#------------------------------------------------------------------------------
#$Date: 2023-08-08 00:55:30 +0300 (Tue, 08 Aug 2023) $
#$Revision: 285571 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/20/7132003.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_7132003
loop_
_publ_author_name
'Goodall, Joe C.'
'Sajjad, Muhammad Arif'
'Thompson, Emily A.'
'Page, Samuel J.'
'Kerrigan, Adam M.'
'Jenkins, Huw T.'
'Lynam, Jason Martin'
'Macgregor, Stuart Alan'
'Weller, Andrew S.'
_publ_section_title
;
 In Crystallo Lattice Adaptivity Triggered by Solid-Gas Reactions of
 Cationic Group 7 Pincer Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03201A
_journal_year                    2023
_chemical_formula_moiety         'C23 H39 N O4 P2 Re, C32 H12 B F24'
_chemical_formula_sum            'C55 H51 B F24 N O4 P2 Re'
_chemical_formula_weight         1504.91
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-06-22 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                107.7110(10)
_cell_angle_beta                 94.0020(10)
_cell_angle_gamma                98.7510(10)
_cell_formula_units_Z            2
_cell_length_a                   12.74810(10)
_cell_length_b                   14.4679(2)
_cell_length_c                   17.4995(2)
_cell_measurement_reflns_used    29016
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      76.5610
_cell_measurement_theta_min      4.1040
_cell_volume                     3015.63(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00 -93.00   0.50    0.40    --  -50.29-133.00 138.00   50
  2  ω   -116.00 -66.00   0.50    0.40    --  -50.29-136.00 -39.00  100
  3  ω    -81.00 -56.00   0.50    0.40    --  -50.29 136.00  24.00   50
  4  ω    -91.00 -66.00   0.50    0.40    --  -50.29 133.00-153.00   50
  5  ω     49.00  96.00   0.50    0.40    --   50.29-133.00 138.00   94
  6  ω     42.00 102.00   0.50    0.40    --   50.29-136.00 -39.00  120
  7  ω     48.00 117.00   0.50    1.50    --  105.75-133.00 138.00  138
  8  ω     49.00 116.00   0.50    1.50    --  105.75-136.00 -39.00  134
  9  ω    109.00 134.00   0.50    1.50    --  105.75 136.00  24.00   50
 10  ω    133.00 158.00   0.50    1.50    --  105.75 133.00-153.00   50
 11  ω    -57.00  22.00   0.50    0.40    --  -50.29  19.00 120.00  158
 12  ω    -49.00  22.00   0.50    0.40    --  -50.29  57.00-150.00  142
 13  ω   -123.00 -59.00   0.50    0.40    --  -50.29 -37.00 120.00  128
 14  ω   -118.00 -67.00   0.50    0.40    --  -50.29 -57.00 -30.00  102
 15  ω   -114.00 -80.00   0.50    0.40    --  -50.29-125.00-180.00   68
 16  ω     39.00  92.00   0.50    1.50    --  105.75 -77.00  30.00  106
 17  ω     98.00 168.00   0.50    1.50    --  105.75  37.00-150.00  140
 18  ω     33.00 112.00   0.50    1.50    --  105.75 -37.00  90.00  158
 19  ω     83.00 108.00   0.50    1.50    --  105.75-110.00 -32.64   50
 20  ω     57.00 105.00   0.50    1.50    --  105.75 -99.00  30.00   96
 21  ω    101.00 177.00   0.50    1.50    --  105.75  19.00 -90.00  152
 22  ω     34.00 112.00   0.50    1.50    --  105.75 -37.00 -90.00  156
 23  ω     71.00 106.00   0.50    1.50    --  105.75 -99.00-150.00   70
 24  ω     48.00  92.00   0.50    1.50    --  105.75 -19.00  30.00   88
 25  ω     45.00 113.00   0.50    1.50    --  105.75 -19.00 150.00  136
 26  ω     34.00  92.00   0.50    1.50    --  105.75 -57.00 120.00  116
 27  ω     58.00 126.00   0.50    1.50    --  105.75 -77.00 120.00  136
 28  ω     37.00  90.00   0.50    1.50    --  105.75 -99.00 -60.00  106
 29  ω     35.00 112.00   0.50    1.50    --  105.75 -19.00 -90.00  154
 30  ω     39.00  65.00   0.50    1.50    --  105.75-125.00 120.00   52
 31  ω    104.00 131.00   0.50    1.50    --  105.75  19.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299467000
_diffrn_orient_matrix_UB_12      0.0429668000
_diffrn_orient_matrix_UB_13      0.0923293000
_diffrn_orient_matrix_UB_21      0.1062257000
_diffrn_orient_matrix_UB_22      0.0574259000
_diffrn_orient_matrix_UB_23      -0.0120849000
_diffrn_orient_matrix_UB_31      -0.0547717000
_diffrn_orient_matrix_UB_32      0.0882091000
_diffrn_orient_matrix_UB_33      0.0012190000
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36432
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.988
_diffrn_reflns_theta_min         3.535
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_preparation
'[(tBuPONOP)ReBr(CO)2] + Na[BarF4] in 1,2-difluorobenzene'
_exptl_crystal_recrystallization_method
'CH2Cl2 solution layered with hexane at room temperature.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.796
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         12178
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0659P)²+5.2978P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11820
_reflns_number_total             12178
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           asw22138
_cod_original_cell_volume        3015.62(6)
_cod_database_code               7132003
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Re1 P2 B1 C40 F24 H40 N1 O4'
_chemical_oxdiff_usercomment     'JG091 - DCM/hex'
_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   0.457
_shelx_estimated_absorpt_t_min   0.339
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-F6 \\sim C31-F4 \\sim C31-F5 \\sim C31-F4A \\sim C31-F6A \\sim C31-F5A
 with sigma of 0.02
 C47-C44 \\sim C47A-C44
 with sigma of 0.02
 F16A-C47 \\sim F16A-C47A
 with sigma of 0.02
 F22-F23 \\sim F22-F24 \\sim F23-F24
 with sigma of 0.04
 C55-F22 \\sim C55-F23 \\sim C55-F24
 with sigma of 0.02
 C39-F10 \\sim C39-F10A \\sim C39-F12A \\sim C39-F11A \\sim C39-F12 \\sim
C39-F11
 with sigma of 0.02
 F6-F4 \\sim F6-F5 \\sim F4-F5 \\sim F4A-F6A \\sim F4A-F5A \\sim F6A-F5A
 with sigma of 0.04
 F18A-F16A \\sim F18A-F17A \\sim F16A-F17A
 with sigma of 0.04
 F10-F12 \\sim F10-F11 \\sim F10A-F12A \\sim F10A-F11A \\sim F12A-F11A \\sim
F12-F11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C47 \\sim C47A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 C47A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F4A)=Sof(F6A)=Sof(F5A)=1-FVAR(1)
 Sof(F6)=Sof(F4)=Sof(F5)=FVAR(1)
 Sof(F10A)=Sof(F12A)=Sof(F11A)=1-FVAR(2)
 Sof(F10)=Sof(F12)=Sof(F11)=FVAR(2)
 Sof(C47A)=Sof(F17B)=Sof(F18B)=1-FVAR(3)
 Sof(C47)=Sof(F18A)=Sof(F17A)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C49(H49), C35(H35), C41(H41), C27(H27), C33(H33), C43(H43),
 C12(H12), C29(H29), C53(H53), C51(H51), C37(H37), C14(H14), C13(H13), C45(H45)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C21(H21A,
 H21B,H21C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.768
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 0.73910(2) 1.07459(2) 0.84815(2) 0.02036(6) Uani 1 1 d . . . . .
