# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1570738'
_audit_update_record             
;
2017-08-24 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;

_vrf_THETM01_2                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Please see the _refine_special_details section of the CIF.
;
_vrf_PLAT088_2                   
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.70 Note
RESPONSE: Please see the _refine_special_details section of the CIF.
;
_vrf_PLAT341_2                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02369 Ang.
RESPONSE: Please see the _refine_special_details section of the CIF.
;
_vrf_PLAT431_2                   
;
PROBLEM: Short Inter HL..A  Contact F3     ..  O10     ..       2.64 Ang.
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# Added during the CSD deposition process: Thursday 24 August 2017 03:46 PM
# end Validation Reply Form

# eb16191_sq
_audit_creation_date             2016-07-20
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C83 H50 Cu2 F9 N8 O10 S3, C F3 O3 S, C2 H3 N + other solvent'
_chemical_formula_sum            'C86 H53 Cu2 F12 N9 O13 S4'
_chemical_formula_weight         1903.69
_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'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.0285(6)
_cell_length_b                   19.1152(9)
_cell_length_c                   21.1384(11)
_cell_angle_alpha                64.740(3)
_cell_angle_beta                 74.232(3)
_cell_angle_gamma                78.345(3)
_cell_volume                     4909.3(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4644
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      22.21
_cell_measurement_theta_min      2.22
_shelx_estimated_absorpt_T_max   0.963
_shelx_estimated_absorpt_T_min   0.814
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0746 before and 0.0502 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0793 before and 0.0507 after correction.
 The Ratio of minimum to maximum transmission is 0.71.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 47951 reflections, Rint = 0.0869
 (11865 with I > 3sig(I), Rint = 0.0460)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1932
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of DCM and acetonitrile by slow evaporation'
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.063
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.814
_diffrn_reflns_theta_max         20.814
_diffrn_reflns_theta_min         1.089
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   Mo-tube
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9503
_reflns_number_total             13413
_reflns_special_details          
;
 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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APEX2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         13413
_refine_ls_number_restraints     1074
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0991
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1783P)²+20.4557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2639
_refine_ls_wR_factor_ref         0.2909
_refine_special_details          
;
The crystals, on the microscope slide and at room temperature, appear very well formed.  However, when flash cooled at 120 K they give a very bad diffraction pattern which is difficult to index.  At 200 K the pattern was indexed using CELL_NOW as a non-merohedral twin.  The two twin components are related by twin law [-1 0 0 / -0.25 1 -0.73 / 0 0 -1] and refined twin scale factor 0.449(2).  One molecule of MeCN was identified but all other electron density pertaining to solvent was handled using the SQUEEZE routine of PLATON.  A total of 262 electrons per unit cell were handled this way.  It is not really possible to identify the correct solvent ratio from this; 262 electrons roughly corresponds with molecules of dichloromethane per asymmetric unit, but the largest residual peak (before using SQUEEZE) was 4.5 electrons high; with DCM it would be much bigger, even for disordered DCM.  The moiety formula is thus reported as "... + solvent".  

Three of the four triflate anions were modelled as disordered over two sites.  Displacement ellipsoid and geometric similarity restraints were used.

The data set was cut at a resolution of 1 A owing to rapidly increasing values of R(merge) at higher resolution.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      20.81 Degree

See above

#===============================================================================
088_ALERT_3_B Poor Data / Parameter Ratio ....................       7.70 Note
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.02369 Ang.

Consequence of poor diffraction, see above

431_ALERT_2_B Short Inter HL..A  Contact F3     ..  O10     ..       2.64 Ang.

Consequence of disorder
#===============================================================================
084_ALERT_3_C High wR2 Value (i.e. > 0.25) ...................       0.29 Report

Weakly diffracting squeezed non-merohedral twin

094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.09 Report
213_ALERT_2_C Atom F5              has ADP max/min Ratio .....        3.2 oblate
213_ALERT_2_C Atom C12             has ADP max/min Ratio .....        4.0 oblate
213_ALERT_2_C Atom C17             has ADP max/min Ratio .....        3.3 oblate
213_ALERT_2_C Atom C73             has ADP max/min Ratio .....        3.6 prolat
234_ALERT_4_C Large Hirshfeld Difference S1     --  O1      ..       0.16 Ang.
234_ALERT_4_C Large Hirshfeld Difference S1     --  O2      ..       0.16 Ang.
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C42 Check
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         S1 Check
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C91 Check
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note

A global displacement ellipsoid restraint was used

364_ALERT_2_C Short   C(sp3)-C(sp)  Bond  C91    -   C92    ..       1.34 Ang.

Acetonitrile solvent

906_ALERT_3_C Large K value in the Analysis of Variance ......      2.856 Check
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.500         92 Report
918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .         11 Check

