# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_ks2
_database_code_depnum_ccdc_archive 'CCDC 2056997'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2019-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C20 H24 Br2 N2 O2 Re), C H2 Cl2'
_chemical_formula_sum            'C41 H50 Br4 Cl2 N4 O4 Re2'
_chemical_formula_weight         1425.79
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9090(4)
_cell_length_b                   31.7496(12)
_cell_length_c                   12.5191(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.998(2)
_cell_angle_gamma                90
_cell_volume                     4978.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20885
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.28
_shelx_estimated_absorpt_T_max   0.791
_shelx_estimated_absorpt_T_min   0.084
_exptl_absorpt_coefficient_mu    8.216
_exptl_absorpt_correction_T_max  0.3713
_exptl_absorpt_correction_T_min  0.2232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2720
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of DCM and pentane  by diffusion'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52668
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         1.283
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5459
_reflns_number_total             10032
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10032
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.007
_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)+(0.0521P)²+6.2207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1214
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C38) = Uanis(C38A) = Uanis(C35) = Uanis(C36) = Uanis(C36A) = Uanis(C37) =
Uanis(C37A)
Uanis(C34) = Uanis(C34A) = Uanis(C33) = Uanis(C33A) = Uanis(C32) = Uanis(C32A)
3. Rigid body (RIGU) restrains
 C41, Cl1, Cl2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(C36A)=Sof(HX)=Sof(HY)=Sof(HZ)=Sof(C37A)=Sof(H0AA)=Sof(H1AA)=Sof(H2AA)=
 Sof(C38A)=Sof(H3AA)=Sof(H4AA)=Sof(H5AA)=1-FVAR(1)
 Sof(C36)=Sof(HO)=Sof(HP)=Sof(HQ)=Sof(C37)=Sof(HR)=Sof(HS)=Sof(HT)=Sof(C38)=
 Sof(HU)=Sof(HV)=Sof(HW)=FVAR(1)
 Sof(C32A)=Sof(H8AA)=Sof(H9AA)=Sof(H0BA)=Sof(C33A)=Sof(H1BA)=Sof(H2BA)=
 Sof(H3BA)=Sof(C34A)=Sof(H4BA)=Sof(H5BA)=Sof(H6BA)=1-FVAR(2)
 Sof(C32)=Sof(HF)=Sof(HG)=Sof(HH)=Sof(C33)=Sof(HI)=Sof(HJ)=Sof(HK)=Sof(C34)=
 Sof(HL)=Sof(HM)=Sof(HN)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C41(H6AA,H7AA)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H), C22(HA), C24(HB), C27(HC), C29(HD), C30(HE), C1(H1), C2(H2), C4(H4),
 C7(H7), C9(H9), C10(H10)
5.c Idealised Me refined as rotating group:
 C32(HF,HG,HH), C33(HI,HJ,HK), C34(HL,HM,HN), C36(HO,HP,HQ), C37(HR,HS,HT),
 C38(HU,HV,HW), C36A(HX,HY,HZ), C37A(H0AA,H1AA,H2AA), C38A(H3AA,H4AA,H5AA),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C32A(H8AA,H9AA,H0BA),
 C33A(H1BA,H2BA,H3BA), C34A(H4BA,H5BA,H6BA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br3 Br 0.62101(8) 0.36373(3) 0.81141(10) 0.0587(3) Uani 1 1 d . . . . .
Br4 Br 0.45853(13) 0.43516(5) 0.45396(14) 0.1024(5) Uani 1 1 d . . . . .
C21 C 0.7571(8) 0.4355(3) 0.6203(10) 0.057(3) Uani 1 1 d . . . . .
H H 0.766813 0.411120 0.581090 0.069 Uiso 1 1 calc R . . . .
C22 C 0.8336(8) 0.4659(3) 0.6399(10) 0.058(3) Uani 1 1 d . . . . .
HA H 0.895878 0.461624 0.615009 0.070 Uiso 1 1 calc R . . . .
C23 C 0.8234(7) 0.5026(3) 0.6949(9) 0.047(3) Uani 1 1 d . . . . .
C24 C 0.7315(7) 0.5070(3) 0.7327(9) 0.048(3) Uani 1 1 d . . . . .
HB H 0.721781 0.530991 0.773113 0.058 Uiso 1 1 calc R . . . .
C25 C 0.6536(7) 0.4757(3) 0.7107(8) 0.044(2) Uani 1 1 d . . . . .
C26 C 0.5513(7) 0.4802(3) 0.7418(8) 0.042(2) Uani 1 1 d . . . . .
C27 C 0.5213(8) 0.5154(3) 0.7913(9) 0.051(3) Uani 1 1 d . . . . .
HC H 0.570241 0.537581 0.812420 0.061 Uiso 1 1 calc R . . . .
C28 C 0.4211(8) 0.5188(3) 0.8101(9) 0.052(3) Uani 1 1 d . . . . .
C29 C 0.3536(9) 0.4845(3) 0.7810(10) 0.065(3) Uani 1 1 d . . . . .
HD H 0.285325 0.484810 0.795262 0.078 Uiso 1 1 calc R . . . .
C30 C 0.3859(8) 0.4504(3) 0.7320(11) 0.065(3) Uani 1 1 d . . . . .
HE H 0.338050 0.427866 0.711054 0.077 Uiso 1 1 calc R . . . .
C31 C 0.9092(8) 0.5371(3) 0.7138(10) 0.060(3) Uani 1 1 d . . . . .
C32 C 0.981(2) 0.5376(8) 0.637(3) 0.077(4) Uani 0.56(3) 1 d . . P A 3
HF H 1.011875 0.509771 0.634974 0.116 Uiso 0.56(3) 1 calc GR . P A 3
HG H 1.038262 0.557806 0.663268 0.116 Uiso 0.56(3) 1 calc GR . P A 3
HH H 0.941175 0.545453 0.564273 0.116 Uiso 0.56(3) 1 calc GR . P A 3
C33 C 0.986(2) 0.5272(8) 0.834(3) 0.077(4) Uani 0.56(3) 1 d . . P A 3
HI H 0.945160 0.530639 0.889758 0.116 Uiso 0.56(3) 1 calc GR . P A 3
HJ H 1.045547 0.546498 0.849197 0.116 Uiso 0.56(3) 1 calc GR . P A 3
HK H 1.011590 0.498475 0.836058 0.116 Uiso 0.56(3) 1 calc GR . P A 3
C34 C 0.856(2) 0.5799(9) 0.714(3) 0.077(4) Uani 0.56(3) 1 d . . P A 3
HL H 0.818355 0.587281 0.639423 0.116 Uiso 0.56(3) 1 calc GR . P A 3
HM H 0.909605 0.601057 0.742515 0.116 Uiso 0.56(3) 1 calc GR . P A 3
HN H 0.805353 0.578656 0.760121 0.116 Uiso 0.56(3) 1 calc GR . P A 3
C35 C 0.3831(10) 0.5591(4) 0.8587(13) 0.083(3) Uani 1 1 d . . . . .
C39 C 0.5996(10) 0.3551(4) 0.5415(12) 0.073(4) Uani 1 1 d . . . . .
C40 C 0.4085(10) 0.3604(3) 0.5991(9) 0.056(3) Uani 1 1 d . . . . .
N3 N 0.6663(6) 0.4400(2) 0.6571(7) 0.050(2) Uani 1 1 d . . . . .
N4 N 0.4838(6) 0.4475(2) 0.7120(7) 0.050(2) Uani 1 1 d . . . . .
O3 O 0.6313(8) 0.3336(3) 0.4967(9) 0.099(3) Uani 1 1 d . . . . .
O4 O 0.3367(7) 0.3412(3) 0.5800(8) 0.090(3) Uani 1 1 d . . . . .
Re2 Re 0.53624(3) 0.39580(2) 0.62542(4) 0.05073(14) Uani 1 1 d . . . . .
C36 C 0.4644(16) 0.5915(7) 0.889(2) 0.083(3) Uani 0.63(2) 1 d . . P B 1
HO H 0.486674 0.600706 0.824615 0.125 Uiso 0.63(2) 1 calc GR . P B 1
HP H 0.525330 0.580130 0.942838 0.125 Uiso 0.63(2) 1 calc GR . P B 1
HQ H 0.435393 0.615200 0.921484 0.125 Uiso 0.63(2) 1 calc GR . P B 1
C37 C 0.3315(18) 0.5463(7) 0.950(2) 0.083(3) Uani 0.63(2) 1 d . . P B 1
HR H 0.385511 0.535470 1.011506 0.125 Uiso 0.63(2) 1 calc GR . P B 1
HS H 0.278506 0.524697 0.923167 0.125 Uiso 0.63(2) 1 calc GR . P B 1
HT H 0.297291 0.570647 0.973409 0.125 Uiso 0.63(2) 1 calc GR . P B 1
C38 C 0.2984(19) 0.5788(7) 0.760(2) 0.083(3) Uani 0.63(2) 1 d . . P B 1
HU H 0.243563 0.558082 0.730609 0.125 Uiso 0.63(2) 1 calc GR . P B 1
HV H 0.333213 0.587101 0.702499 0.125 Uiso 0.63(2) 1 calc GR . P B 1
HW H 0.266235 0.603246 0.785000 0.125 Uiso 0.63(2) 1 calc GR . P B 1
C36A C 0.485(3) 0.5769(12) 0.960(4) 0.083(3) Uani 0.37(2) 1 d . . P B 2
HX H 0.509511 0.554402 1.012762 0.125 Uiso 0.37(2) 1 calc GR . P B 2
HY H 0.460043 0.600303 0.997464 0.125 Uiso 0.37(2) 1 calc GR . P B 2
HZ H 0.542688 0.586162 0.929278 0.125 Uiso 0.37(2) 1 calc GR . P B 2
C37A C 0.292(3) 0.5544(13) 0.913(4) 0.083(3) Uani 0.37(2) 1 d . . P B 2
H0AA H 0.298749 0.527760 0.951541 0.125 Uiso 0.37(2) 1 calc GR . P B 2
H1AA H 0.225456 0.555205 0.857188 0.125 Uiso 0.37(2) 1 calc GR . P B 2
H2AA H 0.294281 0.577310 0.964490 0.125 Uiso 0.37(2) 1 calc GR . P B 2
C38A C 0.358(3) 0.5915(11) 0.773(4) 0.083(3) Uani 0.37(2) 1 d . . P B 2
H3AA H 0.309447 0.579905 0.708039 0.125 Uiso 0.37(2) 1 calc GR . P B 2
H4AA H 0.422928 0.600706 0.754646 0.125 Uiso 0.37(2) 1 calc GR . P B 2
H5AA H 0.324102 0.615238 0.799810 0.125 Uiso 0.37(2) 1 calc GR . P B 2
Br1 Br 0.89357(11) 0.66892(4) -0.04067(12) 0.0771(4) Uani 1 1 d . . . . .
Br2 Br 0.90055(9) 0.58880(4) 0.30529(10) 0.0639(3) Uani 1 1 d . . . . .
C1 C 0.6907(7) 0.6679(3) 0.1409(9) 0.050(3) Uani 1 1 d . . . . .
H1 H 0.659172 0.644271 0.100676 0.060 Uiso 1 1 calc R . . . .
C2 C 0.6262(7) 0.6984(3) 0.1653(9) 0.052(3) Uani 1 1 d . . . . .
H2 H 0.551734 0.694861 0.143824 0.062 Uiso 1 1 calc R . . . .
C3 C 0.6676(7) 0.7343(3) 0.2207(8) 0.045(2) Uani 1 1 d . . . . .
C4 C 0.7782(7) 0.7366(3) 0.2538(8) 0.046(3) Uani 1 1 d . . . . .
H4 H 0.810294 0.760137 0.294114 0.055 Uiso 1 1 calc R . . . .
C5 C 0.8411(7) 0.7054(3) 0.2290(8) 0.045(2) Uani 1 1 d . . . . .
C6 C 0.9588(7) 0.7061(3) 0.2549(9) 0.045(2) Uani 1 1 d . . . . .
C7 C 1.0186(7) 0.7386(3) 0.3133(8) 0.047(3) Uani 1 1 d . . . . .
H7 H 0.983302 0.760774 0.339393 0.056 Uiso 1 1 calc R . . . .
C8 C 1.1292(7) 0.7393(3) 0.3342(8) 0.042(2) Uani 1 1 d . . . . .
C9 C 1.1746(8) 0.7047(3) 0.2921(9) 0.055(3) Uani 1 1 d . . . . .
H9 H 1.249040 0.703527 0.301965 0.066 Uiso 1 1 calc R . . . .
C10 C 1.1148(7) 0.6738(3) 0.2390(8) 0.046(3) Uani 1 1 d . . . . .
H10 H 1.148891 0.651053 0.213439 0.056 Uiso 1 1 calc R . . . .
C11 C 0.5994(7) 0.7701(3) 0.2467(9) 0.051(3) Uani 1 1 d . . . . .
C12 C 0.4808(8) 0.7628(4) 0.1919(11) 0.076(4) Uani 1 1 d . . . . .
H12A H 0.469854 0.764137 0.112534 0.114 Uiso 1 1 calc GR . . . .
H12B H 0.438208 0.784340 0.215912 0.114 Uiso 1 1 calc GR . . . .
H12C H 0.459525 0.735280 0.212652 0.114 Uiso 1 1 calc GR . . . .
C13 C 0.6360(9) 0.8122(3) 0.2062(12) 0.083(4) Uani 1 1 d . . . . .
H13A H 0.707638 0.818742 0.248394 0.125 Uiso 1 1 calc GR . . . .
H13B H 0.587688 0.834512 0.215915 0.125 Uiso 1 1 calc GR . . . .
H13C H 0.635659 0.809884 0.128864 0.125 Uiso 1 1 calc GR . . . .
C14 C 0.6100(9) 0.7712(4) 0.3722(10) 0.076(4) Uani 1 1 d . . . . .
H14A H 0.578605 0.745901 0.394468 0.113 Uiso 1 1 calc GR . . . .
H14B H 0.573102 0.795736 0.390787 0.113 Uiso 1 1 calc GR . . . .
H14C H 0.684863 0.772623 0.410308 0.113 Uiso 1 1 calc GR . . . .
C15 C 1.1923(8) 0.7751(3) 0.4010(10) 0.057(3) Uani 1 1 d . . . . .
C16 C 1.1470(10) 0.8187(4) 0.3575(12) 0.093(4) Uani 1 1 d . . . . .
H16A H 1.153876 0.822427 0.282636 0.139 Uiso 1 1 calc GR . . . .
H16B H 1.186610 0.840696 0.403893 0.139 Uiso 1 1 calc GR . . . .
H16C H 1.072334 0.820347 0.358865 0.139 Uiso 1 1 calc GR . . . .
C17 C 1.3089(8) 0.7745(4) 0.3892(12) 0.089(5) Uani 1 1 d . . . . .
H17A H 1.343030 0.748493 0.419702 0.134 Uiso 1 1 calc GR . . . .
H17B H 1.347466 0.798261 0.428472 0.134 Uiso 1 1 calc GR . . . .
H17C H 1.309178 0.776348 0.311903 0.134 Uiso 1 1 calc GR . . . .
C18 C 1.1905(9) 0.7688(4) 0.5195(10) 0.083(4) Uani 1 1 d . . . . .
H18A H 1.117931 0.771748 0.527430 0.124 Uiso 1 1 calc GR . . . .
H18B H 1.235629 0.789728 0.564689 0.124 Uiso 1 1 calc GR . . . .
H18C H 1.216804 0.740851 0.542980 0.124 Uiso 1 1 calc GR . . . .
C19 C 0.8042(11) 0.5836(4) 0.0425(12) 0.068(4) Uani 1 1 d . . . . .
C20 C 1.0161(9) 0.5886(4) 0.0957(10) 0.062(3) Uani 1 1 d . . . . .
N1 N 0.7965(6) 0.6701(2) 0.1717(7) 0.045(2) Uani 1 1 d . . . . .
N2 N 1.0066(6) 0.6733(2) 0.2196(6) 0.0432(19) Uani 1 1 d . . . . .
O1 O 0.7537(7) 0.5611(3) -0.0043(8) 0.087(3) Uani 1 1 d . . . . .
O2 O 1.0802(7) 0.5686(3) 0.0766(8) 0.088(3) Uani 1 1 d . . . . .
Re1 Re 0.90494(3) 0.62511(2) 0.12715(4) 0.04715(14) Uani 1 1 d . . . . .
C41 C 0.9447(14) 0.6642(5) 0.5364(17) 0.144(6) Uani 1 1 d . U . . .
H6AA H 0.902471 0.654018 0.465250 0.172 Uiso 1 1 calc R . . . .
H7AA H 0.924608 0.647391 0.593827 0.172 Uiso 1 1 calc R . . . .
Cl1 Cl 0.9111(4) 0.71365(14) 0.5512(4) 0.1323(15) Uani 1 1 d . U . . .
Cl2 Cl 1.0799(4) 0.65493(15) 0.5425(4) 0.1338(15) Uani 1 1 d . U . . .
C32A C 0.931(3) 0.5426(11) 0.596(3) 0.077(4) Uani 0.44(3) 1 d . . P A 4
H8AA H 0.953740 0.516006 0.571250 0.116 Uiso 0.44(3) 1 calc GR . P A 4
H9AA H 0.985733 0.563673 0.598483 0.116 Uiso 0.44(3) 1 calc GR . P A 4
H0BA H 0.865421 0.551658 0.544173 0.116 Uiso 0.44(3) 1 calc GR . P A 4
C33A C 1.013(3) 0.5218(10) 0.791(3) 0.077(4) Uani 0.44(3) 1 d . . P A 4
H1BA H 0.999093 0.496452 0.828778 0.116 Uiso 0.44(3) 1 calc GR . P A 4
H2BA H 1.040677 0.543507 0.845219 0.116 Uiso 0.44(3) 1 calc GR . P A 4
H3BA H 1.065161 0.515741 0.749099 0.116 Uiso 0.44(3) 1 calc GR . P A 4
C34A C 0.879(3) 0.5769(12) 0.765(3) 0.077(4) Uani 0.44(3) 1 d . . P A 4
H4BA H 0.808406 0.585946 0.724393 0.116 Uiso 0.44(3) 1 calc GR . P A 4
H5BA H 0.930369 0.598833 0.761920 0.116 Uiso 0.44(3) 1 calc GR . P A 4
H6BA H 0.877992 0.571521 0.840863 0.116 Uiso 0.44(3) 1 calc GR . P A 4


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Br3 Re2 2.5345(12) . ?
Br4 Re2 2.4766(16) . ?
C21 H 0.9400 . ?
C21 C22 1.360(13) . ?
C21 N3 1.366(11) . ?
C22 HA 0.9400 . ?
C22 C23 1.376(13) . ?
C23 C24 1.387(12) . ?
C23 C31 1.535(13) . ?
C24 HB 0.9400 . ?
C24 C25 1.391(12) . ?
C25 C26 1.472(12) . ?
C25 N3 1.350(12) . ?
C26 C27 1.380(13) . ?
C26 N4 1.348(11) . ?
C27 HC 0.9400 . ?
C27 C28 1.374(12) . ?
C28 C29 1.387(14) . ?
C28 C35 1.547(15) . ?
C29 HD 0.9400 . ?
C29 C30 1.359(14) . ?
C30 HE 0.9400 . ?
C30 N4 1.350(11) . ?
C31 C32 1.49(3) . ?
C31 C33 1.62(3) . ?
C31 C34 1.52(3) . ?
C31 C32A 1.58(4) . ?
C31 C33A 1.53(4) . ?
C31 C34A 1.51(4) . ?
C32 HF 0.9700 . ?
C32 HG 0.9700 . ?
C32 HH 0.9700 . ?
C33 HI 0.9700 . ?
C33 HJ 0.9700 . ?
C33 HK 0.9700 . ?
C34 HL 0.9700 . ?
C34 HM 0.9700 . ?
C34 HN 0.9700 . ?
C35 C36 1.45(2) . ?
C35 C37 1.51(3) . ?
C35 C38 1.57(3) . ?
C35 C36A 1.69(4) . ?
C35 C37A 1.49(4) . ?
C35 C38A 1.46(4) . ?
C39 O3 1.030(14) . ?
C39 Re2 1.964(14) . ?
C40 O4 1.087(12) . ?
C40 Re2 1.957(12) . ?
N3 Re2 2.150(7) . ?
N4 Re2 2.163(8) . ?
C36 HO 0.9700 . ?
C36 HP 0.9700 . ?
C36 HQ 0.9700 . ?
C37 HR 0.9700 . ?
C37 HS 0.9700 . ?
C37 HT 0.9700 . ?
C38 HU 0.9700 . ?
C38 HV 0.9700 . ?
C38 HW 0.9700 . ?
C36A HX 0.9700 . ?
C36A HY 0.9700 . ?
C36A HZ 0.9700 . ?
C37A H0AA 0.9700 . ?
C37A H1AA 0.9700 . ?
C37A H2AA 0.9700 . ?
C38A H3AA 0.9700 . ?
C38A H4AA 0.9700 . ?
C38A H5AA 0.9700 . ?
Br1 Re1 2.4940(14) . ?
Br2 Re1 2.5234(12) . ?
C1 H1 0.9400 . ?
C1 C2 1.359(13) . ?
C1 N1 1.328(11) . ?
C2 H2 0.9400 . ?
C2 C3 1.374(13) . ?
C3 C4 1.388(12) . ?
C3 C11 1.521(13) . ?
C4 H4 0.9400 . ?
C4 C5 1.364(12) . ?
C5 C6 1.475(12) . ?
C5 N1 1.378(12) . ?
C6 C7 1.386(13) . ?
C6 N2 1.339(11) . ?
C7 H7 0.9400 . ?
C7 C8 1.387(12) . ?
C8 C9 1.406(13) . ?
C8 C15 1.525(13) . ?
C9 H9 0.9400 . ?
C9 C10 1.325(13) . ?
C10 H10 0.9400 . ?
C10 N2 1.359(10) . ?
C11 C12 1.536(14) . ?
C11 C13 1.543(14) . ?
C11 C14 1.545(15) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 C16 1.549(16) . ?
C15 C17 1.548(13) . ?
C15 C18 1.503(15) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 O1 1.047(13) . ?
C19 Re1 1.971(14) . ?
C20 O2 1.114(12) . ?
C20 Re1 1.958(12) . ?
N1 Re1 2.166(7) . ?
N2 Re1 2.161(7) . ?
C41 H6AA 0.9800 . ?
C41 H7AA 0.9800 . ?
C41 Cl1 1.650(16) . ?
C41 Cl2 1.753(17) . ?
C32A H8AA 0.9700 . ?
C32A H9AA 0.9700 . ?
C32A H0BA 0.9700 . ?
C33A H1BA 0.9700 . ?
C33A H2BA 0.9700 . ?
C33A H3BA 0.9700 . ?
C34A H4BA 0.9700 . ?
C34A H5BA 0.9700 . ?
C34A H6BA 0.9700 . ?

