#------------------------------------------------------------------------------
#$Date: 2020-02-04 22:05:20 +0200 (Tue, 04 Feb 2020) $
#$Revision: 247597 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125656.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_7125656
loop_
_publ_author_name
'Yadav, Pinky'
'Fridman, Natalia'
'Mizrahi, Amir'
'Gross, Zeev'
_publ_section_title
;
Rhenium(i) sapphyrins: remarkable difference between the
C6F5 and CF3-substituted derivatives.
;
_journal_issue 6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first 980
_journal_page_last 983
_journal_paper_doi 10.1039/c9cc08877f
_journal_volume 56
_journal_year 2020
_chemical_formula_moiety 'C31 H12 F12 N5 O3 Re'
_chemical_formula_sum 'C31 H12 F12 N5 O3 Re'
_chemical_formula_weight 916.66
_chemical_name_common 'Gross254b (Pinky)'
_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 mixed
_audit_creation_method SHELXL-2018/3
_audit_update_record
;
2019-08-25 deposited with the CCDC. 2019-12-16 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 101.594(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.9191(10)
_cell_length_b 13.1221(11)
_cell_length_c 19.0424(17)
_cell_measurement_reflns_used 5076
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 25.047
_cell_measurement_theta_min 1.862
_cell_volume 2917.5(4)
_computing_cell_refinement 'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection 'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature 200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type 'APEX2 (Bruker AXS)'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1168
_diffrn_reflns_av_unetI/netI 0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 19449
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full 25.047
_diffrn_reflns_theta_max 25.047
_diffrn_reflns_theta_min 1.862
_exptl_absorpt_coefficient_mu 4.288
_exptl_absorpt_correction_T_max 0.546
_exptl_absorpt_correction_T_min 0.492
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour 'dark brown'
_exptl_crystal_density_diffrn 2.087
_exptl_crystal_description prism
_exptl_crystal_F_000 1760
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.150
_refine_diff_density_max 1.067
_refine_diff_density_min -1.624
_refine_diff_density_rms 0.130
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.985
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 477
_refine_ls_number_reflns 5076
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.985
_refine_ls_R_factor_all 0.0397
_refine_ls_R_factor_gt 0.0321
_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/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0745
_refine_ls_wR_factor_ref 0.0775
_reflns_Friedel_coverage 0.000
_reflns_number_gt 4216
_reflns_number_total 5076
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9cc08877f2.cif
_cod_data_source_block Gross254b
_cod_depositor_comments
'Adding full bibliography for 7125655--7125656.cif.'
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 7125656
_shelx_shelxl_version_number 2018/3