Noted

#===============================================================================
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.551(2) 0.449(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Shared sites
{O7, O7A}
{O11, O11A}
{O12, O12A}
{O4, O4A}
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(O7A)
Uanis(O11) = Uanis(O11A)
Uanis(O12) = Uanis(O12A)
Uanis(O4) = Uanis(O4A)
6. Rigid body (RIGU) restrains
 S3, S3A, F7, F7A, F8, F8A, F9, F9A, O7, O7A, O8, O8A, O9, O9A, C83, C83A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N91, C91, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, F4, F5, F6, O4, O5, O6, C82, S2A, F4A, F5A, F6A, O4A, O5A, O6A, C82A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{S1, F1, F2, F3, O1, O2, O3, C81} sigma for 1-2: 0.02, 1-3: 0.02
as
{S2, F4, F5, F6, O4, O5, O6, C82}
{S1, F1, F2, F3, O1, O2, O3, C81} sigma for 1-2: 0.02, 1-3: 0.02
as
{S2A, F4A, F5A, F6A, O4A, O5A, O6A, C82A}
{S1, F1, F2, F3, O1, O2, O3, C81} sigma for 1-2: 0.02, 1-3: 0.02
as
{S3, F7, F8, F9, O7, O8, O9, C83}
{S1, F1, F2, F3, O1, O2, O3, C81} sigma for 1-2: 0.02, 1-3: 0.02
as
{S3A, F7A, F8A, F9A, O7A, O8A, O9A, C83A}
{S1, F1, F2, F3, O1, O2, O3, C81} sigma for 1-2: 0.02, 1-3: 0.02
as
{S4, F10, F11, F12, O10, O11, O12, C84}
{S1, F1, F2, F3, O1, O2, O3, C81} sigma for 1-2: 0.02, 1-3: 0.02
as
{S4A, F10A, F11A, F12A, O10A, O11A, O12A, C84A}
8. Others
 Sof(S3A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(C83A)=1-
 FVAR(1)
 Sof(S3)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(C83)=FVAR(1)
 Sof(S4A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=
 Sof(C84A)=1-FVAR(2)
 Sof(S4)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C84)=FVAR(2)
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C82A)=1-
 FVAR(3)
 Sof(S2)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(C82)=FVAR(3)
9.a Rotating group:
 O21(H21A,H21B)
9.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C29(H29), C30(H30), C31(H31), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C49(H49), C50(H50), C51(H51),
  C53(H53), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
 C63(H63), C65(H65), C69(H69), C70(H70), C71(H71), C73(H73), C77(H77), C78(H78),
  C79(H79), C80(H80)
9.c Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Cu1 Cu 0.28598(13) 0.17698(10) 0.87708(10) 0.0445(6) Uani 1 1 d . U . . .
Cu2 Cu 0.20710(12) 0.84730(9) 0.62833(9) 0.0373(5) Uani 1 1 d . U . . .
S1 S 0.2692(3) -0.0329(2) 0.9698(2) 0.0515(11) Uani 1 1 d D U . . .
F1 F 0.3494(9) -0.1742(6) 1.0231(7) 0.141(5) Uani 1 1 d D U . . .
F2 F 0.4319(7) -0.0858(8) 1.0147(7) 0.147(5) Uani 1 1 d D U . . .
F3 F 0.4291(9) -0.1033(9) 0.9204(7) 0.167(6) Uani 1 1 d D U . . .
O1 O 0.3132(7) 0.0407(5) 0.9259(5) 0.050(2) Uani 1 1 d D U . . .
O2 O 0.2175(8) -0.0434(7) 1.0423(5) 0.079(4) Uani 1 1 d D U . . .
O3 O 0.2217(8) -0.0594(7) 0.9324(6) 0.086(4) Uani 1 1 d D U . . .
C81 C 0.3778(10) -0.1036(8) 0.9842(8) 0.089(5) Uani 1 1 d D U . . .
S2 S 0.1734(3) 1.0548(2) 0.5854(2) 0.0330(14) Uani 0.797(8) 1 d D U P A 1
F4 F 0.0554(9) 1.1140(11) 0.4971(7) 0.135(6) Uani 0.797(8) 1 d D U P A 1
F5 F 0.1373(13) 1.1953(7) 0.4993(7) 0.137(6) Uani 0.797(8) 1 d D U P A 1
F6 F 0.2076(8) 1.1153(8) 0.4476(5) 0.087(4) Uani 0.797(8) 1 d D U P A 1
O4 O 0.1812(7) 0.9820(5) 0.5776(5) 0.056(2) Uani 0.797(8) 1 d D U P A 1
O5 O 0.2728(9) 1.0711(8) 0.5815(7) 0.065(4) Uani 0.797(8) 1 d D U P A 1
O6 O 0.0951(9) 1.0667(7) 0.6397(6) 0.066(4) Uani 0.797(8) 1 d D U P A 1
C82 C 0.1424(11) 1.1241(9) 0.5029(7) 0.075(4) Uani 0.797(8) 1 d D U P A 1
S2A S 0.2243(15) 1.0530(10) 0.5281(11) 0.086(7) Uani 0.203(8) 1 d D U P A 2
F4A F 0.064(3) 1.084(2) 0.481(3) 0.086(11) Uani 0.203(8) 1 d D U P A 2
F5A F 0.055(3) 1.118(2) 0.568(2) 0.113(11) Uani 0.203(8) 1 d D U P A 2
F6A F 0.130(3) 1.1854(14) 0.460(2) 0.117(12) Uani 0.203(8) 1 d D U P A 2
O4A O 0.1812(7) 0.9820(5) 0.5776(5) 0.056(2) Uani 0.203(8) 1 d D U P A 2
O5A O 0.265(3) 1.0910(18) 0.560(2) 0.092(11) Uani 0.203(8) 1 d D U P A 2
O6A O 0.277(3) 1.055(2) 0.4593(14) 0.092(11) Uani 0.203(8) 1 d D U P A 2
C82A C 0.110(2) 1.1154(13) 0.5080(17) 0.093(9) Uani 0.203(8) 1 d D U P A 2
S3 S 0.2269(5) 0.6274(4) 0.6871(4) 0.052(2) Uani 0.591(8) 1 d D U P A 1
F7 F 0.2184(14) 0.5847(10) 0.8240(7) 0.088(6) Uani 0.591(8) 1 d D U P A 1
F8 F 0.3659(11) 0.5868(10) 0.7600(9) 0.095(6) Uani 0.591(8) 1 d D U P A 1
F9 F 0.2756(13) 0.4944(7) 0.7852(8) 0.092(5) Uani 0.591(8) 1 d D U P A 1
O7 O 0.2276(7) 0.7057(4) 0.6805(5) 0.052(2) Uani 0.591(8) 1 d D U P A 1
O8 O 0.1287(11) 0.6024(12) 0.7040(12) 0.073(6) Uani 0.591(8) 1 d D U P A 1
O9 O 0.3005(14) 0.6073(11) 0.6328(9) 0.085(6) Uani 0.591(8) 1 d D U P A 1
C83 C 0.2751(14) 0.5709(9) 0.7679(9) 0.074(5) Uani 0.591(8) 1 d D U P A 1
S3A S 0.2647(7) 0.6270(5) 0.7234(6) 0.048(3) Uani 0.409(8) 1 d D U P A 2
F7A F 0.2743(18) 0.5892(14) 0.6176(10) 0.085(7) Uani 0.409(8) 1 d D U P A 2
F8A F 0.1316(13) 0.5830(14) 0.6879(16) 0.081(8) Uani 0.409(8) 1 d D U P A 2
F9A F 0.2515(14) 0.4939(8) 0.7199(11) 0.068(6) Uani 0.409(8) 1 d D U P A 2
O7A O 0.2276(7) 0.7057(4) 0.6805(5) 0.052(2) Uani 0.409(8) 1 d D U P A 2
O8A O 0.210(2) 0.5984(14) 0.7981(8) 0.070(7) Uani 0.409(8) 1 d D U P A 2
O9A O 0.3718(11) 0.6107(13) 0.7135(14) 0.069(7) Uani 0.409(8) 1 d D U P A 2