P2 P 0.85160(7) 0.97968(6) 0.77004(5) 0.02431(17) Uani 1 1 d . . . . .
P1 P 0.63908(7) 1.20461(7) 0.88482(6) 0.02741(18) Uani 1 1 d . . . . .
O4 O 0.9182(2) 1.06117(19) 0.73170(17) 0.0301(5) Uani 1 1 d . . . . .
O3 O 0.6767(2) 1.26732(19) 0.82157(17) 0.0318(6) Uani 1 1 d . . . . .
F20 F -0.0762(2) 0.23516(18) 0.4334(2) 0.0514(7) Uani 1 1 d . . . . .
F21 F -0.11159(19) 0.3679(2) 0.51120(16) 0.0452(6) Uani 1 1 d . . . . .
F3 F 0.6638(2) 0.49712(19) 0.82217(18) 0.0467(6) Uani 1 1 d . . . . .
N1 N 0.8004(2) 1.1664(2) 0.77922(17) 0.0211(5) Uani 1 1 d . . . . .
F15 F 0.1924(3) 0.2579(3) 0.8990(2) 0.0594(8) Uani 1 1 d . . . . .
F19 F -0.0913(2) 0.3549(3) 0.38814(18) 0.0604(8) Uani 1 1 d . . . . .
F2 F 0.6136(2) 0.5952(3) 0.92512(17) 0.0663(9) Uani 1 1 d . . . . .
F8 F 0.5423(2) 0.1249(3) 0.48085(17) 0.0641(9) Uani 1 1 d . . . . .
F1 F 0.7118(2) 0.6528(2) 0.8503(2) 0.0569(8) Uani 1 1 d . . . . .
O2 O 0.6271(3) 0.9265(2) 0.9233(2) 0.0471(8) Uani 1 1 d . . . . .
F14 F 0.0278(2) 0.2641(3) 0.9071(3) 0.0716(10) Uani 1 1 d . . . . .
O1 O 0.8896(3) 1.1438(3) 1.00274(18) 0.0485(8) Uani 1 1 d . . . . .
F9 F 0.5973(2) 0.1237(3) 0.5955(2) 0.0660(9) Uani 1 1 d . . . . .
F7 F 0.6156(2) 0.2595(2) 0.5732(3) 0.0785(12) Uani 1 1 d . . . . .
F13 F 0.1477(4) 0.3792(3) 0.98540(18) 0.0877(14) Uani 1 1 d . . . . .
C25 C 0.4592(3) 0.4993(3) 0.7567(2) 0.0247(7) Uani 1 1 d . . . . .
H25 H 0.472692 0.438860 0.762406 0.030 Uiso 1 1 calc R U . . .
F10 F 0.0899(6) 0.0358(9) 0.5767(11) 0.072(4) Uani 0.58(3) 1 d D . P A 1
C40 C 0.1879(3) 0.4105(2) 0.7328(2) 0.0230(6) Uani 1 1 d . . . . .
C42 C 0.1214(3) 0.3746(3) 0.8508(2) 0.0259(7) Uani 1 1 d . . . . .
C49 C 0.1088(3) 0.3710(2) 0.5514(2) 0.0237(6) Uani 1 1 d . . . . .
H49 H 0.063844 0.345352 0.584075 0.028 Uiso 1 1 calc R U . . .
C35 C 0.3674(3) 0.1047(2) 0.5776(2) 0.0266(7) Uani 1 1 d . . . . .
H35 H 0.386032 0.041300 0.557490 0.032 Uiso 1 1 calc R U . . .
C11 C 0.7579(3) 1.2466(2) 0.7782(2) 0.0235(6) Uani 1 1 d . . . . .
C15 C 0.8783(3) 1.1422(3) 0.7319(2) 0.0253(7) Uani 1 1 d . . . . .
C41 C 0.1880(3) 0.3601(2) 0.7899(2) 0.0243(6) Uani 1 1 d . . . . .
H41 H 0.235169 0.314564 0.786944 0.029 Uiso 1 1 calc R U . . .
C48 C 0.2176(3) 0.4064(2) 0.5799(2) 0.0234(6) Uani 1 1 d . . . . .
F12 F 0.2000(12) -0.0531(8) 0.5375(12) 0.115(6) Uani 0.58(3) 1 d D . P A 1
C27 C 0.5140(3) 0.6763(3) 0.7925(2) 0.0279(7) Uani 1 1 d . . . . .
H27 H 0.562609 0.735492 0.821111 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3672(3) 0.4987(2) 0.7078(2) 0.0239(6) Uani 1 1 d . . . . .
C26 C 0.5313(3) 0.5857(3) 0.7971(2) 0.0260(7) Uani 1 1 d . . . . .
C34 C 0.4402(3) 0.1897(3) 0.5848(2) 0.0254(7) Uani 1 1 d . . . . .
C16 C 0.9615(3) 0.9300(3) 0.8093(3) 0.0344(8) Uani 1 1 d . . . . .
C33 C 0.4140(3) 0.2829(2) 0.6149(2) 0.0242(6) Uani 1 1 d . . . . .
H33 H 0.465402 0.339489 0.618630 0.029 Uiso 1 1 calc R U . . .
C43 C 0.0523(3) 0.4416(3) 0.8576(2) 0.0294(7) Uani 1 1 d . . . . .
H43 H 0.005999 0.451026 0.898499 0.035 Uiso 1 1 calc R U . . .
C50 C 0.0644(3) 0.3722(2) 0.4770(2) 0.0268(7) Uani 1 1 d . . . . .
C2 C 0.6676(3) 0.9815(3) 0.8949(2) 0.0318(8) Uani 1 1 d . . . . .
C12 C 0.7928(3) 1.3055(3) 0.7323(2) 0.0297(7) Uani 1 1 d . . . . .
H12 H 0.763137 1.362341 0.733634 0.036 Uiso 1 1 calc R U . . .
