#------------------------------------------------------------------------------
#$Date: 2024-10-06 03:20:07 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295078 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249429.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_7249429
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 Br N4 O3 P Re'
_chemical_formula_sum            'C30 H25 Br N4 O3 P Re'
_chemical_formula_weight         786.62
_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                 102.9290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3314(2)
_cell_length_b                   13.5371(2)
_cell_length_c                   17.3610(3)
_cell_measurement_reflns_used    12870
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.6110
_cell_measurement_theta_min      3.6430
_cell_volume                     2824.62(8)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -117.00 -18.00   1.00    1.00    --  -42.46 -37.00  30.00   99
  2  ω    -81.00  27.00   1.00    1.00    --  -42.46  93.00 -67.00  108
  3  ω     23.00  98.00   1.00    1.00    --   42.46-125.00-150.00   75
  4  ω    101.00 178.00   1.00    1.12    --  100.00  93.00 -67.00   77
  5  ω     27.00 118.00   1.00    1.12    --  100.00-125.00 120.00   91
  6  ω     27.00 118.00   1.00    1.12    --  100.00-125.00  30.00   91
  7  ω     27.00 118.00   1.00    1.12    --  100.00-125.00-120.00   91
  8  ω     74.00 173.00   1.00    1.12    --  100.00  45.00   0.00   99
  9  ω     47.00 178.00   1.00    1.12    --  100.00  15.00 120.00  131
 10  ω     94.00 173.00   1.00    1.12    --  100.00 125.00 150.00   79
 11  ω   -119.00 -10.00   1.00    1.00    --  -42.46 -77.00 -30.00  109
 12  ω   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00-120.00  101
 13  ω   -115.00 -14.00   1.00    1.00    --  -42.46 -57.00 150.00  101
 14  ω     94.00 140.00   1.00    1.12    --  100.00 125.00  30.00   46
 15  ω     71.00 172.00   1.00    1.12    --  100.00  61.00-180.00  101
 16  ω     72.00 176.00   1.00    1.12    --  100.00  30.00 -90.00  104
;
_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      -0.0817770000
_diffrn_orient_matrix_UB_12      -0.0761836000
_diffrn_orient_matrix_UB_13      -0.0468062000
_diffrn_orient_matrix_UB_21      -0.0290889000
_diffrn_orient_matrix_UB_22      0.0724356000
_diffrn_orient_matrix_UB_23      -0.0700478000
_diffrn_orient_matrix_UB_31      0.0942451000
_diffrn_orient_matrix_UB_32      -0.0436512000
_diffrn_orient_matrix_UB_33      -0.0345635000
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        70.648
_diffrn_reflns_theta_max         70.648
_diffrn_reflns_theta_min         4.007
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.932
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.135
_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    1.850
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0302
_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)+(0.0340P)²+4.0831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4982
_reflns_number_total             5354
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra05287k3.cif
_cod_data_source_block           1_gard25y
_cod_database_code               7249429
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C30H25BrN4O3PRe
_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   0.354
_shelx_estimated_absorpt_t_min   0.127
_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. Others
 Fixed Sof: Br1A(0.8) Br1B(0.2) O2A(0.8) O2B(0.2) C9A(0.8) C9B(0.2)
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.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)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_olex2_submission_original_sample_id gard25y
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.634
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 0.59843(2) 0.47283(2) 0.34669(2) 0.01755(7) Uani 1 1 d . . . . .
Br1A Br 0.49653(6) 0.63429(7) 0.37173(4) 0.01993(15) Uani 0.8 1 d . . P A 1
Br1B Br 0.6772(3) 0.3002(4) 0.3465(3) 0.0277(10) Uani 0.2 1 d . . P A -1
P1 P 0.54117(8) 0.48965(7) 0.20043(6) 0.0161(2) Uani 1 1 d . . . . .
O3 O 0.6943(3) 0.4637(2) 0.52756(19) 0.0346(8) Uani 1 1 d . . . . .
O1 O 0.8164(3) 0.5755(3) 0.3358(2) 0.0376(8) Uani 1 1 d . . . . .