C83A C 0.2280(15) 0.5706(10) 0.6855(12) 0.070(6) Uani 0.409(8) 1 d D U P A 2
O21 O 0.2623(7) 0.3292(5) 0.8239(6) 0.057(3) Uani 1 1 d . U . . .
H21A H 0.2485 0.3497 0.7784 0.085 Uiso 1 1 d GR . . . .
H21B H 0.3189 0.3503 0.8197 0.085 Uiso 1 1 d GR . . . .
N1 N 0.2761(8) 0.1785(7) 0.9753(6) 0.042(3) Uani 1 1 d . U . . .
N2 N 0.2027(8) 0.8448(7) 0.7243(6) 0.040(3) Uani 1 1 d . U . . .
N3 N 0.1365(8) 0.1800(7) 0.8952(7) 0.042(3) Uani 1 1 d . U . . .
N4 N 0.0577(8) 0.8410(7) 0.6549(6) 0.035(3) Uani 1 1 d . U . . .
N5 N 0.2939(8) 0.1814(7) 0.7782(6) 0.042(3) Uani 1 1 d . U . . .
N6 N 0.2139(8) 0.8466(7) 0.5305(6) 0.043(3) Uani 1 1 d . U . . .
N7 N 0.4358(8) 0.1796(7) 0.8527(6) 0.045(3) Uani 1 1 d . U . . .
N8 N 0.3567(8) 0.8455(7) 0.6058(6) 0.040(3) Uani 1 1 d . U . . .
C1 C 0.3246(10) 0.1215(9) 1.0221(9) 0.048(4) Uani 1 1 d . U . . .
H1 H 0.3614 0.0804 1.0092 0.058 Uiso 1 1 calc R . . . .
C2 C 0.3240(12) 0.1191(10) 1.0888(9) 0.060(4) Uani 1 1 d . U . . .
H2 H 0.3587 0.0777 1.1216 0.072 Uiso 1 1 calc R . . . .
C3 C 0.2690(10) 0.1816(9) 1.1046(8) 0.045(4) Uani 1 1 d . U . . .
H3 H 0.2652 0.1825 1.1498 0.054 Uiso 1 1 calc R . . . .
C4 C 0.2193(11) 0.2431(9) 1.0552(9) 0.046(4) Uani 1 1 d . U . . .
C5 C 0.2233(9) 0.2364(9) 0.9928(8) 0.042(3) Uani 1 1 d . U . . .
H5 H 0.1863 0.2752 0.9599 0.050 Uiso 1 1 calc R . . . .
C6 C 0.1672(10) 0.3091(10) 1.0681(8) 0.040(4) Uani 1 1 d . U . . .
C7 C 0.1273(12) 0.3698(10) 1.0702(9) 0.052(4) Uani 1 1 d . U . . .
C8 C 0.0838(10) 0.4410(9) 1.0746(8) 0.041(3) Uani 1 1 d . U . . .
C9 C 0.0231(11) 0.4434(10) 1.1402(8) 0.053(4) Uani 1 1 d . U . . .
H9 H 0.0096 0.3971 1.1816 0.063 Uiso 1 1 calc R . . . .
C10 C -0.0152(10) 0.5156(10) 1.1414(8) 0.049(4) Uani 1 1 d . U . . .
H10 H -0.0593 0.5178 1.1836 0.059 Uiso 1 1 calc R . . . .
C11 C 0.0070(9) 0.5836(9) 1.0850(7) 0.039(3) Uani 1 1 d . U . . .
H11 H -0.0191 0.6320 1.0885 0.046 Uiso 1 1 calc R . . . .
C12 C 0.0690(9) 0.5811(9) 1.0217(7) 0.033(3) Uani 1 1 d . U . . .
C13 C 0.1044(9) 0.5115(9) 1.0185(7) 0.033(3) Uani 1 1 d . U . . .
H13 H 0.1461 0.5108 0.9750 0.040 Uiso 1 1 calc R . . . .
C14 C 0.0968(10) 0.6527(9) 0.9638(8) 0.037(3) Uani 1 1 d . U . . .
C15 C 0.1212(11) 0.7091(9) 0.9138(8) 0.045(4) Uani 1 1 d . U . . .
C16 C 0.1612(10) 0.7795(9) 0.8536(7) 0.036(3) Uani 1 1 d . U . . .
C17 C 0.2050(12) 0.8310(9) 0.8614(8) 0.054(4) Uani 1 1 d . U . . .
H17 H 0.2069 0.8266 0.9075 0.065 Uiso 1 1 calc R . . . .
C18 C 0.2471(13) 0.8906(10) 0.8004(8) 0.059(5) Uani 1 1 d . U . . .
H18 H 0.2761 0.9286 0.8049 0.071 Uiso 1 1 calc R . . . .
C19 C 0.2478(11) 0.8957(9) 0.7347(8) 0.049(4) Uani 1 1 d . U . . .
H19 H 0.2806 0.9358 0.6941 0.059 Uiso 1 1 calc R . . . .
C20 C 0.1598(9) 0.7847(8) 0.7857(7) 0.035(3) Uani 1 1 d . U . . .
H20 H 0.1295 0.7472 0.7814 0.042 Uiso 1 1 calc R . . . .
C21 C 0.0840(11) 0.1309(9) 0.9554(9) 0.050(4) Uani 1 1 d . U . . .
H21 H 0.1195 0.0949 0.9907 0.060 Uiso 1 1 calc R . . . .
C22 C -0.0187(12) 0.1283(10) 0.9705(10) 0.061(5) Uani 1 1 d . U . . .
H22 H -0.0515 0.0885 1.0114 0.074 Uiso 1 1 calc R . . . .
C23 C -0.0696(10) 0.1867(9) 0.9228(9) 0.052(4) Uani 1 1 d . U . . .
H23 H -0.1402 0.1906 0.9325 0.062 Uiso 1 1 calc R . . . .
C24 C -0.0182(11) 0.2405(9) 0.8601(8) 0.047(4) Uani 1 1 d . U . . .
C25 C 0.0835(10) 0.2341(9) 0.8493(8) 0.043(4) Uani 1 1 d . U . . .
H25 H 0.1186 0.2705 0.8065 0.051 Uiso 1 1 calc R . . . .
C26 C -0.0657(11) 0.3070(10) 0.8057(9) 0.050(4) Uani 1 1 d . U . . .
C27 C -0.0993(10) 0.3640(9) 0.7636(8) 0.042(4) Uani 1 1 d . U . . .
C28 C -0.1341(9) 0.4360(9) 0.7120(8) 0.037(3) Uani 1 1 d . U . . .
C29 C -0.1847(9) 0.4378(9) 0.6648(8) 0.040(3) Uani 1 1 d . U . . .
H29 H -0.1975 0.3910 0.6645 0.048 Uiso 1 1 calc R . . . .
C30 C -0.2179(10) 0.5108(10) 0.6161(8) 0.048(4) Uani 1 1 d . U . . .
H30 H -0.2529 0.5132 0.5824 0.058 Uiso 1 1 calc R . . . .
C31 C -0.2003(9) 0.5762(9) 0.6171(8) 0.040(4) Uani 1 1 d . U . . .
H31 H -0.2239 0.6246 0.5841 0.048 Uiso 1 1 calc R . . . .
C32 C -0.1488(9) 0.5760(9) 0.6643(7) 0.035(3) Uani 1 1 d . U . . .
C33 C -0.1146(8) 0.5051(9) 0.7119(7) 0.031(3) Uani 1 1 d . U . . .
H33 H -0.0780 0.5033 0.7445 0.037 Uiso 1 1 calc R . . . .
C34 C -0.1261(10) 0.6456(9) 0.6675(8) 0.041(4) Uani 1 1 d . U . . .
C35 C -0.1068(9) 0.7004(9) 0.6711(7) 0.033(3) Uani 1 1 d . U . . .
C36 C -0.0771(11) 0.7681(9) 0.6747(8) 0.044(4) Uani 1 1 d . U . . .
C37 C -0.1430(11) 0.8177(9) 0.6993(7) 0.045(4) Uani 1 1 d . U . . .
H37 H -0.2119 0.8108 0.7152 0.054 Uiso 1 1 calc R . . . .
C38 C -0.1061(11) 0.8788(9) 0.7005(8) 0.048(4) Uani 1 1 d . U . . .
H38 H -0.1504 0.9156 0.7163 0.057 Uiso 1 1 calc R . . . .
C39 C -0.0068(11) 0.8867(9) 0.6792(8) 0.049(4) Uani 1 1 d . U . . .
H39 H 0.0163 0.9282 0.6826 0.059 Uiso 1 1 calc R . . . .
C40 C 0.0236(10) 0.7807(8) 0.6502(7) 0.037(3) Uani 1 1 d . U . . .
H40 H 0.0689 0.7475 0.6303 0.044 Uiso 1 1 calc R . . . .
C41 C 0.2602(13) 0.1212(10) 0.7735(9) 0.065(5) Uani 1 1 d . U . . .
H41 H 0.2340 0.0788 0.8151 0.078 Uiso 1 1 calc R . . . .
C42 C 0.2658(17) 0.1247(11) 0.7071(11) 0.092(7) Uani 1 1 d . U . . .
H42 H 0.2447 0.0828 0.7032 0.111 Uiso 1 1 calc R . . . .
C43 C 0.3000(15) 0.1845(12) 0.6465(10) 0.085(6) Uani 1 1 d . U . . .
H43 H 0.3004 0.1846 0.6015 0.101 Uiso 1 1 calc R . . . .
C44 C 0.3338(11) 0.2449(9) 0.6495(9) 0.055(4) Uani 1 1 d . U . . .
