646(2) 0.55010(17) 0.00885(12) 0.0511(6) Uani 1 1 d . . . . .
H42A H 0.436320 0.595409 0.002093 0.061 Uiso 1 1 calc R . . . .
H42B H 0.376179 0.496508 -0.023122 0.061 Uiso 1 1 calc R . . . .
C43 C 0.2535(2) 0.57437(17) -0.02937(13) 0.0560(6) Uani 1 1 d . . . . .
H43A H 0.275491 0.597233 -0.082457 0.067 Uiso 1 1 calc R . . . .
H43B H 0.189666 0.521824 -0.042710 0.067 Uiso 1 1 calc R . . . .
C44 C 0.2019(2) 0.64028(15) 0.02595(14) 0.0494(6) Uani 1 1 d . . . . .
H44A H 0.119274 0.638440 0.004031 0.059 Uiso 1 1 calc R . . . .
H44B H 0.251030 0.697839 0.020830 0.059 Uiso 1 1 calc R . . . .
C45 C 0.19629(17) 0.62897(13) 0.12036(12) 0.0362(4) Uani 1 1 d . . . . .
H45 H 0.176139 0.681075 0.151376 0.043 Uiso 1 1 calc R . . . .
C46 C 0.10282(19) 0.54946(16) 0.13925(16) 0.0537(6) Uani 1 1 d . . . . .
H46A H 0.097466 0.551568 0.200432 0.064 Uiso 1 1 calc R . . . .
H46B H 0.022974 0.552625 0.115850 0.064 Uiso 1 1 calc R . . . .
C47 C 0.1299(2) 0.46333(15) 0.10489(17) 0.0555(6) Uani 1 1 d . . . . .
H47A H 0.109625 0.452659 0.044195 0.067 Uiso 1 1 calc R . . . .
H47B H 0.077477 0.417490 0.131169 0.067 Uiso 1 1 calc R . . . .
C48 C 0.2623(2) 0.45834(14) 0.12003(15) 0.0492(5) Uani 1 1 d . . . . .
H48A H 0.276780 0.407447 0.084744 0.059 Uiso 1 1 calc R . . . .
H48B H 0.274242 0.449388 0.178876 0.059 Uiso 1 1 calc R . . . .
B1 B 0.61737(18) 0.68419(14) 0.26470(12) 0.0269(4) Uani 1 1 d . . . . .
B2 B 0.34015(18) 0.74304(14) 0.37888(12) 0.0285(4) Uani 1 1 d . . . . .
B3 B 0.45421(18) 0.86185(13) 0.21716(12) 0.0274(4) Uani 1 1 d . . . . .
B4 B 0.32835(18) 0.62166(13) 0.15275(11) 0.0254(4) Uani 1 1 d . . . . .
K1 K 0.14210(4) 0.26336(3) 0.22620(3) 0.04038(10) Uani 1 1 d . . . . .
O1 O 0.33046(15) 0.24515(11) 0.11923(11) 0.0580(4) Uani 1 1 d . . . . .
O2 O 0.08592(17) 0.17376(11) 0.06071(9) 0.0577(4) Uani 1 1 d . . . . .
O3 O -0.08605(14) 0.25441(10) 0.13943(10) 0.0487(4) Uani 1 1 d . . . . .
O4 O -0.03894(13) 0.34135(10) 0.30259(9) 0.0454(3) Uani 1 1 d . . . . .
O5 O 0.20772(14) 0.40834(10) 0.35238(8) 0.0483(4) Uani 1 1 d . . . . .
O6 O 0.39119(14) 0.33417(12) 0.27958(11) 0.0562(4) Uani 1 1 d . . . . .
O7 O 0.17687(19) 0.17084(16) 0.36814(13) 0.0837(6) Uani 1 1 d . . . . .
C51 C 0.4778(2) 0.3325(2) 0.2167(2) 0.0729(8) Uani 1 1 d . . . . .