_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_min 0.512
_shelx_estimated_absorpt_t_max 0.566
_shelx_res_file
;
TITL mo_Gross254b_0m_a.res in P2(1)/n
gross254b.res
created by SHELXL-2018/3 at 09:39:29 on 31-Jul-2019
REM Old TITL mo_Gross254b_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.104, Rweak 0.003, Alpha 0.038, Orientation as input
REM Formula found by SHELXT: C32 N4 O5 F10 Re
CELL 0.71073 11.9191 13.1221 19.0424 90 101.594 90
ZERR 4 0.001 0.0011 0.0017 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H F N O Re
UNIT 124 48 48 20 12 4
L.S. 10
PLAN 20
SIZE 0.15 0.15 0.18
TEMP -73
BOND $H
LIST 6
fmap 2
acta
OMIT 10 0 4
OMIT 10 0 2
OMIT 10 1 5
OMIT 0 1 2
OMIT 10 1 3
OMIT 10 1 1
OMIT 10 2 4
OMIT -7 0 21
REM
REM
REM
WGHT 0.032000
FVAR 0.20969
RE1 6 0.778038 0.552823 0.548857 11.00000 0.02912 0.02694 =
0.02028 -0.00071 -0.00094 -0.00379
F1 3 0.857374 0.269666 0.359047 11.00000 0.10257 0.07886 =
0.06624 -0.01051 0.03551 0.03329
F2 3 0.697150 0.201555 0.364241 11.00000 0.07328 0.10247 =
0.13074 -0.08457 -0.02326 0.00486
F3 3 0.843079 0.178158 0.447862 11.00000 0.09122 0.05527 =
0.07593 -0.00452 0.02179 0.03339
F4 3 0.764590 0.772629 0.311043 11.00000 0.14604 0.08438 =
0.09525 0.04013 0.08171 0.02319
F5 3 0.727507 0.867275 0.391001 11.00000 0.14921 0.06430 =
0.07421 0.00837 0.03707 -0.03990
F6 3 0.595858 0.817339 0.312286 11.00000 0.08186 0.11496 =
0.14972 0.09241 -0.03300 -0.01375
F7 3 0.621927 0.976443 0.552843 11.00000 0.13664 0.03598 =
0.06571 0.00290 0.03011 -0.00809
F8 3 0.648549 0.995075 0.664243 11.00000 0.13949 0.04284 =
0.05379 -0.00811 -0.01497 -0.02578
F9 3 0.480434 0.984608 0.602709 11.00000 0.07541 0.05632 =
0.16337 0.01982 0.01643 0.02833
F10 3 0.512668 0.642314 0.903492 11.00000 0.11535 0.08692 =
0.03991 -0.00419 0.03688 0.00447
F11 3 0.618262 0.510587 0.913006 11.00000 0.09144 0.11085 =
0.03698 0.02232 0.00421 0.01551
F12 3 0.440940 0.500303 0.863925 11.00000 0.08418 0.11585 =
0.05709 0.00305 0.03375 -0.02925
O1 5 0.849855 0.599242 0.708965 11.00000 0.07067 0.04414 =
0.02646 -0.00590 -0.00377 -0.00976
O2 5 0.903240 0.753034 0.534339 11.00000 0.06015 0.04666 =
0.07837 0.01351 -0.00340 -0.02325
O3 5 1.007363 0.444609 0.573945 11.00000 0.03566 0.06726 =
0.05308 0.01718 0.00743 0.00975
N3 4 0.585950 0.693062 0.703930 11.00000 0.04622 0.03972 =
0.02365 0.00055 0.00680 0.00275
N1 4 0.731783 0.523875 0.434257 11.00000 0.04107 0.03778 =
0.02076 -0.00607 0.00676 0.00338
N5 4 0.698348 0.402896 0.553785 11.00000 0.02697 0.03017 =
0.02973 0.00210 -0.00194 -0.00285
N4 4 0.612788 0.491898 0.692362 11.00000 0.04247 0.03373 =
0.02839 0.00556 0.00608 0.00016
AFIX 43
H4 2 0.616107 0.546741 0.666260 11.00000 -1.20000
AFIX 0
N2 4 0.628032 0.790930 0.500189 11.00000 0.04011 0.02793 =
0.03276 0.00352 0.00338 -0.00161
H2 2 0.666092 0.845473 0.489656 11.00000 0.03425
C1 1 0.753464 0.341088 0.441466 11.00000 0.02987 0.03704 =
0.04167 -0.01089 -0.00161 0.00130
C2 1 0.747505 0.433415 0.403354 11.00000 0.03571 0.04213 =
0.02644 -0.01146 -0.00012 0.00345
C3 1 0.741881 0.451485 0.327241 11.00000 0.06172 0.06561 =