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
C22 C21 H 119.7 . . ?
C22 C21 N3 120.6(9) . . ?
N3 C21 H 119.7 . . ?
C21 C22 HA 118.7 . . ?
C21 C22 C23 122.6(9) . . ?
C23 C22 HA 118.7 . . ?
C22 C23 C24 116.6(9) . . ?
C22 C23 C31 122.0(9) . . ?
C24 C23 C31 121.4(9) . . ?
C23 C24 HB 120.1 . . ?
C23 C24 C25 119.8(9) . . ?
C25 C24 HB 120.1 . . ?
C24 C25 C26 122.1(9) . . ?
N3 C25 C24 122.0(8) . . ?
N3 C25 C26 115.9(8) . . ?
C27 C26 C25 124.3(9) . . ?
N4 C26 C25 114.5(9) . . ?
N4 C26 C27 121.1(8) . . ?
C26 C27 HC 119.4 . . ?
C28 C27 C26 121.2(9) . . ?
C28 C27 HC 119.4 . . ?
C27 C28 C29 116.9(9) . . ?
C27 C28 C35 122.2(10) . . ?
C29 C28 C35 120.9(9) . . ?
C28 C29 HD 120.0 . . ?
C30 C29 C28 120.1(10) . . ?
C30 C29 HD 120.0 . . ?
C29 C30 HE 118.6 . . ?
N4 C30 C29 122.8(10) . . ?
N4 C30 HE 118.6 . . ?
C23 C31 C33 104.9(11) . . ?
C23 C31 C32A 102.6(15) . . ?
C32 C31 C23 116.7(14) . . ?
C32 C31 C33 105.4(14) . . ?
C32 C31 C34 110.3(16) . . ?
C34 C31 C23 109.1(12) . . ?
C34 C31 C33 110.2(15) . . ?
C33A C31 C23 111.0(14) . . ?
C33A C31 C32A 107.7(17) . . ?
C34A C31 C23 114.3(15) . . ?
C34A C31 C32A 115(2) . . ?
C34A C31 C33A 105.9(19) . . ?
C31 C32 HF 109.5 . . ?
C31 C32 HG 109.5 . . ?
C31 C32 HH 109.5 . . ?
HF C32 HG 109.5 . . ?
HF C32 HH 109.5 . . ?
HG C32 HH 109.5 . . ?
C31 C33 HI 109.5 . . ?
C31 C33 HJ 109.5 . . ?
C31 C33 HK 109.5 . . ?
HI C33 HJ 109.5 . . ?
HI C33 HK 109.5 . . ?
HJ C33 HK 109.5 . . ?
C31 C34 HL 109.5 . . ?
C31 C34 HM 109.5 . . ?
C31 C34 HN 109.5 . . ?
HL C34 HM 109.5 . . ?
HL C34 HN 109.5 . . ?
HM C34 HN 109.5 . . ?
C28 C35 C38 104.2(12) . . ?
C28 C35 C36A 108.1(14) . . ?
C36 C35 C28 114.4(11) . . ?
C36 C35 C37 114.3(17) . . ?
C36 C35 C38 104.4(15) . . ?
C37 C35 C28 108.4(12) . . ?
C37 C35 C38 110.7(13) . . ?
C37A C35 C28 117.0(18) . . ?
C37A C35 C36A 104(2) . . ?
C38A C35 C28 109.2(17) . . ?
C38A C35 C36A 108(2) . . ?
C38A C35 C37A 110(2) . . ?
O3 C39 Re2 178.9(13) . . ?
O4 C40 Re2 177.1(11) . . ?
C21 N3 Re2 124.4(7) . . ?
C25 N3 C21 118.2(8) . . ?
C25 N3 Re2 117.2(6) . . ?
C26 N4 C30 117.9(9) . . ?
C26 N4 Re2 117.6(6) . . ?
C30 N4 Re2 124.4(7) . . ?
Br4 Re2 Br3 173.39(5) . . ?
C39 Re2 Br3 94.8(4) . . ?
C39 Re2 Br4 90.1(4) . . ?
C39 Re2 N3 96.9(4) . . ?
C39 Re2 N4 171.2(4) . . ?
C40 Re2 Br3 94.8(3) . . ?
C40 Re2 Br4 89.7(3) . . ?
C40 Re2 C39 88.6(5) . . ?
C40 Re2 N3 174.1(4) . . ?
C40 Re2 N4 99.6(4) . . ?
N3 Re2 Br3 87.0(2) . . ?
N3 Re2 Br4 88.0(2) . . ?
N3 Re2 N4 74.8(3) . . ?
N4 Re2 Br3 87.8(2) . . ?
N4 Re2 Br4 86.7(2) . . ?
C35 C36 HO 109.5 . . ?
C35 C36 HP 109.5 . . ?
C35 C36 HQ 109.5 . . ?
HO C36 HP 109.5 . . ?
HO C36 HQ 109.5 . . ?
HP C36 HQ 109.5 . . ?
C35 C37 HR 109.5 . . ?
C35 C37 HS 109.5 . . ?
C35 C37 HT 109.5 . . ?
HR C37 HS 109.5 . . ?
HR C37 HT 109.5 . . ?
HS C37 HT 109.5 . . ?
C35 C38 HU 109.5 . . ?
C35 C38 HV 109.5 . . ?
C35 C38 HW 109.5 . . ?
HU C38 HV 109.5 . . ?
HU C38 HW 109.5 . . ?
HV C38 HW 109.5 . . ?
C35 C36A HX 109.5 . . ?
C35 C36A HY 109.5 . . ?
C35 C36A HZ 109.5 . . ?
HX C36A HY 109.5 . . ?
HX C36A HZ 109.5 . . ?
HY C36A HZ 109.5 . . ?
C35 C37A H0AA 109.5 . . ?
C35 C37A H1AA 109.5 . . ?
C35 C37A H2AA 109.5 . . ?
H0AA C37A H1AA 109.5 . . ?
H0AA C37A H2AA 109.5 . . ?
H1AA C37A H2AA 109.5 . . ?
C35 C38A H3AA 109.5 . . ?
C35 C38A H4AA 109.5 . . ?
C35 C38A H5AA 109.5 . . ?
H3AA C38A H4AA 109.5 . . ?
H3AA C38A H5AA 109.5 . . ?
H4AA C38A H5AA 109.5 . . ?
C2 C1 H1 118.7 . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.7(9) . . ?
C1 C2 H2 119.3 . . ?
C1 C2 C3 121.3(9) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C4 116.1(8) . . ?
C2 C3 C11 123.6(9) . . ?
C4 C3 C11 120.3(9) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.3(9) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 125.2(9) . . ?
C4 C5 N1 120.8(9) . . ?
N1 C5 C6 113.9(8) . . ?
C7 C6 C5 122.8(8) . . ?
N2 C6 C5 116.6(9) . . ?
N2 C6 C7 120.6(8) . . ?
C6 C7 H7 119.0 . . ?
C6 C7 C8 121.9(9) . . ?
C8 C7 H7 119.0 . . ?
C7 C8 C9 114.8(9) . . ?
C7 C8 C15 120.3(8) . . ?
C9 C8 C15 124.9(8) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 C8 121.5(9) . . ?
C10 C9 H9 119.2 . . ?
C9 C10 H10 118.5 . . ?
C9 C10 N2 123.1(9) . . ?
N2 C10 H10 118.5 . . ?
C3 C11 C12 111.0(9) . . ?
C3 C11 C13 109.7(8) . . ?
C3 C11 C14 108.7(8) . . ?
C12 C11 C13 109.6(9) . . ?
C12 C11 C14 106.9(8) . . ?
C13 C11 C14 110.9(10) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 C16 111.6(10) . . ?
C8 C15 C17 109.9(9) . . ?
C17 C15 C16 105.7(10) . . ?
C18 C15 C8 107.9(9) . . ?
C18 C15 C16 111.8(10) . . ?
C18 C15 C17 109.9(10) . . ?
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 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 C19 Re1 177.2(12) . . ?
O2 C20 Re1 178.4(10) . . ?
C1 N1 C5 117.7(8) . . ?
C1 N1 Re1 125.0(7) . . ?
C5 N1 Re1 117.1(6) . . ?
C6 N2 C10 118.0(8) . . ?
C6 N2 Re1 117.3(6) . . ?
C10 N2 Re1 124.6(6) . . ?
Br1 Re1 Br2 171.87(4) . . ?
C19 Re1 Br1 91.3(4) . . ?
C19 Re1 Br2 91.0(4) . . ?
C19 Re1 N1 101.3(4) . . ?
C19 Re1 N2 176.2(4) . . ?
C20 Re1 Br1 93.3(3) . . ?
C20 Re1 Br2 94.7(3) . . ?
C20 Re1 C19 85.2(5) . . ?
C20 Re1 N1 173.5(4) . . ?
C20 Re1 N2 98.5(4) . . ?
N1 Re1 Br1 86.5(2) . . ?
N1 Re1 Br2 85.4(2) . . ?
N2 Re1 Br1 87.7(2) . . ?
N2 Re1 Br2 89.5(2) . . ?
N2 Re1 N1 75.0(3) . . ?
H6AA C41 H7AA 107.4 . . ?
Cl1 C41 H6AA 108.2 . . ?
Cl1 C41 H7AA 108.2 . . ?
Cl1 C41 Cl2 116.2(10) . . ?
Cl2 C41 H6AA 108.2 . . ?
Cl2 C41 H7AA 108.2 . . ?
C31 C32A H8AA 109.5 . . ?
C31 C32A H9AA 109.5 . . ?
C31 C32A H0BA 109.5 . . ?
H8AA C32A H9AA 109.5 . . ?
H8AA C32A H0BA 109.5 . . ?
H9AA C32A H0BA 109.5 . . ?
C31 C33A H1BA 109.5 . . ?
C31 C33A H2BA 109.5 . . ?
C31 C33A H3BA 109.5 . . ?
H1BA C33A H2BA 109.5 . . ?
H1BA C33A H3BA 109.5 . . ?
H2BA C33A H3BA 109.5 . . ?
C31 C34A H4BA 109.5 . . ?
C31 C34A H5BA 109.5 . . ?
C31 C34A H6BA 109.5 . . ?
H4BA C34A H5BA 109.5 . . ?
H4BA C34A H6BA 109.5 . . ?
H5BA C34A H6BA 109.5 . . ?

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
C21 C22 C23 C24 1.7(17) . . . . ?
C21 C22 C23 C31 -178.4(11) . . . . ?
C22 C21 N3 C25 1.7(16) . . . . ?
C22 C21 N3 Re2 177.0(8) . . . . ?
C22 C23 C24 C25 -2.4(15) . . . . ?
C22 C23 C31 C32 22(2) . . . . ?
C22 C23 C31 C33 -93.7(16) . . . . ?
C22 C23 C31 C34 148.2(16) . . . . ?
C22 C23 C31 C32A 48(2) . . . . ?
C22 C23 C31 C33A -66(2) . . . . ?
C22 C23 C31 C34A 174(2) . . . . ?
C23 C24 C25 C26 -175.5(9) . . . . ?
C23 C24 C25 N3 2.9(16) . . . . ?
C24 C23 C31 C32 -157.6(18) . . . . ?
C24 C23 C31 C33 86.2(16) . . . . ?
C24 C23 C31 C34 -31.9(19) . . . . ?
C24 C23 C31 C32A -131.6(18) . . . . ?
C24 C23 C31 C33A 113.5(19) . . . . ?
C24 C23 C31 C34A -6(2) . . . . ?
C24 C25 C26 C27 2.3(16) . . . . ?
C24 C25 C26 N4 178.5(9) . . . . ?
C24 C25 N3 C21 -2.5(15) . . . . ?
C24 C25 N3 Re2 -178.2(8) . . . . ?
C25 C26 C27 C28 174.7(10) . . . . ?
C25 C26 N4 C30 -176.2(9) . . . . ?
C25 C26 N4 Re2 -0.3(11) . . . . ?
C26 C25 N3 C21 176.0(9) . . . . ?
C26 C25 N3 Re2 0.3(11) . . . . ?
C26 C27 C28 C29 2.4(17) . . . . ?
C26 C27 C28 C35 -176.1(11) . . . . ?
C27 C26 N4 C30 0.1(15) . . . . ?
C27 C26 N4 Re2 176.0(7) . . . . ?
C27 C28 C29 C30 -2.7(18) . . . . ?
C27 C28 C35 C36 -4(2) . . . . ?
C27 C28 C35 C37 -133.0(15) . . . . ?
C27 C28 C35 C38 109.1(15) . . . . ?
C27 C28 C35 C36A -42(2) . . . . ?
C27 C28 C35 C37A -158(2) . . . . ?
C27 C28 C35 C38A 76(2) . . . . ?
C28 C29 C30 N4 1.8(19) . . . . ?
C29 C28 C35 C36 177.4(17) . . . . ?
C29 C28 C35 C37 48.6(19) . . . . ?
C29 C28 C35 C38 -69.3(16) . . . . ?
C29 C28 C35 C36A 140.0(19) . . . . ?
C29 C28 C35 C37A 23(3) . . . . ?
C29 C28 C35 C38A -102(2) . . . . ?
C29 C30 N4 C26 -0.5(17) . . . . ?
C29 C30 N4 Re2 -176.1(9) . . . . ?
C31 C23 C24 C25 177.7(10) . . . . ?
C35 C28 C29 C30 175.8(12) . . . . ?
N3 C21 C22 C23 -1.3(18) . . . . ?
N3 C25 C26 C27 -176.1(9) . . . . ?
N3 C25 C26 N4 0.0(13) . . . . ?
N4 C26 C27 C28 -1.1(16) . . . . ?
C1 C2 C3 C4 -2.6(15) . . . . ?
C1 C2 C3 C11 177.8(10) . . . . ?
C2 C1 N1 C5 -1.1(15) . . . . ?
C2 C1 N1 Re1 -175.7(8) . . . . ?
C2 C3 C4 C5 2.1(15) . . . . ?
C2 C3 C11 C12 -6.4(14) . . . . ?
C2 C3 C11 C13 -127.7(11) . . . . ?
C2 C3 C11 C14 110.9(12) . . . . ?
C3 C4 C5 C6 176.3(9) . . . . ?
C3 C4 C5 N1 -1.2(15) . . . . ?
C4 C3 C11 C12 174.1(9) . . . . ?
C4 C3 C11 C13 52.8(13) . . . . ?
C4 C3 C11 C14 -68.6(12) . . . . ?
C4 C5 C6 C7 3.3(16) . . . . ?
C4 C5 C6 N2 -177.1(10) . . . . ?
C4 C5 N1 C1 0.6(14) . . . . ?
C4 C5 N1 Re1 175.6(7) . . . . ?
C5 C6 C7 C8 -178.2(9) . . . . ?
C5 C6 N2 C10 177.8(8) . . . . ?
C5 C6 N2 Re1 1.4(11) . . . . ?
C6 C5 N1 C1 -177.1(9) . . . . ?
C6 C5 N1 Re1 -2.2(11) . . . . ?
C6 C7 C8 C9 -0.2(15) . . . . ?
C6 C7 C8 C15 -178.6(10) . . . . ?
C7 C6 N2 C10 -2.6(14) . . . . ?
C7 C6 N2 Re1 -179.0(7) . . . . ?
C7 C8 C9 C10 -1.4(16) . . . . ?
C7 C8 C15 C16 -49.6(13) . . . . ?
C7 C8 C15 C17 -166.5(10) . . . . ?
C7 C8 C15 C18 73.7(12) . . . . ?
C8 C9 C10 N2 1.1(17) . . . . ?
C9 C8 C15 C16 132.1(11) . . . . ?
C9 C8 C15 C17 15.2(15) . . . . ?
C9 C8 C15 C18 -104.6(12) . . . . ?
C9 C10 N2 C6 1.0(15) . . . . ?
C9 C10 N2 Re1 177.1(8) . . . . ?
C11 C3 C4 C5 -178.3(9) . . . . ?
C15 C8 C9 C10 176.9(10) . . . . ?
N1 C1 C2 C3 2.2(17) . . . . ?
N1 C5 C6 C7 -179.1(9) . . . . ?
N1 C5 C6 N2 0.5(13) . . . . ?
N2 C6 C7 C8 2.2(16) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a loop in oil'
_olex2_submission_original_sample_id KS2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks82-2
_database_code_depnum_ccdc_archive 'CCDC 2057003'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-02-19
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
kevin.schindler@unifr.ch
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H34 N4 O2 Re, 2(F3 P0.5)'
_chemical_formula_sum            'C30 H34 F6 N4 O2 P Re'
_chemical_formula_weight         813.78
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   32.6007(5)
_cell_length_b                   12.21990(10)
_cell_length_c                   18.8003(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.7040(10)
_cell_angle_gamma                90
_cell_volume                     7333.89(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    102336
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.46
_cell_measurement_theta_min      4.34
_shelx_estimated_absorpt_T_max   0.866
_shelx_estimated_absorpt_T_min   0.181
_exptl_absorpt_coefficient_mu    7.427
_exptl_absorpt_correction_T_max  0.7993
_exptl_absorpt_correction_T_min  0.1353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3216
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of DCM and pentane  by slow evaporation'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56792
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.838
_diffrn_reflns_theta_min         4.343
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Primux 100 micro'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6135
_reflns_number_total             6605
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6605
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0708P)²+37.0654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1190
_refine_special_details          
;
splitting and restrain on t-butyl, and on PF6.
squeeze applied (DCM).
constraint applied on H of C19 in order to avoid close contact with H of C9.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H19F-H9
 2.1 with sigma of 0.02
 C5-C13 \\sim C5A-C13
 with sigma of 0.02
 C13-C15 \\sim C13-C15A
 with sigma of 0.02
 C13-C16 \\sim C13-C16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5A) = Uanis(C5) = Uanis(C16A) = Uanis(C16) = Uanis(C15A) = Uanis(C15)
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C19A) = Uanis(C20A) = Uanis(C18A)
Uanis(F4A) = Uanis(F4) = Uanis(F5) = Uanis(F6) = Uanis(F5A) = Uanis(F6A)
Uanis(F3) = Uanis(F2) = Uanis(F1)
4. Others
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C11(H11), C12(H12), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C15(H15A,H15B,H15C), C15A(H15D,H15E,
 H15F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C18(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,
 H20C), C20A(H20D,H20E,H20F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.63321(2) 0.67603(2) 0.48598(2) 0.04099(10) Uani 1 1 d . . . . .
O1 O 0.71845(14) 0.6518(4) 0.5877(3) 0.0801(14) Uani 1 1 d . . . . .
O2 O 0.59705(14) 0.7748(4) 0.6091(2) 0.0696(11) Uani 1 1 d . . . . .
N1 N 0.65126(12) 0.6081(3) 0.3894(2) 0.0422(9) Uani 1 1 d . . . . .
N2 N 0.57888(12) 0.6951(3) 0.3980(2) 0.0406(8) Uani 1 1 d . . . . .
N3 N 0.60999(13) 0.5168(4) 0.5053(2) 0.0489(10) Uani 1 1 d . . . . .
N4 N 0.65293(15) 0.8328(4) 0.4532(2) 0.0512(11) Uani 1 1 d . . . . .
C1 C 0.68483(19) 0.6591(5) 0.5508(3) 0.0531(13) Uani 1 1 d . . . . .
C2 C 0.61115(16) 0.7368(5) 0.5623(3) 0.0520(12) Uani 1 1 d . . . . .
C3 C 0.68789(15) 0.5589(5) 0.3889(3) 0.0501(12) Uani 1 1 d . . . . .
H3 H 0.708431 0.557789 0.432707 0.060 Uiso 1 1 calc R U . . .
C4 C 0.69739(17) 0.5097(5) 0.3282(3) 0.0548(13) Uani 1 1 d . . . . .
H4 H 0.723905 0.475929 0.330773 0.066 Uiso 1 1 calc R U . . .
C5 C 0.6859(6) 0.5511(13) 0.1445(8) 0.119(3) Uani 0.669(13) 1 d D . P A 1
H5A H 0.660085 0.593105 0.128077 0.178 Uiso 0.669(13) 1 calc R U P A 1
H5B H 0.695334 0.520795 0.102340 0.178 Uiso 0.669(13) 1 calc R U P A 1
H5C H 0.707607 0.599131 0.171612 0.178 Uiso 0.669(13) 1 calc R U P A 1
C5A C 0.7071(10) 0.521(2) 0.1593(17) 0.119(3) Uani 0.331(13) 1 d D . P A 2
H5AA H 0.703816 0.498397 0.108387 0.178 Uiso 0.331(13) 1 calc R U P A 2
H5AB H 0.735992 0.507501 0.184712 0.178 Uiso 0.331(13) 1 calc R U P A 2
H5AC H 0.700621 0.598846 0.161610 0.178 Uiso 0.331(13) 1 calc R U P A 2
C6 C 0.63048(16) 0.5646(4) 0.2633(3) 0.0479(11) Uani 1 1 d . . . . .
H6 H 0.609962 0.569557 0.219645 0.058 Uiso 1 1 calc R U . . .
C7 C 0.62277(14) 0.6117(4) 0.3259(2) 0.0407(10) Uani 1 1 d . . . . .
C8 C 0.58308(15) 0.6679(4) 0.3296(3) 0.0411(10) Uani 1 1 d . . . . .
C9 C 0.55271(17) 0.6943(5) 0.2696(3) 0.0515(12) Uani 1 1 d . . . . .
H9 H 0.556731 0.675349 0.222472 0.062 Uiso 1 1 calc DR U . . .
C10 C 0.51623(17) 0.7483(5) 0.2773(3) 0.0586(14) Uani 1 1 d . . . . .
C11 C 0.51183(17) 0.7715(5) 0.3474(3) 0.0566(13) Uani 1 1 d . . . . .
H11 H 0.487090 0.806232 0.355383 0.068 Uiso 1 1 calc R U . . .
C12 C 0.54297(15) 0.7447(5) 0.4052(3) 0.0506(12) Uani 1 1 d . . . . .
H12 H 0.539119 0.761775 0.452659 0.061 Uiso 1 1 calc R U . . .
C13 C 0.6771(2) 0.4544(7) 0.1955(3) 0.077(2) Uani 1 1 d D . . . .
C14 C 0.66813(17) 0.5097(5) 0.2633(3) 0.0527(12) Uani 1 1 d . . . . .
C15 C 0.7186(5) 0.3932(15) 0.2101(7) 0.119(3) Uani 0.669(13) 1 d D . P A 1
H15A H 0.723872 0.363381 0.164460 0.178 Uiso 0.669(13) 1 calc R U P A 1
H15B H 0.717334 0.333320 0.244263 0.178 Uiso 0.669(13) 1 calc R U P A 1
H15C H 0.741181 0.443622 0.231063 0.178 Uiso 0.669(13) 1 calc R U P A 1
C15A C 0.6864(13) 0.3334(17) 0.2159(15) 0.119(3) Uani 0.331(13) 1 d D . P A 2
H15D H 0.695393 0.295692 0.175706 0.178 Uiso 0.331(13) 1 calc R U P A 2
H15E H 0.661056 0.298467 0.225622 0.178 Uiso 0.331(13) 1 calc R U P A 2
H15F H 0.708725 0.329314 0.259490 0.178 Uiso 0.331(13) 1 calc R U P A 2
C16 C 0.6385(5) 0.4073(16) 0.1497(8) 0.119(3) Uani 0.669(13) 1 d D . P A 1
H16A H 0.616845 0.463942 0.139132 0.178 Uiso 0.669(13) 1 calc R U P A 1
H16B H 0.628404 0.346747 0.175726 0.178 Uiso 0.669(13) 1 calc R U P A 1
H16C H 0.644847 0.380116 0.104076 0.178 Uiso 0.669(13) 1 calc R U P A 1
C16A C 0.6392(8) 0.452(3) 0.1330(14) 0.119(3) Uani 0.331(13) 1 d D . P A 2
H16D H 0.633012 0.526102 0.114240 0.178 Uiso 0.331(13) 1 calc R U P A 2
H16E H 0.614944 0.422913 0.150383 0.178 Uiso 0.331(13) 1 calc R U P A 2
H16F H 0.645184 0.404711 0.094166 0.178 Uiso 0.331(13) 1 calc R U P A 2
C17 C 0.4837(2) 0.7840(7) 0.2109(4) 0.081(2) Uani 1 1 d . . . . .
C18 C 0.4682(5) 0.6812(12) 0.1676(7) 0.120(3) Uani 0.762(10) 1 d . . P B 3
H18A H 0.491912 0.644648 0.152744 0.180 Uiso 0.762(10) 1 calc R U P B 3
H18B H 0.447375 0.701498 0.124368 0.180 Uiso 0.762(10) 1 calc R U P B 3
H18C H 0.455517 0.631556 0.197858 0.180 Uiso 0.762(10) 1 calc R U P B 3
C18A C 0.4383(13) 0.735(5) 0.228(2) 0.120(3) Uani 0.238(10) 1 d . . P B 4
H18D H 0.437350 0.655235 0.221944 0.180 Uiso 0.238(10) 1 calc R U P B 4
H18E H 0.414598 0.768210 0.194938 0.180 Uiso 0.238(10) 1 calc R U P B 4
H18F H 0.436489 0.752612 0.278543 0.180 Uiso 0.238(10) 1 calc R U P B 4
C19 C 0.5056(4) 0.8556(14) 0.1608(7) 0.120(3) Uani 0.762(10) 1 d . . P B 3
H19A H 0.519313 0.918094 0.188426 0.180 Uiso 0.762(10) 1 calc R U P B 3
H19B H 0.484587 0.882031 0.119468 0.180 Uiso 0.762(10) 1 calc R U P B 3
H19C H 0.526515 0.811527 0.143017 0.180 Uiso 0.762(10) 1 calc R U P B 3
C19A C 0.4940(14) 0.753(5) 0.139(2) 0.120(3) Uani 0.238(10) 1 d . . P B 4
H19D H 0.475191 0.791335 0.099627 0.180 Uiso 0.238(10) 1 calc R U P B 4
H19E H 0.490450 0.673500 0.131609 0.180 Uiso 0.238(10) 1 calc R U P B 4
H19F H 0.523080 0.772674 0.138528 0.180 Uiso 0.238(10) 1 calc DR U P B 4
C20 C 0.4486(5) 0.8498(15) 0.2298(7) 0.120(3) Uani 0.762(10) 1 d . . P B 3
H20A H 0.434557 0.806898 0.261828 0.180 Uiso 0.762(10) 1 calc R U P B 3
H20B H 0.428485 0.868427 0.185260 0.180 Uiso 0.762(10) 1 calc R U P B 3
H20C H 0.459888 0.917153 0.254612 0.180 Uiso 0.762(10) 1 calc R U P B 3
C20A C 0.4748(15) 0.905(4) 0.218(2) 0.120(3) Uani 0.238(10) 1 d . . P B 4
H20D H 0.466326 0.917719 0.264583 0.180 Uiso 0.238(10) 1 calc R U P B 4
H20E H 0.452198 0.927286 0.178178 0.180 Uiso 0.238(10) 1 calc R U P B 4
H20F H 0.500111 0.947037 0.216536 0.180 Uiso 0.238(10) 1 calc R U P B 4
C21 C 0.57208(19) 0.5022(6) 0.5224(4) 0.0667(16) Uani 1 1 d . . . . .
H21 H 0.555188 0.564914 0.524852 0.080 Uiso 1 1 calc R U . . .
C22 C 0.5567(2) 0.4020(7) 0.5365(4) 0.080(2) Uani 1 1 d . . . . .
H22 H 0.530279 0.395694 0.550194 0.097 Uiso 1 1 calc R U . . .
C23 C 0.5806(3) 0.3097(6) 0.5303(5) 0.081(2) Uani 1 1 d . . . . .
H23 H 0.570250 0.238789 0.537353 0.098 Uiso 1 1 calc R U . . .
C24 C 0.6184(3) 0.3220(5) 0.5142(4) 0.075(2) Uani 1 1 d . . . . .
H24 H 0.635514 0.259963 0.511256 0.090 Uiso 1 1 calc R U . . .
C25 C 0.6324(2) 0.4255(5) 0.5018(3) 0.0616(14) Uani 1 1 d . . . . .
H25 H 0.659376 0.432549 0.490288 0.074 Uiso 1 1 calc R U . . .
C26 C 0.6918(2) 0.8488(6) 0.4396(4) 0.0688(16) Uani 1 1 d . . . . .
H26 H 0.710287 0.788126 0.442460 0.083 Uiso 1 1 calc R U . . .
C27 C 0.7052(3) 0.9490(8) 0.4220(4) 0.091(3) Uani 1 1 d . . . . .
H27 H 0.733029 0.957730 0.414826 0.109 Uiso 1 1 calc R U . . .
C28 C 0.6792(4) 1.0357(8) 0.4146(4) 0.103(3) Uani 1 1 d . . . . .
H28 H 0.688103 1.105079 0.400645 0.124 Uiso 1 1 calc R U . . .
C29 C 0.6403(3) 1.0219(6) 0.4274(4) 0.091(3) Uani 1 1 d . . . . .
H29 H 0.621469 1.082059 0.422834 0.110 Uiso 1 1 calc R U . . .
C30 C 0.6277(2) 0.9200(5) 0.4472(3) 0.0646(15) Uani 1 1 d . . . . .
H30 H 0.600315 0.911882 0.456663 0.078 Uiso 1 1 calc R U . . .
P1 P 0.750000 0.29406(18) 0.500000 0.0683(6) Uani 1 2 d S T P . .
F1 F 0.73215(17) 0.2032(5) 0.5428(3) 0.1235(12) Uani 1 1 d . . . . .
F2 F 0.70705(17) 0.2941(5) 0.4415(3) 0.1235(12) Uani 1 1 d . . . . .
F3 F 0.76691(16) 0.3887(5) 0.4595(3) 0.1235(12) Uani 1 1 d . . . . .
P2 P 0.500000 1.000000 0.500000 0.0630(6) Uani 1 2 d S . P . .
F4 F 0.5007(2) 0.8690(6) 0.5108(4) 0.0965(13) Uani 0.770(6) 1 d . . P C 5
F4A F 0.5382(6) 0.9370(17) 0.5453(13) 0.0965(13) Uani 0.230(6) 1 d . . P C 6
F5 F 0.52756(19) 1.0121(5) 0.5790(4) 0.0965(13) Uani 0.770(6) 1 d . . P C 5
F5A F 0.5202(7) 1.1143(19) 0.5174(14) 0.0965(13) Uani 0.230(6) 1 d . . P C 6
F6 F 0.4594(2) 1.0071(5) 0.5339(4) 0.0965(13) Uani 0.770(6) 1 d . . P C 5
F6A F 0.5225(8) 0.9886(19) 0.4291(15) 0.0965(13) Uani 0.230(6) 1 d . . P C 6