O2A O 0.6963(7) 0.2650(6) 0.3365(5) 0.036(2) Uani 0.8 1 d . . P A 1
O2B O 0.4815(18) 0.6657(15) 0.3733(12) 0.018(6) Uiso 0.2 1 d . . P A -1
N11 N 0.3372(3) 0.4103(2) 0.31819(19) 0.0190(7) Uani 1 1 d . . . . .
N12 N 0.4448(3) 0.3962(2) 0.35839(19) 0.0177(7) Uani 1 1 d . . . . .
N21 N 0.2093(3) 0.5246(2) 0.2414(2) 0.0199(7) Uani 1 1 d . . . . .
N22 N 0.1084(3) 0.4779(3) 0.2262(3) 0.0303(9) Uani 1 1 d . . . . .
C1 C 0.4240(3) 0.4119(3) 0.1501(2) 0.0185(8) Uani 1 1 d . . . . .
C2 C 0.3231(3) 0.4106(3) 0.1757(2) 0.0169(8) Uani 1 1 d . . . . .
C3 C 0.2380(3) 0.3478(3) 0.1390(2) 0.0205(8) Uani 1 1 d . . . . .
H3 H 0.171756 0.346468 0.156056 0.025 Uiso 1 1 calc R U . . .
C4 C 0.2507(3) 0.2872(3) 0.0773(3) 0.0247(9) Uani 1 1 d . . . . .
H4 H 0.193161 0.245241 0.053553 0.030 Uiso 1 1 calc R U . . .
C5 C 0.3487(3) 0.2889(3) 0.0508(2) 0.0252(9) Uani 1 1 d . . . . .
H5 H 0.357060 0.248342 0.009303 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4343(3) 0.3515(3) 0.0868(2) 0.0215(8) Uani 1 1 d . . . . .
H6 H 0.499585 0.353366 0.068508 0.026 Uiso 1 1 calc R U . . .
C7 C 0.3128(3) 0.4725(3) 0.2465(2) 0.0179(8) Uani 1 1 d . . . . .
H7 H 0.371525 0.522678 0.253276 0.021 Uiso 1 1 calc R U . . .
C10 C 0.6547(4) 0.4666(3) 0.4625(3) 0.0232(9) Uani 1 1 d . . . . .
C8 C 0.7344(4) 0.5380(3) 0.3393(2) 0.0244(9) Uani 1 1 d . . . . .
C9A C 0.6604(7) 0.3458(6) 0.3361(5) 0.0257(19) Uani 0.8 1 d . . P A 1
C9B C 0.527(2) 0.601(2) 0.3684(16) 0.025(8) Uiso 0.2 1 d . . P A -1
C11 C 0.2677(3) 0.3496(3) 0.3446(3) 0.0253(9) Uani 1 1 d . . . . .
H11 H 0.191277 0.344669 0.325086 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3306(4) 0.2959(4) 0.4060(3) 0.0298(10) Uani 1 1 d . . . . .
H12 H 0.305632 0.248695 0.436928 0.036 Uiso 1 1 calc R U . . .
C13 C 0.4386(4) 0.3271(3) 0.4117(3) 0.0260(9) Uani 1 1 d . . . . .
H13 H 0.499588 0.302829 0.448316 0.031 Uiso 1 1 calc R U . . .
C21 C 0.1999(4) 0.6211(3) 0.2590(3) 0.0316(10) Uani 1 1 d . . . . .
H21 H 0.257622 0.666534 0.271986 0.038 Uiso 1 1 calc R U . . .
C22 C 0.0902(4) 0.6390(4) 0.2544(3) 0.0388(12) Uani 1 1 d . . . . .
H22 H 0.057411 0.698652 0.263003 0.047 Uiso 1 1 calc R U . . .
C23 C 0.0377(4) 0.5492(4) 0.2339(3) 0.0303(10) Uani 1 1 d . . . . .
H23 H -0.038689 0.539832 0.226478 0.036 Uiso 1 1 calc R U . . .
C31 C 0.6545(3) 0.4604(3) 0.1511(2) 0.0184(8) Uani 1 1 d . . . . .
C32 C 0.6979(3) 0.5316(3) 0.1087(3) 0.0227(9) Uani 1 1 d . . . . .
H32 H 0.666721 0.594504 0.103214 0.027 Uiso 1 1 calc R U . . .
