#------------------------------------------------------------------------------
#$Date: 2024-10-06 03:20:07 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249432.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_7249432
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         'C31 H28 N5 O2 P Re, C F3 O3 S'
_chemical_formula_sum            'C32 H28 F3 N5 O5 P Re S'
_chemical_formula_weight         868.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   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                90
_cell_angle_beta                 111.962(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6364(3)
_cell_length_b                   12.9137(2)
_cell_length_c                   16.6780(3)
_cell_measurement_reflns_used    12601
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.5300
_cell_measurement_theta_min      4.4170
_cell_volume                     3323.04(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  32.00   1.00    1.00    --  -42.46  37.00 -30.00   99
  2  ω    -92.00  -2.00   1.00    1.00    --  -42.46 125.00 -30.00   90
  3  ω     23.00  98.00   1.00    1.00    --   42.46-125.00-180.00   75
  4  ω     17.00 110.00   1.00    2.50    --  100.00 -94.00-120.00   93
  5  ω     94.00 173.00   1.00    2.50    --  100.00 125.00-150.00   79
  6  ω     27.00 118.00   1.00    2.50    --  100.00-125.00-150.00   91
  7  ω     72.00 176.00   1.00    2.50    --  100.00  30.00 120.00  104
  8  ω     47.00 178.00   1.00    2.50    --  100.00  15.00  30.00  131
  9  ω     27.00 126.00   1.00    2.50    --  100.00 -45.00 -60.00   99
 10  ω     18.00 153.00   1.00    2.50    --  100.00 -15.00 150.00  135
 11  ω   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00  30.00  109
 12  ω     10.00 119.00   1.00    1.00    --   42.46  77.00 -90.00  109
 13  ω     14.00 116.00   1.00    1.00    --   42.46  57.00-180.00  102
 14  ω     71.00 132.00   1.00    2.50    --  100.00  61.00 150.00   61
 15  ω     47.00 178.00   1.00    2.50    --  100.00  15.00 -90.00  131
;
_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      -0.0517969000
_diffrn_orient_matrix_UB_12      -0.0866965000
_diffrn_orient_matrix_UB_13      0.0222580000
_diffrn_orient_matrix_UB_21      0.0821701000
_diffrn_orient_matrix_UB_22      -0.0334554000
_diffrn_orient_matrix_UB_23      0.0763169000
_diffrn_orient_matrix_UB_31      -0.0231255000
_diffrn_orient_matrix_UB_32      0.0747272000
_diffrn_orient_matrix_UB_33      0.0601147000
_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  0.0698
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.607
_diffrn_reflns_theta_min         4.460
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.766
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.185
_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    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0501P)²+1.8456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5398
_reflns_number_total             6303
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           3-Re_gard25u
_cod_database_code               7249432
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C32H25N5F3O5PSRe
_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.a Ternary CH refined with riding coordinates:
 C7(H7)
1.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)
1.c Idealised Me refined as rotating group:
 C37(H37a,H37b,H37c), C47(H47a,H47b,H47c), C16(H16a,H16b,H16c)
;
_olex2_submission_original_sample_id gard25u
_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 3.039
_oxdiff_exptl_absorpt_empirical_full_min 0.636
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.51667(2) 0.72885(2) 0.80459(2) 0.01275(8) Uani 1 1 d . . . . .
P1 P 0.40210(6) 0.61277(8) 0.78545(7) 0.0132(2) Uani 1 1 d . . . . .
O1 O 0.6416(2) 0.5850(3) 0.9410(2) 0.0255(7) Uani 1 1 d . . . . .
O2 O 0.4858(2) 0.8444(3) 0.9505(2) 0.0246(7) Uani 1 1 d . . . . .
N1 N 0.6128(2) 0.8320(3) 0.7976(2) 0.0178(8) Uani 1 1 d . . . . .
N11 N 0.3915(2) 0.8146(3) 0.6235(2) 0.0155(7) Uani 1 1 d . . . . .
N12 N 0.4268(2) 0.8326(3) 0.7100(2) 0.0132(7) Uani 1 1 d . . . . .
N21 N 0.4784(2) 0.6690(3) 0.6113(2) 0.0149(7) Uani 1 1 d . . . . .
N22 N 0.5359(2) 0.6620(3) 0.6945(2) 0.0151(7) Uani 1 1 d . . . . .