C32 C 0.3127(3) 0.2952(2) 0.6401(2) 0.0228(6) Uani 1 1 d . . . . .
C18 C 1.0120(4) 0.8624(3) 0.7431(3) 0.0445(10) Uani 1 1 d . . . . .
H18A H 0.959570 0.802517 0.714405 0.067 Uiso 1 1 calc R U . . .
H18B H 1.074257 0.844388 0.767267 0.067 Uiso 1 1 calc R U . . .
H18C H 1.034577 0.896654 0.704883 0.067 Uiso 1 1 calc R U . . .
C29 C 0.3522(3) 0.5911(3) 0.7030(2) 0.0265(7) Uani 1 1 d . . . . .
H29 H 0.291157 0.594299 0.670116 0.032 Uiso 1 1 calc R U . . .
C53 C 0.2792(3) 0.4404(3) 0.5272(2) 0.0280(7) Uani 1 1 d . . . . .
H53 H 0.353820 0.463010 0.542777 0.034 Uiso 1 1 calc R U . . .
C51 C 0.1269(3) 0.4078(3) 0.4267(2) 0.0305(7) Uani 1 1 d . . . . .
H51 H 0.096677 0.408734 0.375759 0.037 Uiso 1 1 calc R U . . .
C37 C 0.2413(3) 0.2080(3) 0.6314(2) 0.0256(7) Uani 1 1 d . . . . .
H37 H 0.172032 0.212675 0.647279 0.031 Uiso 1 1 calc R U . . .
C20 C 0.7687(3) 0.8931(3) 0.6774(2) 0.0326(8) Uani 1 1 d . . . . .
C36 C 0.2671(3) 0.1149(3) 0.6007(2) 0.0273(7) Uani 1 1 d . . . . .
C44 C 0.0524(3) 0.4942(3) 0.8035(2) 0.0286(7) Uani 1 1 d D . . . .
C14 C 0.9160(3) 1.1967(3) 0.6835(2) 0.0303(7) Uani 1 1 d . . . . .
H14 H 0.970358 1.178435 0.650481 0.036 Uiso 1 1 calc R U . . .
F11 F 0.1878(16) 0.0031(18) 0.6610(10) 0.115(7) Uani 0.58(3) 1 d D . P A 1
C19 C 0.9131(4) 0.8737(3) 0.8645(3) 0.0416(9) Uani 1 1 d . . . . .
H19A H 0.888289 0.919939 0.910146 0.062 Uiso 1 1 calc R U . . .
H19B H 0.967684 0.843144 0.884729 0.062 Uiso 1 1 calc R U . . .
H19C H 0.852673 0.822467 0.833568 0.062 Uiso 1 1 calc R U . . .
C13 C 0.8718(3) 1.2789(3) 0.6848(2) 0.0315(7) Uani 1 1 d . . . . .
H13 H 0.896563 1.317621 0.652315 0.038 Uiso 1 1 calc R U . . .
C45 C 0.1186(3) 0.4784(3) 0.7421(2) 0.0249(7) Uani 1 1 d . . . . .
H45 H 0.116454 0.515008 0.705400 0.030 Uiso 1 1 calc R U . . .
C46 C 0.1228(3) 0.3197(3) 0.9102(2) 0.0354(8) Uani 1 1 d . . . . .
C28 C 0.4226(3) 0.6772(3) 0.7442(2) 0.0271(7) Uani 1 1 d . . . . .
C7 C 0.4920(3) 1.1728(3) 0.8519(3) 0.0371(9) Uani 1 1 d . . . . .
F6 F 0.4631(8) 0.8498(4) 0.7885(7) 0.090(6) Uani 0.62(2) 1 d D . P B 1
C23 C 0.7215(4) 0.7980(3) 0.6942(3) 0.0394(9) Uani 1 1 d . . . . .
H23A H 0.778099 0.760086 0.697707 0.059 Uiso 1 1 calc R U . . .
H23B H 0.665517 0.758422 0.650249 0.059 Uiso 1 1 calc R U . . .
H23C H 0.690768 0.814934 0.745393 0.059 Uiso 1 1 calc R U . . .
C54 C -0.0528(3) 0.3333(3) 0.4521(2) 0.0319(7) Uani 1 1 d . . . . .
C39 C 0.1875(3) 0.0244(3) 0.5936(3) 0.0377(9) Uani 1 1 d D . . . .
C10 C 0.4774(4) 1.0838(4) 0.7750(3) 0.0436(10) Uani 1 1 d . . . . .
H10A H 0.519948 1.101048 0.735104 0.065 Uiso 1 1 calc R U . . .
H10B H 0.401760 1.064846 0.752656 0.065 Uiso 1 1 calc R U . . .
H10C H 0.501297 1.028414 0.787929 0.065 Uiso 1 1 calc R U . . .
C52 C 0.2350(3) 0.4420(3) 0.4533(2) 0.0331(8) Uani 1 1 d . . . . .
C9 C 0.4354(4) 1.1414(4) 0.9173(4) 0.0538(12) Uani 1 1 d . . . . .
H9A H 0.469558 1.091359 0.931059 0.081 Uiso 1 1 calc R U . . .
H9B H 0.359897 1.113973 0.896858 0.081 Uiso 1 1 calc R U . . .
H9C H 0.440553 1.198993 0.965657 0.081 Uiso 1 1 calc R U . . .
C38 C 0.5484(3) 0.1776(3) 0.5582(2) 0.0299(7) Uani 1 1 d . . . . .
C30 C 0.6296(3) 0.5824(3) 0.8482(2) 0.0322(8) Uani 1 1 d . . . . .
C1 C 0.8331(3) 1.1189(3) 0.9436(2) 0.0329(8) Uani 1 1 d . . . . .
C31 C 0.4000(3) 0.7733(3) 0.7375(3) 0.0367(9) Uani 1 1 d D . . . .
C17 C 1.0475(4) 1.0178(4) 0.8601(3) 0.0473(11) Uani 1 1 d . . . . .
H17A H 1.081852 1.050843 0.824589 0.071 Uiso 1 1 calc R U . . .
H17B H 1.101351 0.994071 0.888321 0.071 Uiso 1 1 calc R U . . .
H17C H 1.014289 1.064493 0.899716 0.071 Uiso 1 1 calc R U . . .
C22 C 0.6766(3) 0.9478(3) 0.6666(3) 0.0381(9) Uani 1 1 d . . . . .
H22A H 0.646006 0.969033 0.717572 0.057 Uiso 1 1 calc R U . . .
H22B H 0.621099 0.903405 0.624265 0.057 Uiso 1 1 calc R U . . .
H22C H 0.704129 1.005659 0.651052 0.057 Uiso 1 1 calc R U . . .