H51A H 0.558995 0.338685 0.243183 0.087 Uiso 1 1 calc R . . . .
H51B H 0.479590 0.380647 0.183715 0.087 Uiso 1 1 calc R . . . .
C52 C 0.4441(2) 0.2497(2) 0.1611(2) 0.0774(9) Uani 1 1 d . . . . .
H52A H 0.506282 0.246075 0.119812 0.093 Uiso 1 1 calc R . . . .
H52B H 0.438425 0.201425 0.194375 0.093 Uiso 1 1 calc R . . . .
C53 C 0.2951(3) 0.1725(2) 0.05761(19) 0.0771(9) Uani 1 1 d . . . . .
H53A H 0.277256 0.119607 0.084812 0.093 Uiso 1 1 calc R . . . .
H53B H 0.361485 0.168912 0.019731 0.093 Uiso 1 1 calc R . . . .
C54 C 0.1855(3) 0.1806(2) 0.00891(16) 0.0799(9) Uani 1 1 d . . . . .
H54A H 0.200580 0.236514 -0.012935 0.096 Uiso 1 1 calc R . . . .
H54B H 0.167370 0.134970 -0.039038 0.096 Uiso 1 1 calc R . . . .
C55 C -0.0237(3) 0.1825(2) 0.01910(16) 0.0752(9) Uani 1 1 d . . . . .
H55A H -0.048976 0.135250 -0.026788 0.090 Uiso 1 1 calc R . . . .
H55B H -0.009318 0.237193 -0.005130 0.090 Uiso 1 1 calc R . . . .
C56 C -0.1200(3) 0.18072(18) 0.07955(18) 0.0673(8) Uani 1 1 d . . . . .
H56A H -0.197361 0.180769 0.050368 0.081 Uiso 1 1 calc R . . . .
H56B H -0.130094 0.128319 0.107360 0.081 Uiso 1 1 calc R . . . .
C57 C -0.1792(2) 0.26347(17) 0.19602(17) 0.0579(7) Uani 1 1 d . . . . .
H57A H -0.193876 0.215267 0.229845 0.069 Uiso 1 1 calc R . . . .
H57B H -0.254968 0.262780 0.164406 0.069 Uiso 1 1 calc R . . . .
C58 C -0.1406(2) 0.34598(16) 0.25153(16) 0.0527(6) Uani 1 1 d . . . . .
H58A H -0.118971 0.393776 0.217613 0.063 Uiso 1 1 calc R . . . .
H58B H -0.207237 0.356271 0.286838 0.063 Uiso 1 1 calc R . . . .
C59 C 0.0035(2) 0.41904(16) 0.35786(14) 0.0555(6) Uani 1 1 d . . . . .
H59A H -0.060408 0.429390 0.395771 0.067 Uiso 1 1 calc R . . . .
H59B H 0.024469 0.468008 0.325337 0.067 Uiso 1 1 calc R . . . .
C60 C 0.1124(2) 0.41068(17) 0.40742(13) 0.0567(6) Uani 1 1 d . . . . .
H60A H 0.136038 0.459870 0.451578 0.068 Uiso 1 1 calc R . . . .
H60B H 0.094299 0.357588 0.434251 0.068 Uiso 1 1 calc R . . . .
C61 C 0.3196(2) 0.40983(18) 0.39628(15) 0.0605(7) Uani 1 1 d . . . . .
H61A H 0.312000 0.358299 0.425214 0.073 Uiso 1 1 calc R . . . .
H61B H 0.340212 0.460894 0.438565 0.073 Uiso 1 1 calc R . . . .
C62 C 0.4164(2) 0.41209(18) 0.33512(16) 0.0622(7) Uani 1 1 d . . . . .
H62A H 0.419789 0.461222 0.303199 0.075 Uiso 1 1 calc R . . . .
H62B H 0.495483 0.419039 0.364988 0.075 Uiso 1 1 calc R . . . .