C33 C 0.7860(3) 0.5111(3) 0.0745(3) 0.0231(9) Uani 1 1 d . . . . .
H33 H 0.813072 0.560167 0.046338 0.028 Uiso 1 1 calc R U . . .
C34 C 0.8353(3) 0.4173(3) 0.0817(2) 0.0196(8) Uani 1 1 d . . . . .
C35 C 0.7918(3) 0.3466(3) 0.1241(2) 0.0211(8) Uani 1 1 d . . . . .
H35 H 0.822770 0.283632 0.129362 0.025 Uiso 1 1 calc R U . . .
C36 C 0.7039(3) 0.3669(3) 0.1588(2) 0.0218(9) Uani 1 1 d . . . . .
H36 H 0.677396 0.318004 0.187415 0.026 Uiso 1 1 calc R U . . .
C37 C 0.9320(3) 0.3970(3) 0.0450(3) 0.0246(9) Uani 1 1 d . . . . .
H37A H 0.994418 0.436446 0.070580 0.037 Uiso 1 1 calc R U . . .
H37B H 0.912221 0.413064 -0.010184 0.037 Uiso 1 1 calc R U . . .
H37C H 0.951467 0.328283 0.051239 0.037 Uiso 1 1 calc R U . . .
C41 C 0.5019(3) 0.6134(3) 0.1617(2) 0.0176(8) Uani 1 1 d . . . . .
C42 C 0.4278(3) 0.6276(3) 0.0895(2) 0.0195(8) Uani 1 1 d . . . . .
H42 H 0.388004 0.574285 0.063553 0.023 Uiso 1 1 calc R U . . .
C43 C 0.4130(3) 0.7209(3) 0.0561(2) 0.0213(8) Uani 1 1 d . . . . .
H43 H 0.363426 0.729240 0.007665 0.026 Uiso 1 1 calc R U . . .
C44 C 0.4710(3) 0.8028(3) 0.0935(2) 0.0217(8) Uani 1 1 d . . . . .
C45 C 0.5430(3) 0.7878(3) 0.1666(2) 0.0219(8) Uani 1 1 d . . . . .
H45 H 0.581055 0.841416 0.193345 0.026 Uiso 1 1 calc R U . . .
C46 C 0.5590(3) 0.6951(3) 0.2002(2) 0.0206(8) Uani 1 1 d . . . . .
H46 H 0.608120 0.686922 0.248922 0.025 Uiso 1 1 calc R U . . .
C47 C 0.4578(4) 0.9035(3) 0.0563(3) 0.0315(10) Uani 1 1 d . . . . .
H47A H 0.409620 0.942747 0.080351 0.047 Uiso 1 1 calc R U . . .
H47B H 0.426119 0.897226 0.000733 0.047 Uiso 1 1 calc R U . . .
H47C H 0.529288 0.934768 0.063988 0.047 Uiso 1 1 calc R U . . .
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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
-4 -5 -6 0.0813
4 5 6 0.0383
-7 3 6 0.1387
7 -3 -6 0.1387
6 1 -9 0.1000
-6 -1 9 0.1000
-7 1 -4 0.0906
7 -1 4 0.0906
2 7 -7 0.0962
0 -6 8 0.1269
-4 8 1 0.1438
4 -8 -1 0.1838
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
Br1B Re1 Br1A 166.97(11) . . ?
P1 Re1 Br1A 93.22(3) . . ?
P1 Re1 Br1B 96.00(11) . . ?
N12 Re1 Br1A 85.60(9) . . ?
N12 Re1 Br1B 84.48(13) . . ?
N12 Re1 P1 94.78(9) . . ?
C10 Re1 Br1A 86.50(12) . . ?
C10 Re1 Br1B 85.08(16) . . ?
C10 Re1 P1 175.18(12) . . ?
C10 Re1 N12 90.00(15) . . ?
C10 Re1 C9B 85.1(8) . . ?
C8 Re1 Br1A 94.95(13) . . ?
C8 Re1 Br1B 94.75(16) . . ?
C8 Re1 P1 86.72(12) . . ?
C8 Re1 N12 178.37(15) . . ?
C8 Re1 C10 88.50(17) . . ?
C8 Re1 C9B 92.4(8) . . ?
C9A Re1 Br1A 172.3(2) . . ?