F4 F 0.3034(5) 0.7831(5) 0.7461(8) 0.076(4) Uani 0.62(2) 1 d D . P B 1
C21 C 0.8238(4) 0.8700(4) 0.6008(3) 0.0468(11) Uani 1 1 d . . . . .
H21A H 0.853476 0.931658 0.591581 0.070 Uiso 1 1 calc R U . . .
H21B H 0.771618 0.829056 0.554627 0.070 Uiso 1 1 calc R U . . .
H21C H 0.881567 0.834279 0.607160 0.070 Uiso 1 1 calc R U . . .
C3 C 0.6772(4) 1.3052(3) 0.9829(3) 0.0449(10) Uani 1 1 d . . . . .
C47 C -0.0229(18) 0.5669(13) 0.8145(15) 0.037(6) Uani 0.61(3) 1 d D U P C 1
C5 C 0.7932(4) 1.3518(4) 0.9828(3) 0.0546(12) Uani 1 1 d . . . . .
H5A H 0.837011 1.300279 0.970541 0.082 Uiso 1 1 calc R U . . .
H5B H 0.820304 1.399864 1.036175 0.082 Uiso 1 1 calc R U . . .
H5C H 0.796657 1.385250 0.941812 0.082 Uiso 1 1 calc R U . . .
B1 B 0.2730(3) 0.4019(3) 0.6657(2) 0.0231(7) Uani 1 1 d . . . . .
C55 C 0.3024(4) 0.4835(3) 0.4005(3) 0.0438(10) Uani 1 1 d D . . . .
C8 C 0.4442(4) 1.2542(4) 0.8307(4) 0.0527(12) Uani 1 1 d . . . . .
H8A H 0.447369 1.310308 0.879885 0.079 Uiso 1 1 calc R U . . .
H8B H 0.369486 1.228653 0.806887 0.079 Uiso 1 1 calc R U . . .
H8C H 0.484998 1.275822 0.791842 0.079 Uiso 1 1 calc R U . . .
C4 C 0.6093(5) 1.3876(4) 0.9938(4) 0.0645(15) Uani 1 1 d . . . . .
H4A H 0.607013 1.408497 0.945594 0.097 Uiso 1 1 calc R U . . .
H4B H 0.641457 1.444003 1.041188 0.097 Uiso 1 1 calc R U . . .
H4C H 0.536445 1.362225 1.001692 0.097 Uiso 1 1 calc R U . . .
C6 C 0.6682(5) 1.2606(5) 1.0518(3) 0.0600(14) Uani 1 1 d . . . . .
H6A H 0.592693 1.236927 1.054306 0.090 Uiso 1 1 calc R U . . .
H6B H 0.699171 1.311092 1.103134 0.090 Uiso 1 1 calc R U . . .
H6C H 0.706890 1.205370 1.041889 0.090 Uiso 1 1 calc R U . . .
F5 F 0.4175(12) 0.7800(7) 0.6659(5) 0.095(6) Uani 0.62(2) 1 d D . P B 1
F4A F 0.3184(13) 0.7691(7) 0.6865(13) 0.100(11) Uani 0.38(2) 1 d D . P B 2
F6A F 0.384(2) 0.8361(9) 0.8068(7) 0.102(11) Uani 0.38(2) 1 d D . P B 2
F5A F 0.4778(8) 0.8270(9) 0.7171(13) 0.076(8) Uani 0.38(2) 1 d D . P B 2
F22 F 0.2651(4) 0.5577(3) 0.3832(3) 0.0823(12) Uani 1 1 d D . . . .
F23 F 0.2941(4) 0.4215(3) 0.3251(2) 0.0788(11) Uani 1 1 d D . . . .
F24 F 0.3991(3) 0.5136(7) 0.4293(4) 0.208(5) Uani 1 1 d D . . . .
F18A F 0.0303(8) 0.6519(6) 0.8173(18) 0.134(7) Uani 0.61(3) 1 d D . P C 1
F16A F -0.0968(3) 0.5400(3) 0.7494(2) 0.0774(11) Uani 1 1 d D . . . .
F17A F -0.0799(16) 0.5691(19) 0.8675(10) 0.115(7) Uani 0.61(3) 1 d D . P C 1
F10A F 0.1742(15) -0.0396(10) 0.5199(5) 0.075(5) Uani 0.42(3) 1 d D . P A 2
F12A F 0.2228(16) -0.0268(12) 0.6365(13) 0.080(6) Uani 0.42(3) 1 d D . P A 2
F11A F 0.0927(12) 0.0372(11) 0.6113(18) 0.092(8) Uani 0.42(3) 1 d D . P A 2
C47A C -0.010(3) 0.575(2) 0.805(2) 0.034(6) Uani 0.39(3) 1 d D U P C 2
F17B F -0.031(3) 0.621(2) 0.8825(9) 0.107(10) Uani 0.39(3) 1 d . . P C 2
F18B F 0.0262(17) 0.6466(14) 0.7856(12) 0.096(7) Uani 0.39(3) 1 d . . P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
P P 0.2955 0.4335 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0722
-7 7 -2 0.0721
1 9 -2 0.1384
-2 -8 2 0.1042
-7 -2 0 0.0954
-7 6 2 0.0952
0 -9 7 0.0849
3 7 -9 0.0994
7 -1 -6 0.1209
0 4 8 0.1083
5 -8 5 0.0997
0 -4 -8 0.1066
-7 5 -5 0.0517
-6 0 -6 0.0703
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
P2 Re1 P1 155.34(3) . . ?
N1 Re1 P2 77.90(8) . . ?
N1 Re1 P1 78.15(8) . . ?
C2 Re1 P2 100.93(12) . . ?
C2 Re1 P1 101.78(12) . . ?
C2 Re1 N1 170.80(14) . . ?
C1 Re1 P2 95.57(13) . . ?
C1 Re1 P1 95.84(13) . . ?
C1 Re1 N1 104.11(14) . . ?
C1 Re1 C2 85.07(17) . . ?
O4 P2 Re1 101.60(9) . . ?
O4 P2 C16 101.97(16) . . ?
O4 P2 C20 100.42(16) . . ?
C16 P2 Re1 126.01(14) . . ?
C16 P2 C20 114.54(18) . . ?
C20 P2 Re1 107.85(13) . . ?
O3 P1 Re1 100.93(9) . . ?
O3 P1 C7 99.27(16) . . ?
O3 P1 C3 99.62(18) . . ?
C7 P1 Re1 117.50(14) . . ?
C3 P1 Re1 120.20(16) . . ?
C3 P1 C7 113.5(2) . . ?
C15 O4 P2 119.2(2) . . ?
C11 O3 P1 120.8(2) . . ?
C11 N1 Re1 121.0(2) . . ?
C11 N1 C15 118.3(3) . . ?
C15 N1 Re1 120.6(2) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C26 C25 C24 122.0(3) . . ?
C41 C40 B1 123.1(3) . . ?
