#------------------------------------------------------------------------------
#$Date: 2024-10-06 03:20:07 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249435.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_7249435
loop_
_publ_author_name
'Valdivieso, Jorge P.'
'Erickson, Alexander N.'
'Gardinier, James R.'
_publ_section_title
;
 Group 7 carbonyl complexes of a PNN-heteroscorpionate ligand
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              31502
_journal_page_last               31516
_journal_paper_doi               10.1039/D4RA05287K
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C30 H25 N4 O3 P Re, C F3 O3 S'
_chemical_formula_sum            'C31 H25 F3 N4 O6 P Re S'
_chemical_formula_weight         855.78
_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             2024-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-17 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                99.615(2)
_cell_angle_beta                 90.746(2)
_cell_angle_gamma                94.564(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9587(3)
_cell_length_b                   12.2629(4)
_cell_length_c                   14.9571(5)
_cell_measurement_reflns_used    14655
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.6300
_cell_measurement_theta_min      4.3060
_cell_volume                     1614.38(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -10.00   1.00    9.62    --  -42.46 -77.00 -90.00  109
  2  ω    -92.00  -2.00   1.00    9.62    --  -42.46 125.00   0.00   90
  3  ω   -115.00 -14.00   1.00    9.62    --  -42.46 -57.00 150.00  101
  4  ω     27.00 126.00   1.00   38.49    --  100.00 -45.00   0.00   99
  5  ω     94.00 173.00   1.00   38.49    --  100.00 125.00  90.00   79
  6  ω     27.00 118.00   1.00   38.49    --  100.00-125.00  60.00   91
  7  ω     72.00 176.00   1.00   38.49    --  100.00  30.00 -60.00  104
  8  ω     27.00 118.00   1.00   38.49    --  100.00-125.00-150.00   91
  9  ω     67.00 176.00   1.00   38.49    --  100.00  77.00 -90.00  109
 10  ω     74.00 173.00   1.00   38.49    --  100.00  45.00-120.00   99
 11  ω     74.00 173.00   1.00   38.49    --  100.00  45.00   0.00   99
 12  ω     94.00 173.00   1.00   38.49    --  100.00 125.00-120.00   79
 13  ω     27.00 118.00   1.00   38.49    --  100.00-125.00  90.00   91
 14  ω     27.00 118.00   1.00   38.49    --  100.00-125.00 -30.00   91
 15  ω     94.00 173.00   1.00   38.49    --  100.00 125.00-180.00   79
 16  ω     94.00 173.00   1.00   38.49    --  100.00 125.00 -60.00   79
 17  ω     24.00 133.00   1.00   38.49    --  100.00 -77.00-180.00  109
 18  ω   -115.00 -14.00   1.00    9.62    --  -42.46 -57.00 -30.00  101
 19  ω   -117.00 -18.00   1.00    9.62    --  -42.46 -37.00  30.00   99
 20  ω      1.00  83.00   1.00    9.62    --   42.46 -99.00 -90.00   82
 21  ω     10.00 119.00   1.00    9.62    --   42.46  77.00 150.00  109
 22  ω     71.00 172.00   1.00   38.49    --  100.00  61.00  30.00  101
 23  ω     71.00 172.00   1.00   38.49    --  100.00  61.00-180.00  101
 24  ω     47.00 178.00   1.00   38.49    --  100.00  15.00 150.00  131
 25  ω     67.00 176.00   1.00   38.49    --  100.00  77.00  60.00  109
 26  ω     67.00 176.00   1.00   38.49    --  100.00  77.00 -60.00  109
 27  ω     67.00 155.00   1.00   38.49    --  100.00  77.00  90.00   88
 28  ω     67.00 176.00   1.00   38.49    --  100.00  77.00 120.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0571269000
_diffrn_orient_matrix_UB_12      -0.0372032000
_diffrn_orient_matrix_UB_13      0.0877569000
_diffrn_orient_matrix_UB_21      -0.1627011000
_diffrn_orient_matrix_UB_22      -0.0032838000
_diffrn_orient_matrix_UB_23      -0.0356231000
_diffrn_orient_matrix_UB_31      0.0067868000
_diffrn_orient_matrix_UB_32      -0.1222818000
_diffrn_orient_matrix_UB_33      -0.0441662000
_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  0.0745
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29459
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        70.622
_diffrn_reflns_theta_max         70.622
_diffrn_reflns_theta_min         3.668
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.027
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0349
_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)+(0.0471P)²+2.4378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5648
_reflns_number_total             6116
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           2-Re_gard25s
_cod_database_code               7249435
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C31H25F3N4O6PReS
_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.