C9A Re1 Br1B 5.9(3) . . ?
C9A Re1 P1 90.7(2) . . ?
C9A Re1 N12 87.5(3) . . ?
C9A Re1 C10 90.2(3) . . ?
C9A Re1 C8 91.9(3) . . ?
C9A Re1 C9B 173.5(8) . . ?
C9B Re1 Br1A 2.8(8) . . ?
C9B Re1 Br1B 167.7(8) . . ?
C9B Re1 P1 94.4(8) . . ?
C9B Re1 N12 88.1(8) . . ?
C9B Br1A Re1 10(3) . . ?
O2A Br1B Re1 161.5(14) . . ?
O2A Br1B C9A 144.3(19) . . ?
C9A Br1B Re1 17.2(9) . . ?
C1 P1 Re1 116.41(13) . . ?
C31 P1 Re1 112.56(13) . . ?
C31 P1 C1 104.71(18) . . ?
C41 P1 Re1 116.74(13) . . ?
C41 P1 C1 103.51(18) . . ?
C41 P1 C31 101.10(18) . . ?
Br1B O2A C9A 19.2(11) . . ?
N12 N11 C7 120.1(3) . . ?
C11 N11 N12 111.2(3) . . ?
C11 N11 C7 127.8(3) . . ?
N11 N12 Re1 129.9(2) . . ?
C13 N12 Re1 125.3(3) . . ?
C13 N12 N11 104.7(3) . . ?
N22 N21 C7 122.7(3) . . ?
C21 N21 N22 111.7(3) . . ?
C21 N21 C7 125.3(4) . . ?
C23 N22 N21 103.6(4) . . ?
C2 C1 P1 120.8(3) . . ?
C6 C1 P1 120.4(3) . . ?
C6 C1 C2 118.8(4) . . ?
C1 C2 C7 119.1(3) . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 C7 121.2(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.3(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.5(4) . . ?
C6 C5 H5 120.3 . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.1(4) . . ?
C5 C6 H6 119.4 . . ?
N11 C7 C2 109.3(3) . . ?
N11 C7 H7 106.7 . . ?
N21 C7 N11 109.9(3) . . ?
N21 C7 C2 117.0(3) . . ?
N21 C7 H7 106.7 . . ?
C2 C7 H7 106.7 . . ?
O3 C10 Re1 175.1(4) . . ?
O1 C8 Re1 178.7(4) . . ?
Br1B C9A Re1 156.9(12) . . ?
Br1B C9A O2A 16.5(9) . . ?
O2A C9A Re1 173.4(8) . . ?
Br1A C9B Re1 168(3) . . ?
Br1A C9B O2B 7.2(14) . . ?
O2B C9B Re1 173(3) . . ?
N11 C11 H11 126.4 . . ?
N11 C11 C12 107.2(4) . . ?
C12 C11 H11 126.4 . . ?
C11 C12 H12 127.4 . . ?
C11 C12 C13 105.1(4) . . ?
C13 C12 H12 127.4 . . ?
N12 C13 C12 111.8(4) . . ?
N12 C13 H13 124.1 . . ?
C12 C13 H13 124.1 . . ?
N21 C21 H21 126.5 . . ?
N21 C21 C22 107.1(4) . . ?
C22 C21 H21 126.5 . . ?
C21 C22 H22 127.5 . . ?
C21 C22 C23 105.1(4) . . ?
C23 C22 H22 127.5 . . ?
N22 C23 C22 112.5(4) . . ?
N22 C23 H23 123.7 . . ?
C22 C23 H23 123.7 . . ?
C32 C31 P1 121.4(3) . . ?
C32 C31 C36 117.8(4) . . ?
C36 C31 P1 120.8(3) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.5(4) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.9(4) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C37 120.0(4) . . ?
C35 C34 C33 117.5(4) . . ?
C35 C34 C37 122.5(4) . . ?
C34 C35 H35 119.0 . . ?
C36 C35 C34 121.9(4) . . ?
C36 C35 H35 119.0 . . ?
C31 C36 H36 119.8 . . ?
C35 C36 C31 120.5(4) . . ?
C35 C36 H36 119.8 . . ?
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 121.6(3) . . ?
C42 C41 C46 118.8(4) . . ?