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.182(4) . ?
Re1 N2 2.177(4) . ?
Re1 N3 2.145(4) . ?
Re1 N4 2.150(4) . ?
Re1 C1 1.878(6) . ?
Re1 C2 1.883(5) . ?
O1 C1 1.175(7) . ?
O2 C2 1.168(6) . ?
N1 C3 1.338(6) . ?
N1 C7 1.357(6) . ?
N2 C8 1.362(6) . ?
N2 C12 1.349(6) . ?
N3 C21 1.351(7) . ?
N3 C25 1.343(7) . ?
N4 C26 1.357(8) . ?
N4 C30 1.337(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(7) . ?
C4 H4 0.9500 . ?
C4 C14 1.388(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 C13 1.583(16) . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C5A C13 1.53(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(7) . ?
C6 C14 1.399(7) . ?
C7 C8 1.479(6) . ?
C8 C9 1.380(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.393(8) . ?
C10 C11 1.383(8) . ?
C10 C17 1.528(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.368(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.522(7) . ?
C13 C15 1.520(14) . ?
C13 C15A 1.542(19) . ?
C13 C16 1.488(15) . ?
C13 C16A 1.523(19) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?
C17 C18 1.525(16) . ?
C17 C18A 1.69(5) . ?
C17 C19 1.559(18) . ?
C17 C19A 1.51(5) . ?
C17 C20 1.499(16) . ?
C17 C20A 1.51(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.370(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.334(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.381(9) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.364(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.345(14) . ?
C28 H28 0.9500 . ?
C28 C29 1.351(13) . ?
C29 H29 0.9500 . ?
C29 C30 1.384(10) . ?
C30 H30 0.9500 . ?
P1 F1 1.552(5) . ?
P1 F1 1.552(5) 2_656 ?
P1 F2 1.595(5) . ?
P1 F2 1.595(5) 2_656 ?
P1 F3 1.546(5) . ?
P1 F3 1.546(5) 2_656 ?
P2 F4 1.613(7) . ?
P2 F4 1.613(7) 5_676 ?
P2 F4A 1.56(2) . ?
P2 F4A 1.56(2) 5_676 ?
P2 F5 1.579(7) . ?
P2 F5 1.579(7) 5_676 ?
P2 F5A 1.55(2) . ?
P2 F5A 1.55(2) 5_676 ?
P2 F6 1.584(6) 5_676 ?
P2 F6 1.584(6) . ?
P2 F6A 1.65(2) 5_676 ?
P2 F6A 1.65(2) . ?

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
N2 Re1 N1 73.99(14) . . ?
N3 Re1 N1 87.68(15) . . ?
N3 Re1 N2 87.99(16) . . ?
N3 Re1 N4 173.15(16) . . ?
N4 Re1 N1 87.38(16) . . ?
N4 Re1 N2 86.09(16) . . ?
C1 Re1 N1 98.07(19) . . ?
C1 Re1 N2 171.35(19) . . ?
C1 Re1 N3 95.2(2) . . ?
C1 Re1 N4 90.2(2) . . ?
C1 Re1 C2 88.8(2) . . ?
C2 Re1 N1 173.12(18) . . ?
C2 Re1 N2 99.16(18) . . ?
C2 Re1 N3 91.5(2) . . ?
C2 Re1 N4 92.8(2) . . ?
C3 N1 Re1 124.6(3) . . ?
C3 N1 C7 117.4(4) . . ?
C7 N1 Re1 117.9(3) . . ?
C8 N2 Re1 118.0(3) . . ?
C12 N2 Re1 124.2(3) . . ?
C12 N2 C8 117.3(4) . . ?
C21 N3 Re1 122.1(4) . . ?
C25 N3 Re1 122.1(4) . . ?
C25 N3 C21 115.9(5) . . ?
C26 N4 Re1 121.8(4) . . ?
C30 N4 Re1 121.3(4) . . ?
C30 N4 C26 116.8(6) . . ?
O1 C1 Re1 175.2(5) . . ?
O2 C2 Re1 179.2(5) . . ?
N1 C3 H3 118.3 . . ?
N1 C3 C4 123.5(5) . . ?
C4 C3 H3 118.3 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C14 119.8(5) . . ?
C14 C4 H4 120.1 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C13 C5 H5A 109.5 . . ?
C13 C5 H5B 109.5 . . ?
C13 C5 H5C 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
C13 C5A H5AA 109.5 . . ?
C13 C5A H5AB 109.5 . . ?
C13 C5A H5AC 109.5 . . ?
C7 C6 H6 119.6 . . ?
C7 C6 C14 120.9(5) . . ?
C14 C6 H6 119.6 . . ?
N1 C7 C6 121.8(4) . . ?
N1 C7 C8 115.1(4) . . ?
C6 C7 C8 123.1(4) . . ?
N2 C8 C7 114.4(4) . . ?
N2 C8 C9 121.5(4) . . ?
C9 C8 C7 124.0(4) . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.8(5) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 C17 121.0(5) . . ?
C11 C10 C9 116.8(5) . . ?
C11 C10 C17 122.1(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 H11 119.9 . . ?
N2 C12 C11 123.2(5) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C5A C13 C15A 120.5(18) . . ?
C14 C13 C5 105.3(7) . . ?
C14 C13 C5A 112.6(12) . . ?
C14 C13 C15A 106.1(11) . . ?
C14 C13 C16A 113.1(13) . . ?
C15 C13 C5 102.3(10) . . ?
C15 C13 C14 112.4(7) . . ?
C16 C13 C5 100.0(10) . . ?
C16 C13 C14 111.9(8) . . ?
C16 C13 C15 122.1(11) . . ?
C16A C13 C5A 99.2(19) . . ?
C16A C13 C15A 105(2) . . ?
C4 C14 C6 116.5(5) . . ?
C4 C14 C13 121.4(5) . . ?
C6 C14 C13 122.1(5) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C15A H15D 109.5 . . ?
C13 C15A H15E 109.5 . . ?
C13 C15A H15F 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C16A H16D 109.5 . . ?
C13 C16A H16E 109.5 . . ?
C13 C16A H16F 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
C10 C17 C18A 103.3(13) . . ?
C10 C17 C19 109.1(7) . . ?
C18 C17 C10 107.5(7) . . ?
C18 C17 C19 106.4(10) . . ?
C19A C17 C10 114.6(14) . . ?
C19A C17 C18A 117(3) . . ?
C19A C17 C20A 114(3) . . ?
C20 C17 C10 113.3(7) . . ?
C20 C17 C18 112.5(11) . . ?
C20 C17 C19 107.8(11) . . ?
C20A C17 C10 108.5(15) . . ?
C20A C17 C18A 98(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C18A H18D 109.5 . . ?
C17 C18A H18E 109.5 . . ?
C17 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C19A H19D 109.5 . . ?
C17 C19A H19E 109.5 . . ?
C17 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C20A H20D 109.5 . . ?
C17 C20A H20E 109.5 . . ?
C17 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
N3 C21 H21 118.2 . . ?
N3 C21 C22 123.6(7) . . ?
C22 C21 H21 118.2 . . ?
C21 C22 H22 120.8 . . ?
C21 C22 C23 118.3(7) . . ?
C23 C22 H22 120.8 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 C22 119.2(6) . . ?
C24 C23 H23 120.4 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.6(7) . . ?
C25 C24 H24 120.2 . . ?
N3 C25 C24 123.4(6) . . ?
N3 C25 H25 118.3 . . ?
C24 C25 H25 118.3 . . ?
N4 C26 H26 118.9 . . ?
N4 C26 C27 122.2(8) . . ?
C27 C26 H26 118.9 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.4(8) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.7 . . ?
C27 C28 C29 118.6(8) . . ?
C29 C28 H28 120.7 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(9) . . ?
C30 C29 H29 120.0 . . ?
N4 C30 C29 121.9(7) . . ?
N4 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
F1 P1 F1 88.7(6) . 2_656 ?
F1 P1 F2 89.4(3) . . ?
F1 P1 F2 90.7(3) . 2_656 ?
F1 P1 F2 89.4(3) 2_656 2_656 ?
F1 P1 F2 90.7(3) 2_656 . ?
F2 P1 F2 179.9(4) . 2_656 ?
F3 P1 F1 94.1(4) 2_656 . ?
F3 P1 F1 94.1(4) . 2_656 ?
F3 P1 F1 177.2(4) 2_656 2_656 ?
F3 P1 F1 177.2(4) . . ?
F3 P1 F2 90.6(3) . . ?
F3 P1 F2 89.3(3) . 2_656 ?
F3 P1 F2 89.3(3) 2_656 . ?
F3 P1 F2 90.6(3) 2_656 2_656 ?
F3 P1 F3 83.2(5) 2_656 . ?
F4 P2 F6A 91.2(8) 5_676 5_676 ?
F4 P2 F6A 88.8(9) . 5_676 ?
F4A P2 F6A 87.9(12) 5_676 5_676 ?
F4A P2 F6A 92.1(12) . 5_676 ?
F4A P2 F6A 87.9(12) . . ?
F4A P2 F6A 92.1(12) 5_676 . ?
F5 P2 F4 89.1(4) . . ?
F5 P2 F4 90.9(4) 5_676 . ?
F5 P2 F5 180.0 5_676 . ?
F5 P2 F6 88.8(4) . . ?
F5 P2 F6 91.2(4) 5_676 . ?
F5 P2 F6A 59.6(10) . 5_676 ?
F5 P2 F6A 120.4(10) 5_676 5_676 ?
F5A P2 F4A 85.8(12) 5_676 . ?
F5A P2 F4A 94.1(12) . . ?
F5A P2 F5A 180.0 5_676 . ?
F5A P2 F6A 90.4(11) . . ?
F5A P2 F6A 89.6(11) 5_676 . ?
F5A P2 F6A 90.4(11) 5_676 5_676 ?
F5A P2 F6A 89.6(11) . 5_676 ?
F6 P2 F4 90.3(3) 5_676 . ?
F6 P2 F4 89.7(3) . . ?
F6 P2 F6A 150.9(9) 5_676 5_676 ?
F6 P2 F6A 29.1(9) . 5_676 ?
F6A P2 F6A 180.0 5_676 . ?

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 N1 C3 C4 175.2(4) . . . . ?
Re1 N1 C7 C6 -175.8(4) . . . . ?
Re1 N1 C7 C8 3.3(5) . . . . ?
Re1 N2 C8 C7 9.3(5) . . . . ?
Re1 N2 C8 C9 -169.1(4) . . . . ?
Re1 N2 C12 C11 169.2(5) . . . . ?
Re1 N3 C21 C22 -178.6(5) . . . . ?
Re1 N3 C25 C24 179.8(5) . . . . ?
Re1 N4 C26 C27 -177.0(5) . . . . ?
Re1 N4 C30 C29 178.8(5) . . . . ?
N1 C3 C4 C14 0.0(9) . . . . ?
N1 C7 C8 N2 -8.1(6) . . . . ?
N1 C7 C8 C9 170.2(5) . . . . ?
N2 C8 C9 C10 -1.1(8) . . . . ?
N3 C21 C22 C23 -2.4(11) . . . . ?
N4 C26 C27 C28 -2.7(12) . . . . ?
C3 N1 C7 C6 1.4(7) . . . . ?
C3 N1 C7 C8 -179.4(4) . . . . ?
C3 C4 C14 C6 2.3(9) . . . . ?
C3 C4 C14 C13 -178.8(6) . . . . ?
C5 C13 C14 C4 -105.3(10) . . . . ?
C5 C13 C14 C6 73.5(10) . . . . ?
C5A C13 C14 C4 -75.5(18) . . . . ?
C5A C13 C14 C6 103.4(17) . . . . ?
C6 C7 C8 N2 171.0(5) . . . . ?
C6 C7 C8 C9 -10.7(8) . . . . ?
C7 N1 C3 C4 -1.9(8) . . . . ?
C7 C6 C14 C4 -2.7(8) . . . . ?
C7 C6 C14 C13 178.4(6) . . . . ?
C7 C8 C9 C10 -179.4(5) . . . . ?
C8 N2 C12 C11 -2.2(8) . . . . ?
C8 C9 C10 C11 -1.3(9) . . . . ?
C8 C9 C10 C17 176.2(6) . . . . ?
C9 C10 C11 C12 2.0(10) . . . . ?
C9 C10 C17 C18 60.4(11) . . . . ?
C9 C10 C17 C18A 130(2) . . . . ?
C9 C10 C17 C19 -54.6(11) . . . . ?
C9 C10 C17 C19A 2(3) . . . . ?
C9 C10 C17 C20 -174.7(11) . . . . ?
C9 C10 C17 C20A -127(2) . . . . ?
C10 C11 C12 N2 -0.2(10) . . . . ?
C11 C10 C17 C18 -122.2(9) . . . . ?
C11 C10 C17 C18A -53(2) . . . . ?
C11 C10 C17 C19 122.9(9) . . . . ?
C11 C10 C17 C19A 179(3) . . . . ?
C11 C10 C17 C20 2.8(14) . . . . ?
C11 C10 C17 C20A 50(3) . . . . ?
C12 N2 C8 C7 -178.7(4) . . . . ?
C12 N2 C8 C9 2.8(7) . . . . ?
C14 C6 C7 N1 0.9(8) . . . . ?
C14 C6 C7 C8 -178.2(5) . . . . ?
C15 C13 C14 C4 5.3(13) . . . . ?
C15 C13 C14 C6 -175.8(10) . . . . ?
C15A C13 C14 C4 58.3(18) . . . . ?
C15A C13 C14 C6 -122.8(17) . . . . ?
C16 C13 C14 C4 146.9(10) . . . . ?
C16 C13 C14 C6 -34.2(12) . . . . ?
C16A C13 C14 C4 173.1(18) . . . . ?
C16A C13 C14 C6 -8(2) . . . . ?
C17 C10 C11 C12 -175.6(7) . . . . ?
C21 N3 C25 C24 0.5(9) . . . . ?
C21 C22 C23 C24 3.1(11) . . . . ?
C22 C23 C24 C25 -2.0(12) . . . . ?
C23 C24 C25 N3 0.2(11) . . . . ?
C25 N3 C21 C22 0.7(9) . . . . ?
C26 N4 C30 C29 0.5(9) . . . . ?
C26 C27 C28 C29 2.2(12) . . . . ?
C27 C28 C29 C30 -0.4(12) . . . . ?
C28 C29 C30 N4 -0.9(10) . . . . ?
C30 N4 C26 C27 1.3(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.250 0.250 285.3 76.8 '2 DCM'
2 0.250 0.250 0.750 285.3 76.8 '2 DCM'
3 0.750 0.750 0.750 285.3 76.8 '2 DCM'
4 0.750 0.750 0.250 285.3 76.8 '2 DCM'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks113-1_e
_database_code_depnum_ccdc_archive 'CCDC 2057000'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-10-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
kevin.schindler@unifr.ch
fabio.zobi@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H30 Br N4 O2 Re, 1[C5H12]'
_chemical_formula_sum            'C29 H42 Br N4 O2 Re'
_chemical_formula_weight         744.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   15.1687(3)
_cell_length_b                   17.1375(3)
_cell_length_c                   12.0964(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3144.50(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    80065
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.47
_cell_measurement_theta_min      3.65
_shelx_estimated_absorpt_T_max   0.606
_shelx_estimated_absorpt_T_min   0.258
_exptl_absorpt_coefficient_mu    9.278
_exptl_absorpt_correction_T_max  0.1519
_exptl_absorpt_correction_T_min  0.0521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method 'layering DCM and pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38203
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.651
_diffrn_reflns_theta_max         67.651
_diffrn_reflns_theta_min         5.342
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Primux 100 micro'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2806
_reflns_number_total             2838
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.747
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2838
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0234
_refine_ls_restrained_S_all      1.112
_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)+(0.0331P)²+3.8512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0615
_refine_special_details          
;
Br on 2 positions (sof arbitrairely setup at 0.5)
Solvant (probably pentane) has been mask
tert-butyl splitted and refined
;
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
Uanis(C8A) = Uanis(C7) = Uanis(C7A) = Uanis(C9) = Uanis(C9A) = Uanis(C8)
3. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: Br1(0.5) O2(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C15(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C10(H10), C11(H11), C12(H12)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC),
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.46471(2) 0.250000 0.47958(2) 0.03072(9) Uani 1 2 d S T P . .
Br1 Br 0.52306(7) 0.36024(7) 0.35435(9) 0.0427(2) Uani 0.5 1 d . U P A 3
O1 O 0.6276(2) 0.250000 0.6247(3) 0.0590(9) Uani 1 2 d S T P . .
O2 O 0.5558(5) 0.3812(5) 0.3470(8) 0.076(3) Uani 0.5 1 d . U P A 4
N1 N 0.39133(15) 0.32584(13) 0.58524(19) 0.0343(5) Uani 1 1 d . . . . .
N2 N 0.3464(2) 0.250000 0.3713(3) 0.0361(7) Uani 1 2 d S T P A .
N3 N 0.2678(2) 0.250000 0.2187(3) 0.0440(8) Uani 1 2 d S T P A .
C1 C 0.3993(2) 0.40393(17) 0.5871(3) 0.0413(7) Uani 1 1 d . . . . .
H1 H 0.441942 0.427538 0.540291 0.050 Uiso 1 1 calc R U . . .
C2 C 0.3493(2) 0.45097(18) 0.6530(3) 0.0476(8) Uani 1 1 d . . . . .
H2 H 0.358425 0.505799 0.652026 0.057 Uiso 1 1 calc R U . . .
C3 C 0.2846(2) 0.41917(19) 0.7218(3) 0.0495(8) Uani 1 1 d . . . . .
C4 C 0.2775(2) 0.33859(18) 0.7220(3) 0.0445(7) Uani 1 1 d . . . . .
H4 H 0.235241 0.314115 0.768484 0.053 Uiso 1 1 calc R U . . .
C5 C 0.33165(19) 0.29296(17) 0.6549(2) 0.0368(6) Uani 1 1 d . . . . .
C6 C 0.2284(3) 0.4726(2) 0.7940(4) 0.0765(13) Uani 1 1 d . . . . .
C7 C 0.1888(7) 0.5356(5) 0.7228(8) 0.0977(17) Uani 0.644(5) 1 d . U P B 1
H7A H 0.236073 0.566854 0.689767 0.147 Uiso 0.644(5) 1 calc R U P B 1
H7B H 0.151212 0.569306 0.768296 0.147 Uiso 0.644(5) 1 calc R U P B 1
H7C H 0.153373 0.511765 0.664133 0.147 Uiso 0.644(5) 1 calc R U P B 1
C7A C 0.1183(10) 0.4485(8) 0.7496(14) 0.0977(17) Uani 0.356(5) 1 d . . P B 2
H7AA H 0.111994 0.460337 0.670722 0.147 Uiso 0.356(5) 1 calc R U P B 2
H7AB H 0.075583 0.479284 0.791956 0.147 Uiso 0.356(5) 1 calc R U P B 2
H7AC H 0.107437 0.392819 0.761938 0.147 Uiso 0.356(5) 1 calc R U P B 2
C8 C 0.2957(6) 0.5176(5) 0.8775(8) 0.0977(17) Uani 0.644(5) 1 d . . P B 1
H8A H 0.327477 0.479223 0.922339 0.147 Uiso 0.644(5) 1 calc R U P B 1
H8B H 0.262099 0.552470 0.925952 0.147 Uiso 0.644(5) 1 calc R U P B 1
H8C H 0.337979 0.548258 0.834228 0.147 Uiso 0.644(5) 1 calc R U P B 1
C8A C 0.2323(12) 0.5531(9) 0.7760(15) 0.0977(17) Uani 0.356(5) 1 d . U P B 2
H8AA H 0.287769 0.573608 0.805687 0.147 Uiso 0.356(5) 1 calc R U P B 2
H8AB H 0.182580 0.578474 0.813186 0.147 Uiso 0.356(5) 1 calc R U P B 2
H8AC H 0.229321 0.563655 0.696452 0.147 Uiso 0.356(5) 1 calc R U P B 2
C9 C 0.1629(7) 0.4331(5) 0.8642(8) 0.0977(17) Uani 0.644(5) 1 d . . P B 1
H9A H 0.121149 0.404482 0.817467 0.147 Uiso 0.644(5) 1 calc R U P B 1
H9B H 0.130964 0.471934 0.908127 0.147 Uiso 0.644(5) 1 calc R U P B 1
H9C H 0.192941 0.396468 0.913743 0.147 Uiso 0.644(5) 1 calc R U P B 1
C9A C 0.2259(13) 0.4412(9) 0.9067(15) 0.0977(17) Uani 0.356(5) 1 d . . P B 2
H9AA H 0.215785 0.384707 0.903792 0.147 Uiso 0.356(5) 1 calc R U P B 2
H9AB H 0.177967 0.466094 0.948049 0.147 Uiso 0.356(5) 1 calc R U P B 2
H9AC H 0.282139 0.451647 0.943608 0.147 Uiso 0.356(5) 1 calc R U P B 2
C10 C 0.3494(3) 0.250000 0.2632(4) 0.0458(10) Uani 1 2 d S T P . .
H10 H 0.402400 0.250000 0.221375 0.055 Uiso 1 2 calc R U P A .
C11 C 0.2585(3) 0.250000 0.3972(4) 0.0515(11) Uani 1 2 d S T P . .
H11 H 0.235098 0.250000 0.470006 0.062 Uiso 1 2 calc R U P A .
C12 C 0.2103(3) 0.250000 0.3036(4) 0.0537(12) Uani 1 2 d S T P A .
H12 H 0.147837 0.250000 0.298430 0.064 Uiso 1 2 calc R U P . .
C13 C 0.2456(4) 0.250000 0.1026(4) 0.0646(15) Uani 1 2 d S T P . .
H13A H 0.192300 0.281214 0.090836 0.097 Uiso 0.5 1 calc R U P A -1
H13B H 0.235044 0.196323 0.077976 0.097 Uiso 0.5 1 calc R U P A -1
H13C H 0.294439 0.272463 0.060105 0.097 Uiso 0.5 1 calc R U P A -1
C14 C 0.5654(3) 0.250000 0.5706(4) 0.0408(9) Uani 1 2 d S T P A .
C15 C 0.5193(5) 0.3294(6) 0.3980(8) 0.0430(18) Uani 0.5 1 d . U P A 4