C45 C 0.3287(10) 0.2389(9) 0.7202(8) 0.046(4) Uani 1 1 d . U . . .
H45 H 0.3521 0.2793 0.7250 0.056 Uiso 1 1 calc R . . . .
C46 C 0.3692(11) 0.3142(11) 0.5866(9) 0.050(4) Uani 1 1 d . U . . .
C47 C 0.3918(10) 0.3719(10) 0.5371(9) 0.045(4) Uani 1 1 d . U . . .
C48 C 0.4175(10) 0.4434(9) 0.4784(8) 0.043(4) Uani 1 1 d . U . . .
C49 C 0.4792(10) 0.4411(9) 0.4136(9) 0.047(4) Uani 1 1 d . U . . .
H49 H 0.5065 0.3930 0.4096 0.057 Uiso 1 1 calc R . . . .
C50 C 0.4981(10) 0.5109(10) 0.3568(8) 0.048(4) Uani 1 1 d . U . . .
H50 H 0.5383 0.5112 0.3125 0.057 Uiso 1 1 calc R . . . .
C51 C 0.4603(10) 0.5784(9) 0.3633(7) 0.039(3) Uani 1 1 d . U . . .
H51 H 0.4756 0.6255 0.3232 0.047 Uiso 1 1 calc R . . . .
C52 C 0.4004(9) 0.5826(9) 0.4251(7) 0.031(3) Uani 1 1 d . U . . .
C53 C 0.3806(9) 0.5112(9) 0.4844(7) 0.034(3) Uani 1 1 d . U . . .
H53 H 0.3409 0.5115 0.5285 0.041 Uiso 1 1 calc R . . . .
C54 C 0.3587(10) 0.6552(9) 0.4336(7) 0.034(3) Uani 1 1 d . U . . .
C55 C 0.3203(11) 0.7150(10) 0.4374(8) 0.050(4) Uani 1 1 d . U . . .
C56 C 0.2678(10) 0.7816(9) 0.4506(8) 0.047(4) Uani 1 1 d . U . . .
C57 C 0.2192(12) 0.8430(10) 0.4004(9) 0.056(4) Uani 1 1 d . U . . .
H57 H 0.2226 0.8437 0.3546 0.067 Uiso 1 1 calc R . . . .
C58 C 0.1674(12) 0.9012(10) 0.4196(9) 0.058(5) Uani 1 1 d . U . . .
H58 H 0.1311 0.9420 0.3876 0.070 Uiso 1 1 calc R . . . .
C59 C 0.1659(10) 0.9029(9) 0.4843(7) 0.043(4) Uani 1 1 d . U . . .
H59 H 0.1298 0.9452 0.4957 0.052 Uiso 1 1 calc R . . . .
C60 C 0.2668(10) 0.7876(9) 0.5154(8) 0.043(3) Uani 1 1 d . U . . .
H60 H 0.3042 0.7492 0.5482 0.051 Uiso 1 1 calc R . . . .
C61 C 0.4971(10) 0.1289(9) 0.8269(8) 0.046(4) Uani 1 1 d . U . . .
H61 H 0.4703 0.0878 0.8255 0.055 Uiso 1 1 calc R . . . .
C62 C 0.5992(12) 0.1359(10) 0.8024(9) 0.062(5) Uani 1 1 d . U . . .
H62 H 0.6421 0.0987 0.7865 0.075 Uiso 1 1 calc R . . . .
C63 C 0.6367(11) 0.1976(10) 0.8016(8) 0.056(4) Uani 1 1 d . U . . .
H63 H 0.7056 0.2041 0.7836 0.067 Uiso 1 1 calc R . . . .
C64 C 0.5751(11) 0.2492(9) 0.8266(8) 0.046(4) Uani 1 1 d . U . . .
C65 C 0.4751(10) 0.2403(9) 0.8502(8) 0.044(4) Uani 1 1 d . U . . .
H65 H 0.4319 0.2780 0.8652 0.053 Uiso 1 1 calc R . . . .
C66 C 0.6086(11) 0.3162(10) 0.8282(8) 0.052(4) Uani 1 1 d . U . . .
C67 C 0.6279(11) 0.3718(10) 0.8301(8) 0.053(4) Uani 1 1 d . U . . .
C68 C 0.6474(9) 0.4440(10) 0.8276(8) 0.040(3) Uani 1 1 d . U . . .
C69 C 0.7019(10) 0.4407(10) 0.8763(8) 0.049(4) Uani 1 1 d . U . . .
H69 H 0.7256 0.3927 0.9096 0.058 Uiso 1 1 calc R . . . .
C70 C 0.7189(10) 0.5121(11) 0.8726(8) 0.050(4) Uani 1 1 d . U . . .
H70 H 0.7537 0.5118 0.9055 0.060 Uiso 1 1 calc R . . . .
C71 C 0.6878(10) 0.5831(10) 0.8237(8) 0.048(4) Uani 1 1 d . U . . .
H71 H 0.7035 0.6303 0.8213 0.058 Uiso 1 1 calc R . . . .
C72 C 0.6329(9) 0.5831(9) 0.7781(8) 0.042(4) Uani 1 1 d . U . . .
C73 C 0.6143(8) 0.5133(9) 0.7807(7) 0.037(3) Uani 1 1 d . U . . .
H73 H 0.5774 0.5141 0.7487 0.044 Uiso 1 1 calc R . . . .
C74 C 0.5963(11) 0.6554(11) 0.7254(9) 0.050(4) Uani 1 1 d . U . . .
C75 C 0.5635(10) 0.7150(9) 0.6841(9) 0.042(4) Uani 1 1 d . U . . .
C76 C 0.5136(11) 0.7771(9) 0.6349(9) 0.049(4) Uani 1 1 d . U . . .
C77 C 0.5634(11) 0.8318(10) 0.5691(10) 0.071(5) Uani 1 1 d . U . . .
H77 H 0.6340 0.8267 0.5557 0.085 Uiso 1 1 calc R . . . .
C78 C 0.5092(13) 0.8909(11) 0.5261(10) 0.070(5) Uani 1 1 d . U . . .
H78 H 0.5417 0.9288 0.4833 0.084 Uiso 1 1 calc R . . . .
C79 C 0.4063(10) 0.8961(9) 0.5448(8) 0.049(4) Uani 1 1 d . U . . .
H79 H 0.3694 0.9369 0.5133 0.059 Uiso 1 1 calc R . . . .
C80 C 0.4114(10) 0.7882(8) 0.6490(7) 0.037(3) Uani 1 1 d . U . . .
H80 H 0.3768 0.7528 0.6927 0.045 Uiso 1 1 calc R . . . .
S4 S 0.5867(7) -0.0417(5) 0.7419(4) 0.080(3) Uani 0.622(11) 1 d D U P B 1
F10 F 0.5451(17) 0.0779(9) 0.6332(11) 0.124(9) Uani 0.622(11) 1 d D U P B 1
F11 F 0.4855(14) -0.0300(15) 0.6547(11) 0.112(8) Uani 0.622(11) 1 d D U P B 1
F12 F 0.6406(14) -0.0122(15) 0.6054(8) 0.150(11) Uani 0.622(11) 1 d D U P B 1
O10 O 0.4979(13) -0.0214(15) 0.7836(11) 0.146(13) Uani 0.622(11) 1 d D U P B 1
O11 O 0.6730(8) -0.0040(7) 0.7317(6) 0.087(4) Uani 0.622(11) 1 d D U P B 1
O12 O 0.6091(10) -0.1223(6) 0.7495(7) 0.117(5) Uani 0.622(11) 1 d D U P B 1
C84 C 0.5599(13) 0.0029(10) 0.6524(8) 0.082(6) Uani 0.622(11) 1 d D U P B 1
S4A S 0.6258(9) -0.0403(7) 0.7027(7) 0.075(4) Uani 0.378(11) 1 d D U P B 2
F10A F 0.4515(17) -0.022(3) 0.678(2) 0.145(18) Uani 0.378(11) 1 d D U P B 2
F11A F 0.507(3) 0.0827(14) 0.666(2) 0.141(16) Uani 0.378(11) 1 d D U P B 2
F12A F 0.4514(19) -0.004(2) 0.7704(14) 0.136(16) Uani 0.378(11) 1 d D U P B 2
O10A O 0.666(2) -0.0275(16) 0.6287(9) 0.090(12) Uani 0.378(11) 1 d D U P B 2
O11A O 0.6730(8) -0.0040(7) 0.7317(6) 0.087(4) Uani 0.378(11) 1 d D U P B 2
O12A O 0.6091(10) -0.1223(6) 0.7495(7) 0.117(5) Uani 0.378(11) 1 d D U P B 2
C84A C 0.5023(13) 0.0074(12) 0.7033(13) 0.090(10) Uani 0.378(11) 1 d D U P B 2
N91 N 0.351(2) 0.3929(13) 0.8985(16) 0.207(12) Uani 1 1 d . U . . .
C91 C 0.3866(19) 0.4292(14) 0.9271(17) 0.168(11) Uani 1 1 d . U . . .
C92 C 0.413(2) 0.4809(18) 0.9448(19) 0.243(18) Uani 1 1 d . U . . .
H92A H 0.4124 0.5321 0.9053 0.365 Uiso 1 1 calc GR . . . .
H92B H 0.4807 0.4645 0.9543 0.365 Uiso 1 1 calc GR . . . .
H92C H 0.3668 0.4838 0.9878 0.365 Uiso 1 1 calc GR . . . .