C46 C41 P1 119.0(3) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 120.1(4) . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 119.2 . . ?
C42 C43 C44 121.6(4) . . ?
C44 C43 H43 119.2 . . ?
C43 C44 C47 121.7(4) . . ?
C45 C44 C43 117.6(4) . . ?
C45 C44 C47 120.7(4) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 C44 121.3(4) . . ?
C46 C45 H45 119.3 . . ?
C41 C46 H46 119.7 . . ?
C45 C46 C41 120.5(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 . . ?
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 Br1A 2.6057(11) . ?
Re1 Br1B 2.531(5) . ?
Re1 P1 2.4892(10) . ?
Re1 N12 2.209(3) . ?
Re1 C10 1.976(4) . ?
Re1 C8 1.925(4) . ?
Re1 C9A 1.907(9) . ?
Re1 C9B 2.02(3) . ?
Br1A C9B 0.60(3) . ?
Br1B O2A 0.575(5) . ?
Br1B C9A 0.664(6) . ?
P1 C1 1.842(4) . ?
P1 C31 1.837(4) . ?
P1 C41 1.830(4) . ?
O3 C10 1.127(5) . ?
O1 C8 1.145(5) . ?
O2A C9A 1.179(10) . ?
O2B C9B 1.06(3) . ?
N11 N12 1.367(4) . ?
N11 C7 1.477(5) . ?
N11 C11 1.340(5) . ?
N12 C13 1.329(5) . ?
N21 N22 1.367(5) . ?
N21 C7 1.444(5) . ?
N21 C21 1.352(5) . ?
N22 C23 1.327(6) . ?
C1 C2 1.411(5) . ?
C1 C6 1.398(6) . ?
C2 C3 1.389(5) . ?
C2 C7 1.516(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.386(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9800 . ?
C11 H11 0.9300 . ?
C11 C12 1.377(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.379(6) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.359(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.386(7) . ?
C23 H23 0.9300 . ?
C31 C32 1.392(6) . ?
C31 C36 1.399(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.377(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.401(6) . ?
C34 C35 1.387(6) . ?
C34 C37 1.498(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.379(6) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.389(5) . ?
C41 C46 1.399(5) . ?
C42 H42 0.9300 . ?
C42 C43 1.384(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.398(6) . ?
C44 C45 1.391(6) . ?
C44 C47 1.502(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.379(6) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
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 Br1A C9B O2B 148(15) . . . . ?
Re1 Br1B O2A C9A 1(2) . . . . ?
Re1 Br1B C9A O2A -179(3) . . . . ?
Re1 P1 C1 C2 51.4(4) . . . . ?
Re1 P1 C1 C6 -127.3(3) . . . . ?
Re1 P1 C31 C32 -116.3(3) . . . . ?
Re1 P1 C31 C36 60.2(3) . . . . ?
Re1 P1 C41 C42 -152.8(3) . . . . ?
Re1 P1 C41 C46 36.1(4) . . . . ?
Re1 N12 C13 C12 177.8(3) . . . . ?
P1 C1 C2 C3 -177.0(3) . . . . ?
P1 C1 C2 C7 -1.3(5) . . . . ?
P1 C1 C6 C5 176.8(3) . . . . ?
P1 C31 C32 C33 177.2(3) . . . . ?
P1 C31 C36 C35 -177.5(3) . . . . ?
P1 C41 C42 C43 -169.9(3) . . . . ?
P1 C41 C46 C45 170.6(3) . . . . ?
O2A Br1B C9A Re1 179(3) . . . . ?
N11 N12 C13 C12 0.8(5) . . . . ?
N11 C11 C12 C13 -1.5(5) . . . . ?
N12 N11 C7 N21 -145.8(3) . . . . ?
N12 N11 C7 C2 84.6(4) . . . . ?
N12 N11 C11 C12 2.1(5) . . . . ?
N21 N22 C23 C22 -0.7(6) . . . . ?
N21 C21 C22 C23 0.4(6) . . . . ?
N22 N21 C7 N11 -69.3(5) . . . . ?
N22 N21 C7 C2 56.0(5) . . . . ?
N22 N21 C21 C22 -0.9(6) . . . . ?
C1 P1 C31 C32 116.3(3) . . . . ?