C1 C 0.3213(3) 0.5940(3) 0.6736(3) 0.0157(9) Uani 1 1 d . . . . .
C2 C 0.3234(3) 0.6381(3) 0.5973(3) 0.0145(8) Uani 1 1 d . . . . .
C3 C 0.2565(3) 0.6156(4) 0.5187(3) 0.0199(9) Uani 1 1 d . . . . .
H3 H 0.257358 0.645386 0.468304 0.024 Uiso 1 1 calc R U . . .
C4 C 0.1887(3) 0.5502(4) 0.5138(3) 0.0227(10) Uani 1 1 d . . . . .
H4 H 0.144735 0.536631 0.460727 0.027 Uiso 1 1 calc R U . . .
C5 C 0.1873(3) 0.5053(4) 0.5887(3) 0.0222(10) Uani 1 1 d . . . . .
H5 H 0.142680 0.460589 0.586438 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2531(3) 0.5277(4) 0.6671(3) 0.0194(9) Uani 1 1 d . . . . .
H6 H 0.251643 0.497382 0.717089 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3902(3) 0.7118(3) 0.5865(3) 0.0149(9) Uani 1 1 d . . . . .
H7 H 0.370681 0.723519 0.523995 0.018 Uiso 1 1 calc R U . . .
C8 C 0.5958(3) 0.6387(4) 0.8884(3) 0.0188(9) Uani 1 1 d . . . . .
C9 C 0.4979(3) 0.7988(3) 0.8956(3) 0.0165(9) Uani 1 1 d . . . . .
C11 C 0.3420(3) 0.8947(3) 0.5815(3) 0.0194(9) Uani 1 1 d . . . . .
H11 H 0.310504 0.899009 0.522329 0.023 Uiso 1 1 calc R U . . .
C12 C 0.3466(3) 0.9689(3) 0.6417(3) 0.0194(9) Uani 1 1 d . . . . .
H12 H 0.319704 1.033406 0.632171 0.023 Uiso 1 1 calc R U . . .
C13 C 0.4004(3) 0.9264(3) 0.7206(3) 0.0187(9) Uani 1 1 d . . . . .
H13 H 0.415763 0.959765 0.773693 0.022 Uiso 1 1 calc R U . . .
C15 C 0.6617(3) 0.8797(4) 0.7802(3) 0.0234(10) Uani 1 1 d . . . . .
C16 C 0.7237(3) 0.9415(4) 0.7583(4) 0.0392(14) Uani 1 1 d . . . . .
H16a H 0.708707 0.940201 0.696840 0.059 Uiso 1 1 calc R U . . .
H16b H 0.780781 0.913366 0.786638 0.059 Uiso 1 1 calc R U . . .
H16c H 0.722492 1.011574 0.776940 0.059 Uiso 1 1 calc R U . . .
C21 C 0.5097(3) 0.6243(3) 0.5560(3) 0.0190(9) Uani 1 1 d . . . . .
H21 H 0.481742 0.618976 0.496383 0.023 Uiso 1 1 calc R U . . .
C22 C 0.5910(3) 0.5880(4) 0.6050(3) 0.0202(9) Uani 1 1 d . . . . .
H22 H 0.628861 0.552884 0.585238 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6052(3) 0.6147(3) 0.6900(3) 0.0170(9) Uani 1 1 d . . . . .
H23 H 0.655950 0.601236 0.737165 0.020 Uiso 1 1 calc R U . . .
C31 C 0.3350(3) 0.6519(3) 0.8450(3) 0.0161(9) Uani 1 1 d . . . . .
C32 C 0.3638(3) 0.6355(3) 0.9335(3) 0.0185(9) Uani 1 1 d . . . . .
H32 H 0.413267 0.595970 0.960834 0.022 Uiso 1 1 calc R U . . .
C33 C 0.3193(3) 0.6777(4) 0.9817(3) 0.0218(10) Uani 1 1 d . . . . .
H33 H 0.338809 0.664855 1.040789 0.026 Uiso 1 1 calc R U . . .
C34 C 0.2461(3) 0.7389(4) 0.9431(3) 0.0223(10) Uani 1 1 d . . . . .
C35 C 0.2175(3) 0.7554(4) 0.8539(3) 0.0232(10) Uani 1 1 d . . . . .
H35 H 0.168667 0.796091 0.826840 0.028 Uiso 1 1 calc R U . . .