;
_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.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C23(H23), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_olex2_submission_original_sample_id gard25s
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.841
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 0.35701(2) 0.63441(2) 0.24457(2) 0.02102(8) Uani 1 1 d . . . . .
P1 P 0.58689(11) 0.69558(8) 0.33887(7) 0.0195(2) Uani 1 1 d . . . . .
O3 O 0.0828(4) 0.5531(3) 0.1150(2) 0.0330(7) Uani 1 1 d . . . . .
O2 O 0.1334(4) 0.7416(3) 0.3791(2) 0.0353(7) Uani 1 1 d . . . . .
O1 O 0.2945(4) 0.4296(3) 0.3355(2) 0.0370(8) Uani 1 1 d . . . . .
N11 N 0.5017(4) 0.7895(3) 0.1159(2) 0.0230(7) Uani 1 1 d . . . . .
N12 N 0.3902(4) 0.7768(3) 0.1744(2) 0.0234(7) Uani 1 1 d . . . . .
N21 N 0.6298(4) 0.6227(3) 0.1116(2) 0.0222(7) Uani 1 1 d . . . . .
N22 N 0.5224(4) 0.5628(3) 0.1512(2) 0.0214(7) Uani 1 1 d . . . . .
C1 C 0.7230(5) 0.7939(3) 0.2972(3) 0.0226(8) Uani 1 1 d . . . . .
C2 C 0.7389(5) 0.8056(3) 0.2057(3) 0.0224(8) Uani 1 1 d . . . . .
C3 C 0.8465(5) 0.8851(3) 0.1836(3) 0.0252(9) Uani 1 1 d . . . . .
H3 H 0.857515 0.892319 0.123032 0.030 Uiso 1 1 calc R U . . .
C4 C 0.9378(5) 0.9538(4) 0.2495(3) 0.0284(9) Uani 1 1 d . . . . .
H4 H 1.007152 1.007296 0.233496 0.034 Uiso 1 1 calc R U . . .
C5 C 0.9231(5) 0.9411(4) 0.3394(3) 0.0284(9) Uani 1 1 d . . . . .
H5 H 0.983320 0.985771 0.384457 0.034 Uiso 1 1 calc R U . . .
C6 C 0.8188(5) 0.8616(4) 0.3619(3) 0.0261(9) Uani 1 1 d . . . . .
H6 H 0.811876 0.852768 0.422299 0.031 Uiso 1 1 calc R U . . .
C7 C 0.6468(5) 0.7444(3) 0.1238(3) 0.0229(8) Uani 1 1 d . . . . .
H7 H 0.702186 0.761502 0.071076 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4734(5) 0.8681(4) 0.0657(3) 0.0286(9) Uani 1 1 d . . . . .
H11 H 0.534593 0.891860 0.021789 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3390(5) 0.9059(4) 0.0911(3) 0.0311(10) Uani 1 1 d . . . . .
H12 H 0.289882 0.959804 0.068327 0.037 Uiso 1 1 calc R U . . .
C13 C 0.2907(5) 0.8468(4) 0.1583(3) 0.0283(9) Uani 1 1 d . . . . .
H13 H 0.200888 0.854957 0.188190 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7172(5) 0.5549(4) 0.0599(3) 0.0280(9) Uani 1 1 d . . . . .
H21 H 0.797443 0.576727 0.026290 0.034 Uiso 1 1 calc R U . . .
C22 C 0.6670(5) 0.4484(4) 0.0655(3) 0.0304(10) Uani 1 1 d . . . . .
H22 H 0.705851 0.383687 0.037328 0.036 Uiso 1 1 calc R U . . .
C23 C 0.5443(5) 0.4571(4) 0.1227(3) 0.0273(9) Uani 1 1 d . . . . .
H23 H 0.486374 0.397200 0.138495 0.033 Uiso 1 1 calc R U . . .
C31 C 0.6969(5) 0.5799(3) 0.3508(3) 0.0213(8) Uani 1 1 d . . . . .
C32 C 0.8309(5) 0.5624(4) 0.3072(3) 0.0267(9) Uani 1 1 d . . . . .
H32 H 0.869312 0.612266 0.271161 0.032 Uiso 1 1 calc R U . . .