0.02741 -0.01118 0.00591 0.00997
AFIX 43
H3 2 0.749798 0.401512 0.292468 11.00000 -1.20000
AFIX 0
C4 1 0.723444 0.551762 0.315047 11.00000 0.05379 0.06584 =
0.02938 0.00052 0.00866 0.00348
AFIX 43
H4A 2 0.719162 0.586130 0.270678 11.00000 -1.20000
AFIX 0
C5 1 0.711580 0.596516 0.381318 11.00000 0.04151 0.05169 =
0.01790 0.00466 -0.00460 -0.00387
C6 1 0.676921 0.694825 0.397308 11.00000 0.03968 0.04024 =
0.02563 0.00699 0.00391 0.00100
C7 1 0.629916 0.706418 0.458992 11.00000 0.03422 0.03517 =
0.02607 0.00443 0.00064 0.00286
C8 1 0.582103 0.625384 0.493951 11.00000 0.02432 0.02727 =
0.02799 0.00175 -0.00511 0.00147
AFIX 13
H8 2 0.524761 0.579353 0.464035 11.00000 -1.20000
AFIX 0
C9 1 0.558082 0.662972 0.555903 11.00000 0.03654 0.03296 =
0.02759 0.00368 0.00631 -0.00474
H9 2 0.522815 0.628764 0.590322 11.00000 0.06900
C10 1 0.590628 0.767987 0.562428 11.00000 0.03150 0.02750 =
0.03130 0.00292 -0.00206 0.00228
C11 1 0.585402 0.832657 0.620321 11.00000 0.04036 0.02997 =
0.03352 -0.00338 0.00025 -0.00077
C12 1 0.574044 0.794257 0.687190 11.00000 0.04063 0.03176 =
0.03220 -0.00309 0.00123 0.00511
C13 1 0.543953 0.845730 0.747122 11.00000 0.05007 0.04563 =
0.04147 -0.01250 0.00167 0.00253
AFIX 43
H13 2 0.532204 0.916967 0.750862 11.00000 -1.20000
AFIX 0
C14 1 0.535227 0.775182 0.797365 11.00000 0.05701 0.05981 =
0.03032 -0.01226 0.00938 0.00079
AFIX 43
H14 2 0.515516 0.787516 0.842535 11.00000 -1.20000
AFIX 0
C15 1 0.561399 0.677623 0.769696 11.00000 0.03734 0.05215 =
0.03016 -0.00528 0.00353 0.00102
C16 1 0.562169 0.578291 0.797097 11.00000 0.03655 0.05487 =
0.02735 0.00232 0.00472 -0.00175
C17 1 0.585727 0.491409 0.758783 11.00000 0.03795 0.04538 =
0.03336 0.00965 0.00270 -0.00267
C18 1 0.588329 0.387720 0.782605 11.00000 0.06909 0.05277 =
0.03981 0.02092 0.01498 -0.00628
AFIX 43
H18 2 0.573166 0.364285 0.826975 11.00000 -1.20000
AFIX 0
C19 1 0.616490 0.329214 0.729977 11.00000 0.06095 0.03184 =
0.04566 0.01345 0.00560 -0.00142
AFIX 43
H19 2 0.623511 0.257087 0.730964 11.00000 -1.20000
AFIX 0
C20 1 0.633994 0.394691 0.672296 11.00000 0.03220 0.03039 =
0.03395 0.00796 -0.00118 -0.00441
C21 1 0.664695 0.355481 0.610571 11.00000 0.02373 0.03051 =
0.03675 0.00618 -0.00117 -0.00212
C22 1 0.662556 0.247783 0.597900 11.00000 0.03835 0.02845 =
0.05383 0.00404 0.00079 -0.00394
AFIX 43
H22 2 0.640526 0.197408 0.628317 11.00000 -1.20000
AFIX 0
C23 1 0.696553 0.229749 0.536402 11.00000 0.04686 0.02776 =
0.05553 -0.00458 0.00465 -0.00126
AFIX 43
H23 2 0.703397 0.164868 0.515531 11.00000 -1.20000
AFIX 0
C24 1 0.721030 0.327247 0.507443 11.00000 0.03147 0.02709 =
0.04153 -0.00617 -0.00452 0.00014
C25 1 0.787131 0.247757 0.403903 11.00000 0.05461 0.05081 =
0.04974 -0.01741 -0.00201 0.00905
C26 1 0.690359 0.784974 0.351647 11.00000 0.05909 0.05511 =
0.03879 0.01489 0.00636 -0.00303
C27 1 0.584962 0.945702 0.610955 11.00000 0.06787 0.03231 =
0.03743 -0.00062 0.00132 0.00616
C28 1 0.534168 0.558191 0.869086 11.00000 0.05152 0.07442 =
0.03104 0.00599 0.00846 0.00140
C29 1 0.814960 0.581159 0.649539 11.00000 0.04331 0.02739 =