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Br1 2.5782(14) 7_565 ?
Re1 Br1 2.5783(14) . ?
Re1 N1 2.136(2) . ?
Re1 N1 2.136(2) 7_565 ?
Re1 N2 2.222(3) . ?
Re1 C14 1.883(5) . ?
Re1 C15 1.874(11) . ?
Re1 C15 1.874(11) 7_565 ?
O1 C14 1.148(6) . ?
O2 C15 1.214(11) . ?
N1 C1 1.344(4) . ?
N1 C5 1.359(4) . ?
N2 C10 1.308(6) . ?
N2 C11 1.369(6) . ?
N3 C10 1.350(6) . ?
N3 C12 1.347(7) . ?
N3 C13 1.444(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.364(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.397(5) . ?
C3 C4 1.385(5) . ?
C3 C6 1.526(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.395(4) . ?
C5 C5 1.472(6) 7_565 ?
C6 C7 1.506(11) . ?
C6 C7A 1.802(18) . ?
C6 C8 1.630(11) . ?
C6 C8A 1.398(17) . ?
C6 C9 1.472(9) . ?
C6 C9A 1.466(18) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.348(7) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

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
Br1 Re1 Br1 94.24(4) 7_565 . ?
N1 Re1 Br1 94.85(6) 7_565 7_565 ?
N1 Re1 Br1 94.85(6) . . ?
N1 Re1 Br1 167.53(6) . 7_565 ?
N1 Re1 Br1 167.53(6) 7_565 . ?
N1 Re1 N1 74.97(12) . 7_565 ?
N1 Re1 N2 86.08(10) . . ?
N1 Re1 N2 86.08(10) 7_565 . ?
N2 Re1 Br1 86.04(6) . . ?
N2 Re1 Br1 86.04(6) . 7_565 ?
C14 Re1 Br1 93.72(10) . 7_565 ?
C14 Re1 Br1 93.72(10) . . ?
C14 Re1 N1 94.19(13) . . ?
C14 Re1 N1 94.19(13) . 7_565 ?
C14 Re1 N2 179.65(16) . . ?
C15 Re1 N1 170.9(2) 7_565 . ?
C15 Re1 N1 95.9(2) . . ?
C15 Re1 N2 92.7(3) . . ?
C15 Re1 N2 92.7(3) 7_565 . ?
C15 Re1 C14 87.1(3) . . ?
C15 Re1 C14 87.1(3) 7_565 . ?
C15 Re1 C15 93.2(5) 7_565 . ?
C1 N1 Re1 124.7(2) . . ?
C1 N1 C5 117.6(3) . . ?
C5 N1 Re1 117.76(18) . . ?
C10 N2 Re1 124.1(3) . . ?
C10 N2 C11 105.3(4) . . ?
C11 N2 Re1 130.7(3) . . ?
C10 N3 C13 127.0(4) . . ?
C12 N3 C10 106.8(4) . . ?
C12 N3 C13 126.2(4) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(3) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C6 120.0(3) . . ?
C4 C3 C2 116.4(3) . . ?
C4 C3 C6 123.6(3) . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.8(3) . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C5 114.50(16) . 7_565 ?
C4 C5 C5 124.10(18) . 7_565 ?
C3 C6 C7A 102.1(5) . . ?
C3 C6 C8 106.7(4) . . ?
C7 C6 C3 109.0(4) . . ?
C7 C6 C8 105.3(6) . . ?
C8A C6 C3 118.6(7) . . ?
C8A C6 C7A 102.7(11) . . ?
C8A C6 C9A 120.6(10) . . ?
C9 C6 C3 115.5(4) . . ?
C9 C6 C7 113.0(6) . . ?
C9 C6 C8 106.5(6) . . ?
C9A C6 C3 109.0(6) . . ?
C9A C6 C7A 99.7(10) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C7A H7AA 109.5 . . ?
C6 C7A H7AB 109.5 . . ?
C6 C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C8A H8AA 109.5 . . ?
C6 C8A H8AB 109.5 . . ?
C6 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C9A H9AA 109.5 . . ?
C6 C9A H9AB 109.5 . . ?
C6 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
N2 C10 N3 111.5(4) . . ?
N2 C10 H10 124.2 . . ?
N3 C10 H10 124.2 . . ?
N2 C11 H11 125.2 . . ?
C12 C11 N2 109.6(4) . . ?
C12 C11 H11 125.2 . . ?
N3 C12 C11 106.8(4) . . ?
N3 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 Re1 179.0(4) . . ?
O2 C15 Re1 178.6(8) . . ?

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 N1 C1 C2 177.7(2) . . . . ?
Re1 N1 C5 C4 -176.3(2) . . . . ?
Re1 N1 C5 C5 5.4(2) . . . 7_565 ?
Re1 N2 C10 N3 180.000(0) . . . . ?
Re1 N2 C11 C12 180.000(0) . . . . ?
N1 C1 C2 C3 -1.2(5) . . . . ?
N2 C11 C12 N3 0.000(0) . . . . ?
C1 N1 C5 C4 3.1(4) . . . . ?
C1 N1 C5 C5 -175.2(2) . . . 7_565 ?
C1 C2 C3 C4 2.5(5) . . . . ?
C1 C2 C3 C6 -179.3(4) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
C2 C3 C6 C7 52.0(7) . . . . ?
C2 C3 C6 C7A 122.6(7) . . . . ?
C2 C3 C6 C8 -61.2(6) . . . . ?
C2 C3 C6 C8A 10.8(13) . . . . ?
C2 C3 C6 C9 -179.4(6) . . . . ?
C2 C3 C6 C9A -132.5(9) . . . . ?
C3 C4 C5 N1 -1.7(5) . . . . ?
C3 C4 C5 C5 176.4(2) . . . 7_565 ?
C4 C3 C6 C7 -129.9(6) . . . . ?
C4 C3 C6 C7A -59.3(7) . . . . ?
C4 C3 C6 C8 116.9(5) . . . . ?
C4 C3 C6 C8A -171.1(11) . . . . ?
C4 C3 C6 C9 -1.3(9) . . . . ?
C4 C3 C6 C9A 45.6(10) . . . . ?
C5 N1 C1 C2 -1.7(5) . . . . ?
C6 C3 C4 C5 -179.3(4) . . . . ?
C10 N2 C11 C12 0.000(0) . . . . ?
C10 N3 C12 C11 0.000(0) . . . . ?
C11 N2 C10 N3 0.000(0) . . . . ?
C12 N3 C10 N2 0.000(0) . . . . ?
C13 N3 C10 N2 180.000(0) . . . . ?
C13 N3 C12 C11 180.000(0) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.968 0.500 386.3 112.2 '2 C5H12'
2 0.500 -0.493 0.000 386.3 112.2 '2 C5H12'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'mounted on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks87-2_tw
_database_code_depnum_ccdc_archive 'CCDC 2057005'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-03-10
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
kevin.schindler@unifr.ch
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H36 N6 O2 Re, F6 P'
_chemical_formula_sum            'C28 H36 F6 N6 O2 P Re'
_chemical_formula_weight         819.80
_chemical_melting_point          ?
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'
P P 0.1023 0.0942 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.3996(3)
_cell_length_b                   13.8863(3)
_cell_length_c                   19.1424(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.747(2)
_cell_angle_gamma                90
_cell_volume                     3238.21(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39263
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      1.47
_shelx_estimated_absorpt_T_max   0.773
_shelx_estimated_absorpt_T_min   0.216
_exptl_absorpt_coefficient_mu    3.872
_exptl_absorpt_correction_T_max  0.5838
_exptl_absorpt_correction_T_min  0.1485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, , Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6440
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.320
_diffrn_reflns_theta_min         1.823
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5655
_reflns_number_total             6440
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.044
_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)+(0.0296P)²+6.4110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0698
_refine_special_details          'refined as twin (BASF: 0.0452(7))'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9548(7)
 0.0452(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C19(H19), C20(H20),
 C21(H21), C23(H23), C24(H24), C25(H25)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C26(H26A,
 H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.46512(2) 0.30633(2) 0.14116(2) 0.04055(6) Uani 1 1 d . . . . .
O1 O 0.2797(3) 0.3799(3) 0.0264(2) 0.0819(12) Uani 1 1 d . . . . .
O2 O 0.5619(3) 0.2145(3) 0.02301(19) 0.0749(11) Uani 1 1 d . . . . .
N1 N 0.4041(3) 0.3643(2) 0.23247(16) 0.0413(7) Uani 1 1 d . . . . .
N2 N 0.5834(3) 0.2615(2) 0.23474(17) 0.0406(7) Uani 1 1 d . . . . .
N3 N 0.3760(3) 0.1776(2) 0.15727(18) 0.0438(8) Uani 1 1 d . . . . .
N4 N 0.2405(3) 0.0773(3) 0.1592(2) 0.0573(10) Uani 1 1 d . . . . .
N5 N 0.5594(3) 0.4367(2) 0.14101(18) 0.0461(8) Uani 1 1 d . . . . .
N6 N 0.6967(3) 0.5359(3) 0.1420(2) 0.0565(9) Uani 1 1 d . . . . .
C1 C 0.3123(3) 0.4159(3) 0.2276(2) 0.0487(10) Uani 1 1 d . . . . .
H1 H 0.276005 0.435333 0.182251 0.058 Uiso 1 1 calc R U . . .
C2 C 0.2681(3) 0.4421(3) 0.2853(2) 0.0472(10) Uani 1 1 d . . . . .
H2 H 0.203634 0.479199 0.278742 0.057 Uiso 1 1 calc R U . . .
C3 C 0.3178(3) 0.4141(3) 0.3533(2) 0.0422(8) Uani 1 1 d . . . . .
C4 C 0.4167(3) 0.3634(3) 0.3585(2) 0.0415(9) Uani 1 1 d . . . . .
H4 H 0.455914 0.345775 0.403533 0.050 Uiso 1 1 calc R U . . .
C5 C 0.4571(3) 0.3390(3) 0.2985(2) 0.0374(8) Uani 1 1 d . . . . .
C6 C 0.5614(3) 0.2844(3) 0.2998(2) 0.0385(8) Uani 1 1 d . . . . .
C7 C 0.6332(3) 0.2611(3) 0.3616(2) 0.0438(9) Uani 1 1 d . . . . .
H7 H 0.615344 0.277615 0.405661 0.053 Uiso 1 1 calc R U . . .
C8 C 0.7320(3) 0.2132(3) 0.3598(2) 0.0456(9) Uani 1 1 d . . . . .
C9 C 0.7509(4) 0.1890(3) 0.2928(2) 0.0518(10) Uani 1 1 d . . . . .
H9 H 0.815045 0.155554 0.288204 0.062 Uiso 1 1 calc R U . . .
C10 C 0.6759(4) 0.2139(3) 0.2331(2) 0.0494(10) Uani 1 1 d . . . . .
H10 H 0.691048 0.196140 0.188546 0.059 Uiso 1 1 calc R U . . .
C11 C 0.2653(4) 0.4324(3) 0.4180(2) 0.0477(10) Uani 1 1 d . . . . .
C12 C 0.1687(5) 0.5014(5) 0.4014(3) 0.090(2) Uani 1 1 d . . . . .
H12A H 0.193819 0.563088 0.386867 0.136 Uiso 1 1 calc R U . . .
H12B H 0.136661 0.509973 0.443521 0.136 Uiso 1 1 calc R U . . .
H12C H 0.113973 0.475121 0.363323 0.136 Uiso 1 1 calc R U . . .
C13 C 0.2253(6) 0.3354(5) 0.4408(4) 0.095(2) Uani 1 1 d . . . . .
H13A H 0.172256 0.308360 0.402125 0.142 Uiso 1 1 calc R U . . .
H13B H 0.191156 0.344429 0.481984 0.142 Uiso 1 1 calc R U . . .
H13C H 0.287166 0.291867 0.452835 0.142 Uiso 1 1 calc R U . . .
C14 C 0.3491(5) 0.4725(5) 0.4790(3) 0.0845(19) Uani 1 1 d . . . . .
H14A H 0.406485 0.425176 0.493538 0.127 Uiso 1 1 calc R U . . .
H14B H 0.313407 0.486977 0.518747 0.127 Uiso 1 1 calc R U . . .
H14C H 0.380982 0.530805 0.463766 0.127 Uiso 1 1 calc R U . . .
C15 C 0.8154(4) 0.1927(4) 0.4275(3) 0.0578(11) Uani 1 1 d . . . . .
C16 C 0.7625(5) 0.1279(5) 0.4756(3) 0.090(2) Uani 1 1 d . . . . .
H16A H 0.694640 0.156905 0.483531 0.136 Uiso 1 1 calc R U . . .
H16B H 0.812171 0.119950 0.520839 0.136 Uiso 1 1 calc R U . . .
H16C H 0.746985 0.065484 0.453255 0.136 Uiso 1 1 calc R U . . .
C17 C 0.9167(5) 0.1418(7) 0.4121(4) 0.114(3) Uani 1 1 d . . . . .
H17A H 0.969297 0.133558 0.456065 0.170 Uiso 1 1 calc R U . . .
H17B H 0.949510 0.180181 0.379212 0.170 Uiso 1 1 calc R U . . .
H17C H 0.896198 0.079307 0.391250 0.170 Uiso 1 1 calc R U . . .
C18 C 0.8477(6) 0.2868(4) 0.4648(4) 0.103(3) Uani 1 1 d . . . . .
H18A H 0.881266 0.328256 0.434124 0.155 Uiso 1 1 calc R U . . .
H18B H 0.899744 0.274748 0.508484 0.155 Uiso 1 1 calc R U . . .
H18C H 0.782984 0.318016 0.475920 0.155 Uiso 1 1 calc R U . . .
C19 C 0.4182(4) 0.0879(3) 0.1762(3) 0.0582(11) Uani 1 1 d . . . . .
H19 H 0.493093 0.071754 0.186073 0.070 Uiso 1 1 calc R U . . .
C20 C 0.3348(5) 0.0269(4) 0.1783(3) 0.0643(13) Uani 1 1 d . . . . .
H20 H 0.340820 -0.038645 0.190688 0.077 Uiso 1 1 calc R U . . .
C21 C 0.2693(4) 0.1678(3) 0.1481(3) 0.0525(11) Uani 1 1 d . . . . .
H21 H 0.219100 0.218357 0.135307 0.063 Uiso 1 1 calc R U . . .
C22 C 0.1288(5) 0.0392(4) 0.1513(4) 0.0806(17) Uani 1 1 d . . . . .
H22A H 0.084290 0.082887 0.173585 0.121 Uiso 1 1 calc R U . . .
H22B H 0.130727 -0.023417 0.173977 0.121 Uiso 1 1 calc R U . . .
H22C H 0.097255 0.032940 0.101216 0.121 Uiso 1 1 calc R U . . .
C23 C 0.5199(5) 0.5287(4) 0.1321(3) 0.0732(15) Uani 1 1 d . . . . .
H23 H 0.445640 0.546564 0.126604 0.088 Uiso 1 1 calc R U . . .
C24 C 0.6048(5) 0.5895(4) 0.1324(4) 0.0811(17) Uani 1 1 d . . . . .
H24 H 0.600461 0.656777 0.126991 0.097 Uiso 1 1 calc R U . . .
C25 C 0.6661(4) 0.4440(3) 0.1469(2) 0.0510(10) Uani 1 1 d . . . . .
H25 H 0.714850 0.391568 0.153662 0.061 Uiso 1 1 calc R U . . .
C26 C 0.8096(4) 0.5710(4) 0.1444(3) 0.0739(15) Uani 1 1 d . . . . .
H26A H 0.860902 0.518260 0.156663 0.111 Uiso 1 1 calc R U . . .
H26B H 0.825971 0.621410 0.179904 0.111 Uiso 1 1 calc R U . . .
H26C H 0.816210 0.596525 0.098209 0.111 Uiso 1 1 calc R U . . .
C27 C 0.3514(4) 0.3518(3) 0.0697(2) 0.0547(11) Uani 1 1 d . . . . .
C28 C 0.5265(4) 0.2494(3) 0.0687(2) 0.0524(11) Uani 1 1 d . . . . .
P1 P -0.00863(12) 0.29877(13) 0.20229(10) 0.0787(4) Uani 1 1 d . . . . .
F1 F 0.0331(4) 0.2663(5) 0.1329(2) 0.143(2) Uani 1 1 d . . . . .
F2 F 0.1096(3) 0.2744(3) 0.2443(3) 0.1183(15) Uani 1 1 d . . . . .
F3 F -0.0502(6) 0.3287(4) 0.2700(3) 0.168(3) Uani 1 1 d . . . . .
F4 F -0.1246(3) 0.3166(5) 0.1564(3) 0.161(2) Uani 1 1 d . . . . .
F5 F -0.0426(4) 0.1900(3) 0.2152(3) 0.1193(16) Uani 1 1 d . . . . .
F6 F 0.0262(4) 0.4061(4) 0.1940(3) 0.149(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.184(3) . ?
Re1 N2 2.184(3) . ?
Re1 N3 2.154(3) . ?
Re1 N5 2.156(3) . ?
Re1 C27 1.881(5) . ?
Re1 C28 1.877(5) . ?
O1 C27 1.164(6) . ?
O2 C28 1.156(5) . ?
N1 C1 1.333(5) . ?
N1 C5 1.358(5) . ?
N2 C6 1.361(5) . ?
N2 C10 1.330(5) . ?
N3 C19 1.373(5) . ?
N3 C21 1.309(6) . ?
N4 C20 1.353(6) . ?
N4 C21 1.334(6) . ?
N4 C22 1.464(6) . ?
N5 C23 1.367(6) . ?
N5 C25 1.311(6) . ?
N6 C24 1.346(7) . ?
N6 C25 1.339(6) . ?
N6 C26 1.475(6) . ?
C1 H1 0.9400 . ?
C1 C2 1.370(6) . ?
C2 H2 0.9400 . ?
C2 C3 1.388(6) . ?
C3 C4 1.401(6) . ?
C3 C11 1.524(5) . ?
C4 H4 0.9400 . ?
C4 C5 1.378(5) . ?
C5 C6 1.495(5) . ?
C6 C7 1.378(5) . ?
C7 H7 0.9400 . ?
C7 C8 1.400(6) . ?
C8 C9 1.387(6) . ?
C8 C15 1.527(6) . ?
C9 H9 0.9400 . ?
C9 C10 1.376(6) . ?
C10 H10 0.9400 . ?
C11 C12 1.520(7) . ?
C11 C13 1.527(7) . ?
C11 C14 1.517(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 C16 1.521(8) . ?
C15 C17 1.517(7) . ?
C15 C18 1.507(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19 0.9400 . ?
C19 C20 1.342(7) . ?
C20 H20 0.9400 . ?
C21 H21 0.9400 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23 0.9400 . ?
C23 C24 1.349(8) . ?
C24 H24 0.9400 . ?
C25 H25 0.9400 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
P1 F1 1.578(5) . ?
P1 F2 1.571(4) . ?
P1 F3 1.539(5) . ?
P1 F4 1.559(4) . ?
P1 F5 1.600(4) . ?
P1 F6 1.567(5) . ?