C33 C 0.9078(5) 0.4715(4) 0.3169(3) 0.0308(10) Uani 1 1 d . . . . .
H33 H 0.996624 0.460662 0.286411 0.037 Uiso 1 1 calc R U . . .
C34 C 0.8551(5) 0.3954(4) 0.3715(3) 0.0284(9) Uani 1 1 d . . . . .
C35 C 0.7200(5) 0.4122(4) 0.4139(3) 0.0264(9) Uani 1 1 d . . . . .
H35 H 0.682068 0.362283 0.450114 0.032 Uiso 1 1 calc R U . . .
C36 C 0.6404(5) 0.5020(4) 0.4033(3) 0.0243(8) Uani 1 1 d . . . . .
H36 H 0.548918 0.510609 0.431190 0.029 Uiso 1 1 calc R U . . .
C37 C 0.9428(6) 0.2981(4) 0.3840(4) 0.0405(12) Uani 1 1 d . . . . .
H37A H 0.995023 0.314006 0.441754 0.061 Uiso 1 1 calc R U . . .
H37B H 1.013686 0.285790 0.336556 0.061 Uiso 1 1 calc R U . . .
H37C H 0.875130 0.232849 0.381675 0.061 Uiso 1 1 calc R U . . .
C41 C 0.5554(5) 0.7638(3) 0.4543(3) 0.0214(8) Uani 1 1 d . . . . .
C42 C 0.6324(5) 0.7410(4) 0.5303(3) 0.0262(9) Uani 1 1 d . . . . .
H42 H 0.705712 0.690832 0.522891 0.031 Uiso 1 1 calc R U . . .
C43 C 0.5997(5) 0.7930(4) 0.6164(3) 0.0291(9) Uani 1 1 d . . . . .
H43 H 0.651742 0.777273 0.666315 0.035 Uiso 1 1 calc R U . . .
C44 C 0.4913(6) 0.8679(4) 0.6299(3) 0.0294(9) Uani 1 1 d . . . . .
C45 C 0.4176(5) 0.8937(4) 0.5537(3) 0.0270(9) Uani 1 1 d . . . . .
H45 H 0.346324 0.945433 0.561276 0.032 Uiso 1 1 calc R U . . .
C46 C 0.4504(5) 0.8425(3) 0.4670(3) 0.0245(8) Uani 1 1 d . . . . .
H46 H 0.401861 0.860902 0.416971 0.029 Uiso 1 1 calc R U . . .
C47 C 0.4491(7) 0.9187(5) 0.7242(3) 0.0406(12) Uani 1 1 d . . . . .
H47A H 0.431616 0.995159 0.725287 0.061 Uiso 1 1 calc R U . . .
H47B H 0.529193 0.914081 0.766322 0.061 Uiso 1 1 calc R U . . .
H47C H 0.359778 0.879283 0.740933 0.061 Uiso 1 1 calc R U . . .
C10 C 0.1841(6) 0.5806(4) 0.1609(3) 0.0291(10) Uani 1 1 d . . . . .
C9 C 0.2180(5) 0.7038(4) 0.3298(3) 0.0270(9) Uani 1 1 d . . . . .
C8 C 0.3219(5) 0.5048(4) 0.3007(3) 0.0285(9) Uani 1 1 d . . . . .
S1 S 0.16872(12) 0.20968(9) 0.11721(7) 0.0256(2) Uani 1 1 d . . . . .
F1 F -0.0460(4) 0.2483(3) 0.0096(2) 0.0454(7) Uani 1 1 d . . . . .
F2 F -0.1039(5) 0.2663(4) 0.1488(3) 0.0753(13) Uani 1 1 d . . . . .
F3 F -0.0929(4) 0.1043(3) 0.0725(3) 0.0682(12) Uani 1 1 d . . . . .
O4 O 0.2193(5) 0.3247(3) 0.1254(3) 0.0557(12) Uani 1 1 d . . . . .
O5 O 0.2255(5) 0.1403(4) 0.0403(2) 0.0488(10) Uani 1 1 d . . . . .
O6 O 0.1688(4) 0.1642(3) 0.1994(2) 0.0347(7) Uani 1 1 d . . . . .
C14 C -0.0288(6) 0.2068(4) 0.0864(3) 0.0366(11) 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'
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'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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
-6 1 1 0.0399
6 -1 -1 0.0479
0 7 2 0.0438
0 -7 -2 0.0010
-1 0 9 0.0152
1 0 -9 0.0182
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
N12 Re1 P1 91.27(10) . . ?