0.03324 -0.00251 0.01261 -0.00246
C30 1 0.855875 0.678463 0.538456 11.00000 0.04193 0.03427 =
0.03648 0.00223 -0.00727 -0.00494
C31 1 0.920352 0.485505 0.563376 11.00000 0.02823 0.04433 =
0.02652 0.00231 0.00471 -0.00525
HKLF 4
REM mo_Gross254b_0m_a.res in P2(1)/n
REM wR2 = 0.0775, GooF = S = 0.985, Restrained GooF = 0.985 for all data
REM R1 = 0.0321 for 4216 Fo > 4sig(Fo) and 0.0397 for all 5076 data
REM 477 parameters refined using 0 restraints
END
WGHT 0.0320 0.0000
REM Highest difference peak 1.067, deepest hole -1.624, 1-sigma level 0.130
Q1 1 0.7379 0.5494 0.5885 11.00000 0.05 1.07
Q2 1 0.8268 0.5493 0.5109 11.00000 0.05 1.04
Q3 1 0.7416 0.6110 0.6332 11.00000 0.05 0.92
Q4 1 0.8310 0.6060 0.6100 11.00000 0.05 0.78
Q5 1 0.7202 0.5002 0.4875 11.00000 0.05 0.71
Q6 1 0.6520 0.7483 0.2807 11.00000 0.05 0.68
Q7 1 0.8308 0.4927 0.6047 11.00000 0.05 0.66
Q8 1 0.6406 0.8533 0.3616 11.00000 0.05 0.66
Q9 1 0.7203 0.6111 0.4918 11.00000 0.05 0.63
Q10 1 0.7833 0.8149 0.3699 11.00000 0.05 0.61
Q11 1 0.8174 0.6182 0.5528 11.00000 0.05 0.57
Q12 1 0.6033 0.6496 0.6822 11.00000 0.05 0.51
Q13 1 0.8996 0.6025 0.6686 11.00000 0.05 0.48
Q14 1 0.6623 0.5574 0.3520 11.00000 0.05 0.48
Q15 1 0.5609 0.8273 0.3075 11.00000 0.05 0.47
Q16 1 0.5950 0.5471 0.7915 11.00000 0.05 0.44
Q17 1 0.6667 0.3823 0.5811 11.00000 0.05 0.43
Q18 1 0.5958 0.6831 0.7348 11.00000 0.05 0.41
Q19 1 0.6296 0.6408 0.5345 11.00000 0.05 0.41
Q20 1 0.5476 0.9953 0.6642 11.00000 0.05 0.41
;
_shelx_res_checksum 92920
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
Re1 Re 0.77804(2) 0.55282(2) 0.54886(2) 0.02627(8) Uani 1 1 d . .
F1 F 0.8574(4) 0.2697(3) 0.3590(2) 0.0800(12) Uani 1 1 d . .
F2 F 0.6971(4) 0.2016(4) 0.3642(3) 0.1083(19) Uani 1 1 d . .
F3 F 0.8431(4) 0.1782(3) 0.4479(2) 0.0734(11) Uani 1 1 d . .
F4 F 0.7646(4) 0.7726(3) 0.3110(2) 0.1005(16) Uani 1 1 d . .
F5 F 0.7275(4) 0.8673(3) 0.3910(2) 0.0939(15) Uani 1 1 d . .
F6 F 0.5959(4) 0.8173(4) 0.3123(3) 0.123(2) Uani 1 1 d . .
F7 F 0.6219(4) 0.9764(2) 0.5528(2) 0.0781(12) Uani 1 1 d . .
F8 F 0.6485(4) 0.9951(3) 0.66424(19) 0.0835(13) Uani 1 1 d . .
F9 F 0.4804(4) 0.9846(3) 0.6027(3) 0.0994(15) Uani 1 1 d . .
F10 F 0.5127(4) 0.6423(3) 0.90349(19) 0.0778(11) Uani 1 1 d . .
F11 F 0.6183(4) 0.5106(4) 0.91301(19) 0.0810(12) Uani 1 1 d . .
F12 F 0.4409(4) 0.5003(4) 0.8639(2) 0.0830(12) Uani 1 1 d . .
O1 O 0.8499(4) 0.5992(3) 0.70896(19) 0.0490(9) Uani 1 1 d . .
O2 O 0.9032(4) 0.7530(3) 0.5343(2) 0.0641(12) Uani 1 1 d . .
O3 O 1.0074(3) 0.4446(3) 0.5739(2) 0.0522(10) Uani 1 1 d . .
N3 N 0.5860(4) 0.6931(3) 0.7039(2) 0.0366(9) Uani 1 1 d . .
N1 N 0.7318(3) 0.5239(3) 0.4343(2) 0.0331(9) Uani 1 1 d . .
N5 N 0.6983(3) 0.4029(3) 0.5538(2) 0.0300(8) Uani 1 1 d . .
N4 N 0.6128(3) 0.4919(3) 0.6924(2) 0.0350(9) Uani 1 1 d . .
H4 H 0.616107 0.546741 0.666260 0.042 Uiso 1 1 calc R U
N2 N 0.6280(4) 0.7909(3) 0.5002(2) 0.0342(9) Uani 1 1 d . .
H2 H 0.666(4) 0.845(4) 0.490(3) 0.034(13) Uiso 1 1 d . .
C1 C 0.7535(4) 0.3411(4) 0.4415(3) 0.0374(11) Uani 1 1 d . .
C2 C 0.7475(4) 0.4334(3) 0.4034(3) 0.0356(11) Uani 1 1 d . .