C45 C40 C41 115.7(3) . . ?
C45 C40 B1 120.8(3) . . ?
C41 C42 C46 121.1(3) . . ?
C43 C42 C41 120.5(3) . . ?
C43 C42 C46 118.4(3) . . ?
C48 C49 H49 118.9 . . ?
C50 C49 H49 118.9 . . ?
C50 C49 C48 122.2(3) . . ?
C34 C35 H35 120.9 . . ?
C36 C35 H35 120.9 . . ?
C36 C35 C34 118.2(3) . . ?
O3 C11 N1 118.3(3) . . ?
O3 C11 C12 119.0(3) . . ?
N1 C11 C12 122.7(3) . . ?
O4 C15 N1 118.1(3) . . ?
O4 C15 C14 119.7(3) . . ?
N1 C15 C14 122.2(3) . . ?
C40 C41 H41 118.8 . . ?
C42 C41 C40 122.3(3) . . ?
C42 C41 H41 118.8 . . ?
C49 C48 C53 115.4(3) . . ?
C49 C48 B1 123.3(3) . . ?
C53 C48 B1 121.1(3) . . ?
C26 C27 H27 121.3 . . ?
C26 C27 C28 117.5(3) . . ?
C28 C27 H27 121.3 . . ?
C25 C24 C29 115.7(3) . . ?
C25 C24 B1 124.6(3) . . ?
C29 C24 B1 119.4(3) . . ?
C25 C26 C30 120.0(3) . . ?
C27 C26 C25 121.3(3) . . ?
C27 C26 C30 118.6(3) . . ?
C35 C34 C33 121.3(3) . . ?
C35 C34 C38 117.7(3) . . ?
C33 C34 C38 121.0(3) . . ?
C18 C16 P2 113.5(3) . . ?
C18 C16 C19 110.5(3) . . ?
C18 C16 C17 109.2(4) . . ?
C19 C16 P2 106.4(3) . . ?
C17 C16 P2 107.9(3) . . ?
C17 C16 C19 109.3(4) . . ?
C34 C33 H33 119.3 . . ?
C34 C33 C32 121.5(3) . . ?
C32 C33 H33 119.3 . . ?
C42 C43 H43 120.8 . . ?
C44 C43 C42 118.5(3) . . ?
C44 C43 H43 120.8 . . ?
C49 C50 C54 118.3(3) . . ?
C51 C50 C49 121.1(3) . . ?
C51 C50 C54 120.6(3) . . ?
O2 C2 Re1 178.7(4) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 C11 117.6(3) . . ?
C13 C12 H12 121.2 . . ?
C33 C32 B1 123.2(3) . . ?
C37 C32 C33 115.6(3) . . ?
C37 C32 B1 120.7(3) . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C24 C29 H29 118.8 . . ?
C28 C29 C24 122.5(3) . . ?
C28 C29 H29 118.8 . . ?
C48 C53 H53 118.8 . . ?
C52 C53 C48 122.3(3) . . ?
C52 C53 H53 118.8 . . ?
C50 C51 H51 121.2 . . ?
C52 C51 C50 117.6(3) . . ?
C52 C51 H51 121.2 . . ?
C32 C37 H37 118.5 . . ?
C36 C37 C32 123.0(3) . . ?
C36 C37 H37 118.5 . . ?
C23 C20 P2 109.2(3) . . ?
C23 C20 C22 108.3(3) . . ?
C22 C20 P2 102.7(3) . . ?
C21 C20 P2 115.9(3) . . ?
C21 C20 C23 111.0(4) . . ?
C21 C20 C22 109.2(3) . . ?
C35 C36 C37 120.5(3) . . ?
C35 C36 C39 119.1(3) . . ?
C37 C36 C39 120.5(3) . . ?
C43 C44 C45 120.7(3) . . ?
C43 C44 C47 116.2(14) . . ?
C43 C44 C47A 126(2) . . ?
C45 C44 C47 123.2(14) . . ?
C45 C44 C47A 113(2) . . ?
C15 C14 H14 121.1 . . ?
C13 C14 C15 117.8(3) . . ?
C13 C14 H14 121.1 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C13 C14 121.3(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C40 C45 H45 118.8 . . ?
C44 C45 C40 122.3(3) . . ?
C44 C45 H45 118.8 . . ?
F15 C46 F14 105.5(4) . . ?
F15 C46 C42 113.9(3) . . ?
F14 C46 C42 112.0(4) . . ?
F13 C46 F15 105.9(4) . . ?
F13 C46 F14 106.6(4) . . ?
F13 C46 C42 112.3(4) . . ?
C27 C28 C31 119.6(3) . . ?
C29 C28 C27 121.0(3) . . ?
C29 C28 C31 119.4(3) . . ?
C10 C7 P1 105.0(3) . . ?
C10 C7 C9 109.0(4) . . ?
C10 C7 C8 107.8(4) . . ?
C9 C7 P1 108.7(3) . . ?
C8 C7 P1 114.6(3) . . ?
C8 C7 C9 111.4(4) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
F20 C54 F21 105.0(3) . . ?
F20 C54 C50 112.0(3) . . ?
F21 C54 C50 112.4(3) . . ?
F19 C54 F20 106.7(3) . . ?
F19 C54 F21 106.7(3) . . ?
F19 C54 C50 113.4(3) . . ?
F10 C39 C36 111.5(6) . . ?
F10 C39 F11 105.1(9) . . ?
F12 C39 F10 105.3(9) . . ?
F12 C39 C36 114.2(6) . . ?
F12 C39 F11 107.6(10) . . ?
F11 C39 C36 112.5(8) . . ?
F10A C39 C36 111.6(7) . . ?
F12A C39 C36 111.7(8) . . ?
F12A C39 F10A 101.6(10) . . ?
F11A C39 C36 116.9(8) . . ?
F11A C39 F10A 106.2(11) . . ?
F11A C39 F12A 107.7(10) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C53 C52 C51 121.2(3) . . ?
C53 C52 C55 120.7(4) . . ?
C51 C52 C55 118.0(4) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
F8 C38 F9 102.2(3) . . ?
F8 C38 C34 112.4(3) . . ?
F9 C38 C34 111.9(3) . . ?
F7 C38 F8 109.8(4) . . ?
F7 C38 F9 105.0(4) . . ?
F7 C38 C34 114.6(3) . . ?
F3 C30 F2 106.3(4) . . ?
F3 C30 F1 106.3(3) . . ?
F3 C30 C26 112.8(3) . . ?
F2 C30 F1 106.0(4) . . ?
F2 C30 C26 112.5(3) . . ?
F1 C30 C26 112.4(3) . . ?
O1 C1 Re1 178.1(4) . . ?
F6 C31 C28 113.2(4) . . ?
F6 C31 F5 104.4(7) . . ?