_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
Cu1 O1 2.349(8) . ?
Cu1 O21 2.620(9) . ?
Cu1 N1 2.055(12) . ?
Cu1 N3 2.020(11) . ?
Cu1 N5 2.029(12) . ?
Cu1 N7 2.029(11) . ?
Cu2 O4 2.321(8) . ?
Cu2 O4A 2.321(8) . ?
Cu2 O7 2.436(7) . ?
Cu2 O7A 2.436(7) . ?
Cu2 N2 1.992(11) . ?
Cu2 N4 2.032(11) . ?
Cu2 N6 2.051(12) . ?
Cu2 N8 2.019(11) . ?
S1 O1 1.465(8) . ?
S1 O2 1.451(9) . ?
S1 O3 1.447(9) . ?
S1 C81 1.819(14) . ?
F1 C81 1.323(15) . ?
F2 C81 1.288(15) . ?
F3 C81 1.344(14) . ?
S2 O4 1.449(9) . ?
S2 O5 1.462(10) . ?
S2 O6 1.419(10) . ?
S2 C82 1.788(13) . ?
F4 C82 1.319(15) . ?
F5 C82 1.318(15) . ?
F6 C82 1.324(15) . ?
S2A O4A 1.442(15) . ?
S2A O5A 1.445(16) . ?
S2A O6A 1.433(17) . ?
S2A C82A 1.830(19) . ?
F4A C82A 1.32(2) . ?
F5A C82A 1.31(2) . ?
F6A C82A 1.317(19) . ?
S3 O7 1.444(9) . ?
S3 O8 1.452(13) . ?
S3 O9 1.452(13) . ?
S3 C83 1.817(15) . ?
F7 C83 1.333(17) . ?
F8 C83 1.319(17) . ?
F9 C83 1.346(16) . ?
S3A O7A 1.460(11) . ?
S3A O8A 1.469(14) . ?
S3A O9A 1.446(14) . ?
S3A C83A 1.804(17) . ?
F7A C83A 1.326(18) . ?
F8A C83A 1.316(18) . ?
F9A C83A 1.346(17) . ?
O21 H21A 0.9303 . ?
O21 H21B 0.9282 . ?
N1 C1 1.333(18) . ?
N1 C5 1.334(17) . ?
N2 C19 1.380(17) . ?
N2 C20 1.396(17) . ?
N3 C21 1.341(18) . ?
N3 C25 1.337(17) . ?
N4 C39 1.288(16) . ?
N4 C40 1.383(17) . ?
N5 C41 1.379(18) . ?
N5 C45 1.300(17) . ?
N6 C59 1.317(17) . ?
N6 C60 1.328(17) . ?
N7 C61 1.355(17) . ?
N7 C65 1.357(17) . ?
N8 C79 1.342(17) . ?
N8 C80 1.346(17) . ?
C1 H1 0.9500 . ?
C1 C2 1.39(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.40(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.41(2) . ?
C4 C5 1.364(19) . ?
C4 C6 1.42(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.20(2) . ?
C7 C8 1.40(2) . ?
C8 C9 1.43(2) . ?
C8 C13 1.38(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.38(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.36(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(18) . ?
C12 C13 1.348(19) . ?
C12 C14 1.43(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.173(19) . ?
C15 C16 1.48(2) . ?
C16 C17 1.346(19) . ?
C16 C20 1.402(18) . ?
C17 H17 0.9500 . ?
C17 C18 1.38(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.347(19) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.40(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.37(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.40(2) . ?
C24 C25 1.372(19) . ?
C24 C26 1.49(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.180(19) . ?
C27 C28 1.44(2) . ?
C28 C29 1.361(18) . ?
C28 C33 1.400(18) . ?
C29 H29 0.9500 . ?
C29 C30 1.41(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.333(19) . ?
C31 H31 0.9500 . ?
C31 C32 1.381(18) . ?
C32 C33 1.383(19) . ?
C32 C34 1.46(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.170(18) . ?
C35 C36 1.47(2) . ?
C36 C37 1.353(19) . ?
C36 C40 1.398(19) . ?
C37 H37 0.9500 . ?
C37 C38 1.38(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.36(2) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C41 C42 1.36(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.35(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.37(2) . ?
C44 C45 1.43(2) . ?
C44 C46 1.47(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.18(2) . ?
C47 C48 1.43(2) . ?
C48 C49 1.42(2) . ?
C48 C53 1.341(19) . ?
C49 H49 0.9500 . ?
C49 C50 1.38(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.342(19) . ?
C51 H51 0.9500 . ?
C51 C52 1.373(18) . ?
C52 C53 1.418(19) . ?
C52 C54 1.46(2) . ?
C53 H53 0.9500 . ?
C54 C55 1.188(19) . ?
C55 C56 1.43(2) . ?
C56 C57 1.41(2) . ?
C56 C60 1.419(19) . ?
C57 H57 0.9500 . ?
C57 C58 1.35(2) . ?
C58 H58 0.9500 . ?
C58 C59 1.38(2) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C61 C62 1.40(2) . ?
C62 H62 0.9500 . ?
C62 C63 1.38(2) . ?
C63 H63 0.9500 . ?
C63 C64 1.36(2) . ?
C64 C65 1.375(19) . ?
C64 C66 1.47(2) . ?
C65 H65 0.9500 . ?
C66 C67 1.17(2) . ?
C67 C68 1.44(2) . ?
C68 C69 1.415(19) . ?
C68 C73 1.36(2) . ?
C69 H69 0.9500 . ?
C69 C70 1.40(2) . ?
C70 H70 0.9500 . ?
C70 C71 1.38(2) . ?
C71 H71 0.9500 . ?
C71 C72 1.389(19) . ?
C72 C73 1.39(2) . ?
C72 C74 1.46(2) . ?
C73 H73 0.9500 . ?
C74 C75 1.20(2) . ?
C75 C76 1.41(2) . ?
C76 C77 1.43(2) . ?
C76 C80 1.374(19) . ?
C77 H77 0.9500 . ?
C77 C78 1.35(2) . ?
C78 H78 0.9500 . ?
C78 C79 1.38(2) . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
S4 O10 1.406(13) . ?
S4 O11 1.451(12) . ?
S4 O12 1.456(12) . ?
S4 C84 1.826(16) . ?
F10 C84 1.301(17) . ?
F11 C84 1.303(17) . ?
F12 C84 1.361(17) . ?
S4A O10A 1.439(15) . ?
S4A O11A 1.438(13) . ?
S4A O12A 1.480(14) . ?
S4A C84A 1.788(17) . ?
F10A C84A 1.318(19) . ?
F11A C84A 1.318(19) . ?
F12A C84A 1.348(18) . ?
N91 C91 1.33(4) . ?
C91 C92 1.34(3) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 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
O1 Cu1 O21 177.7(3) . . ?
N1 Cu1 O1 90.4(4) . . ?
N1 Cu1 O21 88.6(4) . . ?
N3 Cu1 O1 94.8(4) . . ?