C3 C 0.7419(6) 0.4515(4) 0.3272(3) 0.0520(15) Uani 1 1 d . .
H3 H 0.749798 0.401512 0.292468 0.062 Uiso 1 1 calc R U
C4 C 0.7234(5) 0.5518(4) 0.3150(3) 0.0496(14) Uani 1 1 d . .
H4A H 0.719162 0.586130 0.270678 0.060 Uiso 1 1 calc R U
C5 C 0.7116(5) 0.5965(4) 0.3813(3) 0.0385(12) Uani 1 1 d . .
C6 C 0.6769(4) 0.6948(4) 0.3973(3) 0.0356(11) Uani 1 1 d . .
C7 C 0.6299(4) 0.7064(3) 0.4590(2) 0.0326(10) Uani 1 1 d . .
C8 C 0.5821(4) 0.6254(3) 0.4940(2) 0.0280(10) Uani 1 1 d . .
H8 H 0.524761 0.579353 0.464035 0.034 Uiso 1 1 calc R U
C9 C 0.5581(4) 0.6630(3) 0.5559(3) 0.0324(10) Uani 1 1 d . .
H9 H 0.523(5) 0.629(5) 0.590(4) 0.069(19) Uiso 1 1 d . .
C10 C 0.5906(4) 0.7680(3) 0.5624(2) 0.0313(10) Uani 1 1 d . .
C11 C 0.5854(4) 0.8327(3) 0.6203(3) 0.0356(11) Uani 1 1 d . .
C12 C 0.5740(4) 0.7943(3) 0.6872(3) 0.0357(11) Uani 1 1 d . .
C13 C 0.5440(5) 0.8457(4) 0.7471(3) 0.0468(13) Uani 1 1 d . .
H13 H 0.532204 0.916967 0.750862 0.056 Uiso 1 1 calc R U
C14 C 0.5352(5) 0.7752(4) 0.7974(3) 0.0490(14) Uani 1 1 d . .
H14 H 0.515516 0.787516 0.842535 0.059 Uiso 1 1 calc R U
C15 C 0.5614(4) 0.6776(4) 0.7697(3) 0.0403(12) Uani 1 1 d . .
C16 C 0.5622(4) 0.5783(4) 0.7971(3) 0.0398(12) Uani 1 1 d . .
C17 C 0.5857(4) 0.4914(4) 0.7588(3) 0.0395(12) Uani 1 1 d . .
C18 C 0.5883(5) 0.3877(4) 0.7826(3) 0.0533(15) Uani 1 1 d . .
H18 H 0.573166 0.364285 0.826975 0.064 Uiso 1 1 calc R U
C19 C 0.6165(5) 0.3292(4) 0.7300(3) 0.0469(14) Uani 1 1 d . .
H19 H 0.623511 0.257087 0.730964 0.056 Uiso 1 1 calc R U
C20 C 0.6340(4) 0.3947(3) 0.6723(3) 0.0333(11) Uani 1 1 d . .
C21 C 0.6647(4) 0.3555(3) 0.6106(3) 0.0313(10) Uani 1 1 d . .
C22 C 0.6626(4) 0.2478(4) 0.5979(3) 0.0414(12) Uani 1 1 d . .
H22 H 0.640526 0.197408 0.628317 0.050 Uiso 1 1 calc R U
C23 C 0.6966(5) 0.2297(4) 0.5364(3) 0.0442(13) Uani 1 1 d . .
H23 H 0.703397 0.164868 0.515531 0.053 Uiso 1 1 calc R U
C24 C 0.7210(4) 0.3272(3) 0.5074(3) 0.0350(11) Uani 1 1 d . .
C25 C 0.7871(5) 0.2478(4) 0.4039(3) 0.0535(15) Uani 1 1 d . .
C26 C 0.6904(5) 0.7850(4) 0.3516(3) 0.0515(15) Uani 1 1 d . .
C27 C 0.5850(6) 0.9457(4) 0.6110(3) 0.0472(14) Uani 1 1 d . .
C28 C 0.5342(5) 0.5582(5) 0.8691(3) 0.0523(15) Uani 1 1 d . .
C29 C 0.8150(4) 0.5812(3) 0.6495(3) 0.0340(11) Uani 1 1 d . .
C30 C 0.8559(5) 0.6785(4) 0.5385(3) 0.0397(12) Uani 1 1 d . .