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
N2 Re1 N1 74.24(12) . . ?
N3 Re1 N1 85.86(13) . . ?
N3 Re1 N2 85.99(13) . . ?
N3 Re1 N5 171.98(13) . . ?
N5 Re1 N1 87.74(13) . . ?
N5 Re1 N2 87.64(13) . . ?
C27 Re1 N1 97.66(16) . . ?
C27 Re1 N2 171.87(16) . . ?
C27 Re1 N3 92.75(17) . . ?
C27 Re1 N5 92.88(17) . . ?
C28 Re1 N1 174.68(16) . . ?
C28 Re1 N2 100.58(16) . . ?
C28 Re1 N3 92.61(16) . . ?
C28 Re1 N5 93.33(16) . . ?
C28 Re1 C27 87.5(2) . . ?
C1 N1 Re1 124.1(3) . . ?
C1 N1 C5 117.6(3) . . ?
C5 N1 Re1 118.0(3) . . ?
C6 N2 Re1 117.8(3) . . ?
C10 N2 Re1 125.0(3) . . ?
C10 N2 C6 117.3(4) . . ?
C19 N3 Re1 127.7(3) . . ?
C21 N3 Re1 126.8(3) . . ?
C21 N3 C19 105.5(4) . . ?
C20 N4 C22 126.5(5) . . ?
C21 N4 C20 106.7(4) . . ?
C21 N4 C22 126.9(5) . . ?
C23 N5 Re1 127.1(3) . . ?
C25 N5 Re1 127.2(3) . . ?
C25 N5 C23 105.7(4) . . ?
C24 N6 C26 126.6(4) . . ?
C25 N6 C24 107.0(4) . . ?
C25 N6 C26 126.3(4) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(4) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.5(4) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 115.9(4) . . ?
C2 C3 C11 122.2(4) . . ?
C4 C3 C11 121.8(4) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 H4 119.5 . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 C6 114.5(3) . . ?
C4 C5 C6 124.0(3) . . ?
N2 C6 C5 115.0(3) . . ?
N2 C6 C7 121.5(4) . . ?
C7 C6 C5 123.4(3) . . ?
C6 C7 H7 119.4 . . ?
C6 C7 C8 121.2(4) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C15 121.7(4) . . ?
C9 C8 C7 115.8(4) . . ?
C9 C8 C15 122.4(4) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
N2 C10 C9 123.9(4) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
C3 C11 C13 107.2(4) . . ?
C12 C11 C3 112.1(4) . . ?
C12 C11 C13 109.3(5) . . ?
C14 C11 C3 110.6(4) . . ?
C14 C11 C12 109.2(5) . . ?
C14 C11 C13 108.3(5) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C8 108.9(4) . . ?
C17 C15 C8 112.1(4) . . ?
C17 C15 C16 108.0(5) . . ?
C18 C15 C8 108.6(4) . . ?
C18 C15 C16 109.4(5) . . ?
C18 C15 C17 109.8(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 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19 125.6 . . ?
C20 C19 N3 108.8(4) . . ?
C20 C19 H19 125.6 . . ?
N4 C20 H20 126.4 . . ?
C19 C20 N4 107.3(4) . . ?
C19 C20 H20 126.4 . . ?
N3 C21 N4 111.7(4) . . ?
N3 C21 H21 124.1 . . ?
N4 C21 H21 124.1 . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 H23 125.6 . . ?
C24 C23 N5 108.8(5) . . ?
C24 C23 H23 125.6 . . ?
N6 C24 C23 107.1(5) . . ?
N6 C24 H24 126.4 . . ?
C23 C24 H24 126.4 . . ?
N5 C25 N6 111.2(4) . . ?
N5 C25 H25 124.4 . . ?
N6 C25 H25 124.4 . . ?
N6 C26 H26A 109.5 . . ?
N6 C26 H26B 109.5 . . ?
N6 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O1 C27 Re1 178.7(4) . . ?
O2 C28 Re1 178.4(4) . . ?
F1 P1 F5 89.9(3) . . ?
F2 P1 F1 87.0(3) . . ?
F2 P1 F5 88.0(3) . . ?
F3 P1 F1 179.0(3) . . ?
F3 P1 F2 93.1(4) . . ?
F3 P1 F4 90.7(4) . . ?
F3 P1 F5 89.2(3) . . ?
F3 P1 F6 88.3(3) . . ?
F4 P1 F1 89.1(3) . . ?
F4 P1 F2 175.5(3) . . ?
F4 P1 F5 89.7(3) . . ?
F4 P1 F6 92.0(3) . . ?
F6 P1 F1 92.7(3) . . ?
F6 P1 F2 90.5(2) . . ?
F6 P1 F5 177.0(3) . . ?

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 N1 C1 C2 172.0(3) . . . . ?
Re1 N1 C5 C4 -172.5(3) . . . . ?
Re1 N1 C5 C6 8.0(4) . . . . ?
Re1 N2 C6 C5 -0.4(4) . . . . ?
Re1 N2 C6 C7 -178.3(3) . . . . ?
Re1 N2 C10 C9 177.9(3) . . . . ?
Re1 N3 C19 C20 -177.9(3) . . . . ?
Re1 N3 C21 N4 176.8(3) . . . . ?
Re1 N5 C23 C24 -177.4(4) . . . . ?
Re1 N5 C25 N6 177.6(3) . . . . ?
N1 C1 C2 C3 -0.8(7) . . . . ?
N1 C5 C6 N2 -4.9(5) . . . . ?
N1 C5 C6 C7 172.9(4) . . . . ?
N2 C6 C7 C8 0.3(6) . . . . ?
N3 C19 C20 N4 1.3(6) . . . . ?
N5 C23 C24 N6 -0.4(7) . . . . ?
C1 N1 C5 C4 1.6(6) . . . . ?
C1 N1 C5 C6 -177.9(4) . . . . ?
C1 C2 C3 C4 3.3(6) . . . . ?
C1 C2 C3 C11 -173.4(4) . . . . ?
C2 C3 C4 C5 -3.5(6) . . . . ?
C2 C3 C11 C12 -12.1(6) . . . . ?
C2 C3 C11 C13 107.7(5) . . . . ?
C2 C3 C11 C14 -134.3(5) . . . . ?
C3 C4 C5 N1 1.1(6) . . . . ?
C3 C4 C5 C6 -179.6(4) . . . . ?
C4 C3 C11 C12 171.3(5) . . . . ?
C4 C3 C11 C13 -68.8(6) . . . . ?
C4 C3 C11 C14 49.1(6) . . . . ?
C4 C5 C6 N2 175.7(4) . . . . ?
C4 C5 C6 C7 -6.5(6) . . . . ?
C5 N1 C1 C2 -1.7(6) . . . . ?
C5 C6 C7 C8 -177.4(4) . . . . ?
C6 N2 C10 C9 -1.7(6) . . . . ?
C6 C7 C8 C9 -1.7(6) . . . . ?
C6 C7 C8 C15 176.0(4) . . . . ?
C7 C8 C9 C10 1.4(6) . . . . ?
C7 C8 C15 C16 61.6(6) . . . . ?
C7 C8 C15 C17 -178.9(5) . . . . ?
C7 C8 C15 C18 -57.4(6) . . . . ?
C8 C9 C10 N2 0.3(7) . . . . ?
C9 C8 C15 C16 -120.8(5) . . . . ?
C9 C8 C15 C17 -1.4(7) . . . . ?
C9 C8 C15 C18 120.1(6) . . . . ?
C10 N2 C6 C5 179.3(4) . . . . ?
C10 N2 C6 C7 1.4(6) . . . . ?
C11 C3 C4 C5 173.3(4) . . . . ?
C15 C8 C9 C10 -176.3(4) . . . . ?
C19 N3 C21 N4 -0.7(5) . . . . ?
C20 N4 C21 N3 1.5(5) . . . . ?
C21 N3 C19 C20 -0.4(5) . . . . ?
C21 N4 C20 C19 -1.7(6) . . . . ?
C22 N4 C20 C19 177.4(5) . . . . ?
C22 N4 C21 N3 -177.6(5) . . . . ?
C23 N5 C25 N6 -0.1(5) . . . . ?
C24 N6 C25 N5 -0.1(6) . . . . ?
C25 N5 C23 C24 0.4(6) . . . . ?
C25 N6 C24 C23 0.3(7) . . . . ?
C26 N6 C24 C23 178.5(5) . . . . ?
C26 N6 C25 N5 -178.3(4) . . . . ?

_olex2_submission_original_sample_id KS87-2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9548(7)
2 0.0452(7)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks42
_database_code_depnum_ccdc_archive 'CCDC 2056998'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-05-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
''
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H24 Br Cl N2 O2 Re, C H Cl3'
_chemical_formula_sum            'C21 H25 Br Cl4 N2 O2 Re'
_chemical_formula_weight         745.34
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.4068(8)
_cell_length_b                   13.9121(6)
_cell_length_c                   16.1781(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2792.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6740
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      1.93
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.343
_exptl_absorpt_coefficient_mu    6.184
_exptl_absorpt_correction_T_max  0.4015
_exptl_absorpt_correction_T_min  0.2857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, , Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_recrystallization_method 
'recrystallised from a mixture of chloroform and pentane by solvent layering'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10710
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.247
_diffrn_reflns_theta_min         1.931
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1960
_reflns_number_total             2916
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.187
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2916
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0778
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1209P)²+31.6071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2417
_refine_special_details          'chloroform is on a special position (Part -1)'
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl3) = Uanis(Cl2) = Uanis(Cl4)
3. Others
 Fixed Sof: C11(0.5) H11(0.5) Cl2(0.5) Cl3(0.5) Cl4(0.5)
4.a Free rotating group:
 C11(Cl2,Cl3,Cl4)
4.b Ternary CH refined with riding coordinates:
 C11(H11)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.36354(7) 0.250000 0.48545(5) 0.0655(3) Uani 1 2 d S T P . .
Br1 Br 0.5369(3) 0.250000 0.5632(2) 0.1178(10) Uani 1 2 d S T P . .
Cl1 Cl 0.2083(4) 0.250000 0.3967(3) 0.0692(12) Uani 1 2 d S T P . .
O1 O 0.2557(13) 0.3949(13) 0.5982(10) 0.139(6) Uani 1 1 d . . . . .
N1 N 0.4385(9) 0.1555(7) 0.3943(6) 0.062(3) Uani 1 1 d . . . . .
C1 C 0.4386(13) 0.0604(9) 0.4001(9) 0.073(4) Uani 1 1 d . . . . .
H1 H 0.409040 0.032073 0.447717 0.087 Uiso 1 1 calc R U . . .
C2 C 0.4794(11) 0.0017(9) 0.3405(8) 0.066(3) Uani 1 1 d . . . . .
H2 H 0.478533 -0.065358 0.347556 0.080 Uiso 1 1 calc R U . . .
C3 C 0.5227(12) 0.0422(9) 0.2688(8) 0.065(3) Uani 1 1 d . . . . .
C4 C 0.5228(11) 0.1422(8) 0.2655(8) 0.063(3) Uani 1 1 d . . . . .
H4 H 0.551697 0.173312 0.218922 0.075 Uiso 1 1 calc R U . . .
C5 C 0.4828(10) 0.1945(8) 0.3273(8) 0.057(3) Uani 1 1 d . . . . .
C6 C 0.5695(14) -0.0200(9) 0.1993(9) 0.077(4) Uani 1 1 d . . . . .
C7 C 0.5221(16) 0.0148(13) 0.1169(9) 0.103(6) Uani 1 1 d . . . . .
H7A H 0.444579 0.006113 0.117350 0.154 Uiso 1 1 calc R U . . .
H7B H 0.553128 -0.022069 0.071860 0.154 Uiso 1 1 calc R U . . .
H7C H 0.538819 0.082355 0.109308 0.154 Uiso 1 1 calc R U . . .
C8 C 0.6900(17) -0.0088(14) 0.2000(11) 0.105(6) Uani 1 1 d . . . . .
H8A H 0.708588 0.057469 0.187941 0.158 Uiso 1 1 calc R U . . .
H8B H 0.721539 -0.050504 0.158502 0.158 Uiso 1 1 calc R U . . .
H8C H 0.717742 -0.026078 0.254088 0.158 Uiso 1 1 calc R U . . .
C9 C 0.5451(18) -0.1253(10) 0.2108(12) 0.110(7) Uani 1 1 d . . . . .
H9A H 0.574093 -0.146853 0.263293 0.165 Uiso 1 1 calc R U . . .
H9B H 0.577910 -0.161798 0.166274 0.165 Uiso 1 1 calc R U . . .
H9C H 0.467738 -0.135061 0.210084 0.165 Uiso 1 1 calc R U . . .
C10 C 0.2942(15) 0.3482(15) 0.5592(11) 0.090(5) Uani 1 1 d . . . . .
C11 C 0.2744(7) 0.2653(8) 0.0662(5) 0.114(12) Uani 0.5 1 d G . P A -1
H11 H 0.215864 0.232145 0.035928 0.136 Uiso 0.5 1 calc R U P A -1
Cl2 Cl 0.2762(11) 0.2185(7) 0.1689(7) 0.155(3) Uani 0.5 1 d G . P A -1
Cl3 Cl 0.2446(12) 0.3907(8) 0.0656(8) 0.155(3) Uani 0.5 1 d G . P A -1
Cl4 Cl 0.3974(11) 0.2404(13) 0.0134(6) 0.155(3) Uani 0.5 1 d G . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Br1 2.491(4) . ?
Re1 Cl1 2.403(5) . ?
Re1 N1 2.184(10) . ?
Re1 N1 2.184(10) 7_565 ?
Re1 C10 2.01(2) . ?
Re1 C10 2.01(2) 7_565 ?
O1 C10 1.02(2) . ?
N1 C1 1.326(16) . ?
N1 C5 1.332(15) . ?
C1 H1 0.9400 . ?
C1 C2 1.360(18) . ?
C2 H2 0.9400 . ?
C2 C3 1.397(18) . ?
C3 C4 1.392(16) . ?
C3 C6 1.534(18) . ?
C4 H4 0.9400 . ?
C4 C5 1.333(17) . ?
C5 C5 1.54(2) 7_565 ?
C6 C7 1.54(2) . ?
C6 C8 1.50(3) . ?
C6 C9 1.507(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C11 H11 0.9900 . ?
C11 Cl2 1.7832 . ?
C11 Cl3 1.7843 . ?
C11 Cl4 1.7833 . ?

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
Cl1 Re1 Br1 173.63(15) . . ?
N1 Re1 Br1 88.5(3) 7_565 . ?
N1 Re1 Br1 88.5(3) . . ?
N1 Re1 Cl1 86.4(3) . . ?
N1 Re1 Cl1 86.4(3) 7_565 . ?
N1 Re1 N1 74.1(5) . 7_565 ?
C10 Re1 Br1 94.0(5) . . ?
C10 Re1 Br1 94.0(5) 7_565 . ?
C10 Re1 Cl1 90.7(5) 7_565 . ?
C10 Re1 Cl1 90.7(5) . . ?
C10 Re1 N1 173.6(5) . . ?
C10 Re1 N1 100.0(6) . 7_565 ?
C10 Re1 N1 100.0(6) 7_565 . ?
C10 Re1 N1 173.6(5) 7_565 7_565 ?
C10 Re1 C10 85.7(10) 7_565 . ?
C1 N1 Re1 123.6(9) . . ?
C1 N1 C5 117.6(11) . . ?
C5 N1 Re1 118.7(8) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.3(13) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.3(12) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C6 121.8(11) . . ?
C4 C3 C2 115.8(12) . . ?
C4 C3 C6 122.4(12) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.1(12) . . ?
C5 C4 H4 119.4 . . ?
N1 C5 C4 122.8(11) . . ?
N1 C5 C5 114.1(7) . 7_565 ?
C4 C5 C5 123.1(7) . 7_565 ?
C3 C6 C7 108.3(12) . . ?
C8 C6 C3 108.2(13) . . ?
C8 C6 C7 110.7(14) . . ?
C8 C6 C9 107.5(15) . . ?
C9 C6 C3 112.5(13) . . ?
C9 C6 C7 109.6(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 Re1 176(2) . . ?
Cl2 C11 H11 107.5 . . ?
Cl2 C11 Cl3 111.4 . . ?
Cl2 C11 Cl4 111.4 . . ?
Cl3 C11 H11 107.5 . . ?
Cl4 C11 H11 107.5 . . ?
Cl4 C11 Cl3 111.4 . . ?

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 N1 C1 C2 175.7(11) . . . . ?
Re1 N1 C5 C4 -174.7(10) . . . . ?
Re1 N1 C5 C5 4.9(10) . . . 7_565 ?
N1 C1 C2 C3 -1(2) . . . . ?
C1 N1 C5 C4 3(2) . . . . ?
C1 N1 C5 C5 -177.9(10) . . . 7_565 ?
C1 C2 C3 C4 2(2) . . . . ?
C1 C2 C3 C6 -179.8(14) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C2 C3 C6 C7 131.6(16) . . . . ?
C2 C3 C6 C8 -108.3(16) . . . . ?
C2 C3 C6 C9 10(2) . . . . ?
C3 C4 C5 N1 -2(2) . . . . ?
C3 C4 C5 C5 178.9(10) . . . 7_565 ?
C4 C3 C6 C7 -50(2) . . . . ?
C4 C3 C6 C8 70.2(18) . . . . ?
C4 C3 C6 C9 -171.3(16) . . . . ?
C5 N1 C1 C2 -1(2) . . . . ?
C6 C3 C4 C5 -179.2(13) . . . . ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks47
_database_code_depnum_ccdc_archive 'CCDC 2057001'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-05-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
''
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H30 Br N4 O2 Re'
_chemical_formula_sum            'C24 H30 Br N4 O2 Re'
_chemical_formula_weight         672.63
_chemical_melting_point          ?
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'
Br Br -0.6763 1.2805 '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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   14.2929(3)
_cell_length_b                   17.3769(3)
_cell_length_c                   10.1717(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2526.31(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    47432
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.89
_cell_measurement_theta_min      6.70
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.476
_exptl_absorpt_correction_T_max  0.2679
_exptl_absorpt_correction_T_min  0.0792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_recrystallization_method 
'recrystallised from a mixture of ??? and ??? by solvent layering'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0075
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25845
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.380
_diffrn_reflns_theta_min         6.698
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Primux 100 micro'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2323
_reflns_number_total             2383
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00140(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0227
_refine_ls_restrained_S_all      1.116
_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)+(0.0270P)²+6.3734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0574
_refine_special_details          
'tertbutyl group is spiltted and restraints were applied on the two parts'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C8 \\sim C6-C7A
 with sigma of 0.02
 C6-C7 \\sim C6-C9A
 with sigma of 0.02
 C6-C9 \\sim C6-C8A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C8A) = Uanis(C8) = Uanis(C7A) = Uanis(C7) = Uanis(C9A)
4. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: H13A(0.5) H13B(0.5) H13C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C10(H10), C11(H11), C12(H12)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC),
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.48020(2) 0.250000 0.51525(2) 0.02058(10) Uani 1 2 d S T P . .
Br1 Br 0.63786(4) 0.250000 0.64201(6) 0.04694(17) Uani 1 2 d S T P . .
O1 O 0.5358(2) 0.12897(17) 0.3147(3) 0.0506(7) Uani 1 1 d . . . . .
N1 N 0.43309(17) 0.32552(14) 0.6727(2) 0.0218(5) Uani 1 1 d . . . . .
N2 N 0.3383(3) 0.250000 0.4460(4) 0.0237(7) Uani 1 2 d S T P . .
N3 N 0.1850(3) 0.250000 0.4319(4) 0.0304(9) Uani 1 2 d S T P . .
C1 C 0.4384(2) 0.40277(18) 0.6694(3) 0.0283(7) Uani 1 1 d . . . . .
H1 H 0.466164 0.426015 0.596880 0.034 Uiso 1 1 calc R . . . .
C2 C 0.4047(3) 0.44888(18) 0.7682(3) 0.0332(8) Uani 1 1 d . . . . .
H2 H 0.410371 0.502053 0.761693 0.040 Uiso 1 1 calc R . . . .
C3 C 0.3620(3) 0.41661(18) 0.8780(3) 0.0306(7) Uani 1 1 d . . . . .
C4 C 0.3599(2) 0.33653(18) 0.8830(3) 0.0251(6) Uani 1 1 d . . . . .
H4 H 0.333944 0.312168 0.955824 0.030 Uiso 1 1 calc R . . . .
C5 C 0.3957(2) 0.29269(16) 0.7812(3) 0.0207(6) Uani 1 1 d . . . . .
C6 C 0.3178(4) 0.4657(2) 0.9867(4) 0.0482(11) Uani 1 1 d D . . . .
C7 C 0.2085(8) 0.4559(5) 0.9670(8) 0.092(2) Uani 0.716(7) 1 d D . . A 1
H7A H 0.190665 0.477033 0.883457 0.138 Uiso 0.716(7) 1 calc GR . . A 1
H7B H 0.176016 0.482582 1.035903 0.138 Uiso 0.716(7) 1 calc GR . . A 1
H7C H 0.192625 0.402273 0.969677 0.138 Uiso 0.716(7) 1 calc GR . . A 1
C7A C 0.2446(17) 0.5157(12) 0.9266(19) 0.092(2) Uani 0.284(7) 1 d D . . A 2
H7AA H 0.271640 0.544953 0.856124 0.138 Uiso 0.284(7) 1 calc GR . . A 2
H7AB H 0.220290 0.550086 0.992028 0.138 Uiso 0.284(7) 1 calc GR . . A 2
H7AC H 0.194910 0.484202 0.892966 0.138 Uiso 0.284(7) 1 calc GR . . A 2
C8 C 0.3383(9) 0.5498(5) 0.9741(9) 0.092(2) Uani 0.716(7) 1 d D . . A 1
H8A H 0.404818 0.557452 0.970811 0.138 Uiso 0.716(7) 1 calc GR . . A 1
H8B H 0.312957 0.576629 1.048390 0.138 Uiso 0.716(7) 1 calc GR . . A 1
H8C H 0.310449 0.569134 0.894842 0.138 Uiso 0.716(7) 1 calc GR . . A 1
C8A C 0.3913(16) 0.5197(12) 1.045(2) 0.092(2) Uani 0.284(7) 1 d D . . A 2
H8AA H 0.434685 0.490642 1.096820 0.138 Uiso 0.284(7) 1 calc GR . . A 2
H8AB H 0.361043 0.557487 1.099025 0.138 Uiso 0.284(7) 1 calc GR . . A 2
H8AC H 0.424222 0.545101 0.974830 0.138 Uiso 0.284(7) 1 calc GR . . A 2
C9 C 0.3449(9) 0.4348(5) 1.1185(8) 0.092(2) Uani 0.716(7) 1 d D . . A 1
H9A H 0.319280 0.384134 1.129276 0.138 Uiso 0.716(7) 1 calc GR . . A 1
H9B H 0.320843 0.468024 1.185926 0.138 Uiso 0.716(7) 1 calc GR . . A 1
H9C H 0.411805 0.432510 1.124808 0.138 Uiso 0.716(7) 1 calc GR . . A 1
C9A C 0.278(2) 0.4175(11) 1.106(2) 0.092(2) Uani 0.284(7) 1 d D . . A 2
H9AA H 0.224620 0.388733 1.078383 0.138 Uiso 0.284(7) 1 calc GR . . A 2
H9AB H 0.261028 0.451724 1.176137 0.138 Uiso 0.284(7) 1 calc GR . . A 2
H9AC H 0.325802 0.382628 1.136949 0.138 Uiso 0.284(7) 1 calc GR . . A 2
C10 C 0.2594(3) 0.250000 0.5132(5) 0.0272(10) Uani 1 2 d S T P . .
H10 H 0.255616 0.250000 0.604452 0.033 Uiso 1 2 calc RS T P . .
C11 C 0.2179(4) 0.250000 0.3060(5) 0.0396(12) Uani 1 2 d S T P . .
H11 H 0.182687 0.250000 0.229106 0.047 Uiso 1 2 calc RS T P . .
C12 C 0.3114(4) 0.250000 0.3159(5) 0.0375(12) Uani 1 2 d S T P . .
H12 H 0.352428 0.250000 0.244877 0.045 Uiso 1 2 calc RS T P . .
C13 C 0.0866(4) 0.250000 0.4715(6) 0.0427(13) Uani 1 2 d S T P . .
H13A H 0.081648 0.233352 0.561217 0.064 Uiso 0.5 1 calc GR . . B -1
H13B H 0.052030 0.215582 0.415959 0.064 Uiso 0.5 1 calc GR . . B -1
H13C H 0.061686 0.301066 0.463314 0.064 Uiso 0.5 1 calc GR . . B -1
C14 C 0.5157(2) 0.1745(2) 0.3908(4) 0.0322(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Br1 2.5963(6) . ?
Re1 N1 2.177(2) 7_565 ?
Re1 N1 2.177(2) . ?
Re1 N2 2.147(4) . ?
Re1 C14 1.892(4) . ?
Re1 C14 1.892(4) 7_565 ?
O1 C14 1.143(5) . ?
N1 C1 1.345(4) . ?
N1 C5 1.353(4) . ?
N2 C10 1.318(6) . ?
N2 C12 1.378(6) . ?
N3 C10 1.347(6) . ?
N3 C11 1.364(7) . ?
N3 C13 1.462(7) . ?
C1 H1 0.9300 . ?
C1 C2 1.373(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(5) . ?
C3 C4 1.393(4) . ?
C3 C6 1.532(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.384(4) . ?
C5 C5 1.484(6) 7_565 ?
C6 C7 1.584(12) . ?
C6 C7A 1.491(17) . ?
C6 C8 1.496(10) . ?
C6 C8A 1.528(18) . ?
C6 C9 1.494(10) . ?
C6 C9A 1.580(17) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7A H7AA 0.9600 . ?
C7A H7AB 0.9600 . ?
C7A H7AC 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9600 . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.340(8) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