C63 C 0.2855(3) 0.1576(2) 0.4040(2) 0.0905(10) Uani 1 1 d . . . . .
H63A H 0.298814 0.101765 0.380391 0.136 Uiso 1 1 calc GR . . . .
H63B H 0.279398 0.159068 0.464476 0.136 Uiso 1 1 calc GR . . . .
H63C H 0.353033 0.202672 0.391896 0.136 Uiso 1 1 calc GR . . . .
C64 C 0.0759(4) 0.1077(4) 0.3859(3) 0.1234(17) Uani 1 1 d D . . . .
H64A H 0.060847 0.116737 0.446014 0.148 Uiso 0.734(13) 1 calc R . P A 1
H64B H 0.094407 0.050387 0.373697 0.148 Uiso 0.734(13) 1 calc R . P A 1
H64C H 0.103216 0.073149 0.426173 0.148 Uiso 0.266(13) 1 calc R . P A 2
H64D H 0.016888 0.137150 0.413775 0.148 Uiso 0.266(13) 1 calc R . P A 2
C66 C -0.0090(3) 0.0171(3) 0.2025(3) 0.1057(14) Uani 1 1 d . . . . .
H66A H 0.012552 0.025062 0.145183 0.159 Uiso 0.734(13) 1 calc GR . P A 1
H66B H -0.086256 -0.023972 0.201701 0.159 Uiso 0.734(13) 1 calc GR . P A 1
H66C H 0.053526 -0.004679 0.230212 0.159 Uiso 0.734(13) 1 calc GR . P A 1
H66D H -0.032993 0.027081 0.146566 0.159 Uiso 0.28(3) 1 calc GR . P B 2
H66E H -0.078991 -0.014631 0.228238 0.159 Uiso 0.28(3) 1 calc GR . P B 2
H66F H 0.053785 -0.016153 0.198466 0.159 Uiso 0.28(3) 1 calc GR . P B 2
O8 O -0.0196(8) 0.1025(4) 0.2497(4) 0.0640(15) Uani 0.72(3) 1 d . . P A 1
C65 C -0.0315(4) 0.1103(5) 0.3377(4) 0.085(2) Uani 0.734(13) 1 d D . P A 1
H65A H -0.097640 0.063519 0.350609 0.101 Uiso 0.734(13) 1 calc R . P A 1
H65B H -0.055136 0.165015 0.355515 0.101 Uiso 0.734(13) 1 calc R . P A 1
O8A O 0.027(2) 0.0812(13) 0.2423(7) 0.065(5) Uani 0.28(3) 1 d . . P A 2
C65A C 0.019(2) 0.0543(12) 0.3207(8) 0.116(10) Uani 0.266(13) 1 d D . P A 2
H65C H -0.067455 0.039058 0.332299 0.139 Uiso 0.266(13) 1 calc R . P A 2
H65D H 0.049686 0.001070 0.318033 0.139 Uiso 0.266(13) 1 calc R . 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -5 -20 0.1979
-13 10 -12 0.0938
13 -10 12 0.0938
9 15 -6 0.0860
-9 -15 6 0.0860
9 12 10 0.0918
-6 -12 17 0.1291
0 -4 23 0.1508
-9 -14 -4 0.0695
-7 -10 -14 0.1160
-12 11 12 0.1313
14 -13 -7 0.0879
-1 22 1 0.0693
-2 22 -4 0.0724
1 -22 -1 0.0116
-7 17 11 0.1110
-9 20 -8 0.0731
3 -22 2 0.0115
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
B2 Re1 B1 115.06(7) . . ?
B3 Re1 B1 113.03(7) . . ?
B3 Re1 B2 99.20(7) . . ?
B4 Re1 B1 101.95(7) . . ?
B4 Re1 B2 115.82(7) . . ?
B4 Re1 B3 112.36(7) . . ?
C12 C11 B1 108.85(16) . . ?