C31 C 0.9204(4) 0.4855(4) 0.5634(2) 0.0331(10) Uani 1 1 d . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.02912(13) 0.02694(11) 0.02028(11) -0.00071(7) -0.00094(8) -0.00379(7)
F1 0.103(3) 0.079(3) 0.066(3) -0.011(2) 0.036(2) 0.033(2)
F2 0.073(3) 0.102(3) 0.131(4) -0.085(3) -0.023(3) 0.005(2)
F3 0.091(3) 0.055(2) 0.076(3) -0.0045(18) 0.022(2) 0.0334(19)
F4 0.146(4) 0.084(3) 0.095(3) 0.040(2) 0.082(3) 0.023(3)
F5 0.149(4) 0.064(2) 0.074(3) 0.008(2) 0.037(3) -0.040(3)
F6 0.082(3) 0.115(4) 0.150(5) 0.092(3) -0.033(3) -0.014(3)
F7 0.137(4) 0.0360(17) 0.066(3) 0.0029(16) 0.030(3) -0.008(2)
F8 0.139(4) 0.0428(19) 0.054(2) -0.0081(16) -0.015(2) -0.026(2)
F9 0.075(3) 0.056(2) 0.163(5) 0.020(3) 0.016(3) 0.028(2)
F10 0.115(3) 0.087(3) 0.040(2) -0.0042(18) 0.037(2) 0.004(2)
F11 0.091(3) 0.111(3) 0.037(2) 0.022(2) 0.004(2) 0.016(2)
F12 0.084(3) 0.116(3) 0.057(3) 0.003(2) 0.034(2) -0.029(3)
O1 0.071(3) 0.044(2) 0.026(2) -0.0059(15) -0.0038(18) -0.0098(18)
O2 0.060(3) 0.047(2) 0.078(3) 0.014(2) -0.003(2) -0.023(2)
O3 0.036(2) 0.067(3) 0.053(3) 0.0172(18) 0.007(2) 0.0098(17)
N3 0.046(3) 0.040(2) 0.024(2) 0.0005(16) 0.0068(19) 0.0028(18)
N1 0.041(3) 0.038(2) 0.021(2) -0.0061(16) 0.0068(18) 0.0034(17)
N5 0.027(2) 0.0302(19) 0.030(2) 0.0021(16) -0.0019(17) -0.0028(16)
N4 0.042(2) 0.034(2) 0.028(2) 0.0056(16) 0.0061(18) 0.0002(18)
N2 0.040(2) 0.028(2) 0.033(2) 0.0035(16) 0.0034(19) -0.0016(17)
C1 0.030(3) 0.037(3) 0.042(3) -0.011(2) -0.002(2) 0.001(2)
C2 0.036(3) 0.042(3) 0.026(3) -0.0115(19) 0.000(2) 0.003(2)
C3 0.062(4) 0.066(4) 0.027(3) -0.011(2) 0.006(3) 0.010(3)
C4 0.054(4) 0.066(4) 0.029(3) 0.001(2) 0.009(3) 0.003(3)
C5 0.042(3) 0.052(3) 0.018(2) 0.005(2) -0.005(2) -0.004(2)
C6 0.040(3) 0.040(3) 0.026(3) 0.0070(19) 0.004(2) 0.001(2)
C7 0.034(3) 0.035(2) 0.026(2) 0.0044(18) 0.001(2) 0.0029(19)
C8 0.024(2) 0.027(2) 0.028(2) 0.0018(17) -0.0051(19) 0.0015(17)
C9 0.037(3) 0.033(2) 0.028(3) 0.0037(19) 0.006(2) -0.005(2)
C10 0.032(3) 0.028(2) 0.031(3) 0.0029(18) -0.002(2) 0.0023(18)
C11 0.040(3) 0.030(2) 0.034(3) -0.0034(19) 0.000(2) -0.001(2)
C12 0.041(3) 0.032(2) 0.032(3) -0.0031(19) 0.001(2) 0.0051(19)
C13 0.050(3) 0.046(3) 0.041(3) -0.013(2) 0.002(3) 0.003(2)
C14 0.057(4) 0.060(3) 0.030(3) -0.012(2) 0.009(3) 0.001(3)
C15 0.037(3) 0.052(3) 0.030(3) -0.005(2) 0.004(2) 0.001(2)