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 Br1 84.44(7) . . ?
N1 Re1 Br1 84.45(7) 7_565 . ?
N1 Re1 N1 74.15(13) . 7_565 ?
N2 Re1 Br1 169.38(10) . . ?
N2 Re1 N1 87.08(10) . . ?
N2 Re1 N1 87.08(10) . 7_565 ?
C14 Re1 Br1 95.70(10) 7_565 . ?
C14 Re1 Br1 95.69(10) . . ?
C14 Re1 N1 173.13(12) . . ?
C14 Re1 N1 173.13(12) 7_565 7_565 ?
C14 Re1 N1 99.02(12) . 7_565 ?
C14 Re1 N1 99.02(12) 7_565 . ?
C14 Re1 N2 91.95(12) 7_565 . ?
C14 Re1 N2 91.95(12) . . ?
C14 Re1 C14 87.8(2) . 7_565 ?
C1 N1 Re1 124.5(2) . . ?
C1 N1 C5 117.6(3) . . ?
C5 N1 Re1 117.92(19) . . ?
C10 N2 Re1 129.6(3) . . ?
C10 N2 C12 105.1(4) . . ?
C12 N2 Re1 125.3(3) . . ?
C10 N3 C11 107.7(4) . . ?
C10 N3 C13 126.1(4) . . ?
C11 N3 C13 126.2(4) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.0(3) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.4(3) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 116.2(3) . . ?
C2 C3 C6 122.4(3) . . ?
C4 C3 C6 121.3(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.0(3) . . ?
C5 C4 H4 119.5 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C5 114.95(16) . 7_565 ?
C4 C5 C5 123.41(18) . 7_565 ?
C3 C6 C7 104.9(4) . . ?
C3 C6 C9A 114.0(7) . . ?
C7A C6 C3 108.5(8) . . ?
C7A C6 C8A 106.4(13) . . ?
C7A C6 C9A 112.0(15) . . ?
C8 C6 C3 113.6(4) . . ?
C8 C6 C7 106.7(6) . . ?
C8A C6 C3 109.7(8) . . ?
C8A C6 C9A 105.9(14) . . ?
C9 C6 C3 109.9(4) . . ?
C9 C6 C7 109.3(6) . . ?
C9 C6 C8 112.1(6) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C7A H7AA 109.5 . . ?
C6 C7A H7AB 109.5 . . ?
C6 C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C8A H8AA 109.5 . . ?
C6 C8A H8AB 109.5 . . ?
C6 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C9A H9AA 109.5 . . ?
C6 C9A H9AB 109.5 . . ?
C6 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
N2 C10 N3 110.9(4) . . ?
N2 C10 H10 124.5 . . ?
N3 C10 H10 124.5 . . ?
N3 C11 H11 127.1 . . ?
C12 C11 N3 105.9(4) . . ?
C12 C11 H11 127.1 . . ?
N2 C12 H12 124.8 . . ?
C11 C12 N2 110.5(5) . . ?
C11 C12 H12 124.8 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 Re1 178.9(3) . . ?

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 N1 C1 C2 177.4(3) . . . . ?
Re1 N1 C5 C4 -176.8(2) . . . . ?
Re1 N1 C5 C5 2.7(2) . . . 7_565 ?
Re1 N2 C10 N3 180.000(0) . . . . ?
Re1 N2 C12 C11 180.000(0) . . . . ?
N1 C1 C2 C3 -0.4(6) . . . . ?
N3 C11 C12 N2 0.000(1) . . . . ?
C1 N1 C5 C4 3.0(4) . . . . ?
C1 N1 C5 C5 -177.4(2) . . . 7_565 ?
C1 C2 C3 C4 2.7(5) . . . . ?
C1 C2 C3 C6 -176.0(4) . . . . ?
C2 C3 C4 C5 -2.1(5) . . . . ?
C2 C3 C6 C7 106.8(5) . . . . ?
C2 C3 C6 C7A 57.7(12) . . . . ?
C2 C3 C6 C8 -9.3(8) . . . . ?
C2 C3 C6 C8A -58.1(11) . . . . ?
C2 C3 C6 C9 -135.8(6) . . . . ?
C2 C3 C6 C9A -176.7(14) . . . . ?
C3 C4 C5 N1 -0.8(5) . . . . ?
C3 C4 C5 C5 179.7(2) . . . 7_565 ?
C4 C3 C6 C7 -71.8(5) . . . . ?
C4 C3 C6 C7A -120.9(12) . . . . ?
C4 C3 C6 C8 172.1(6) . . . . ?
C4 C3 C6 C8A 123.2(11) . . . . ?
C4 C3 C6 C9 45.5(7) . . . . ?
C4 C3 C6 C9A 4.7(15) . . . . ?
C5 N1 C1 C2 -2.5(5) . . . . ?
C6 C3 C4 C5 176.6(3) . . . . ?
C10 N2 C12 C11 0.000(0) . . . . ?
C10 N3 C11 C12 0.000(1) . . . . ?
C11 N3 C10 N2 0.000(1) . . . . ?
C12 N2 C10 N3 0.000(1) . . . . ?
C13 N3 C10 N2 180.000(1) . . . . ?
C13 N3 C11 C12 180.000(0) . . . . ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks46-1_sq
_database_code_depnum_ccdc_archive 'CCDC 2056999'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-05-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
''
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H29 Br N3 O2 Re'
_chemical_formula_sum            'C25 H29 Br N3 O2 Re'
_chemical_formula_weight         669.62
_chemical_melting_point          ?
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'
Br Br -0.6763 1.2805 '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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   13.5302(2)
_cell_length_b                   34.6388(7)
_cell_length_c                   15.2486(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7146.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    72577
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.57
_cell_measurement_theta_min      4.55
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.132
_exptl_absorpt_coefficient_mu    8.104
_exptl_absorpt_correction_T_max  0.4878
_exptl_absorpt_correction_T_min  0.0390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2608
_exptl_crystal_recrystallization_method 
'recrystallised from a mixture of chloroform and pentane by solvent layering'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42653
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.204
_diffrn_reflns_theta_min         6.787
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Primux 100 micro'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3029
_reflns_number_total             3229
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0439
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0832P)²+13.7639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1329
_refine_special_details          
'solvent were squeezed and tert-butyl group splitted, restraints were applied to the different parts.'
_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. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C9) = Uanis(C7) = Uanis(C8) = Uanis(C7A) = Uanis(C8A) =
Uanis(C9A)
3. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C10(H10), C11(H11), C12(H12)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC),
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.500000 0.68567(2) 0.28720(2) 0.06752(17) Uani 1 2 d S T P . .
Br1 Br 0.500000 0.62446(2) 0.18915(6) 0.0826(3) Uani 1 2 d S T P . .
O1 O 0.3422(3) 0.72583(12) 0.1782(3) 0.0892(11) Uani 1 1 d . . . . .
N1 N 0.5967(3) 0.65272(12) 0.3734(3) 0.0702(10) Uani 1 1 d . . . . .
N2 N 0.500000 0.7310(2) 0.3826(4) 0.0775(15) Uani 1 2 d S T P . .
C1 C 0.6957(4) 0.65323(17) 0.3712(4) 0.0793(13) Uani 1 1 d . . . . .
H1 H 0.726815 0.670025 0.330461 0.095 Uiso 1 1 calc R U . . .
C2 C 0.7538(4) 0.63155(17) 0.4229(4) 0.0817(14) Uani 1 1 d . . . . .
H2 H 0.823614 0.633339 0.417570 0.098 Uiso 1 1 calc R U . . .
C3 C 0.7131(5) 0.60672(18) 0.4836(4) 0.0845(14) Uani 1 1 d . . . . .
C4 C 0.6120(4) 0.60518(18) 0.4870(4) 0.0803(14) Uani 1 1 d . . . . .
H4 H 0.580859 0.588180 0.527386 0.096 Uiso 1 1 calc R U . . .
C5 C 0.5532(4) 0.62835(16) 0.4318(4) 0.0749(12) Uani 1 1 d . . . . .
C6 C 0.7791(5) 0.5811(2) 0.5425(5) 0.1054(14) Uani 1 1 d . . . . .
C7 C 0.8402(11) 0.6076(4) 0.6044(11) 0.1054(14) Uani 0.620(19) 1 d . . P A 1
H7A H 0.864959 0.629806 0.571253 0.158 Uiso 0.620(19) 1 calc R U P A 1
H7B H 0.896011 0.593014 0.628441 0.158 Uiso 0.620(19) 1 calc R U P A 1
H7C H 0.797993 0.616621 0.652412 0.158 Uiso 0.620(19) 1 calc R U P A 1
C7A C 0.7260(16) 0.5684(8) 0.6266(17) 0.1054(14) Uani 0.380(19) 1 d . . P A 2
H7AA H 0.704360 0.591273 0.659227 0.158 Uiso 0.380(19) 1 calc R U P A 2
H7AB H 0.771287 0.553215 0.662947 0.158 Uiso 0.380(19) 1 calc R U P A 2
H7AC H 0.668316 0.552651 0.611325 0.158 Uiso 0.380(19) 1 calc R U P A 2
C8 C 0.8346(11) 0.5538(4) 0.4721(10) 0.1054(14) Uani 0.620(19) 1 d . . P A 1
H8A H 0.786138 0.543437 0.430481 0.158 Uiso 0.620(19) 1 calc R U P A 1
H8B H 0.867038 0.532398 0.502819 0.158 Uiso 0.620(19) 1 calc R U P A 1
H8C H 0.884178 0.568915 0.440351 0.158 Uiso 0.620(19) 1 calc R U P A 1
C8A C 0.8696(19) 0.6087(7) 0.5693(18) 0.1054(14) Uani 0.380(19) 1 d . . P A 2
H8AA H 0.911462 0.613269 0.517901 0.158 Uiso 0.380(19) 1 calc R U P A 2
H8AB H 0.908804 0.596206 0.615401 0.158 Uiso 0.380(19) 1 calc R U P A 2
H8AC H 0.843904 0.633311 0.591033 0.158 Uiso 0.380(19) 1 calc R U P A 2
C9 C 0.7190(10) 0.5520(5) 0.5972(10) 0.1054(14) Uani 0.620(19) 1 d . . P A 1
H9A H 0.678044 0.566014 0.639628 0.158 Uiso 0.620(19) 1 calc R U P A 1
H9B H 0.764274 0.534768 0.628565 0.158 Uiso 0.620(19) 1 calc R U P A 1
H9C H 0.676522 0.536793 0.558347 0.158 Uiso 0.620(19) 1 calc R U P A 1
C9A C 0.8535(17) 0.5573(8) 0.5009(17) 0.1054(14) Uani 0.380(19) 1 d . . P A 2
H9AA H 0.821280 0.536555 0.467783 0.158 Uiso 0.380(19) 1 calc R U P A 2
H9AB H 0.896564 0.546058 0.545797 0.158 Uiso 0.380(19) 1 calc R U P A 2
H9AC H 0.893018 0.573161 0.460860 0.158 Uiso 0.380(19) 1 calc R U P A 2
C10 C 0.5843(5) 0.74663(18) 0.4125(4) 0.0905(16) Uani 1 1 d . . . . .
H10 H 0.644930 0.736482 0.391266 0.109 Uiso 1 1 calc R U . . .
C11 C 0.5883(6) 0.7763(2) 0.4718(4) 0.103(2) Uani 1 1 d . . . . .
H11 H 0.650076 0.786009 0.491446 0.124 Uiso 1 1 calc R U . . .
C12 C 0.500000 0.7919(4) 0.5029(7) 0.115(3) Uani 1 2 d S T P . .
H12 H 0.500000 0.812603 0.543926 0.138 Uiso 1 2 calc R U P . .
C13 C 0.4028(4) 0.71100(17) 0.2194(3) 0.0747(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Br1 2.5944(9) . ?
Re1 N1 2.178(4) 12_655 ?
Re1 N1 2.178(4) . ?
Re1 N2 2.140(7) . ?
Re1 C13 1.889(6) . ?
Re1 C13 1.889(6) 12_655 ?
O1 C13 1.154(7) . ?
N1 C1 1.341(7) . ?
N1 C5 1.360(7) . ?
N2 C10 1.342(8) . ?
N2 C10 1.342(8) 12_655 ?
C1 H1 0.9500 . ?
C1 C2 1.343(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.379(8) . ?
C3 C4 1.371(9) . ?
C3 C6 1.546(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.409(8) . ?
C5 C5 1.441(11) 12_655 ?
C6 C7 1.555(16) . ?
C6 C7A 1.53(2) . ?
C6 C8 1.615(18) . ?
C6 C8A 1.61(3) . ?
C6 C9 1.539(16) . ?
C6 C9A 1.45(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.370(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(9) . ?
C12 H12 0.9500 . ?

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 Br1 85.39(11) . . ?
N1 Re1 Br1 85.39(11) 12_655 . ?
N1 Re1 N1 73.8(2) . 12_655 ?
N2 Re1 Br1 172.38(18) . . ?
N2 Re1 N1 88.52(18) . . ?
N2 Re1 N1 88.52(18) . 12_655 ?
C13 Re1 Br1 93.68(16) . . ?
C13 Re1 Br1 93.68(16) 12_655 . ?
C13 Re1 N1 98.96(19) . 12_655 ?
C13 Re1 N1 172.8(2) 12_655 12_655 ?
C13 Re1 N1 98.96(19) 12_655 . ?
C13 Re1 N1 172.77(19) . . ?
C13 Re1 N2 91.8(2) . . ?
C13 Re1 N2 91.8(2) 12_655 . ?
C13 Re1 C13 88.2(3) . 12_655 ?
C1 N1 Re1 125.3(4) . . ?
C1 N1 C5 117.1(5) . . ?
C5 N1 Re1 117.5(3) . . ?
C10 N2 Re1 121.8(4) 12_655 . ?
C10 N2 Re1 121.8(4) . . ?
C10 N2 C10 116.3(7) 12_655 . ?
N1 C1 H1 117.9 . . ?
N1 C1 C2 124.3(5) . . ?
C2 C1 H1 117.9 . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.6(5) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C6 121.2(6) . . ?
C4 C3 C2 116.6(5) . . ?
C4 C3 C6 122.2(6) . . ?
C3 C4 H4 119.4 . . ?
C3 C4 C5 121.2(5) . . ?
C5 C4 H4 119.4 . . ?
N1 C5 C4 120.1(5) . . ?
N1 C5 C5 115.6(3) . 12_655 ?
C4 C5 C5 124.3(3) . 12_655 ?
C3 C6 C7 108.6(8) . . ?
C3 C6 C8 102.7(7) . . ?
C3 C6 C8A 104.3(9) . . ?
C7 C6 C8 120.1(11) . . ?
C7A C6 C3 112.3(10) . . ?
C7A C6 C8A 108.3(12) . . ?
C9 C6 C3 112.7(7) . . ?
C9 C6 C7 109.7(8) . . ?
C9 C6 C8 102.9(11) . . ?
C9A C6 C3 118.3(11) . . ?
C9A C6 C7A 122.0(14) . . ?
C9A C6 C8A 85.4(17) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C7A H7AA 109.5 . . ?
C6 C7A H7AB 109.5 . . ?
C6 C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C8A H8AA 109.5 . . ?
C6 C8A H8AB 109.5 . . ?
C6 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C9A H9AA 109.5 . . ?
C6 C9A H9AB 109.5 . . ?
C6 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
N2 C10 H10 117.9 . . ?
N2 C10 C11 124.1(7) . . ?
C11 C10 H10 117.9 . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.8(8) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C11 117.8(10) . 12_655 ?
C11 C12 H12 121.1 12_655 . ?
C11 C12 H12 121.1 . . ?
O1 C13 Re1 178.6(5) . . ?