C36 C 0.2603(3) 0.7124(3) 0.8050(3) 0.0181(9) Uani 1 1 d . . . . .
H36 H 0.239609 0.723531 0.745670 0.022 Uiso 1 1 calc R U . . .
C37 C 0.2000(3) 0.7875(4) 0.9960(4) 0.0315(12) Uani 1 1 d . . . . .
H37a H 0.166570 0.735729 1.010948 0.047 Uiso 1 1 calc R U . . .
H37b H 0.162283 0.841290 0.963101 0.047 Uiso 1 1 calc R U . . .
H37c H 0.241935 0.816346 1.047884 0.047 Uiso 1 1 calc R U . . .
C41 C 0.4317(3) 0.4771(3) 0.8138(3) 0.0159(9) Uani 1 1 d . . . . .
C42 C 0.4923(3) 0.4347(3) 0.7838(3) 0.0187(9) Uani 1 1 d . . . . .
H42 H 0.517145 0.476015 0.753577 0.022 Uiso 1 1 calc R U . . .
C43 C 0.5158(3) 0.3312(4) 0.7988(3) 0.0199(9) Uani 1 1 d . . . . .
H43 H 0.556084 0.303915 0.778184 0.024 Uiso 1 1 calc R U . . .
C44 C 0.4804(3) 0.2681(3) 0.8437(3) 0.0186(9) Uani 1 1 d . . . . .
C45 C 0.4202(3) 0.3106(4) 0.8740(3) 0.0190(9) Uani 1 1 d . . . . .
H45 H 0.396058 0.269238 0.904793 0.023 Uiso 1 1 calc R U . . .
C46 C 0.3954(3) 0.4139(3) 0.8590(3) 0.0182(9) Uani 1 1 d . . . . .
H46 H 0.354641 0.440792 0.879141 0.022 Uiso 1 1 calc R U . . .
C47 C 0.5076(3) 0.1556(4) 0.8598(3) 0.0255(10) Uani 1 1 d . . . . .
H47a H 0.508439 0.125457 0.807507 0.038 Uiso 1 1 calc R U . . .
H47b H 0.467236 0.118751 0.877899 0.038 Uiso 1 1 calc R U . . .
H47c H 0.564481 0.151477 0.904186 0.038 Uiso 1 1 calc R U . . .
S1 S 0.35402(7) 0.80508(9) 0.34502(7) 0.0205(2) Uani 1 1 d . . . . .
F1 F 0.45102(19) 0.9713(2) 0.3679(2) 0.0405(8) Uani 1 1 d . . . . .
F2 F 0.48682(19) 0.8701(3) 0.47830(19) 0.0355(7) Uani 1 1 d . . . . .
F3 F 0.51789(18) 0.8292(3) 0.3687(2) 0.0395(8) Uani 1 1 d . . . . .
O3 O 0.3326(2) 0.8117(3) 0.2532(2) 0.0258(7) Uani 1 1 d . . . . .
O4 O 0.2983(2) 0.8630(3) 0.3764(2) 0.0333(8) Uani 1 1 d . . . . .
O5 O 0.3747(2) 0.7028(3) 0.3815(2) 0.0382(10) Uani 1 1 d . . . . .
C14 C 0.4583(3) 0.8723(4) 0.3924(3) 0.0242(10) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.3331 0.5567 '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
-9 0 9 0.0289
9 0 -9 0.0269
7 0 4 0.1337
-7 0 -4 0.1337
-7 5 7 0.0837
7 -5 -7 0.0587
-3 4 10 0.0427
6 -4 5 0.1400
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
N1 Re1 P1 169.78(10) . . ?
N1 Re1 N12 84.33(13) . . ?
N1 Re1 N22 81.33(14) . . ?
N12 Re1 P1 89.53(9) . . ?
N22 Re1 P1 90.01(9) . . ?
N22 Re1 N12 84.82(13) . . ?
C8 Re1 P1 90.69(13) . . ?
C8 Re1 N1 95.51(16) . . ?
C8 Re1 N12 179.53(16) . . ?
C8 Re1 N22 95.60(16) . . ?
C9 Re1 P1 92.56(13) . . ?
C9 Re1 N1 95.67(16) . . ?
C9 Re1 N12 90.79(15) . . ?
C9 Re1 N22 174.89(15) . . ?
C9 Re1 C8 88.79(18) . . ?
C1 P1 Re1 117.62(14) . . ?
C31 P1 Re1 112.37(14) . . ?