C16 0.037(3) 0.055(3) 0.027(3) 0.002(2) 0.005(2) -0.002(2)
C17 0.038(3) 0.045(3) 0.033(3) 0.010(2) 0.003(2) -0.003(2)
C18 0.069(4) 0.053(3) 0.040(3) 0.021(3) 0.015(3) -0.006(3)
C19 0.061(4) 0.032(3) 0.046(3) 0.013(2) 0.006(3) -0.001(2)
C20 0.032(3) 0.030(2) 0.034(3) 0.0080(19) -0.001(2) -0.0044(19)
C21 0.024(2) 0.031(2) 0.037(3) 0.0062(19) -0.001(2) -0.0021(18)
C22 0.038(3) 0.028(2) 0.054(3) 0.004(2) 0.001(3) -0.004(2)
C23 0.047(3) 0.028(2) 0.056(4) -0.005(2) 0.005(3) -0.001(2)
C24 0.031(3) 0.027(2) 0.042(3) -0.0062(19) -0.005(2) 0.0001(19)
C25 0.055(4) 0.051(3) 0.050(4) -0.017(3) -0.002(3) 0.009(3)
C26 0.059(4) 0.055(3) 0.039(3) 0.015(3) 0.006(3) -0.003(3)
C27 0.068(4) 0.032(3) 0.037(3) -0.001(2) 0.001(3) 0.006(2)
C28 0.052(4) 0.074(4) 0.031(3) 0.006(3) 0.008(3) 0.001(3)
C29 0.043(3) 0.027(2) 0.033(3) -0.0025(19) 0.013(2) -0.0025(19)
C30 0.042(3) 0.034(3) 0.036(3) 0.002(2) -0.007(2) -0.005(2)
C31 0.028(3) 0.044(3) 0.027(3) 0.002(2) 0.005(2) -0.005(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C31 Re1 C29 85.7(2)
C31 Re1 C30 88.8(2)
C29 Re1 C30 85.3(2)
C31 Re1 N1 96.01(18)
C29 Re1 N1 178.26(17)
C30 Re1 N1 94.40(19)
C31 Re1 N5 87.60(17)
C29 Re1 N5 98.37(17)
C30 Re1 N5 174.61(19)
N1 Re1 N5 82.05(15)
C31 Re1 C8 164.02(17)
C29 Re1 C8 110.24(18)
C30 Re1 C8 93.38(18)
N1 Re1 C8 68.05(15)
N5 Re1 C8 89.06(14)
C15 N3 C12 109.2(4)
C2 N1 C5 108.0(4)
C2 N1 Re1 124.0(3)
C5 N1 Re1 126.0(3)
C21 N5 C24 107.5(4)
C21 N5 Re1 129.5(3)
C24 N5 Re1 118.2(3)
C17 N4 C20 110.2(4)
C17 N4 H4 124.9
C20 N4 H4 124.9
C7 N2 C10 111.3(4)
C7 N2 H2 117(3)
C10 N2 H2 129(3)
C24 C1 C2 125.5(4)
C24 C1 C25 117.8(5)
C2 C1 C25 116.4(5)
N1 C2 C1 121.8(5)
N1 C2 C3 107.9(4)
C1 C2 C3 129.9(4)
C4 C3 C2 107.7(5)
C4 C3 H3 126.2
C2 C3 H3 126.2
C3 C4 C5 107.0(5)
C3 C4 H4A 126.5
C5 C4 H4A 126.5
N1 C5 C6 119.6(5)
N1 C5 C4 109.3(5)
C6 C5 C4 131.0(5)
C5 C6 C7 117.6(4)
C5 C6 C26 121.9(5)
C7 C6 C26 120.4(5)
N2 C7 C6 128.6(4)
N2 C7 C8 106.4(4)
C6 C7 C8 124.7(4)
C9 C8 C7 107.8(4)
C9 C8 Re1 96.6(3)
C7 C8 Re1 92.9(3)
C9 C8 H8 118.3
C7 C8 H8 118.3
Re1 C8 H8 118.3
C8 C9 C10 108.9(4)
C8 C9 H9 128(4)
C10 C9 H9 123(4)
N2 C10 C11 128.0(4)
N2 C10 C9 105.3(4)
C11 C10 C9 126.7(4)
C12 C11 C10 121.6(4)
C12 C11 C27 117.8(4)
C10 C11 C27 120.4(5)
N3 C12 C11 122.5(4)
N3 C12 C13 107.7(4)
C11 C12 C13 129.8(5)
C14 C13 C12 108.0(5)
C14 C13 H13 126.0
C12 C13 H13 126.0
C13 C14 C15 107.3(5)