F4 C31 C28 112.7(4) . . ?
F4 C31 F6 108.6(6) . . ?
F4 C31 F5 107.2(7) . . ?
F5 C31 C28 110.2(4) . . ?
F4A C31 C28 116.9(5) . . ?
F4A C31 F6A 104.6(10) . . ?
F6A C31 C28 114.0(5) . . ?
F5A C31 C28 115.4(5) . . ?
F5A C31 F4A 103.2(10) . . ?
F5A C31 F6A 100.7(9) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C5 C3 P1 106.2(3) . . ?
C5 C3 C4 107.6(4) . . ?
C5 C3 C6 110.5(5) . . ?
C4 C3 P1 113.2(4) . . ?
C6 C3 P1 108.9(3) . . ?
C6 C3 C4 110.3(4) . . ?
F18A C47 C44 108.7(19) . . ?
F18A C47 F16A 106(2) . . ?
F16A C47 C44 110.0(9) . . ?
F17A C47 C44 116(2) . . ?
F17A C47 F18A 115.0(13) . . ?
F17A C47 F16A 100.6(17) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C48 B1 C40 111.5(3) . . ?
C48 B1 C24 110.4(3) . . ?
C48 B1 C32 103.4(3) . . ?
C24 B1 C40 103.5(3) . . ?
C24 B1 C32 115.6(3) . . ?
C32 B1 C40 112.7(3) . . ?
F22 C55 C52 112.3(4) . . ?
F23 C55 C52 112.9(4) . . ?
F23 C55 F22 98.3(4) . . ?
F24 C55 C52 114.0(4) . . ?
F24 C55 F22 108.0(5) . . ?
F24 C55 F23 110.2(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
F16A C47A C44 110.1(13) . . ?
F16A C47A F17B 115(3) . . ?
F17B C47A C44 111(3) . . ?
F18B C47A C44 122(4) . . ?
F18B C47A F16A 98(3) . . ?
F18B C47A F17B 100.8(19) . . ?
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 P2 2.3541(9) . ?
Re1 P1 2.3845(9) . ?
Re1 N1 2.150(3) . ?
Re1 C2 1.928(4) . ?
Re1 C1 1.864(4) . ?
P2 O4 1.679(3) . ?
P2 C16 1.850(4) . ?
P2 C20 1.853(4) . ?
P1 O3 1.682(3) . ?
P1 C7 1.867(4) . ?
P1 C3 1.857(5) . ?
O4 C15 1.346(4) . ?
O3 C11 1.344(4) . ?
F20 C54 1.337(5) . ?
F21 C54 1.338(5) . ?
F3 C30 1.331(5) . ?
N1 C11 1.356(4) . ?
N1 C15 1.357(4) . ?
F15 C46 1.336(5) . ?
F19 C54 1.332(5) . ?
F2 C30 1.336(5) . ?
F8 C38 1.327(5) . ?
F1 C30 1.335(5) . ?
O2 C2 1.139(5) . ?
F14 C46 1.336(5) . ?
O1 C1 1.144(5) . ?
F9 C38 1.351(5) . ?
F7 C38 1.295(5) . ?
F13 C46 1.321(5) . ?
C25 H25 0.9500 . ?
C25 C24 1.399(5) . ?
C25 C26 1.388(5) . ?
F10 C39 1.306(8) . ?
C40 C41 1.405(5) . ?
C40 C45 1.400(5) . ?
C40 B1 1.642(5) . ?
C42 C41 1.395(5) . ?
C42 C43 1.390(5) . ?
C42 C46 1.489(5) . ?
C49 H49 0.9500 . ?
C49 C48 1.403(5) . ?
C49 C50 1.388(5) . ?
C35 H35 0.9500 . ?
C35 C34 1.391(5) . ?
C35 C36 1.383(5) . ?
C11 C12 1.385(5) . ?
C15 C14 1.386(5) . ?
C41 H41 0.9500 . ?
C48 C53 1.404(5) . ?
C48 B1 1.637(5) . ?
F12 C39 1.285(9) . ?
C27 H27 0.9500 . ?
C27 C26 1.387(5) . ?
C27 C28 1.395(5) . ?
C24 C29 1.405(5) . ?
C24 B1 1.639(5) . ?
C26 C30 1.503(5) . ?
C34 C33 1.391(5) . ?
C34 C38 1.503(5) . ?
C16 C18 1.523(6) . ?
C16 C19 1.544(6) . ?
C16 C17 1.536(6) . ?
C33 H33 0.9500 . ?
C33 C32 1.413(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.384(5) . ?
C50 C51 1.388(5) . ?
C50 C54 1.498(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(5) . ?
C32 C37 1.399(5) . ?
C32 B1 1.640(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C29 H29 0.9500 . ?
C29 C28 1.379(5) . ?
C53 H53 0.9500 . ?
C53 C52 1.383(6) . ?
C51 H51 0.9500 . ?
C51 C52 1.387(6) . ?
C37 H37 0.9500 . ?
C37 C36 1.390(5) . ?
C20 C23 1.536(5) . ?
C20 C22 1.545(5) . ?
C20 C21 1.526(6) . ?
C36 C39 1.497(5) . ?
C44 C45 1.397(5) . ?
C44 C47 1.509(11) . ?
C44 C47A 1.506(15) . ?
C14 H14 0.9500 . ?
C14 C13 1.385(5) . ?
F11 C39 1.307(10) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C13 H13 0.9500 . ?
C45 H45 0.9500 . ?
C28 C31 1.498(5) . ?
C7 C10 1.530(7) . ?
C7 C9 1.540(6) . ?
C7 C8 1.533(6) . ?
F6 C31 1.302(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C39 F10A 1.320(9) . ?
C39 F12A 1.307(10) . ?
C39 F11A 1.295(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C52 C55 1.497(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C31 F4 1.275(7) . ?
C31 F5 1.317(7) . ?
C31 F4A 1.304(8) . ?
C31 F6A 1.326(9) . ?
C31 F5A 1.303(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C3 C5 1.529(7) . ?
C3 C4 1.551(7) . ?
C3 C6 1.534(7) . ?
C47 F18A 1.30(3) . ?
C47 F16A 1.344(11) . ?
C47 F17A 1.21(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C55 F22 1.342(6) . ?
C55 F23 1.337(5) . ?
C55 F24 1.257(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
F16A C47A 1.345(15) . ?
C47A F17B 1.38(4) . ?
C47A F18B 1.22(6) . ?
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 P2 O4 C15 -18.1(3) . . . . ?
Re1 P2 C16 C18 173.9(2) . . . . ?
Re1 P2 C16 C19 52.1(3) . . . . ?
Re1 P2 C16 C17 -65.1(4) . . . . ?
Re1 P2 C20 C23 -88.2(3) . . . . ?