N22 Re1 P1 80.72(9) . . ?
N22 Re1 N12 84.38(13) . . ?
C10 Re1 P1 175.23(13) . . ?
C10 Re1 N12 87.80(15) . . ?
C10 Re1 N22 94.53(16) . . ?
C9 Re1 P1 96.76(13) . . ?
C9 Re1 N12 94.29(16) . . ?
C9 Re1 N22 177.11(16) . . ?
C9 Re1 C10 87.97(18) . . ?
C8 Re1 P1 91.48(13) . . ?
C8 Re1 N12 176.94(16) . . ?
C8 Re1 N22 94.74(16) . . ?
C8 Re1 C10 89.35(18) . . ?
C8 Re1 C9 86.73(19) . . ?
C1 P1 Re1 116.94(13) . . ?
C31 P1 Re1 111.88(13) . . ?
C31 P1 C1 103.08(19) . . ?
C31 P1 C41 105.53(18) . . ?
C41 P1 Re1 115.00(14) . . ?
C41 P1 C1 103.04(19) . . ?
N12 N11 C7 122.6(3) . . ?
N12 N11 C11 110.7(4) . . ?
C11 N11 C7 125.0(4) . . ?
N11 N12 Re1 123.8(3) . . ?
C13 N12 Re1 128.2(3) . . ?
C13 N12 N11 105.4(3) . . ?
N22 N21 C7 124.5(3) . . ?
C21 N21 N22 110.7(3) . . ?
C21 N21 C7 124.8(4) . . ?
N21 N22 Re1 124.8(3) . . ?
C23 N22 Re1 129.4(3) . . ?
C23 N22 N21 105.7(4) . . ?
C2 C1 P1 125.1(3) . . ?
C6 C1 P1 117.0(3) . . ?
C6 C1 C2 117.9(4) . . ?
C1 C2 C7 127.9(4) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 C7 112.9(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 118.7 . . ?
C5 C6 C1 122.5(4) . . ?
C5 C6 H6 118.7 . . ?
N11 C7 N21 111.0(3) . . ?
N11 C7 C2 112.1(3) . . ?
N11 C7 H7 105.0 . . ?
N21 C7 C2 117.4(3) . . ?
N21 C7 H7 105.0 . . ?
C2 C7 H7 105.0 . . ?
N11 C11 H11 126.2 . . ?
N11 C11 C12 107.5(4) . . ?
C12 C11 H11 126.2 . . ?
C11 C12 H12 127.3 . . ?
C11 C12 C13 105.3(4) . . ?
C13 C12 H12 127.3 . . ?
N12 C13 C12 111.0(4) . . ?
N12 C13 H13 124.5 . . ?
C12 C13 H13 124.5 . . ?
N21 C21 H21 126.2 . . ?
N21 C21 C22 107.7(4) . . ?
C22 C21 H21 126.2 . . ?
C21 C22 H22 127.3 . . ?
C21 C22 C23 105.4(4) . . ?
C23 C22 H22 127.3 . . ?
N22 C23 C22 110.4(4) . . ?
N22 C23 H23 124.8 . . ?
C22 C23 H23 124.8 . . ?
C32 C31 P1 123.1(3) . . ?
C32 C31 C36 118.3(4) . . ?
C36 C31 P1 118.5(3) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(4) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.2 . . ?
C32 C33 C34 121.5(4) . . ?
C34 C33 H33 119.2 . . ?
C33 C34 C37 121.1(4) . . ?
C35 C34 C33 117.8(4) . . ?
C35 C34 C37 121.2(4) . . ?
C34 C35 H35 119.4 . . ?
C34 C35 C36 121.2(4) . . ?
C36 C35 H35 119.4 . . ?
C31 C36 H36 119.7 . . ?
C35 C36 C31 120.5(4) . . ?
C35 C36 H36 119.7 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 P1 123.0(3) . . ?
C46 C41 P1 118.2(3) . . ?
C46 C41 C42 118.8(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 C41 120.1(4) . . ?
C43 C42 H42 119.9 . . ?
C42 C43 H43 119.3 . . ?
C44 C43 C42 121.5(4) . . ?
C44 C43 H43 119.3 . . ?
C43 C44 C45 118.5(4) . . ?
C43 C44 C47 121.2(4) . . ?
C45 C44 C47 120.3(4) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 C44 120.4(4) . . ?