C18 C11 C12 114.43(17) . . ?
C18 C11 B1 107.59(17) . . ?
C13 C12 C11 115.76(19) . . ?
C14 C13 C12 114.14(19) . . ?
C13 C14 C15 115.42(18) . . ?
C14 C15 B1 107.13(17) . . ?
C16 C15 C14 113.15(17) . . ?
C16 C15 B1 110.14(16) . . ?
C17 C16 C15 116.03(18) . . ?
C18 C17 C16 114.45(18) . . ?
C17 C18 C11 115.21(17) . . ?
C22 C21 B2 108.06(17) . . ?
C28 C21 C22 113.94(17) . . ?
C28 C21 B2 108.94(17) . . ?
C23 C22 C21 116.45(18) . . ?
C22 C23 C24 113.97(18) . . ?
C23 C24 C25 114.96(19) . . ?
C24 C25 C26 114.48(17) . . ?
C24 C25 B2 109.37(17) . . ?
C26 C25 B2 106.63(16) . . ?
C27 C26 C25 116.14(18) . . ?
C26 C27 C28 114.24(18) . . ?
C27 C28 C21 114.61(19) . . ?
C32 C31 C38 113.77(18) . . ?
C32 C31 B3 108.66(18) . . ?
C38 C31 B3 108.21(16) . . ?
C33 C32 C31 115.85(18) . . ?
C32 C33 C34 115.6(2) . . ?
C33 C34 C35 115.86(19) . . ?
C34 C35 C36 114.07(17) . . ?
C34 C35 B3 109.29(16) . . ?
C36 C35 B3 108.25(15) . . ?
C37 C36 C35 115.01(17) . . ?
C36 C37 C38 114.45(17) . . ?
C37 C38 C31 115.21(17) . . ?
C42 C41 C48 113.99(17) . . ?
C42 C41 B4 108.24(16) . . ?
C48 C41 B4 108.75(16) . . ?
C43 C42 C41 115.24(18) . . ?
C44 C43 C42 115.01(18) . . ?
C43 C44 C45 116.11(17) . . ?
C44 C45 B4 107.69(16) . . ?
C46 C45 C44 114.01(17) . . ?
C46 C45 B4 109.10(16) . . ?
C47 C46 C45 115.09(19) . . ?
C46 C47 C48 113.60(19) . . ?
C47 C48 C41 115.90(17) . . ?
C11 B1 Re1 116.72(13) . . ?
C15 B1 Re1 135.57(13) . . ?
C15 B1 C11 107.56(15) . . ?
C21 B2 Re1 131.94(13) . . ?
C21 B2 C25 107.64(15) . . ?
C25 B2 Re1 120.42(13) . . ?
C31 B3 Re1 135.96(13) . . ?
C31 B3 C35 107.19(15) . . ?
C35 B3 Re1 116.69(12) . . ?
C41 B4 Re1 133.26(12) . . ?
C41 B4 C45 107.63(15) . . ?
C45 B4 Re1 119.10(13) . . ?
O1 K1 O2 60.32(5) . . ?
O1 K1 O3 113.82(5) . . ?
O1 K1 O4 157.26(5) . . ?
O1 K1 O5 112.96(5) . . ?
O1 K1 O6 58.84(5) . . ?
O1 K1 O7 106.01(6) . . ?
O1 K1 O8 114.1(2) . . ?
O1 K1 O8A 102.1(5) . . ?
O2 K1 O3 58.54(5) . . ?
O2 K1 O6 119.17(5) . . ?
O2 K1 O7 120.83(6) . . ?
O2 K1 O8 75.25(15) . . ?
O2 K1 O8A 72.2(2) . . ?
O3 K1 O7 125.23(6) . . ?
O3 K1 O8 71.56(15) . . ?
O3 K1 O8A 81.6(6) . . ?
O4 K1 O2 117.26(5) . . ?