N3 Cu1 O21 87.3(4) . . ?
N3 Cu1 N1 91.0(4) . . ?
N3 Cu1 N5 88.6(5) . . ?
N3 Cu1 N7 176.3(5) . . ?
N5 Cu1 O1 92.5(4) . . ?
N5 Cu1 O21 88.5(4) . . ?
N5 Cu1 N1 177.1(5) . . ?
N5 Cu1 N7 88.9(4) . . ?
N7 Cu1 O1 88.0(4) . . ?
N7 Cu1 O21 90.0(4) . . ?
N7 Cu1 N1 91.4(4) . . ?
O4 Cu2 O7 177.6(3) . . ?
O4A Cu2 O7A 177.6(3) . . ?
N2 Cu2 O4 92.9(4) . . ?
N2 Cu2 O4A 92.9(4) . . ?
N2 Cu2 O7 88.2(4) . . ?
N2 Cu2 O7A 88.2(4) . . ?
N2 Cu2 N4 89.8(4) . . ?
N2 Cu2 N6 178.3(5) . . ?
N2 Cu2 N8 89.6(4) . . ?
N4 Cu2 O4 90.1(4) . . ?
N4 Cu2 O4A 90.1(4) . . ?
N4 Cu2 O7 87.8(4) . . ?
N4 Cu2 O7A 87.8(4) . . ?
N4 Cu2 N6 90.8(4) . . ?
N6 Cu2 O4 88.7(4) . . ?
N6 Cu2 O4A 88.7(4) . . ?
N6 Cu2 O7 90.2(4) . . ?
N6 Cu2 O7A 90.2(4) . . ?
N8 Cu2 O4 93.9(4) . . ?
N8 Cu2 O4A 93.9(4) . . ?
N8 Cu2 O7 88.2(4) . . ?
N8 Cu2 O7A 88.2(4) . . ?
N8 Cu2 N4 176.0(4) . . ?
N8 Cu2 N6 89.7(4) . . ?
O1 S1 C81 102.8(6) . . ?
O2 S1 O1 116.4(6) . . ?
O2 S1 C81 102.4(6) . . ?
O3 S1 O1 114.6(6) . . ?
O3 S1 O2 115.7(7) . . ?
O3 S1 C81 101.8(7) . . ?
S1 O1 Cu1 146.6(6) . . ?
F1 C81 S1 109.8(10) . . ?
F1 C81 F3 106.8(13) . . ?
F2 C81 S1 109.8(11) . . ?
F2 C81 F1 111.3(13) . . ?
F2 C81 F3 110.9(13) . . ?
F3 C81 S1 108.2(10) . . ?
O4 S2 O5 109.0(7) . . ?
O4 S2 C82 102.1(6) . . ?
O5 S2 C82 104.0(7) . . ?
O6 S2 O4 116.7(7) . . ?
O6 S2 O5 117.5(8) . . ?
O6 S2 C82 105.4(7) . . ?
S2 O4 Cu2 147.8(6) . . ?
F4 C82 S2 111.0(11) . . ?
F4 C82 F6 105.7(13) . . ?
F5 C82 S2 110.2(11) . . ?
F5 C82 F4 108.0(14) . . ?
F5 C82 F6 110.9(13) . . ?
F6 C82 S2 110.9(10) . . ?
O4A S2A O5A 115.2(15) . . ?
O4A S2A C82A 98.9(11) . . ?
O5A S2A C82A 102.7(13) . . ?
O6A S2A O4A 116.3(15) . . ?
O6A S2A O5A 117.1(16) . . ?
O6A S2A C82A 102.6(13) . . ?
S2A O4A Cu2 145.8(10) . . ?
F4A C82A S2A 107.5(15) . . ?
F5A C82A S2A 107.6(15) . . ?
F5A C82A F4A 111.0(19) . . ?
F5A C82A F6A 111.3(19) . . ?
F6A C82A S2A 110.9(17) . . ?
F6A C82A F4A 108.5(18) . . ?
O7 S3 O8 115.1(9) . . ?
O7 S3 O9 113.8(9) . . ?
O7 S3 C83 101.2(7) . . ?
O8 S3 C83 104.4(9) . . ?
O9 S3 O8 116.3(11) . . ?
O9 S3 C83 103.3(9) . . ?
S3 O7 Cu2 158.0(6) . . ?
F7 C83 S3 111.9(12) . . ?
F7 C83 F9 106.1(14) . . ?
F8 C83 S3 111.3(12) . . ?
F8 C83 F7 107.6(15) . . ?
F8 C83 F9 109.6(15) . . ?
F9 C83 S3 110.2(12) . . ?
O7A S3A O8A 113.0(11) . . ?
O7A S3A C83A 101.6(8) . . ?
O8A S3A C83A 104.1(11) . . ?
O9A S3A O7A 116.0(11) . . ?
O9A S3A O8A 115.3(13) . . ?
O9A S3A C83A 104.7(10) . . ?
S3A O7A Cu2 159.0(6) . . ?
F7A C83A S3A 110.8(13) . . ?
F7A C83A F9A 106.7(16) . . ?
F8A C83A S3A 111.1(14) . . ?
F8A C83A F7A 107.9(17) . . ?
F8A C83A F9A 108.4(16) . . ?
F9A C83A S3A 111.8(13) . . ?
Cu1 O21 H21A 111.9 . . ?
Cu1 O21 H21B 112.0 . . ?
H21A O21 H21B 106.8 . . ?
C1 N1 Cu1 119.7(10) . . ?
C1 N1 C5 119.0(13) . . ?
C5 N1 Cu1 121.2(10) . . ?
C19 N2 Cu2 123.7(10) . . ?
C19 N2 C20 116.5(12) . . ?
C20 N2 Cu2 119.5(9) . . ?
C21 N3 Cu1 122.2(10) . . ?
C25 N3 Cu1 121.8(10) . . ?
C25 N3 C21 115.9(12) . . ?
C39 N4 Cu2 124.5(10) . . ?
C39 N4 C40 117.9(12) . . ?
C40 N4 Cu2 117.5(9) . . ?
C41 N5 Cu1 118.0(10) . . ?
C45 N5 Cu1 122.2(10) . . ?
C45 N5 C41 119.8(13) . . ?
C59 N6 Cu2 120.6(11) . . ?
C59 N6 C60 121.1(13) . . ?
C60 N6 Cu2 118.4(10) . . ?
C61 N7 Cu1 120.8(10) . . ?
C61 N7 C65 118.2(12) . . ?
C65 N7 Cu1 120.1(10) . . ?
C79 N8 Cu2 122.2(10) . . ?
C79 N8 C80 117.1(12) . . ?
C80 N8 Cu2 120.4(9) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(15) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 122.1 . . ?
C1 C2 C3 115.7(16) . . ?
C3 C2 H2 122.1 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(15) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C6 123.0(15) . . ?
C5 C4 C3 116.3(15) . . ?
C5 C4 C6 120.8(15) . . ?
N1 C5 C4 123.8(15) . . ?
N1 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C7 C6 C4 172.0(18) . . ?
C6 C7 C8 177.3(17) . . ?
C7 C8 C9 120.7(15) . . ?
C13 C8 C7 122.0(14) . . ?
C13 C8 C9 117.0(14) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 C8 117.7(15) . . ?
C10 C9 H9 121.1 . . ?
C9 C10 H10 118.4 . . ?
C11 C10 C9 123.2(14) . . ?
C11 C10 H10 118.4 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 118.9(15) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C14 118.8(14) . . ?
C13 C12 C11 119.0(14) . . ?
C13 C12 C14 122.2(13) . . ?
C8 C13 H13 118.0 . . ?
C12 C13 C8 124.0(13) . . ?
C12 C13 H13 118.0 . . ?
C15 C14 C12 176.3(16) . . ?
C14 C15 C16 174.1(16) . . ?
C17 C16 C15 123.9(13) . . ?
C17 C16 C20 121.2(14) . . ?
C20 C16 C15 114.6(13) . . ?
C16 C17 H17 120.8 . . ?
C16 C17 C18 118.3(14) . . ?
C18 C17 H17 120.8 . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.2(16) . . ?
C19 C18 H18 119.4 . . ?
N2 C19 H19 118.8 . . ?
C18 C19 N2 122.5(15) . . ?
C18 C19 H19 118.8 . . ?
N2 C20 C16 120.3(13) . . ?
N2 C20 H20 119.8 . . ?
C16 C20 H20 119.8 . . ?
N3 C21 H21 117.4 . . ?
N3 C21 C22 125.2(15) . . ?
C22 C21 H21 117.4 . . ?
C21 C22 H22 122.0 . . ?
C23 C22 C21 116.1(16) . . ?