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 N1 C1 C2 -177.4(4) . . . . ?
Re1 N1 C5 C4 177.6(4) . . . . ?
Re1 N1 C5 C5 -2.3(4) . . . 12_655 ?
Re1 N2 C10 C11 178.3(5) . . . . ?
N1 C1 C2 C3 -0.2(10) . . . . ?
N2 C10 C11 C12 -0.9(11) . . . . ?
C1 N1 C5 C4 0.4(8) . . . . ?
C1 N1 C5 C5 -179.5(4) . . . 12_655 ?
C1 C2 C3 C4 0.9(10) . . . . ?
C1 C2 C3 C6 178.9(6) . . . . ?
C2 C3 C4 C5 -0.9(10) . . . . ?
C2 C3 C6 C7 65.3(11) . . . . ?
C2 C3 C6 C7A 157.4(13) . . . . ?
C2 C3 C6 C8 -62.9(10) . . . . ?
C2 C3 C6 C8A 40.4(14) . . . . ?
C2 C3 C6 C9 -172.9(10) . . . . ?
C2 C3 C6 C9A -52.1(15) . . . . ?
C3 C4 C5 N1 0.3(9) . . . . ?
C3 C4 C5 C5 -179.9(5) . . . 12_655 ?
C4 C3 C6 C7 -116.7(10) . . . . ?
C4 C3 C6 C7A -24.7(16) . . . . ?
C4 C3 C6 C8 115.1(9) . . . . ?
C4 C3 C6 C8A -141.7(13) . . . . ?
C4 C3 C6 C9 5.1(14) . . . . ?
C4 C3 C6 C9A 125.9(14) . . . . ?
C5 N1 C1 C2 -0.4(9) . . . . ?
C6 C3 C4 C5 -178.9(6) . . . . ?
C10 N2 C10 C11 1.4(12) 12_655 . . . ?
C10 C11 C12 C11 0.2(15) . . . 12_655 ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.098 0.000 0.329 1355 316 '6 CHCl3'
2 -0.090 0.500 0.101 1355 316 '6 CHCl3'

_platon_squeeze_void_probe_radius 1.20
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks67-3
_database_code_depnum_ccdc_archive 'CCDC 2057002'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-02-21
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
kevin.schindler@unifr.ch
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H39 Br N2 O2 P Re'
_chemical_formula_sum            'C38 H39 Br N2 O2 P Re'
_chemical_formula_weight         852.79
_chemical_melting_point          ?
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'
Br Br -0.6763 1.2805 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.8689(3)
_cell_length_b                   13.4662(2)
_cell_length_c                   28.4268(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7223.0(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    115397
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.27
_cell_measurement_theta_min      6.17
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.559
_exptl_absorpt_correction_T_max  0.3682
_exptl_absorpt_correction_T_min  0.1239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3376
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of DCM and pentane  by solvent layering'
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            94678
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.998
_diffrn_reflns_theta_min         6.174
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Primux 100 micro'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6107
_reflns_number_total             6632
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6632
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0204
_refine_ls_restrained_S_all      1.036
_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)+(0.0296P)²+6.6998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0528
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16A-C15A
 2.6 with sigma of 0.01
 C16A-C14A
 2.6 with sigma of 0.01
3. Rigid bond restraints
 C18, C18A, C19, C19A, C20, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14, C14A, C15, C15A, C16, C16A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20 \\sim C20A: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
5. Others
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C11(H11), C12(H12), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
6.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15(H15A,H15B,H15C), C15A(H15D,
 H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C18(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,
 H20C), C20A(H20D,H20E,H20F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.37421(2) 0.55665(2) 0.38213(2) 0.02798(5) Uani 1 1 d . . . . .
Br1 Br 0.31804(2) 0.71802(2) 0.41768(2) 0.04125(7) Uani 1 1 d . . . . .
P1 P 0.42416(3) 0.40582(4) 0.35862(2) 0.02833(12) Uani 1 1 d . . . . .
O1 O 0.40253(11) 0.64042(17) 0.28406(7) 0.0546(5) Uani 1 1 d . . . . .
O2 O 0.51801(10) 0.63271(17) 0.41537(7) 0.0533(5) Uani 1 1 d . . . . .
N1 N 0.33398(10) 0.49365(15) 0.44742(7) 0.0304(4) Uani 1 1 d . . . . .
N2 N 0.26404(10) 0.51973(14) 0.36833(7) 0.0289(4) Uani 1 1 d . . . . .
C1 C 0.39328(13) 0.60998(19) 0.32161(10) 0.0366(5) Uani 1 1 d . . . . .
C2 C 0.46404(13) 0.60145(19) 0.40255(9) 0.0361(5) Uani 1 1 d . . . . .
C3 C 0.37176(13) 0.4798(2) 0.48704(9) 0.0377(6) Uani 1 1 d . . . . .
H3 H 0.418995 0.499512 0.487274 0.045 Uiso 1 1 calc R U . . .
C4 C 0.34433(15) 0.4383(2) 0.52696(9) 0.0438(7) Uani 1 1 d . . . . .
H4 H 0.372670 0.431659 0.553541 0.053 Uiso 1 1 calc R U . . .
C5 C 0.27436(14) 0.4059(2) 0.52815(9) 0.0433(6) Uani 1 1 d . . . . .
C6 C 0.23487(13) 0.4222(2) 0.48771(9) 0.0372(5) Uani 1 1 d . . . . .
H6 H 0.187491 0.403200 0.486934 0.045 Uiso 1 1 calc R U . . .
C7 C 0.26493(12) 0.46632(18) 0.44848(8) 0.0309(5) Uani 1 1 d . . . . .
C8 C 0.22469(12) 0.48567(17) 0.40487(8) 0.0292(5) Uani 1 1 d . . . . .
C9 C 0.15266(13) 0.47003(18) 0.40086(9) 0.0325(5) Uani 1 1 d . . . . .
H9 H 0.127609 0.446388 0.426715 0.039 Uiso 1 1 calc R U . . .
C10 C 0.11670(13) 0.48869(18) 0.35925(9) 0.0344(5) Uani 1 1 d . . . . .
C11 C 0.15803(14) 0.5237(2) 0.32211(9) 0.0373(5) Uani 1 1 d . . . . .
H11 H 0.136974 0.537886 0.293311 0.045 Uiso 1 1 calc R U . . .
C12 C 0.22976(13) 0.53728(19) 0.32783(9) 0.0352(5) Uani 1 1 d . . . . .
H12 H 0.255897 0.559865 0.302240 0.042 Uiso 1 1 calc R U . . .
C13 C 0.24295(17) 0.3545(3) 0.57143(10) 0.0628(9) Uani 1 1 d . . . . .
C14 C 0.2940(3) 0.2804(6) 0.5910(2) 0.0933(14) Uani 0.783(5) 1 d . U P A 1
H14A H 0.304169 0.230996 0.567626 0.140 Uiso 0.783(5) 1 calc R U P A 1
H14B H 0.273624 0.249198 0.618181 0.140 Uiso 0.783(5) 1 calc R U P A 1
H14C H 0.337106 0.313507 0.599806 0.140 Uiso 0.783(5) 1 calc R U P A 1
C14A C 0.2920(10) 0.338(2) 0.6115(7) 0.0924(15) Uani 0.217(5) 1 d D U P A 2
H14D H 0.333280 0.303002 0.600580 0.139 Uiso 0.217(5) 1 calc R U P A 2
H14E H 0.268553 0.298732 0.635095 0.139 Uiso 0.217(5) 1 calc R U P A 2
H14F H 0.305764 0.400436 0.624608 0.139 Uiso 0.217(5) 1 calc R U P A 2
C15 C 0.1718(3) 0.3108(5) 0.56248(18) 0.0882(14) Uani 0.783(5) 1 d . U P A 1
H15A H 0.140570 0.361365 0.550784 0.132 Uiso 0.783(5) 1 calc R U P A 1
H15B H 0.153121 0.284283 0.591263 0.132 Uiso 0.783(5) 1 calc R U P A 1
H15C H 0.175875 0.258646 0.539633 0.132 Uiso 0.783(5) 1 calc R U P A 1
C15A C 0.2256(11) 0.2318(14) 0.5526(6) 0.0910(15) Uani 0.217(5) 1 d D U P A 2
H15D H 0.197177 0.233430 0.524573 0.136 Uiso 0.217(5) 1 calc R U P A 2
H15E H 0.200587 0.196701 0.576855 0.136 Uiso 0.217(5) 1 calc R U P A 2
H15F H 0.269524 0.198595 0.546088 0.136 Uiso 0.217(5) 1 calc R U P A 2
C16 C 0.2341(4) 0.4377(5) 0.61045(18) 0.0924(14) Uani 0.783(5) 1 d . U P A 1
H16A H 0.279893 0.462632 0.619179 0.139 Uiso 0.783(5) 1 calc R U P A 1
H16B H 0.211246 0.409801 0.637583 0.139 Uiso 0.783(5) 1 calc R U P A 1
H16C H 0.205756 0.490956 0.598212 0.139 Uiso 0.783(5) 1 calc R U P A 1
C16A C 0.1685(9) 0.3952(16) 0.5809(6) 0.0908(15) Uani 0.217(5) 1 d D U P A 2
H16D H 0.170882 0.465881 0.585184 0.136 Uiso 0.217(5) 1 calc R U P A 2
H16E H 0.149598 0.365006 0.608810 0.136 Uiso 0.217(5) 1 calc R U P A 2
H16F H 0.138243 0.380376 0.554667 0.136 Uiso 0.217(5) 1 calc R U P A 2
C17 C 0.03759(14) 0.4684(2) 0.35421(10) 0.0425(6) Uani 1 1 d . . . . .
C18 C 0.0233(3) 0.3611(5) 0.3556(2) 0.0639(11) Uani 0.630(4) 1 d . U P B 3
H18A H 0.047290 0.329125 0.329991 0.096 Uiso 0.630(4) 1 calc R U P B 3
H18B H -0.026807 0.349883 0.352917 0.096 Uiso 0.630(4) 1 calc R U P B 3
H18C H 0.039982 0.334251 0.384872 0.096 Uiso 0.630(4) 1 calc R U P B 3
C18A C 0.0373(5) 0.3643(8) 0.3244(4) 0.0624(14) Uani 0.370(4) 1 d . U P B 4
H18D H 0.057427 0.375489 0.293788 0.094 Uiso 0.370(4) 1 calc R U P B 4
H18E H -0.010475 0.340971 0.321036 0.094 Uiso 0.370(4) 1 calc R U P B 4
H18F H 0.064936 0.315411 0.340761 0.094 Uiso 0.370(4) 1 calc R U P B 4
C19 C -0.0027(3) 0.5200(5) 0.3960(2) 0.0607(10) Uani 0.630(4) 1 d . U P B 3
H19A H 0.011825 0.490725 0.425211 0.091 Uiso 0.630(4) 1 calc R U P B 3
H19B H -0.052869 0.511229 0.392001 0.091 Uiso 0.630(4) 1 calc R U P B 3
H19C H 0.008216 0.589632 0.396224 0.091 Uiso 0.630(4) 1 calc R U P B 3
C19A C 0.0040(5) 0.4368(8) 0.4007(4) 0.0620(11) Uani 0.370(4) 1 d . U P B 4
H19D H 0.026847 0.377702 0.411948 0.093 Uiso 0.370(4) 1 calc R U P B 4
H19E H -0.045514 0.423861 0.395944 0.093 Uiso 0.370(4) 1 calc R U P B 4
H19F H 0.009554 0.488973 0.423399 0.093 Uiso 0.370(4) 1 calc R U P B 4
C20 C 0.0029(5) 0.5453(9) 0.3295(4) 0.0607(11) Uani 0.370(4) 1 d . U P B 4
H20A H -0.003613 0.601249 0.349955 0.091 Uiso 0.370(4) 1 calc R U P B 4
H20B H -0.042427 0.522177 0.318739 0.091 Uiso 0.370(4) 1 calc R U P B 4
H20C H 0.031163 0.564717 0.302956 0.091 Uiso 0.370(4) 1 calc R U P B 4
C20A C 0.0057(3) 0.5152(5) 0.3084(2) 0.0553(11) Uani 0.630(4) 1 d . U P B 3
H20D H 0.016194 0.584901 0.307635 0.083 Uiso 0.630(4) 1 calc R U P B 3
H20E H -0.044710 0.505726 0.308149 0.083 Uiso 0.630(4) 1 calc R U P B 3
H20F H 0.026147 0.483523 0.281343 0.083 Uiso 0.630(4) 1 calc R U P B 3
C21 C 0.37557(12) 0.33698(18) 0.31306(9) 0.0315(5) Uani 1 1 d . . . . .
C22 C 0.30398(13) 0.31444(18) 0.32004(9) 0.0353(5) Uani 1 1 d . . . . .
H22 H 0.282613 0.330749 0.348487 0.042 Uiso 1 1 calc R U . . .
C23 C 0.26447(14) 0.26844(19) 0.28546(10) 0.0404(6) Uani 1 1 d . . . . .
H23 H 0.216980 0.253916 0.290874 0.048 Uiso 1 1 calc R U . . .
C24 C 0.29491(15) 0.2440(2) 0.24305(10) 0.0454(6) Uani 1 1 d . . . . .
H24 H 0.268183 0.212838 0.219848 0.054 Uiso 1 1 calc R U . . .
C25 C 0.36507(16) 0.2658(2) 0.23516(10) 0.0488(7) Uani 1 1 d . . . . .
H25 H 0.385721 0.249329 0.206493 0.059 Uiso 1 1 calc R U . . .
C26 C 0.40548(15) 0.3123(2) 0.26972(9) 0.0426(6) Uani 1 1 d . . . . .
H26 H 0.452820 0.326974 0.263867 0.051 Uiso 1 1 calc R U . . .
C27 C 0.51482(12) 0.40675(19) 0.33481(8) 0.0329(5) Uani 1 1 d . . . . .
C28 C 0.55112(14) 0.3172(2) 0.32945(10) 0.0420(6) Uani 1 1 d . . . . .
H28 H 0.529217 0.258104 0.338106 0.050 Uiso 1 1 calc R U . . .
C29 C 0.61906(14) 0.3151(2) 0.31150(11) 0.0484(7) Uani 1 1 d . . . . .
H29 H 0.641995 0.254614 0.307297 0.058 Uiso 1 1 calc R U . . .
C30 C 0.65313(14) 0.4024(2) 0.29974(10) 0.0471(7) Uani 1 1 d . . . . .
H30 H 0.699397 0.401156 0.288472 0.056 Uiso 1 1 calc R U . . .
C31 C 0.61795(14) 0.4912(2) 0.30486(10) 0.0429(6) Uani 1 1 d . . . . .
H31 H 0.640567 0.550242 0.296907 0.051 Uiso 1 1 calc R U . . .
C32 C 0.54882(13) 0.49350(19) 0.32184(9) 0.0356(5) Uani 1 1 d . . . . .
H32 H 0.525259 0.553907 0.324494 0.043 Uiso 1 1 calc R U . . .
C33 C 0.43519(13) 0.31901(18) 0.40809(8) 0.0327(5) Uani 1 1 d . . . . .
C34 C 0.49418(14) 0.3304(2) 0.43723(9) 0.0418(6) Uani 1 1 d . . . . .
H34 H 0.529490 0.375429 0.429050 0.050 Uiso 1 1 calc R U . . .
C35 C 0.50072(16) 0.2753(2) 0.47833(10) 0.0514(7) Uani 1 1 d . . . . .
H35 H 0.540675 0.282642 0.497175 0.062 Uiso 1 1 calc R U . . .
C36 C 0.44801(19) 0.2099(2) 0.49118(11) 0.0559(8) Uani 1 1 d . . . . .
H36 H 0.452007 0.173620 0.518888 0.067 Uiso 1 1 calc R U . . .
C37 C 0.38925(19) 0.1984(2) 0.46275(11) 0.0540(8) Uani 1 1 d . . . . .
H37 H 0.353628 0.154277 0.471410 0.065 Uiso 1 1 calc R U . . .
C38 C 0.38304(15) 0.2522(2) 0.42130(10) 0.0416(6) Uani 1 1 d . . . . .
H38 H 0.343482 0.243414 0.402239 0.050 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Br1 2.6204(3) . ?
Re1 P1 2.3367(6) . ?
Re1 N1 2.177(2) . ?
Re1 N2 2.1731(19) . ?
Re1 C1 1.899(3) . ?
Re1 C2 1.890(3) . ?
P1 C21 1.838(2) . ?
P1 C27 1.840(2) . ?
P1 C33 1.840(2) . ?
O1 C1 1.157(3) . ?
O2 C2 1.160(3) . ?
N1 C3 1.346(3) . ?
N1 C7 1.354(3) . ?
N2 C8 1.357(3) . ?
N2 C12 1.342(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.367(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.391(4) . ?
C5 C6 1.388(4) . ?
C5 C13 1.531(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(3) . ?
C7 C8 1.477(3) . ?
C8 C9 1.380(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.387(4) . ?
C10 C11 1.394(4) . ?
C10 C17 1.524(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.375(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.495(7) . ?
C13 C14A 1.484(17) . ?
C13 C15 1.487(6) . ?
C13 C15A 1.77(2) . ?
C13 C16 1.585(7) . ?
C13 C16A 1.533(17) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15A H15D 0.9600 . ?
C15A H15E 0.9600 . ?
C15A H15F 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16A H16D 0.9600 . ?
C16A H16E 0.9600 . ?
C16A H16F 0.9600 . ?
C17 C18 1.470(7) . ?
C17 C18A 1.638(10) . ?
C17 C19 1.572(6) . ?
C17 C19A 1.525(11) . ?
C17 C20 1.413(11) . ?
C17 C20A 1.567(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18A H18D 0.9600 . ?
C18A H18E 0.9600 . ?
C18A H18F 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C21 C22 1.399(3) . ?
C21 C26 1.395(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.380(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.376(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.374(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.392(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.395(4) . ?
C27 C32 1.383(4) . ?
C28 H28 0.9300 . ?
C28 C29 1.380(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.381(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.376(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.391(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.396(4) . ?
C33 C38 1.385(4) . ?
C34 H34 0.9300 . ?
C34 C35 1.389(4) . ?
C35 H35 0.9300 . ?
C35 C36 1.378(5) . ?
C36 H36 0.9300 . ?
C36 C37 1.381(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.389(4) . ?
C38 H38 0.9300 . ?

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
P1 Re1 Br1 173.845(16) . . ?
N1 Re1 Br1 81.57(5) . . ?
N1 Re1 P1 92.62(5) . . ?
N2 Re1 Br1 82.67(5) . . ?
N2 Re1 P1 97.78(5) . . ?
N2 Re1 N1 74.41(7) . . ?
C1 Re1 Br1 96.45(8) . . ?
C1 Re1 P1 89.61(8) . . ?
C1 Re1 N1 170.34(9) . . ?
C1 Re1 N2 95.99(9) . . ?
C2 Re1 Br1 88.83(7) . . ?
C2 Re1 P1 90.21(8) . . ?
C2 Re1 N1 100.08(9) . . ?
C2 Re1 N2 170.43(9) . . ?
C2 Re1 C1 89.29(11) . . ?
C21 P1 Re1 116.03(8) . . ?
C21 P1 C27 102.00(11) . . ?
C21 P1 C33 105.93(11) . . ?
C27 P1 Re1 118.31(8) . . ?
C27 P1 C33 100.38(11) . . ?
C33 P1 Re1 112.29(8) . . ?
C3 N1 Re1 125.64(16) . . ?
C3 N1 C7 117.0(2) . . ?
C7 N1 Re1 117.40(15) . . ?
C8 N2 Re1 117.57(15) . . ?
C12 N2 Re1 125.16(16) . . ?
C12 N2 C8 116.9(2) . . ?
O1 C1 Re1 177.2(2) . . ?
O2 C2 Re1 177.2(2) . . ?
N1 C3 H3 118.3 . . ?
N1 C3 C4 123.4(2) . . ?
C4 C3 H3 118.3 . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.5(2) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C13 121.9(2) . . ?
C6 C5 C4 116.1(2) . . ?
C6 C5 C13 122.0(2) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.0(2) . . ?
C7 C6 H6 119.5 . . ?
N1 C7 C6 121.9(2) . . ?
N1 C7 C8 115.3(2) . . ?
C6 C7 C8 122.7(2) . . ?
N2 C8 C7 114.9(2) . . ?
N2 C8 C9 121.8(2) . . ?
C9 C8 C7 123.3(2) . . ?
C8 C9 H9 119.2 . . ?
C8 C9 C10 121.6(2) . . ?
C10 C9 H9 119.2 . . ?
C9 C10 C11 115.7(2) . . ?
C9 C10 C17 121.8(2) . . ?
C11 C10 C17 122.5(2) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 C10 120.4(2) . . ?
C12 C11 H11 119.8 . . ?
N2 C12 C11 123.5(2) . . ?
N2 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
C5 C13 C15A 104.5(6) . . ?
C5 C13 C16 106.5(3) . . ?
C5 C13 C16A 109.5(7) . . ?
C14 C13 C5 110.6(3) . . ?
C14 C13 C16 106.2(4) . . ?
C14A C13 C5 116.4(8) . . ?
C14A C13 C15A 101.9(14) . . ?
C14A C13 C16A 119.4(10) . . ?
C15 C13 C5 113.0(3) . . ?
C15 C13 C14 112.4(5) . . ?
C15 C13 C16 107.7(4) . . ?
C16A C13 C15A 102.6(8) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14A H14D 109.5 . . ?
C13 C14A H14E 109.5 . . ?
C13 C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C15A H15D 109.5 . . ?
C13 C15A H15E 109.5 . . ?
C13 C15A H15F 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C16A H16D 109.5 . . ?
C13 C16A H16E 109.5 . . ?
C13 C16A H16F 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
C10 C17 C18A 101.8(4) . . ?
C10 C17 C19 108.9(3) . . ?
C10 C17 C19A 112.1(4) . . ?
C10 C17 C20A 112.4(3) . . ?
C18 C17 C10 110.7(3) . . ?
C18 C17 C19 109.0(4) . . ?
C18 C17 C20A 110.3(4) . . ?
C19A C17 C18A 102.1(6) . . ?
C20 C17 C10 111.6(5) . . ?
C20 C17 C18A 111.6(6) . . ?
C20 C17 C19A 116.3(6) . . ?
C20A C17 C19 105.3(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C18A H18D 109.5 . . ?
C17 C18A H18E 109.5 . . ?
C17 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C19A H19D 109.5 . . ?
C17 C19A H19E 109.5 . . ?
C17 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C20A H20D 109.5 . . ?
C17 C20A H20E 109.5 . . ?
C17 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C22 C21 P1 119.42(19) . . ?
C26 C21 P1 122.74(18) . . ?
C26 C21 C22 117.7(2) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.2(2) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.2 . . ?
C25 C24 C23 119.6(3) . . ?
C25 C24 H24 120.2 . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.6(3) . . ?
C25 C26 H26 119.7 . . ?
C28 C27 P1 119.39(19) . . ?
C32 C27 P1 122.36(19) . . ?
C32 C27 C28 118.2(2) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 C27 121.0(3) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.3(3) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.3(2) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.6(3) . . ?
C32 C31 H31 119.7 . . ?
C27 C32 C31 120.6(2) . . ?
C27 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 P1 118.3(2) . . ?
C38 C33 P1 122.63(19) . . ?
C38 C33 C34 118.5(2) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 C33 120.7(3) . . ?
C35 C34 H34 119.6 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.0(3) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 H36 120.1 . . ?
C35 C36 C37 119.8(3) . . ?
C37 C36 H36 120.1 . . ?
C36 C37 H37 119.8 . . ?
C36 C37 C38 120.4(3) . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 120.6(3) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?