O4 K1 O3 58.73(5) . . ?
O4 K1 O5 59.40(5) . . ?
O4 K1 O6 118.26(5) . . ?
O4 K1 O7 94.40(5) . . ?
O4 K1 O8 85.0(2) . . ?
O4 K1 O8A 98.0(6) . . ?
O5 K1 O2 157.06(5) . . ?
O5 K1 O3 113.08(5) . . ?
O5 K1 O6 58.86(5) . . ?
O5 K1 O7 81.84(6) . . ?
O5 K1 O8 124.49(18) . . ?
O5 K1 O8A 129.8(2) . . ?
O6 K1 O3 156.60(5) . . ?
O6 K1 O7 77.13(5) . . ?
O6 K1 O8 131.73(16) . . ?
O6 K1 O8A 121.0(6) . . ?
O7 K1 O8A 53.8(4) . . ?
O8 K1 O7 58.31(10) . . ?
C52 O1 K1 114.58(15) . . ?
C53 O1 K1 111.53(15) . . ?
C53 O1 C52 113.5(2) . . ?
C54 O2 K1 114.23(16) . . ?
C54 O2 C55 113.7(2) . . ?
C55 O2 K1 116.77(14) . . ?
C56 O3 K1 112.63(13) . . ?
C56 O3 C57 112.5(2) . . ?
C57 O3 K1 111.96(13) . . ?
C58 O4 K1 117.77(13) . . ?
C58 O4 C59 111.62(18) . . ?
C59 O4 K1 116.34(13) . . ?
C60 O5 K1 110.24(13) . . ?
C60 O5 C61 112.00(17) . . ?
C61 O5 K1 111.95(14) . . ?
C51 O6 K1 116.40(16) . . ?
C62 O6 K1 117.14(14) . . ?
C62 O6 C51 112.7(2) . . ?
C63 O7 K1 129.19(19) . . ?
C63 O7 C64 111.3(3) . . ?
C64 O7 K1 115.9(2) . . ?
O6 C51 C52 109.2(2) . . ?
O1 C52 C51 108.7(2) . . ?
O1 C53 C54 109.2(2) . . ?
O2 C54 C53 109.9(2) . . ?
O2 C55 C56 109.7(2) . . ?
O3 C56 C55 108.1(2) . . ?
O3 C57 C58 108.91(18) . . ?
O4 C58 C57 108.51(19) . . ?
O4 C59 C60 108.68(19) . . ?
O5 C60 C59 108.35(18) . . ?
O5 C61 C62 108.88(18) . . ?
O6 C62 C61 109.1(2) . . ?
O7 C64 C65 112.1(4) . . ?
C65A C64 O7 116.3(7) . . ?
C66 O8 K1 122.5(5) . . ?
C65 O8 K1 102.8(4) . . ?
C65 O8 C66 120.0(5) . . ?
O8 C65 C64 114.8(5) . . ?
C66 O8A K1 141.0(8) . . ?
C66 O8A C65A 99.3(13) . . ?
C65A O8A K1 119.4(9) . . ?
C64 C65A O8A 118.6(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
Re1 B1 2.304(2) . ?
Re1 B2 2.2993(19) . ?
Re1 B3 2.290(2) . ?
Re1 B4 2.2894(19) . ?
C11 C12 1.540(3) . ?
C11 C18 1.536(3) . ?
C11 B1 1.598(3) . ?
C12 C13 1.528(3) . ?
C13 C14 1.516(3) . ?
C14 C15 1.540(3) . ?
C15 C16 1.534(3) . ?
C15 B1 1.595(3) . ?
C16 C17 1.520(3) . ?
C17 C18 1.515(3) . ?
C21 C22 1.542(3) . ?
C21 C28 1.528(3) . ?
C21 B2 1.599(3) . ?
C22 C23 1.521(3) . ?
C23 C24 1.527(4) . ?
C24 C25 1.537(3) . ?