C23 C22 H22 122.0 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.5(14) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C26 125.0(14) . . ?
C25 C24 C23 117.8(15) . . ?
C25 C24 C26 117.1(15) . . ?
N3 C25 C24 124.2(15) . . ?
N3 C25 H25 117.9 . . ?
C24 C25 H25 117.9 . . ?
C27 C26 C24 174.1(17) . . ?
C26 C27 C28 175.8(16) . . ?
C29 C28 C27 121.6(14) . . ?
C29 C28 C33 120.6(14) . . ?
C33 C28 C27 117.8(13) . . ?
C28 C29 H29 120.7 . . ?
C28 C29 C30 118.6(14) . . ?
C30 C29 H29 120.7 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.4(13) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 118.9 . . ?
C30 C31 C32 122.2(14) . . ?
C32 C31 H31 118.9 . . ?
C31 C32 C33 118.4(14) . . ?
C31 C32 C34 124.8(14) . . ?
C33 C32 C34 116.8(12) . . ?
C28 C33 H33 120.1 . . ?
C32 C33 C28 119.9(12) . . ?
C32 C33 H33 120.1 . . ?
C35 C34 C32 178.6(17) . . ?
C34 C35 C36 177.1(15) . . ?
C37 C36 C35 122.7(13) . . ?
C37 C36 C40 120.1(14) . . ?
C40 C36 C35 117.2(13) . . ?
C36 C37 H37 121.3 . . ?
C36 C37 C38 117.4(14) . . ?
C38 C37 H37 121.3 . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.5(15) . . ?
C39 C38 H38 119.7 . . ?
N4 C39 C38 123.5(15) . . ?
N4 C39 H39 118.2 . . ?
C38 C39 H39 118.2 . . ?
N4 C40 C36 120.5(13) . . ?
N4 C40 H40 119.8 . . ?
C36 C40 H40 119.8 . . ?
N5 C41 H41 121.2 . . ?
C42 C41 N5 117.5(16) . . ?
C42 C41 H41 121.2 . . ?
C41 C42 H42 118.3 . . ?
C43 C42 C41 123.4(17) . . ?
C43 C42 H42 118.3 . . ?
C42 C43 H43 119.8 . . ?
C42 C43 C44 120.4(17) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C45 114.9(15) . . ?
C43 C44 C46 124.5(16) . . ?
C45 C44 C46 120.5(14) . . ?
N5 C45 C44 123.9(14) . . ?
N5 C45 H45 118.0 . . ?
C44 C45 H45 118.0 . . ?
C47 C46 C44 176.0(18) . . ?
C46 C47 C48 178.1(19) . . ?
C49 C48 C47 119.0(15) . . ?
C53 C48 C47 119.9(14) . . ?
C53 C48 C49 121.1(14) . . ?
C48 C49 H49 121.2 . . ?
C50 C49 C48 117.6(14) . . ?
C50 C49 H49 121.2 . . ?
C49 C50 H50 119.6 . . ?
C51 C50 C49 120.7(13) . . ?
C51 C50 H50 119.6 . . ?
C50 C51 H51 118.5 . . ?
C50 C51 C52 123.0(14) . . ?
C52 C51 H51 118.5 . . ?
C51 C52 C53 117.1(13) . . ?
C51 C52 C54 124.1(13) . . ?
C53 C52 C54 118.8(12) . . ?
C48 C53 C52 120.4(12) . . ?
C48 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C55 C54 C52 175.3(16) . . ?
C54 C55 C56 173.0(17) . . ?
C57 C56 C55 122.3(15) . . ?
C57 C56 C60 118.2(14) . . ?
C60 C56 C55 119.5(15) . . ?
C56 C57 H57 121.2 . . ?
C58 C57 C56 117.6(15) . . ?
C58 C57 H57 121.2 . . ?
C57 C58 H58 119.1 . . ?
C57 C58 C59 121.8(16) . . ?
C59 C58 H58 119.1 . . ?
N6 C59 C58 120.7(15) . . ?
N6 C59 H59 119.7 . . ?
C58 C59 H59 119.7 . . ?
N6 C60 C56 120.4(14) . . ?
N6 C60 H60 119.8 . . ?
C56 C60 H60 119.8 . . ?
N7 C61 H61 119.5 . . ?
N7 C61 C62 121.1(14) . . ?
C62 C61 H61 119.5 . . ?
C61 C62 H62 120.5 . . ?
C63 C62 C61 119.1(16) . . ?
C63 C62 H62 120.5 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 C62 120.0(14) . . ?
C64 C63 H63 120.0 . . ?
C63 C64 C65 119.1(15) . . ?
C63 C64 C66 123.8(14) . . ?
C65 C64 C66 117.1(15) . . ?
N7 C65 C64 122.5(15) . . ?
N7 C65 H65 118.8 . . ?
C64 C65 H65 118.8 . . ?
C67 C66 C64 174.9(18) . . ?
C66 C67 C68 175.2(18) . . ?
C69 C68 C67 117.9(15) . . ?
C73 C68 C67 121.5(13) . . ?
C73 C68 C69 120.6(15) . . ?
C68 C69 H69 121.8 . . ?
C70 C69 C68 116.3(15) . . ?
C70 C69 H69 121.8 . . ?
C69 C70 H70 118.2 . . ?
C71 C70 C69 123.6(13) . . ?
C71 C70 H70 118.2 . . ?
C70 C71 H71 121.1 . . ?
C70 C71 C72 117.8(15) . . ?
C72 C71 H71 121.1 . . ?
C71 C72 C74 121.3(15) . . ?
C73 C72 C71 120.0(15) . . ?
C73 C72 C74 118.7(14) . . ?
C68 C73 C72 121.7(13) . . ?
C68 C73 H73 119.1 . . ?
C72 C73 H73 119.1 . . ?
C75 C74 C72 177.6(17) . . ?
C74 C75 C76 169.9(16) . . ?
C75 C76 C77 123.7(14) . . ?
C80 C76 C75 120.3(15) . . ?
C80 C76 C77 116.0(15) . . ?
C76 C77 H77 120.3 . . ?
C78 C77 C76 119.5(15) . . ?
C78 C77 H77 120.3 . . ?
C77 C78 H78 120.1 . . ?
C77 C78 C79 119.9(16) . . ?
C79 C78 H78 120.1 . . ?
N8 C79 C78 122.4(15) . . ?
N8 C79 H79 118.8 . . ?
C78 C79 H79 118.8 . . ?
N8 C80 C76 125.0(14) . . ?
N8 C80 H80 117.5 . . ?
C76 C80 H80 117.5 . . ?
O10 S4 O11 116.4(12) . . ?
O10 S4 O12 118.2(12) . . ?
O10 S4 C84 102.5(11) . . ?
O11 S4 O12 114.3(8) . . ?
O11 S4 C84 101.8(8) . . ?
O12 S4 C84 99.5(8) . . ?
F10 C84 S4 108.8(13) . . ?
F10 C84 F11 115.5(16) . . ?
F10 C84 F12 107.5(16) . . ?
F11 C84 S4 106.8(13) . . ?
F11 C84 F12 108.9(16) . . ?
F12 C84 S4 109.1(12) . . ?
O10A S4A O12A 113.6(13) . . ?
O10A S4A C84A 103.9(12) . . ?
O11A S4A O10A 115.7(13) . . ?
O11A S4A O12A 113.7(10) . . ?
O11A S4A C84A 105.1(10) . . ?
O12A S4A C84A 103.0(10) . . ?
F10A C84A S4A 110.4(15) . . ?
F10A C84A F12A 105.9(17) . . ?
F11A C84A S4A 109.0(15) . . ?
F11A C84A F10A 111.4(18) . . ?
F11A C84A F12A 108.5(17) . . ?
F12A C84A S4A 111.6(14) . . ?
N91 C91 C92 167(4) . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O21 H21A F9A 0.93 2.50 2.974(18) 111.9 .
O21 H21B N91 0.93 2.31 2.97(3) 127.6 .