C46 C45 H45 119.8 . . ?
C41 C46 H46 119.7 . . ?
C45 C46 C41 120.7(4) . . ?
C45 C46 H46 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C10 Re1 177.4(4) . . ?
O2 C9 Re1 177.8(4) . . ?
O1 C8 Re1 176.6(4) . . ?
O4 S1 O5 114.2(3) . . ?
O4 S1 O6 116.1(2) . . ?
O4 S1 C14 103.2(3) . . ?
O5 S1 C14 102.2(3) . . ?
O6 S1 O5 114.6(2) . . ?
O6 S1 C14 104.1(2) . . ?
F1 C14 S1 110.6(4) . . ?
F2 C14 S1 112.5(4) . . ?
F2 C14 F1 106.7(4) . . ?
F2 C14 F3 107.9(5) . . ?
F3 C14 S1 111.3(4) . . ?
F3 C14 F1 107.6(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 P1 2.4734(10) . ?
Re1 N12 2.185(3) . ?
Re1 N22 2.183(4) . ?
Re1 C10 1.978(5) . ?
Re1 C9 1.936(5) . ?
Re1 C8 1.924(5) . ?
P1 C1 1.835(4) . ?
P1 C31 1.822(4) . ?
P1 C41 1.825(4) . ?
O3 C10 1.125(6) . ?
O2 C9 1.136(6) . ?
O1 C8 1.144(6) . ?
N11 N12 1.353(5) . ?
N11 C7 1.463(5) . ?
N11 C11 1.354(5) . ?
N12 C13 1.332(6) . ?
N21 N22 1.365(5) . ?
N21 C7 1.469(5) . ?
N21 C21 1.344(6) . ?
N22 C23 1.326(6) . ?
C1 C2 1.407(6) . ?
C1 C6 1.399(6) . ?
C2 C3 1.399(6) . ?
C2 C7 1.521(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.360(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(7) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.364(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.402(7) . ?
C23 H23 0.9300 . ?
C31 C32 1.389(6) . ?
C31 C36 1.403(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.383(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.398(6) . ?
C34 C35 1.388(7) . ?
C34 C37 1.515(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.389(6) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.401(6) . ?
C41 C46 1.393(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.385(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.383(7) . ?
C44 C45 1.403(6) . ?
C44 C47 1.509(7) . ?
C45 H45 0.9300 . ?
C45 C46 1.389(6) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
S1 O4 1.432(4) . ?
S1 O5 1.436(4) . ?
S1 O6 1.432(3) . ?
S1 C14 1.818(5) . ?
F1 C14 1.344(6) . ?
F2 C14 1.313(7) . ?
F3 C14 1.321(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 P1 C1 C2 -25.3(4) . . . . ?
Re1 P1 C1 C6 155.2(3) . . . . ?
Re1 P1 C31 C32 107.1(4) . . . . ?
Re1 P1 C31 C36 -70.0(3) . . . . ?
Re1 P1 C41 C42 136.2(3) . . . . ?
Re1 P1 C41 C46 -44.1(4) . . . . ?
Re1 N12 C13 C12 -163.0(3) . . . . ?
Re1 N22 C23 C22 -177.7(3) . . . . ?
P1 C1 C2 C3 179.2(3) . . . . ?
P1 C1 C2 C7 2.3(6) . . . . ?
P1 C1 C6 C5 -178.1(4) . . . . ?
P1 C31 C32 C33 -178.3(4) . . . . ?
P1 C31 C36 C35 179.7(3) . . . . ?
P1 C41 C42 C43 -177.9(3) . . . . ?
P1 C41 C46 C45 177.4(3) . . . . ?
N11 N12 C13 C12 -1.1(5) . . . . ?
N11 C11 C12 C13 0.3(5) . . . . ?
N12 N11 C7 N21 63.4(5) . . . . ?
N12 N11 C7 C2 -70.1(5) . . . . ?
N12 N11 C11 C12 -1.1(5) . . . . ?
N21 N22 C23 C22 0.7(5) . . . . ?
N21 C21 C22 C23 0.5(5) . . . . ?
N22 N21 C7 N11 -45.0(5) . . . . ?
N22 N21 C7 C2 85.7(5) . . . . ?
N22 N21 C21 C22 -0.1(5) . . . . ?
C1 P1 C31 C32 -19.4(4) . . . . ?
C1 P1 C31 C36 163.5(3) . . . . ?