C1 P1 C31 C36 -67.1(4) . . . . ?
C1 P1 C41 C42 -23.5(4) . . . . ?
C1 P1 C41 C46 165.4(3) . . . . ?
C1 C2 C3 C4 -0.6(6) . . . . ?
C1 C2 C7 N11 -95.8(4) . . . . ?
C1 C2 C7 N21 138.5(4) . . . . ?
C2 C1 C6 C5 -2.0(6) . . . . ?
C2 C3 C4 C5 -0.4(6) . . . . ?
C3 C2 C7 N11 79.8(4) . . . . ?
C3 C2 C7 N21 -45.8(5) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
C4 C5 C6 C1 1.0(6) . . . . ?
C6 C1 C2 C3 1.7(6) . . . . ?
C6 C1 C2 C7 177.4(3) . . . . ?
C7 N11 N12 Re1 11.8(5) . . . . ?
C7 N11 N12 C13 -171.5(3) . . . . ?
C7 N11 C11 C12 170.8(4) . . . . ?
C7 N21 N22 C23 174.3(4) . . . . ?
C7 N21 C21 C22 -174.0(4) . . . . ?
C7 C2 C3 C4 -176.2(4) . . . . ?
C11 N11 N12 Re1 -178.5(3) . . . . ?
C11 N11 N12 C13 -1.8(4) . . . . ?
C11 N11 C7 N21 46.4(5) . . . . ?
C11 N11 C7 C2 -83.2(5) . . . . ?
C11 C12 C13 N12 0.4(5) . . . . ?
C21 N21 N22 C23 0.9(5) . . . . ?
C21 N21 C7 N11 103.1(5) . . . . ?
C21 N21 C7 C2 -131.6(4) . . . . ?
C21 C22 C23 N22 0.2(6) . . . . ?
C31 P1 C1 C2 176.4(3) . . . . ?
C31 P1 C1 C6 -2.3(4) . . . . ?
C31 P1 C41 C42 84.8(3) . . . . ?
C31 P1 C41 C46 -86.4(3) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C32 C31 C36 C35 -0.8(6) . . . . ?
C32 C33 C34 C35 0.1(6) . . . . ?
C32 C33 C34 C37 -179.2(4) . . . . ?
C33 C34 C35 C36 -0.5(6) . . . . ?
C34 C35 C36 C31 0.8(6) . . . . ?
C36 C31 C32 C33 0.5(6) . . . . ?
C37 C34 C35 C36 178.8(4) . . . . ?
C41 P1 C1 C2 -78.1(3) . . . . ?
C41 P1 C1 C6 103.2(3) . . . . ?
C41 P1 C31 C32 9.0(4) . . . . ?
C41 P1 C31 C36 -174.5(3) . . . . ?
C41 C42 C43 C44 -0.3(6) . . . . ?
C42 C41 C46 C45 -0.8(6) . . . . ?
C42 C43 C44 C45 -1.2(6) . . . . ?
C42 C43 C44 C47 178.1(4) . . . . ?
C43 C44 C45 C46 1.6(6) . . . . ?
C44 C45 C46 C41 -0.7(6) . . . . ?
C46 C41 C42 C43 1.3(6) . . . . ?
C47 C44 C45 C46 -177.6(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
-4.0032 -5.0066 -5.9927 0.9893 0.1736 0.0484
4.0032 5.0066 5.9927 -0.9893 -0.1736 -0.0484
-7.0012 3.0013 6.0063 0.0628 0.0003 -0.9984
7.0012 -3.0013 -6.0063 -0.0628 -0.0003 0.9984
5.9990 0.9976 -9.0085 -0.1449 0.5288 0.8332
-5.9990 -0.9976 9.0085 0.1449 -0.5288 -0.8332
-7.0047 0.9950 -3.9935 0.6839 0.5556 -0.5656
7.0047 -0.9950 3.9935 -0.6839 -0.5556 0.5656
1.9970 6.9987 -7.0082 -0.3685 0.9398 0.1249
0.0041 -5.9970 8.0054 0.0818 -0.9953 -0.0145
-4.0027 8.0011 0.9987 -0.3290 0.6260 -0.7610
4.0027 -8.0011 -0.9987 0.3290 -0.6260 0.7610