C31 P1 C1 102.82(19) . . ?
C31 P1 C41 106.5(2) . . ?
C41 P1 Re1 116.66(13) . . ?
C41 P1 C1 99.07(19) . . ?
C15 N1 Re1 168.1(4) . . ?
N12 N11 C7 122.4(3) . . ?
C11 N11 N12 111.1(4) . . ?
C11 N11 C7 124.7(4) . . ?
N11 N12 Re1 124.8(3) . . ?
C13 N12 Re1 129.6(3) . . ?
C13 N12 N11 105.4(3) . . ?
N22 N21 C7 123.9(3) . . ?
C21 N21 N22 111.3(3) . . ?
C21 N21 C7 124.6(4) . . ?
N21 N22 Re1 124.6(3) . . ?
C23 N22 Re1 129.7(3) . . ?
C23 N22 N21 105.5(3) . . ?
C2 C1 P1 126.9(3) . . ?
C6 C1 P1 114.8(3) . . ?
C6 C1 C2 118.3(4) . . ?
C1 C2 C7 128.8(4) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 C7 112.3(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 121.9(4) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.3(4) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.3(4) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 H6 118.8 . . ?
C5 C6 C1 122.3(4) . . ?
C5 C6 H6 118.8 . . ?
N11 C7 N21 111.5(3) . . ?
N11 C7 C2 114.4(3) . . ?
N11 C7 H7 104.8 . . ?
N21 C7 C2 115.2(3) . . ?
N21 C7 H7 104.8 . . ?
C2 C7 H7 104.8 . . ?
O1 C8 Re1 177.2(4) . . ?
O2 C9 Re1 178.1(4) . . ?
N11 C11 H11 126.2 . . ?
N11 C11 C12 107.6(4) . . ?
C12 C11 H11 126.2 . . ?
C11 C12 H12 127.6 . . ?
C11 C12 C13 104.8(4) . . ?
C13 C12 H12 127.6 . . ?
N12 C13 C12 111.2(4) . . ?
N12 C13 H13 124.4 . . ?
C12 C13 H13 124.4 . . ?
N1 C15 C16 179.4(6) . . ?
C15 C16 H16a 109.5 . . ?
C15 C16 H16b 109.5 . . ?
C15 C16 H16c 109.5 . . ?
H16a C16 H16b 109.5 . . ?
H16a C16 H16c 109.5 . . ?
H16b C16 H16c 109.5 . . ?
N21 C21 H21 126.7 . . ?
N21 C21 C22 106.7(4) . . ?
C22 C21 H21 126.7 . . ?
C21 C22 H22 127.0 . . ?
C21 C22 C23 105.9(4) . . ?
C23 C22 H22 127.0 . . ?
N22 C23 C22 110.6(4) . . ?
N22 C23 H23 124.7 . . ?
C22 C23 H23 124.7 . . ?
C32 C31 P1 119.9(3) . . ?
C32 C31 C36 118.7(4) . . ?
C36 C31 P1 120.6(3) . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.5(4) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.2(4) . . ?
C34 C33 H33 119.4 . . ?
C33 C34 C35 118.0(4) . . ?
C33 C34 C37 120.9(5) . . ?
C35 C34 C37 121.0(5) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.3(4) . . ?
C36 C35 H35 119.3 . . ?
C31 C36 H36 119.9 . . ?
C35 C36 C31 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
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 116.3(3) . . ?
C46 C41 P1 124.8(3) . . ?
C46 C41 C42 118.8(4) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.3(4) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 119.4 . . ?
C44 C43 C42 121.2(4) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 C45 118.4(4) . . ?
C43 C44 C47 120.2(4) . . ?
C45 C44 C47 121.5(4) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 C44 121.2(4) . . ?
C46 C45 H45 119.4 . . ?
C41 C46 H46 120.0 . . ?
C45 C46 C41 120.1(4) . . ?
C45 C46 H46 120.0 . . ?
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 S1 O5 115.4(2) . . ?
O3 S1 C14 104.4(2) . . ?
O4 S1 O3 114.9(2) . . ?
O4 S1 O5 114.1(2) . . ?
O4 S1 C14 103.5(2) . . ?
O5 S1 C14 102.3(2) . . ?
F1 C14 S1 111.0(3) . . ?
F2 C14 S1 110.7(3) . . ?
F2 C14 F1 107.8(4) . . ?