Re1 P2 C20 C22 26.6(3) . . . . ?
Re1 P2 C20 C21 145.6(3) . . . . ?
Re1 P1 O3 C11 -10.2(3) . . . . ?
Re1 P1 C7 C10 -27.5(3) . . . . ?
Re1 P1 C7 C9 88.9(3) . . . . ?
Re1 P1 C7 C8 -145.6(3) . . . . ?
Re1 P1 C3 C5 57.6(4) . . . . ?
Re1 P1 C3 C4 175.5(3) . . . . ?
Re1 P1 C3 C6 -61.4(4) . . . . ?
Re1 N1 C11 O3 0.2(4) . . . . ?
Re1 N1 C11 C12 -177.7(3) . . . . ?
Re1 N1 C15 O4 -2.2(4) . . . . ?
Re1 N1 C15 C14 176.7(3) . . . . ?
P2 O4 C15 N1 15.0(4) . . . . ?
P2 O4 C15 C14 -163.9(3) . . . . ?
P1 O3 C11 N1 7.8(4) . . . . ?
P1 O3 C11 C12 -174.3(3) . . . . ?
O4 P2 C16 C18 -72.0(3) . . . . ?
O4 P2 C16 C19 166.2(3) . . . . ?
O4 P2 C16 C17 49.0(3) . . . . ?
O4 P2 C20 C23 165.9(3) . . . . ?
O4 P2 C20 C22 -79.3(3) . . . . ?
O4 P2 C20 C21 39.7(3) . . . . ?
O4 C15 C14 C13 179.3(3) . . . . ?
O3 P1 C7 C10 80.0(3) . . . . ?
O3 P1 C7 C9 -163.5(3) . . . . ?
O3 P1 C7 C8 -38.1(4) . . . . ?
O3 P1 C3 C5 -51.1(4) . . . . ?
O3 P1 C3 C4 66.8(4) . . . . ?
O3 P1 C3 C6 -170.1(4) . . . . ?
O3 C11 C12 C13 -176.2(3) . . . . ?
N1 C11 C12 C13 1.7(6) . . . . ?
N1 C15 C14 C13 0.4(6) . . . . ?
C25 C24 C29 C28 -0.5(5) . . . . ?
C25 C24 B1 C40 91.5(4) . . . . ?
C25 C24 B1 C48 -149.0(3) . . . . ?
C25 C24 B1 C32 -32.2(5) . . . . ?
C25 C26 C30 F3 29.3(5) . . . . ?
C25 C26 C30 F2 -91.0(4) . . . . ?
C25 C26 C30 F1 149.5(3) . . . . ?
C42 C43 C44 C45 1.6(5) . . . . ?
C42 C43 C44 C47 -179.1(7) . . . . ?
C42 C43 C44 C47A -175.0(12) . . . . ?
C49 C48 C53 C52 2.1(5) . . . . ?
C49 C48 B1 C40 -30.9(4) . . . . ?
C49 C48 B1 C24 -145.4(3) . . . . ?
C49 C48 B1 C32 90.4(4) . . . . ?
C49 C50 C51 C52 0.0(5) . . . . ?
C49 C50 C54 F20 -71.4(4) . . . . ?
C49 C50 C54 F21 46.6(4) . . . . ?
C49 C50 C54 F19 167.8(3) . . . . ?
C35 C34 C33 C32 0.5(5) . . . . ?
C35 C34 C38 F8 59.8(5) . . . . ?
C35 C34 C38 F9 -54.6(5) . . . . ?
C35 C34 C38 F7 -174.0(4) . . . . ?
C35 C36 C39 F10 -147.4(9) . . . . ?
C35 C36 C39 F12 -28.2(13) . . . . ?
C35 C36 C39 F11 94.7(14) . . . . ?
C35 C36 C39 F10A -53.6(11) . . . . ?
C35 C36 C39 F12A 59.3(13) . . . . ?
C35 C36 C39 F11A -176.0(16) . . . . ?
C11 N1 C15 O4 -178.4(3) . . . . ?
C11 N1 C15 C14 0.5(5) . . . . ?
C11 C12 C13 C14 -0.7(6) . . . . ?
C15 N1 C11 O3 176.4(3) . . . . ?
C15 N1 C11 C12 -1.6(5) . . . . ?
C15 C14 C13 C12 -0.2(6) . . . . ?
C41 C40 C45 C44 -0.9(5) . . . . ?
C41 C40 B1 C48 145.0(3) . . . . ?
C41 C40 B1 C24 -96.3(4) . . . . ?
C41 C40 B1 C32 29.3(5) . . . . ?
C41 C42 C43 C44 -0.9(5) . . . . ?
C41 C42 C46 F15 0.2(5) . . . . ?
C41 C42 C46 F14 -119.5(4) . . . . ?
C41 C42 C46 F13 120.6(4) . . . . ?
C48 C49 C50 C51 0.8(5) . . . . ?
C48 C49 C50 C54 -179.7(3) . . . . ?
C48 C53 C52 C51 -1.4(6) . . . . ?
C48 C53 C52 C55 176.9(3) . . . . ?
C27 C26 C30 F3 -151.8(3) . . . . ?
C27 C26 C30 F2 88.0(4) . . . . ?
C27 C26 C30 F1 -31.6(5) . . . . ?
C27 C28 C31 F6 -9.3(9) . . . . ?
C27 C28 C31 F4 -133.0(7) . . . . ?
C27 C28 C31 F5 107.2(8) . . . . ?
C27 C28 C31 F4A 174.6(14) . . . . ?
C27 C28 C31 F6A -63.0(14) . . . . ?
C27 C28 C31 F5A 52.9(11) . . . . ?
C24 C25 C26 C27 1.7(5) . . . . ?
C24 C25 C26 C30 -179.4(3) . . . . ?
C24 C29 C28 C27 0.7(5) . . . . ?
C24 C29 C28 C31 -178.7(3) . . . . ?
C26 C25 C24 C29 -0.7(5) . . . . ?
C26 C25 C24 B1 -173.6(3) . . . . ?
C26 C27 C28 C29 0.3(5) . . . . ?
C26 C27 C28 C31 179.7(3) . . . . ?
C34 C35 C36 C37 -1.2(5) . . . . ?
C34 C35 C36 C39 -179.9(3) . . . . ?
C34 C33 C32 C37 -0.9(5) . . . . ?
C34 C33 C32 B1 -172.4(3) . . . . ?
C16 P2 O4 C15 -149.2(3) . . . . ?
C16 P2 C20 C23 57.5(3) . . . . ?
C16 P2 C20 C22 172.2(3) . . . . ?
C16 P2 C20 C21 -68.7(3) . . . . ?
C33 C34 C38 F8 -119.9(4) . . . . ?
C33 C34 C38 F9 125.8(4) . . . . ?