C1 P1 C41 C42 -95.4(4) . . . . ?
C1 P1 C41 C46 84.3(4) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C1 C2 C7 N11 78.2(5) . . . . ?
C1 C2 C7 N21 -52.0(6) . . . . ?
C2 C1 C6 C5 2.4(6) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C2 C7 N11 -98.9(4) . . . . ?
C3 C2 C7 N21 130.9(4) . . . . ?
C3 C4 C5 C6 -0.4(7) . . . . ?
C4 C5 C6 C1 -1.5(7) . . . . ?
C6 C1 C2 C3 -1.3(6) . . . . ?
C6 C1 C2 C7 -178.3(4) . . . . ?
C7 N11 N12 Re1 -29.9(5) . . . . ?
C7 N11 N12 C13 167.2(4) . . . . ?
C7 N11 C11 C12 -166.5(4) . . . . ?
C7 N21 N22 Re1 -2.1(5) . . . . ?
C7 N21 N22 C23 179.4(4) . . . . ?
C7 N21 C21 C22 -179.9(4) . . . . ?
C7 C2 C3 C4 176.9(4) . . . . ?
C11 N11 N12 Re1 164.2(3) . . . . ?
C11 N11 N12 C13 1.4(5) . . . . ?
C11 N11 C7 N21 -132.8(4) . . . . ?
C11 N11 C7 C2 93.7(5) . . . . ?
C11 C12 C13 N12 0.5(5) . . . . ?
C21 N21 N22 Re1 178.2(3) . . . . ?
C21 N21 N22 C23 -0.3(4) . . . . ?
C21 N21 C7 N11 134.7(4) . . . . ?
C21 N21 C7 C2 -94.5(5) . . . . ?
C21 C22 C23 N22 -0.8(5) . . . . ?
C31 P1 C1 C2 97.9(4) . . . . ?
C31 P1 C1 C6 -81.6(4) . . . . ?
C31 P1 C41 C42 12.4(4) . . . . ?
C31 P1 C41 C46 -168.0(3) . . . . ?
C31 C32 C33 C34 -0.9(7) . . . . ?
C32 C31 C36 C35 2.4(6) . . . . ?
C32 C33 C34 C35 1.9(7) . . . . ?
C32 C33 C34 C37 -178.0(5) . . . . ?
C33 C34 C35 C36 -0.6(7) . . . . ?
C34 C35 C36 C31 -1.5(7) . . . . ?
C36 C31 C32 C33 -1.2(7) . . . . ?
C37 C34 C35 C36 179.3(5) . . . . ?
C41 P1 C1 C2 -152.5(4) . . . . ?
C41 P1 C1 C6 28.1(4) . . . . ?
C41 P1 C31 C32 -127.2(4) . . . . ?
C41 P1 C31 C36 55.8(4) . . . . ?
C41 C42 C43 C44 0.1(7) . . . . ?
C42 C41 C46 C45 -3.0(6) . . . . ?
C42 C43 C44 C45 -2.2(7) . . . . ?
C42 C43 C44 C47 176.0(5) . . . . ?
C43 C44 C45 C46 1.8(7) . . . . ?
C44 C45 C46 C41 0.8(7) . . . . ?
C46 C41 C42 C43 2.5(7) . . . . ?
C47 C44 C45 C46 -176.5(5) . . . . ?
O4 S1 C14 F1 58.0(4) . . . . ?
O4 S1 C14 F2 -61.2(5) . . . . ?
O4 S1 C14 F3 177.5(4) . . . . ?
O5 S1 C14 F1 -60.8(4) . . . . ?
O5 S1 C14 F2 180.0(4) . . . . ?
O5 S1 C14 F3 58.7(4) . . . . ?
O6 S1 C14 F1 179.6(4) . . . . ?
O6 S1 C14 F2 60.4(4) . . . . ?
O6 S1 C14 F3 -60.8(4) . . . . ?
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
-6.0000 1.0000 1.0000 0.3933 0.9373 -0.2072
6.0000 -1.0000 -1.0000 -0.3933 -0.9373 0.2072
0.0000 7.0000 2.0000 -0.0849 -0.0942 -0.9443
-0.0000 -7.0000 -2.0000 0.0849 0.0942 0.9443
-1.0000 0.0000 9.0000 0.8469 -0.1579 -0.4043
1.0000 -0.0000 -9.0000 -0.8469 0.1579 0.4043