F3 C14 S1 111.5(3) . . ?
F3 C14 F1 107.7(4) . . ?
F3 C14 F2 108.0(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 2.3510(10) . ?
Re1 N1 2.118(4) . ?
Re1 N12 2.180(3) . ?
Re1 N22 2.158(4) . ?
Re1 C8 1.914(5) . ?
Re1 C9 1.890(5) . ?
P1 C1 1.863(4) . ?
P1 C31 1.821(4) . ?
P1 C41 1.833(4) . ?
O1 C8 1.154(6) . ?
O2 C9 1.167(6) . ?
N1 C15 1.141(6) . ?
N11 N12 1.358(5) . ?
N11 C7 1.461(5) . ?
N11 C11 1.344(6) . ?
N12 C13 1.324(6) . ?
N21 N22 1.363(5) . ?
N21 C7 1.474(5) . ?
N21 C21 1.347(6) . ?
N22 C23 1.331(5) . ?
C1 C2 1.406(6) . ?
C1 C6 1.393(6) . ?
C2 C3 1.397(6) . ?
C2 C7 1.524(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.369(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.398(6) . ?
C13 H13 0.9300 . ?
C15 C16 1.453(7) . ?
C16 H16a 0.9600 . ?
C16 H16b 0.9600 . ?
C16 H16c 0.9600 . ?
C21 H21 0.9300 . ?
C21 C22 1.375(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.392(6) . ?
C23 H23 0.9300 . ?
C31 C32 1.387(6) . ?
C31 C36 1.407(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.393(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.391(7) . ?
C34 C35 1.398(7) . ?
C34 C37 1.506(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.383(7) . ?
C36 H36 0.9300 . ?
C37 H37a 0.9600 . ?
C37 H37b 0.9600 . ?
C37 H37c 0.9600 . ?
C41 C42 1.395(6) . ?
C41 C46 1.391(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.389(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.378(7) . ?
C44 C45 1.392(7) . ?
C44 C47 1.515(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.391(6) . ?
C46 H46 0.9300 . ?
C47 H47a 0.9600 . ?
C47 H47b 0.9600 . ?
C47 H47c 0.9600 . ?
S1 O3 1.439(3) . ?
S1 O4 1.434(4) . ?
S1 O5 1.441(4) . ?
S1 C14 1.834(5) . ?
F1 C14 1.334(6) . ?
F2 C14 1.330(6) . ?
F3 C14 1.320(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 3.5(4) . . . . ?
Re1 P1 C1 C6 -177.4(3) . . . . ?
Re1 P1 C31 C32 -77.2(4) . . . . ?
Re1 P1 C31 C36 93.2(3) . . . . ?
Re1 P1 C41 C42 -45.9(4) . . . . ?
Re1 P1 C41 C46 137.1(3) . . . . ?
Re1 N12 C13 C12 176.2(3) . . . . ?
Re1 N22 C23 C22 -177.0(3) . . . . ?
P1 C1 C2 C3 -179.6(3) . . . . ?
P1 C1 C2 C7 -0.6(6) . . . . ?
P1 C1 C6 C5 179.9(4) . . . . ?
P1 C31 C32 C33 170.9(3) . . . . ?
P1 C31 C36 C35 -169.8(3) . . . . ?
P1 C41 C42 C43 -177.1(3) . . . . ?
P1 C41 C46 C45 177.3(3) . . . . ?
N11 N12 C13 C12 1.3(5) . . . . ?
N11 C11 C12 C13 -0.7(5) . . . . ?
N12 N11 C7 N21 -57.6(5) . . . . ?
N12 N11 C7 C2 75.2(5) . . . . ?
N12 N11 C11 C12 1.5(5) . . . . ?
N21 N22 C23 C22 -2.2(5) . . . . ?
N21 C21 C22 C23 -0.6(5) . . . . ?
N22 N21 C7 N11 52.7(5) . . . . ?
N22 N21 C7 C2 -79.7(5) . . . . ?
N22 N21 C21 C22 -0.8(5) . . . . ?
C1 P1 C31 C32 155.3(4) . . . . ?
C1 P1 C31 C36 -34.3(4) . . . . ?
C1 P1 C41 C42 81.4(3) . . . . ?
C1 P1 C41 C46 -95.6(4) . . . . ?
C1 C2 C3 C4 -0.8(6) . . . . ?
C1 C2 C7 N11 -67.5(5) . . . . ?