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 C21 C22 -54.3(2) . . . . ?
Re1 P1 C21 C26 120.7(2) . . . . ?
Re1 P1 C27 C28 167.12(18) . . . . ?
Re1 P1 C27 C32 -12.9(2) . . . . ?
Re1 P1 C33 C34 -81.3(2) . . . . ?
Re1 P1 C33 C38 89.7(2) . . . . ?
Re1 N1 C3 C4 -178.8(2) . . . . ?
Re1 N1 C7 C6 177.59(19) . . . . ?
Re1 N1 C7 C8 -1.6(3) . . . . ?
Re1 N2 C8 C7 -7.3(3) . . . . ?
Re1 N2 C8 C9 173.18(18) . . . . ?
Re1 N2 C12 C11 -172.1(2) . . . . ?
P1 C21 C22 C23 175.85(19) . . . . ?
P1 C21 C26 C25 -175.8(2) . . . . ?
P1 C27 C28 C29 179.7(2) . . . . ?
P1 C27 C32 C31 178.7(2) . . . . ?
P1 C33 C34 C35 172.0(2) . . . . ?
P1 C33 C38 C37 -170.6(2) . . . . ?
N1 C3 C4 C5 1.2(5) . . . . ?
N1 C7 C8 N2 5.8(3) . . . . ?
N1 C7 C8 C9 -174.7(2) . . . . ?
N2 C8 C9 C10 -0.2(4) . . . . ?
C3 N1 C7 C6 -2.7(3) . . . . ?
C3 N1 C7 C8 178.1(2) . . . . ?
C3 C4 C5 C6 -2.6(4) . . . . ?
C3 C4 C5 C13 177.0(3) . . . . ?
C4 C5 C6 C7 1.4(4) . . . . ?
C4 C5 C13 C14 -43.2(5) . . . . ?
C4 C5 C13 C14A -2.2(13) . . . . ?
C4 C5 C13 C15 -170.2(4) . . . . ?
C4 C5 C13 C15A -113.6(8) . . . . ?
C4 C5 C13 C16 71.8(4) . . . . ?
C4 C5 C13 C16A 137.0(9) . . . . ?
C5 C6 C7 N1 1.3(4) . . . . ?
C5 C6 C7 C8 -179.6(2) . . . . ?
C6 C5 C13 C14 136.3(4) . . . . ?
C6 C5 C13 C14A 177.3(13) . . . . ?
C6 C5 C13 C15 9.3(6) . . . . ?
C6 C5 C13 C15A 65.9(8) . . . . ?
C6 C5 C13 C16 -108.7(4) . . . . ?
C6 C5 C13 C16A -43.4(10) . . . . ?
C6 C7 C8 N2 -173.4(2) . . . . ?
C6 C7 C8 C9 6.1(4) . . . . ?
C7 N1 C3 C4 1.5(4) . . . . ?
C7 C8 C9 C10 -179.7(2) . . . . ?
C8 N2 C12 C11 0.8(4) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C8 C9 C10 C17 178.0(2) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C9 C10 C17 C18 -68.0(4) . . . . ?
C9 C10 C17 C18A -102.5(5) . . . . ?
C9 C10 C17 C19 51.8(4) . . . . ?
C9 C10 C17 C19A 5.9(6) . . . . ?
C9 C10 C17 C20 138.3(6) . . . . ?
C9 C10 C17 C20A 168.1(3) . . . . ?
C10 C11 C12 N2 -0.8(4) . . . . ?
C11 C10 C17 C18 109.6(4) . . . . ?
C11 C10 C17 C18A 75.1(5) . . . . ?
C11 C10 C17 C19 -130.6(4) . . . . ?
C11 C10 C17 C19A -176.5(5) . . . . ?
C11 C10 C17 C20 -44.1(6) . . . . ?
C11 C10 C17 C20A -14.3(4) . . . . ?
C12 N2 C8 C7 179.3(2) . . . . ?
C12 N2 C8 C9 -0.3(3) . . . . ?
C13 C5 C6 C7 -178.2(3) . . . . ?
C17 C10 C11 C12 -177.5(3) . . . . ?
C21 P1 C27 C28 -64.3(2) . . . . ?
C21 P1 C27 C32 115.7(2) . . . . ?
C21 P1 C33 C34 151.12(19) . . . . ?
C21 P1 C33 C38 -37.9(2) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C22 C21 C26 C25 -0.7(4) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C23 C24 C25 C26 0.1(5) . . . . ?
C24 C25 C26 C21 0.4(5) . . . . ?
C26 C21 C22 C23 0.7(4) . . . . ?
C27 P1 C21 C22 175.7(2) . . . . ?
C27 P1 C21 C26 -9.4(2) . . . . ?
C27 P1 C33 C34 45.3(2) . . . . ?
C27 P1 C33 C38 -143.7(2) . . . . ?
C27 C28 C29 C30 1.9(5) . . . . ?
C28 C27 C32 C31 -1.3(4) . . . . ?
C28 C29 C30 C31 -1.8(4) . . . . ?
C29 C30 C31 C32 0.2(4) . . . . ?
C30 C31 C32 C27 1.4(4) . . . . ?
C32 C27 C28 C29 -0.3(4) . . . . ?
C33 P1 C21 C22 71.1(2) . . . . ?
C33 P1 C21 C26 -114.0(2) . . . . ?
C33 P1 C27 C28 44.7(2) . . . . ?
C33 P1 C27 C32 -135.4(2) . . . . ?
C33 C34 C35 C36 -1.2(4) . . . . ?
C34 C33 C38 C37 0.3(4) . . . . ?
C34 C35 C36 C37 0.9(5) . . . . ?
C35 C36 C37 C38 0.1(5) . . . . ?
C36 C37 C38 C33 -0.7(5) . . . . ?
C38 C33 C34 C35 0.6(4) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with oil'
_olex2_submission_original_sample_id KS67-3
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ks108
_database_code_depnum_ccdc_archive 'CCDC 2057004'
loop_
_audit_author_name
_audit_author_address
'Aurelien Crochet'
;University of Fribourg, Chemistry Department
Switzerland
;
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
kevin.schindler@unifr.ch
aurelien.crochet@unifr.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H35 N5 O2 Re, F6 P'
_chemical_formula_sum            'C29 H35 F6 N5 O2 P Re'
_chemical_formula_weight         816.79
_chemical_melting_point          ?
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'
P P 0.1023 0.0942 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.1948(10)
_cell_length_b                   12.3447(3)
_cell_length_c                   28.1669(9)
_cell_angle_alpha                90
_cell_angle_beta                 144.0940(10)
_cell_angle_gamma                90
_cell_volume                     6565.1(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19662
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      1.45
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.819
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, , Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'orangish red'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3232
_exptl_crystal_recrystallization_method 'layering of DCM and pentane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.235
_diffrn_reflns_theta_min         1.455
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4690
_reflns_number_total             6603
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6603
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.060
_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)+(0.0487P)²+27.0923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1105
_refine_special_details          ?
_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 Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C19(H19), C20(H20),
 C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.38805(2) 0.30894(2) 0.52723(2) 0.05011(11) Uani 1 1 d . . . . .
O1 O 0.2706(3) 0.1732(5) 0.3743(3) 0.0770(16) Uani 1 1 d . . . . .
O2 O 0.2737(3) 0.4629(6) 0.4580(4) 0.096(2) Uani 1 1 d . . . . .
N1 N 0.4810(2) 0.4002(4) 0.6376(3) 0.0463(12) Uani 1 1 d . . . . .
N2 N 0.4802(3) 0.2188(4) 0.5879(3) 0.0512(13) Uani 1 1 d . . . . .
N3 N 0.3929(3) 0.2168(5) 0.5968(3) 0.0552(14) Uani 1 1 d . . . . .
N4 N 0.3981(4) 0.0788(7) 0.6506(4) 0.089(2) Uani 1 1 d . . . . .
N5 N 0.3993(3) 0.3976(5) 0.4718(3) 0.0562(14) Uani 1 1 d . . . . .
C1 C 0.4783(4) 0.4910(6) 0.6599(4) 0.0581(17) Uani 1 1 d . . . . .
H1 H 0.434224 0.514392 0.629730 0.070 Uiso 1 1 calc R U . . .
C2 C 0.5366(4) 0.5531(6) 0.7251(4) 0.0583(17) Uani 1 1 d . . . . .
H2 H 0.531604 0.616316 0.738141 0.070 Uiso 1 1 calc R U . . .
C3 C 0.6026(4) 0.5200(6) 0.7708(4) 0.0577(17) Uani 1 1 d . . . . .
C4 C 0.6059(3) 0.4245(6) 0.7484(4) 0.0523(15) Uani 1 1 d . . . . .
H4 H 0.649583 0.399276 0.778380 0.063 Uiso 1 1 calc R U . . .
C5 C 0.5455(3) 0.3656(5) 0.6822(3) 0.0443(14) Uani 1 1 d . . . . .
C6 C 0.5447(3) 0.2635(6) 0.6543(3) 0.0463(14) Uani 1 1 d . . . . .
C7 C 0.6049(4) 0.2151(6) 0.6914(4) 0.0569(18) Uani 1 1 d . . . . .
H7 H 0.648846 0.247341 0.736817 0.068 Uiso 1 1 calc R U . . .
C8 C 0.6007(4) 0.1192(7) 0.6618(4) 0.065(2) Uani 1 1 d . . . . .
C9 C 0.5340(4) 0.0743(7) 0.5944(4) 0.067(2) Uani 1 1 d . . . . .
H9 H 0.528340 0.010231 0.572259 0.080 Uiso 1 1 calc R U . . .
C10 C 0.4759(4) 0.1253(6) 0.5604(4) 0.0607(18) Uani 1 1 d . . . . .
H10 H 0.431752 0.092888 0.516269 0.073 Uiso 1 1 calc R U . . .
C11 C 0.6699(4) 0.5888(6) 0.8413(4) 0.0649(19) Uani 1 1 d . . . . .
C12 C 0.6537(5) 0.6921(8) 0.8535(7) 0.121(4) Uani 1 1 d . . . . .
H12A H 0.618280 0.732846 0.804001 0.181 Uiso 1 1 calc R U . . .
H12B H 0.696029 0.734649 0.895498 0.181 Uiso 1 1 calc R U . . .
H12C H 0.636502 0.674004 0.868656 0.181 Uiso 1 1 calc R U . . .
C13 C 0.7027(5) 0.6158(9) 0.8233(6) 0.106(4) Uani 1 1 d . . . . .
H13A H 0.710184 0.550107 0.812707 0.160 Uiso 1 1 calc R U . . .
H13B H 0.747204 0.651864 0.869183 0.160 Uiso 1 1 calc R U . . .
H13C H 0.671264 0.662282 0.776842 0.160 Uiso 1 1 calc R U . . .
C14 C 0.7230(5) 0.5220(8) 0.9188(5) 0.100(3) Uani 1 1 d . . . . .
H14A H 0.704227 0.507937 0.932517 0.150 Uiso 1 1 calc R U . . .
H14B H 0.766623 0.561448 0.962029 0.150 Uiso 1 1 calc R U . . .
H14C H 0.731577 0.454628 0.910767 0.150 Uiso 1 1 calc R U . . .
C15 C 0.6664(4) 0.0633(8) 0.7031(5) 0.084(3) Uani 1 1 d . . . . .
C16 C 0.7146(6) 0.1497(12) 0.7233(8) 0.147(6) Uani 1 1 d . . . . .
H16A H 0.691559 0.176406 0.673965 0.220 Uiso 1 1 calc R U . . .
H16B H 0.758998 0.117277 0.755959 0.220 Uiso 1 1 calc R U . . .
H16C H 0.722739 0.208653 0.752441 0.220 Uiso 1 1 calc R U . . .
C17 C 0.7055(6) 0.0173(12) 0.7807(6) 0.156(6) Uani 1 1 d . . . . .
H17A H 0.710775 0.072034 0.809602 0.234 Uiso 1 1 calc R U . . .
H17B H 0.751362 -0.007013 0.813161 0.234 Uiso 1 1 calc R U . . .
H17C H 0.679360 -0.042733 0.769372 0.234 Uiso 1 1 calc R U . . .
C18 C 0.6490(5) -0.0204(10) 0.6505(6) 0.131(5) Uani 1 1 d . . . . .
H18A H 0.622523 -0.077944 0.640563 0.197 Uiso 1 1 calc R U . . .
H18B H 0.691962 -0.048887 0.677119 0.197 Uiso 1 1 calc R U . . .
H18C H 0.621154 0.011952 0.599995 0.197 Uiso 1 1 calc R U . . .
C19 C 0.3978(4) 0.1115(7) 0.6041(5) 0.073(2) Uani 1 1 d . . . . .
H19 H 0.400640 0.065252 0.580696 0.088 Uiso 1 1 calc R U . . .
C20 C 0.3926(9) 0.1722(10) 0.6733(8) 0.140(5) Uani 1 1 d . . . . .
H20 H 0.390862 0.176885 0.704634 0.169 Uiso 1 1 calc R U . . .
C21 C 0.3901(8) 0.2561(8) 0.6384(8) 0.124(4) Uani 1 1 d . . . . .
H21 H 0.387018 0.329143 0.643231 0.149 Uiso 1 1 calc R U . . .
C22 C 0.3975(6) -0.0265(10) 0.6671(7) 0.127(4) Uani 1 1 d . . . . .
H22A H 0.395885 -0.076170 0.639387 0.191 Uiso 1 1 calc R U . . .
H22B H 0.356590 -0.036895 0.648915 0.191 Uiso 1 1 calc R U . . .
H22C H 0.439578 -0.039292 0.724320 0.191 Uiso 1 1 calc R U . . .
C23 C 0.4071(4) 0.3464(8) 0.4368(5) 0.070(2) Uani 1 1 d . . . . .
H23 H 0.407930 0.271122 0.436320 0.084 Uiso 1 1 calc R U . . .
C24 C 0.4138(5) 0.4041(10) 0.4029(6) 0.092(3) Uani 1 1 d . . . . .
H24 H 0.419512 0.367187 0.379698 0.110 Uiso 1 1 calc R U . . .
C25 C 0.4125(6) 0.5139(14) 0.4008(7) 0.128(5) Uani 1 1 d . . . . .
H25 H 0.416544 0.553586 0.376651 0.154 Uiso 1 1 calc R U . . .
C26 C 0.4054(5) 0.5568(12) 0.4334(6) 0.109(4) Uani 1 1 d . . . . .
H26 H 0.404577 0.632122 0.433369 0.131 Uiso 1 1 calc R U . . .
C27 C 0.3989(4) 0.5051(7) 0.4693(5) 0.070(2) Uani 1 1 d . . . . .
H27 H 0.394000 0.545193 0.492584 0.084 Uiso 1 1 calc R U . . .
C28 C 0.3159(4) 0.2237(6) 0.4337(5) 0.0606(18) Uani 1 1 d . . . . .
C29 C 0.3180(4) 0.4016(7) 0.4853(4) 0.064(2) Uani 1 1 d . . . . .
P1 P 0.4491(2) 0.8075(2) 0.5740(2) 0.1104(10) Uani 1 1 d . . . . .
F1 F 0.4948(4) 0.7040(6) 0.6064(5) 0.142(3) Uani 1 1 d . . . . .
F2 F 0.3812(5) 0.7395(7) 0.4978(7) 0.206(5) Uani 1 1 d . . . . .
F3 F 0.4013(5) 0.9081(6) 0.5371(5) 0.188(4) Uani 1 1 d . . . . .
F4 F 0.5150(5) 0.8771(8) 0.6466(5) 0.187(4) Uani 1 1 d . . . . .
F5 F 0.4450(7) 0.7778(7) 0.6239(8) 0.206(5) Uani 1 1 d . . . . .
F6 F 0.4580(5) 0.8375(5) 0.5282(4) 0.143(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.194(5) . ?
Re1 N2 2.180(5) . ?
Re1 N3 2.160(5) . ?
Re1 N5 2.163(6) . ?
Re1 C28 1.879(8) . ?
Re1 C29 1.863(9) . ?
O1 C28 1.167(9) . ?
O2 C29 1.194(9) . ?
N1 C1 1.322(8) . ?
N1 C5 1.358(7) . ?
N2 C6 1.350(8) . ?
N2 C10 1.333(9) . ?
N3 C19 1.306(10) . ?
N3 C21 1.335(10) . ?
N4 C19 1.364(10) . ?
N4 C20 1.398(13) . ?
N4 C22 1.385(12) . ?
N5 C23 1.357(9) . ?
N5 C27 1.329(10) . ?
C1 H1 0.9300 . ?
C1 C2 1.379(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(10) . ?
C3 C4 1.381(9) . ?
C3 C11 1.546(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.383(8) . ?
C5 C6 1.475(9) . ?
C6 C7 1.388(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.389(10) . ?
C8 C9 1.385(10) . ?
C8 C15 1.522(10) . ?
C9 H9 0.9300 . ?
C9 C10 1.381(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.519(11) . ?
C11 C13 1.532(12) . ?
C11 C14 1.524(12) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.562(16) . ?
C15 C17 1.493(14) . ?
C15 C18 1.493(12) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.386(14) . ?
C21 H21 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23 0.9300 . ?
C23 C24 1.340(12) . ?
C24 H24 0.9300 . ?
C24 C25 1.356(17) . ?
C25 H25 0.9300 . ?
C25 C26 1.230(16) . ?
C26 H26 0.9300 . ?
C26 C27 1.349(12) . ?
C27 H27 0.9300 . ?
P1 F1 1.568(7) . ?
P1 F2 1.578(10) . ?
P1 F3 1.549(7) . ?
P1 F4 1.546(9) . ?
P1 F5 1.557(10) . ?
P1 F6 1.578(8) . ?

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
N2 Re1 N1 73.9(2) . . ?
N3 Re1 N1 88.4(2) . . ?
N3 Re1 N2 88.1(2) . . ?
N3 Re1 N5 171.8(2) . . ?
N5 Re1 N1 85.9(2) . . ?
N5 Re1 N2 84.6(2) . . ?
C28 Re1 N1 172.9(3) . . ?
C28 Re1 N2 99.6(3) . . ?
C28 Re1 N3 94.3(3) . . ?
C28 Re1 N5 90.7(3) . . ?
C29 Re1 N1 98.3(3) . . ?
C29 Re1 N2 172.0(3) . . ?
C29 Re1 N3 93.4(3) . . ?
C29 Re1 N5 93.2(3) . . ?
C29 Re1 C28 88.1(3) . . ?
C1 N1 Re1 124.7(4) . . ?
C1 N1 C5 117.8(5) . . ?
C5 N1 Re1 117.3(4) . . ?
C6 N2 Re1 117.8(4) . . ?
C10 N2 Re1 123.5(4) . . ?
C10 N2 C6 118.6(6) . . ?
C19 N3 Re1 125.2(5) . . ?
C19 N3 C21 108.0(7) . . ?
C21 N3 Re1 126.7(6) . . ?
C19 N4 C20 106.9(8) . . ?
C19 N4 C22 127.5(10) . . ?
C22 N4 C20 125.3(9) . . ?
C23 N5 Re1 121.9(5) . . ?
C27 N5 Re1 122.9(5) . . ?
C27 N5 C23 115.2(7) . . ?
N1 C1 H1 117.9 . . ?
N1 C1 C2 124.2(7) . . ?
C2 C1 H1 117.9 . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 118.9(7) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 117.2(6) . . ?
C2 C3 C11 122.2(6) . . ?
C4 C3 C11 120.6(6) . . ?
C3 C4 H4 119.3 . . ?
C3 C4 C5 121.3(6) . . ?
C5 C4 H4 119.3 . . ?
N1 C5 C4 120.6(6) . . ?
N1 C5 C6 115.0(5) . . ?
C4 C5 C6 124.4(6) . . ?
N2 C6 C5 115.5(5) . . ?
N2 C6 C7 120.6(6) . . ?
C7 C6 C5 123.9(6) . . ?
C6 C7 H7 119.4 . . ?
C6 C7 C8 121.2(6) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C15 121.9(7) . . ?
C9 C8 C7 116.9(7) . . ?
C9 C8 C15 121.2(7) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 C8 119.6(7) . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 123.1(7) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C12 C11 C3 111.7(7) . . ?
C12 C11 C13 110.3(8) . . ?
C12 C11 C14 108.8(8) . . ?
C13 C11 C3 108.6(6) . . ?
C14 C11 C3 108.8(7) . . ?
C14 C11 C13 108.5(8) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 C16 108.8(8) . . ?
C17 C15 C8 107.0(8) . . ?
C17 C15 C16 108.4(10) . . ?
C18 C15 C8 112.5(7) . . ?
C18 C15 C16 107.4(9) . . ?
C18 C15 C17 112.6(10) . . ?
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 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 N4 110.5(8) . . ?
N3 C19 H19 124.7 . . ?
N4 C19 H19 124.7 . . ?
N4 C20 H20 127.9 . . ?
C21 C20 N4 104.3(8) . . ?
C21 C20 H20 127.9 . . ?
N3 C21 C20 110.2(9) . . ?
N3 C21 H21 124.9 . . ?
C20 C21 H21 124.9 . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 H23 119.9 . . ?
C24 C23 N5 120.1(9) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 118.5 . . ?
C23 C24 C25 123.1(11) . . ?
C25 C24 H24 118.5 . . ?
C24 C25 H25 122.7 . . ?
C26 C25 C24 114.6(14) . . ?
C26 C25 H25 122.7 . . ?
C25 C26 H26 116.9 . . ?
C25 C26 C27 126.3(15) . . ?
C27 C26 H26 116.9 . . ?
N5 C27 C26 120.8(10) . . ?
N5 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
O1 C28 Re1 177.9(7) . . ?
O2 C29 Re1 178.3(7) . . ?
F1 P1 F2 88.3(5) . . ?
F1 P1 F6 87.6(4) . . ?
F3 P1 F1 176.7(5) . . ?
F3 P1 F2 89.1(5) . . ?
F3 P1 F5 91.7(5) . . ?
F3 P1 F6 90.3(5) . . ?
F4 P1 F1 92.7(6) . . ?
F4 P1 F2 177.9(6) . . ?
F4 P1 F3 89.8(6) . . ?
F4 P1 F5 88.1(6) . . ?
F4 P1 F6 89.2(5) . . ?
F5 P1 F1 90.6(4) . . ?
F5 P1 F2 93.7(7) . . ?
F5 P1 F6 176.7(7) . . ?
F6 P1 F2 89.0(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 N1 C1 C2 -173.5(5) . . . . ?
Re1 N1 C5 C4 174.1(5) . . . . ?
Re1 N1 C5 C6 -5.9(7) . . . . ?
Re1 N2 C6 C5 4.9(7) . . . . ?
Re1 N2 C6 C7 -174.1(5) . . . . ?
Re1 N2 C10 C9 173.1(6) . . . . ?
Re1 N3 C19 N4 -178.6(5) . . . . ?
Re1 N3 C21 C20 178.1(9) . . . . ?
Re1 N5 C23 C24 179.8(6) . . . . ?
Re1 N5 C27 C26 -179.4(6) . . . . ?
N1 C1 C2 C3 0.1(11) . . . . ?
N1 C5 C6 N2 0.7(8) . . . . ?
N1 C5 C6 C7 179.7(6) . . . . ?
N2 C6 C7 C8 -0.5(11) . . . . ?
N4 C20 C21 N3 0.9(17) . . . . ?
N5 C23 C24 C25 -0.6(15) . . . . ?
C1 N1 C5 C4 -0.4(9) . . . . ?
C1 N1 C5 C6 179.6(6) . . . . ?
C1 C2 C3 C4 -0.9(10) . . . . ?
C1 C2 C3 C11 175.9(7) . . . . ?
C2 C3 C4 C5 1.1(10) . . . . ?
C2 C3 C11 C12 1.2(11) . . . . ?
C2 C3 C11 C13 -120.7(8) . . . . ?
C2 C3 C11 C14 121.3(8) . . . . ?
C3 C4 C5 N1 -0.4(10) . . . . ?
C3 C4 C5 C6 179.6(6) . . . . ?
C4 C3 C11 C12 177.9(8) . . . . ?
C4 C3 C11 C13 56.0(10) . . . . ?
C4 C3 C11 C14 -62.0(9) . . . . ?
C4 C5 C6 N2 -179.4(6) . . . . ?
C4 C5 C6 C7 -0.4(10) . . . . ?
C5 N1 C1 C2 0.6(10) . . . . ?
C5 C6 C7 C8 -179.4(6) . . . . ?
C6 N2 C10 C9 -3.0(11) . . . . ?
C6 C7 C8 C9 -0.6(11) . . . . ?
C6 C7 C8 C15 -178.2(8) . . . . ?
C7 C8 C9 C10 -0.1(12) . . . . ?
C7 C8 C15 C16 -46.2(11) . . . . ?
C7 C8 C15 C17 70.8(12) . . . . ?
C7 C8 C15 C18 -165.0(9) . . . . ?
C8 C9 C10 N2 1.9(12) . . . . ?
C9 C8 C15 C16 136.4(9) . . . . ?
C9 C8 C15 C17 -106.6(10) . . . . ?
C9 C8 C15 C18 17.6(14) . . . . ?
C10 N2 C6 C5 -178.7(6) . . . . ?
C10 N2 C6 C7 2.2(10) . . . . ?
C11 C3 C4 C5 -175.8(6) . . . . ?
C15 C8 C9 C10 177.5(8) . . . . ?
C19 N3 C21 C20 -0.7(15) . . . . ?
C19 N4 C20 C21 -0.8(15) . . . . ?
C20 N4 C19 N3 0.4(12) . . . . ?
C21 N3 C19 N4 0.2(11) . . . . ?
C22 N4 C19 N3 174.9(9) . . . . ?
C22 N4 C20 C21 -175.4(11) . . . . ?
C23 N5 C27 C26 0.4(11) . . . . ?
C23 C24 C25 C26 0.7(18) . . . . ?
C24 C25 C26 C27 -0.3(18) . . . . ?
C25 C26 C27 N5 -0.3(16) . . . . ?
C27 N5 C23 C24 0.0(11) . . . . ?

_olex2_exptl_crystal_mounting_method 'mounted on nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