C25 C26 1.543(3) . ?
C25 B2 1.602(3) . ?
C26 C27 1.520(3) . ?
C27 C28 1.523(3) . ?
C31 C32 1.540(3) . ?
C31 C38 1.541(3) . ?
C31 B3 1.596(3) . ?
C32 C33 1.514(4) . ?
C33 C34 1.516(4) . ?
C34 C35 1.527(3) . ?
C35 C36 1.532(3) . ?
C35 B3 1.607(3) . ?
C36 C37 1.513(3) . ?
C37 C38 1.528(3) . ?
C41 C42 1.533(3) . ?
C41 C48 1.537(3) . ?
C41 B4 1.591(3) . ?
C42 C43 1.522(3) . ?
C43 C44 1.516(3) . ?
C44 C45 1.545(3) . ?
C45 C46 1.531(3) . ?
C45 B4 1.596(3) . ?
C46 C47 1.516(3) . ?
C47 C48 1.525(3) . ?
K1 O1 2.7983(16) . ?
K1 O2 2.8496(16) . ?
K1 O3 2.8617(15) . ?
K1 O4 2.8368(15) . ?
K1 O5 2.8456(16) . ?
K1 O6 2.8616(16) . ?
K1 O7 2.915(2) . ?
K1 O8 2.884(4) . ?
K1 O8A 2.964(15) . ?
O1 C52 1.415(3) . ?
O1 C53 1.413(3) . ?
O2 C54 1.403(3) . ?
O2 C55 1.430(3) . ?
O3 C56 1.406(3) . ?
O3 C57 1.421(3) . ?
O4 C58 1.412(3) . ?
O4 C59 1.422(3) . ?
O5 C60 1.408(3) . ?
O5 C61 1.423(3) . ?
O6 C51 1.419(3) . ?
O6 C62 1.414(3) . ?
O7 C63 1.407(3) . ?
O7 C64 1.408(4) . ?
C51 C52 1.476(4) . ?
C53 C54 1.483(4) . ?
C55 C56 1.468(4) . ?
C57 C58 1.476(4) . ?
C59 C60 1.485(3) . ?
C61 C62 1.479(4) . ?
C64 C65 1.432(6) . ?
C64 C65A 1.326(12) . ?
C66 O8 1.509(10) . ?
C66 O8A 1.131(14) . ?
O8 C65 1.412(9) . ?
O8A C65A 1.372(19) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.4377 -5.0832 -20.0261 -0.1455 0.4930 -0.8578
-13.0435 9.7061 -11.6682 0.2307 -0.7759 -0.5871
13.0435 -9.7061 11.6682 -0.2307 0.7759 0.5871
9.0552 14.9638 -6.2044 -0.9919 0.0255 -0.1247
-9.0552 -14.9638 6.2044 0.9919 -0.0255 0.1247
8.5330 11.8673 9.7140 -0.8258 0.0209 0.5635
-6.0693 -11.8930 17.2056 0.7557 -0.0199 0.6546
-0.3837 -3.8228 22.5404 0.1975 -0.0058 0.9803
-9.2984 -13.8881 -3.9049 0.9465 -0.0242 -0.3217
-7.4637 -9.6094 -13.8812 0.6848 -0.0172 -0.7285
-11.7991 11.1438 12.2658 0.1583 -0.8546 0.4946
13.5894 -12.6735 -6.9826 -0.1766 0.9517 -0.2513
-1.4187 22.0701 0.7682 -0.7541 -0.6444 0.1270
-1.7411 22.3636 -3.8951 -0.7576 -0.6476 -0.0817
1.3784 -21.9768 -1.2918 0.7516 0.6423 -0.1502
-7.2208 17.2787 11.0230 -0.2868 -0.8117 0.5089
-9.2128 19.6501 -8.0443 -0.3131 -0.8849 -0.3448
3.2446 -22.4920 1.5733 0.6880 0.7256 -0.0089