C1 C2 C7 N21 63.6(6) . . . . ?
C2 C1 C6 C5 -0.9(6) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C3 C2 C7 N11 111.5(4) . . . . ?
C3 C2 C7 N21 -117.4(4) . . . . ?
C3 C4 C5 C6 0.7(7) . . . . ?
C4 C5 C6 C1 -0.1(7) . . . . ?
C6 C1 C2 C3 1.4(6) . . . . ?
C6 C1 C2 C7 -179.7(4) . . . . ?
C7 N11 N12 Re1 17.6(5) . . . . ?
C7 N11 N12 C13 -167.2(4) . . . . ?
C7 N11 C11 C12 166.6(4) . . . . ?
C7 N21 N22 Re1 -8.2(5) . . . . ?
C7 N21 N22 C23 176.7(4) . . . . ?
C7 N21 C21 C22 -175.6(4) . . . . ?
C7 C2 C3 C4 -179.9(4) . . . . ?
C11 N11 N12 Re1 -176.9(3) . . . . ?
C11 N11 N12 C13 -1.7(5) . . . . ?
C11 N11 C7 N21 139.0(4) . . . . ?
C11 N11 C7 C2 -88.2(5) . . . . ?
C11 C12 C13 N12 -0.4(5) . . . . ?
C21 N21 N22 Re1 177.0(3) . . . . ?
C21 N21 N22 C23 1.8(5) . . . . ?
C21 N21 C7 N11 -133.1(4) . . . . ?
C21 N21 C7 C2 94.5(5) . . . . ?
C21 C22 C23 N22 1.8(5) . . . . ?
C31 P1 C1 C2 127.6(4) . . . . ?
C31 P1 C1 C6 -53.4(4) . . . . ?
C31 P1 C41 C42 -172.2(3) . . . . ?
C31 P1 C41 C46 10.8(4) . . . . ?
C31 C32 C33 C34 -1.3(7) . . . . ?
C32 C31 C36 C35 0.7(6) . . . . ?
C32 C33 C34 C35 1.0(7) . . . . ?
C32 C33 C34 C37 -177.8(4) . . . . ?
C33 C34 C35 C36 0.1(7) . . . . ?
C34 C35 C36 C31 -1.0(7) . . . . ?
C36 C31 C32 C33 0.4(6) . . . . ?
C37 C34 C35 C36 178.9(4) . . . . ?
C41 P1 C1 C2 -123.1(4) . . . . ?
C41 P1 C1 C6 56.0(4) . . . . ?
C41 P1 C31 C32 51.7(4) . . . . ?
C41 P1 C31 C36 -137.9(4) . . . . ?
C41 C42 C43 C44 -0.3(7) . . . . ?
C42 C41 C46 C45 0.4(6) . . . . ?
C42 C43 C44 C45 0.0(7) . . . . ?
C42 C43 C44 C47 -179.5(4) . . . . ?
C43 C44 C45 C46 0.5(6) . . . . ?
C44 C45 C46 C41 -0.7(7) . . . . ?
C46 C41 C42 C43 0.1(6) . . . . ?
C47 C44 C45 C46 -180.0(4) . . . . ?
O3 S1 C14 F1 61.6(4) . . . . ?
O3 S1 C14 F2 -178.8(3) . . . . ?
O3 S1 C14 F3 -58.5(4) . . . . ?
O4 S1 C14 F1 -59.0(4) . . . . ?
O4 S1 C14 F2 60.7(4) . . . . ?
O4 S1 C14 F3 -179.1(3) . . . . ?
O5 S1 C14 F1 -177.8(4) . . . . ?
O5 S1 C14 F2 -58.2(4) . . . . ?
O5 S1 C14 F3 62.1(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
-8.9999 0.0000 9.0000 0.6665 -0.0527 0.7492
8.9999 -0.0000 -9.0000 -0.6665 0.0527 -0.7492
7.0000 -0.0000 4.0000 -0.2735 0.8805 0.0786
-7.0000 0.0000 -4.0000 0.2735 -0.8805 -0.0786
-6.9999 5.0000 7.0000 0.0849 -0.2082 0.9563
6.9999 -5.0000 -7.0000 -0.0849 0.2082 -0.9563
-2.9999 4.0000 10.0000 0.0312 0.3828 0.9694
6.0000 -4.0000 5.0000 0.1473 1.0084 -0.1371