C13 C14 H14 126.4
C15 C14 H14 126.4
N3 C15 C16 119.7(4)
N3 C15 C14 107.9(5)
C16 C15 C14 132.4(5)
C15 C16 C17 123.0(5)
C15 C16 C28 121.2(5)
C17 C16 C28 115.8(5)
N4 C17 C16 125.7(5)
N4 C17 C18 107.7(5)
C16 C17 C18 126.7(5)
C19 C18 C17 107.2(5)
C19 C18 H18 126.4
C17 C18 H18 126.4
C18 C19 C20 108.7(5)
C18 C19 H19 125.7
C20 C19 H19 125.7
N4 C20 C21 132.2(4)
N4 C20 C19 106.2(4)
C21 C20 C19 121.6(4)
N5 C21 C20 131.4(4)
N5 C21 C22 108.2(4)
C20 C21 C22 120.4(4)
C23 C22 C21 108.9(4)
C23 C22 H22 125.5
C21 C22 H22 125.5
C22 C23 C24 107.3(4)
C22 C23 H23 126.3
C24 C23 H23 126.3
N5 C24 C1 127.0(4)
N5 C24 C23 108.0(5)
C1 C24 C23 124.8(4)
F3 C25 F2 106.9(5)
F3 C25 F1 104.5(5)
F2 C25 F1 105.8(5)
F3 C25 C1 114.0(5)
F2 C25 C1 112.2(5)
F1 C25 C1 112.7(5)
F6 C26 F4 108.3(6)
F6 C26 F5 102.2(5)
F4 C26 F5 104.2(5)
F6 C26 C6 114.5(5)
F4 C26 C6 114.4(5)
F5 C26 C6 112.0(5)
F8 C27 F9 106.6(5)
F8 C27 F7 104.9(5)
F9 C27 F7 104.2(5)
F8 C27 C11 114.3(5)
F9 C27 C11 112.1(5)
F7 C27 C11 113.9(4)
F11 C28 F12 106.9(5)
F11 C28 F10 106.0(5)
F12 C28 F10 105.5(5)
F11 C28 C16 112.4(5)
F12 C28 C16 111.6(5)
F10 C28 C16 113.8(5)
O1 C29 Re1 172.1(5)
O2 C30 Re1 178.0(5)
O3 C31 Re1 178.4(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C31 1.883(5)
Re1 C29 1.915(5)
Re1 C30 1.921(5)
Re1 N1 2.174(4)
Re1 N5 2.195(4)
Re1 C8 2.544(4)
F1 C25 1.342(7)
F2 C25 1.328(7)
F3 C25 1.325(7)
F4 C26 1.297(7)
F5 C26 1.338(7)
F6 C26 1.293(7)
F7 C27 1.333(7)
F8 C27 1.309(6)
F9 C27 1.326(7)
F10 C28 1.335(7)
F11 C28 1.326(7)
F12 C28 1.333(7)
O1 C29 1.149(6)
O2 C30 1.140(6)
O3 C31 1.149(6)
N3 C15 1.357(6)
N3 C12 1.366(6)
N1 C2 1.355(6)
N1 C5 1.373(6)
N5 C21 1.375(6)
N5 C24 1.390(6)
N4 C17 1.367(6)
N4 C20 1.370(6)
N4 H4 0.8800
N2 C7 1.361(6)
N2 C10 1.381(6)
N2 H2 0.89(5)
C1 C24 1.399(7)
C1 C2 1.407(7)
C1 C25 1.513(7)
C2 C3 1.457(8)
C3 C4 1.347(7)
C3 H3 0.9500
C4 C5 1.424(8)
C4 H4A 0.9500
C5 C6 1.406(7)
C6 C7 1.408(7)
C6 C26 1.496(7)
C7 C8 1.432(6)
C8 C9 1.361(7)
C8 H8 1.0000
C9 C10 1.430(6)
C9 H9 0.96(7)
C10 C11 1.402(7)
C11 C12 1.401(7)
C11 C27 1.494(6)
C12 C13 1.432(7)
C13 C14 1.350(8)
C13 H13 0.9500
C14 C15 1.442(7)
C14 H14 0.9500
C15 C16 1.403(7)
C16 C17 1.412(7)
C16 C28 1.498(8)
C17 C18 1.433(7)
C18 C19 1.357(8)
C18 H18 0.9500
C19 C20 1.442(7)
C19 H19 0.9500
C20 C21 1.398(7)
C21 C22 1.433(6)
C22 C23 1.335(8)
C22 H22 0.9500
C23 C24 1.446(7)
C23 H23 0.9500