C33 C34 C38 F7 6.4(6) . . . . ?
C33 C32 C37 C36 0.4(5) . . . . ?
C33 C32 B1 C40 -150.7(3) . . . . ?
C33 C32 B1 C48 88.8(4) . . . . ?
C33 C32 B1 C24 -32.0(5) . . . . ?
C43 C42 C41 C40 -0.8(5) . . . . ?
C43 C42 C46 F15 -179.4(4) . . . . ?
C43 C42 C46 F14 60.9(5) . . . . ?
C43 C42 C46 F13 -59.0(5) . . . . ?
C43 C44 C45 C40 -0.7(5) . . . . ?
C43 C44 C47 F18A 128(2) . . . . ?
C43 C44 C47 F16A -117(2) . . . . ?
C43 C44 C47 F17A -3.2(18) . . . . ?
C43 C44 C47A F16A -102(3) . . . . ?
C43 C44 C47A F17B 26(4) . . . . ?
C43 C44 C47A F18B 144(2) . . . . ?
C50 C49 C48 C53 -1.8(5) . . . . ?
C50 C49 C48 B1 -177.5(3) . . . . ?
C50 C51 C52 C53 0.3(6) . . . . ?
C50 C51 C52 C55 -178.1(3) . . . . ?
C32 C37 C36 C35 0.7(6) . . . . ?
C32 C37 C36 C39 179.4(3) . . . . ?
C29 C24 B1 C40 -81.2(4) . . . . ?
C29 C24 B1 C48 38.2(4) . . . . ?
C29 C24 B1 C32 155.1(3) . . . . ?
C29 C28 C31 F6 170.1(8) . . . . ?
C29 C28 C31 F4 46.4(8) . . . . ?
C29 C28 C31 F5 -73.4(8) . . . . ?
C29 C28 C31 F4A -6.1(15) . . . . ?
C29 C28 C31 F6A 116.4(13) . . . . ?
C29 C28 C31 F5A -127.7(11) . . . . ?
C53 C48 B1 C40 153.6(3) . . . . ?
C53 C48 B1 C24 39.2(4) . . . . ?
C53 C48 B1 C32 -85.1(4) . . . . ?
C53 C52 C55 F22 -122.3(4) . . . . ?
C53 C52 C55 F23 127.7(4) . . . . ?
C53 C52 C55 F24 0.9(8) . . . . ?
C51 C50 C54 F20 108.1(4) . . . . ?
C51 C50 C54 F21 -133.9(4) . . . . ?
C51 C50 C54 F19 -12.7(5) . . . . ?
C51 C52 C55 F22 56.1(5) . . . . ?
C51 C52 C55 F23 -53.9(6) . . . . ?
C51 C52 C55 F24 179.4(6) . . . . ?
C37 C32 B1 C40 38.2(4) . . . . ?
C37 C32 B1 C48 -82.3(4) . . . . ?
C37 C32 B1 C24 156.9(3) . . . . ?
C37 C36 C39 F10 33.8(10) . . . . ?
C37 C36 C39 F12 153.1(13) . . . . ?
C37 C36 C39 F11 -84.0(15) . . . . ?
C37 C36 C39 F10A 127.6(10) . . . . ?
C37 C36 C39 F12A -119.5(13) . . . . ?
C37 C36 C39 F11A 5.2(16) . . . . ?
C20 P2 O4 C15 92.7(3) . . . . ?
C20 P2 C16 C18 35.4(4) . . . . ?
C20 P2 C16 C19 -86.3(3) . . . . ?
C20 P2 C16 C17 156.5(3) . . . . ?
C36 C35 C34 C33 0.6(5) . . . . ?
C36 C35 C34 C38 -179.0(3) . . . . ?
C45 C40 C41 C42 1.6(5) . . . . ?
C45 C40 B1 C48 -42.5(4) . . . . ?
C45 C40 B1 C24 76.2(4) . . . . ?
C45 C40 B1 C32 -158.3(3) . . . . ?
C45 C44 C47 F18A -52.3(19) . . . . ?
C45 C44 C47 F16A 63(3) . . . . ?
C45 C44 C47 F17A 176.1(15) . . . . ?
C45 C44 C47A F16A 81(4) . . . . ?
C45 C44 C47A F17B -151(3) . . . . ?
C45 C44 C47A F18B -33(2) . . . . ?
C46 C42 C41 C40 179.6(3) . . . . ?
C46 C42 C43 C44 178.7(3) . . . . ?
C28 C27 C26 C25 -1.5(5) . . . . ?
C28 C27 C26 C30 179.6(3) . . . . ?
C7 P1 O3 C11 -130.8(3) . . . . ?
C7 P1 C3 C5 -155.7(3) . . . . ?
C7 P1 C3 C4 -37.8(4) . . . . ?
C7 P1 C3 C6 85.3(4) . . . . ?
C54 C50 C51 C52 -179.5(3) . . . . ?
C38 C34 C33 C32 -179.9(3) . . . . ?
C3 P1 O3 C11 113.3(3) . . . . ?
C3 P1 C7 C10 -175.2(3) . . . . ?
C3 P1 C7 C9 -58.7(4) . . . . ?
C3 P1 C7 C8 66.7(4) . . . . ?
C47 C44 C45 C40 -180.0(8) . . . . ?
B1 C40 C41 C42 174.5(3) . . . . ?
B1 C40 C45 C44 -173.9(3) . . . . ?
B1 C48 C53 C52 177.9(3) . . . . ?
B1 C24 C29 C28 172.8(3) . . . . ?
B1 C32 C37 C36 172.1(3) . . . . ?
C47A C44 C45 C40 176.3(10) . . . . ?
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
1.0015 0.0016 -0.0017 0.0299 0.1065 -0.0547
-6.6862 6.5990 -2.0755 -0.1083 -0.3062 0.9458
1.2801 8.8331 -1.9692 0.2360 0.6670 0.7066
-2.1313 -8.4601 1.8145 -0.2598 -0.7342 -0.6273
-7.4661 -2.2522 -0.0624 -0.3261 -0.9217 0.2102
-6.7165 5.9465 1.7231 0.2135 -0.3928 0.8945
0.2007 -8.6655 7.2879 0.3066 -0.5644 -0.7665
2.6969 6.8667 -8.6940 -0.4269 0.7859 0.4474
7.0841 -1.1299 -6.2637 -0.4147 0.7633 -0.4953
0.2660 4.1415 7.9194 0.9171 0.1704 0.3604
5.2169 -7.6567 5.0306 0.2917 0.0537 -0.9550
-0.2315 -4.1900 -7.8826 -0.9148 -0.1699 -0.3665
-6.8387 5.0473 -4.9198 -0.4422 -0.3771 0.8138
-6.3563 -0.0993 -5.6593 -0.7171 -0.6125 0.3325