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
Cu1 N1 C1 C2 178.3(12) . . . . ?
Cu1 N1 C5 C4 -175.6(10) . . . . ?
Cu1 N3 C21 C22 -178.1(13) . . . . ?
Cu1 N3 C25 C24 -177.7(11) . . . . ?
Cu1 N5 C41 C42 180.0(15) . . . . ?
Cu1 N5 C45 C44 -178.8(11) . . . . ?
Cu1 N7 C61 C62 172.6(12) . . . . ?
Cu1 N7 C65 C64 -172.9(11) . . . . ?
Cu2 N2 C19 C18 -177.2(12) . . . . ?
Cu2 N2 C20 C16 176.3(9) . . . . ?
Cu2 N4 C39 C38 -176.2(12) . . . . ?
Cu2 N4 C40 C36 173.3(10) . . . . ?
Cu2 N6 C59 C58 -177.7(11) . . . . ?
Cu2 N6 C60 C56 175.3(10) . . . . ?
Cu2 N8 C79 C78 -174.2(12) . . . . ?
Cu2 N8 C80 C76 173.0(11) . . . . ?
O1 S1 C81 F1 -179.2(10) . . . . ?
O1 S1 C81 F2 58.1(12) . . . . ?
O1 S1 C81 F3 -63.1(12) . . . . ?
O2 S1 O1 Cu1 -57.3(12) . . . . ?
O2 S1 C81 F1 59.7(12) . . . . ?
O2 S1 C81 F2 -63.0(12) . . . . ?
O2 S1 C81 F3 175.8(11) . . . . ?
O3 S1 O1 Cu1 82.2(12) . . . . ?
O3 S1 C81 F1 -60.3(12) . . . . ?
O3 S1 C81 F2 177.0(11) . . . . ?
O3 S1 C81 F3 55.9(12) . . . . ?
C81 S1 O1 Cu1 -168.2(10) . . . . ?
O4 S2 C82 F4 63.6(13) . . . . ?
O4 S2 C82 F5 -176.8(12) . . . . ?
O4 S2 C82 F6 -53.6(12) . . . . ?
O5 S2 O4 Cu2 73.7(13) . . . . ?
O5 S2 C82 F4 177.0(13) . . . . ?
O5 S2 C82 F5 -63.4(14) . . . . ?
O5 S2 C82 F6 59.8(13) . . . . ?
O6 S2 O4 Cu2 -62.4(14) . . . . ?
O6 S2 C82 F4 -58.8(14) . . . . ?
O6 S2 C82 F5 60.8(14) . . . . ?
O6 S2 C82 F6 -176.0(11) . . . . ?
C82 S2 O4 Cu2 -176.7(11) . . . . ?
O4A S2A C82A F4A -59(2) . . . . ?
O4A S2A C82A F5A 60(2) . . . . ?
O4A S2A C82A F6A -178(2) . . . . ?
O5A S2A O4A Cu2 -96(2) . . . . ?
O5A S2A C82A F4A -178(3) . . . . ?
O5A S2A C82A F5A -58(3) . . . . ?
O5A S2A C82A F6A 64(3) . . . . ?
O6A S2A O4A Cu2 46(2) . . . . ?
O6A S2A C82A F4A 60(3) . . . . ?
O6A S2A C82A F5A 180(3) . . . . ?
O6A S2A C82A F6A -58(3) . . . . ?
C82A S2A O4A Cu2 155.3(15) . . . . ?
O7 S3 C83 F7 59.2(15) . . . . ?
O7 S3 C83 F8 -61.2(14) . . . . ?
O7 S3 C83 F9 177.0(13) . . . . ?
O8 S3 O7 Cu2 -71(2) . . . . ?
O8 S3 C83 F7 -60.6(16) . . . . ?
O8 S3 C83 F8 178.9(15) . . . . ?
O8 S3 C83 F9 57.2(16) . . . . ?
O9 S3 O7 Cu2 67(2) . . . . ?
O9 S3 C83 F7 177.3(15) . . . . ?
O9 S3 C83 F8 56.8(16) . . . . ?
O9 S3 C83 F9 -64.9(15) . . . . ?
C83 S3 O7 Cu2 177.2(17) . . . . ?
O7A S3A C83A F7A 63.9(17) . . . . ?
O7A S3A C83A F8A -56.0(17) . . . . ?
O7A S3A C83A F9A -177.2(15) . . . . ?
O8A S3A O7A Cu2 85(2) . . . . ?
O8A S3A C83A F7A -178.6(18) . . . . ?
O8A S3A C83A F8A 62(2) . . . . ?
O8A S3A C83A F9A -59.7(18) . . . . ?
O9A S3A O7A Cu2 -51(2) . . . . ?
O9A S3A C83A F7A -57.2(19) . . . . ?
O9A S3A C83A F8A -177.1(18) . . . . ?
O9A S3A C83A F9A 61.7(18) . . . . ?
C83A S3A O7A Cu2 -164.2(19) . . . . ?
N1 C1 C2 C3 0(2) . . . . ?
N3 C21 C22 C23 -8(3) . . . . ?
N5 C41 C42 C43 -2(3) . . . . ?
N7 C61 C62 C63 -3(2) . . . . ?
C1 N1 C5 C4 3(2) . . . . ?
C1 C2 C3 C4 -1(2) . . . . ?
C2 C3 C4 C5 3(2) . . . . ?
C2 C3 C4 C6 -176.7(14) . . . . ?
C3 C4 C5 N1 -5(2) . . . . ?
C5 N1 C1 C2 -1(2) . . . . ?
C6 C4 C5 N1 175.5(13) . . . . ?
C7 C8 C9 C10 178.2(13) . . . . ?
C7 C8 C13 C12 -176.0(13) . . . . ?
C8 C9 C10 C11 -4(2) . . . . ?
C9 C8 C13 C12 -1.6(19) . . . . ?
C9 C10 C11 C12 2(2) . . . . ?
C10 C11 C12 C13 0.3(19) . . . . ?
C10 C11 C12 C14 -176.6(12) . . . . ?
C11 C12 C13 C8 -0.5(19) . . . . ?
C13 C8 C9 C10 3.8(19) . . . . ?
C14 C12 C13 C8 176.3(12) . . . . ?
C15 C16 C17 C18 174.4(15) . . . . ?
C15 C16 C20 N2 -174.8(11) . . . . ?
C16 C17 C18 C19 -2(3) . . . . ?
C17 C16 C20 N2 -1(2) . . . . ?
C17 C18 C19 N2 3(3) . . . . ?
C19 N2 C20 C16 1.9(18) . . . . ?
C20 N2 C19 C18 -3(2) . . . . ?
C20 C16 C17 C18 1(2) . . . . ?
C21 N3 C25 C24 -1(2) . . . . ?
C21 C22 C23 C24 6(2) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?
C22 C23 C24 C26 -178.4(15) . . . . ?
C23 C24 C25 N3 0(2) . . . . ?
C25 N3 C21 C22 5(2) . . . . ?
C26 C24 C25 N3 176.4(13) . . . . ?
C27 C28 C29 C30 179.2(13) . . . . ?
C27 C28 C33 C32 -178.4(12) . . . . ?
C28 C29 C30 C31 0(2) . . . . ?
C29 C28 C33 C32 1.3(19) . . . . ?
C29 C30 C31 C32 1(2) . . . . ?
C30 C31 C32 C33 0(2) . . . . ?
C30 C31 C32 C34 179.2(13) . . . . ?
C31 C32 C33 C28 -1.1(18) . . . . ?
C33 C28 C29 C30 -1(2) . . . . ?
C34 C32 C33 C28 179.7(12) . . . . ?
C35 C36 C37 C38 179.6(14) . . . . ?
C35 C36 C40 N4 -177.1(12) . . . . ?
C36 C37 C38 C39 -2(2) . . . . ?
C37 C36 C40 N4 4(2) . . . . ?
C37 C38 C39 N4 2(2) . . . . ?
C39 N4 C40 C36 -3(2) . . . . ?
C40 N4 C39 C38 0(2) . . . . ?
C40 C36 C37 C38 -1(2) . . . . ?
C41 N5 C45 C44 1(2) . . . . ?
C41 C42 C43 C44 2(4) . . . . ?
C42 C43 C44 C45 -1(3) . . . . ?
C42 C43 C44 C46 -178(2) . . . . ?
C43 C44 C45 N5 -1(2) . . . . ?
C45 N5 C41 C42 1(2) . . . . ?
C46 C44 C45 N5 176.6(14) . . . . ?
C47 C48 C49 C50 176.4(13) . . . . ?
C47 C48 C53 C52 -176.0(12) . . . . ?
C48 C49 C50 C51 1(2) . . . . ?
C49 C48 C53 C52 2(2) . . . . ?
C49 C50 C51 C52 -1(2) . . . . ?
C50 C51 C52 C53 1(2) . . . . ?
C50 C51 C52 C54 179.8(13) . . . . ?
C51 C52 C53 C48 -1.6(19) . . . . ?
C53 C48 C49 C50 -1(2) . . . . ?
C54 C52 C53 C48 179.8(12) . . . . ?
C55 C56 C57 C58 176.7(15) . . . . ?
C55 C56 C60 N6 -176.2(13) . . . . ?
C56 C57 C58 C59 3(3) . . . . ?
C57 C56 C60 N6 6(2) . . . . ?
C57 C58 C59 N6 -1(2) . . . . ?
C59 N6 C60 C56 -4(2) . . . . ?
C60 N6 C59 C58 2(2) . . . . ?
C60 C56 C57 C58 -5(2) . . . . ?
C61 N7 C65 C64 -4(2) . . . . ?
C61 C62 C63 C64 2(3) . . . . ?
C62 C63 C64 C65 -2(2) . . . . ?
C62 C63 C64 C66 179.7(15) . . . . ?
C63 C64 C65 N7 3(2) . . . . ?
C65 N7 C61 C62 4(2) . . . . ?
C66 C64 C65 N7 -178.5(13) . . . . ?
C67 C68 C69 C70 -179.6(13) . . . . ?
C67 C68 C73 C72 179.9(13) . . . . ?
C68 C69 C70 C71 -2(2) . . . . ?
C69 C68 C73 C72 1(2) . . . . ?
C69 C70 C71 C72 3(2) . . . . ?
C70 C71 C72 C73 -3(2) . . . . ?
C70 C71 C72 C74 179.3(13) . . . . ?
C71 C72 C73 C68 1(2) . . . . ?
C73 C68 C69 C70 0(2) . . . . ?
C74 C72 C73 C68 179.0(13) . . . . ?
C74 C75 C76 C77 -129(9) . . . . ?
C74 C75 C76 C80 52(10) . . . . ?
C75 C76 C77 C78 -178.1(17) . . . . ?
C75 C76 C80 N8 -180.0(13) . . . . ?
C76 C77 C78 C79 -3(3) . . . . ?
C77 C76 C80 N8 0(2) . . . . ?
C77 C78 C79 N8 2(3) . . . . ?
C79 N8 C80 C76 -1(2) . . . . ?
C80 N8 C79 C78 0(2) . . . . ?
C80 C76 C77 C78 1(2) . . . . ?
O10 S4 C84 F10 63.1(18) . . . . ?
O10 S4 C84 F11 -62.3(18) . . . . ?
O10 S4 C84 F12 -179.9(17) . . . . ?
O11 S4 C84 F10 -57.7(16) . . . . ?
O11 S4 C84 F11 177.0(14) . . . . ?
O11 S4 C84 F12 59.4(15) . . . . ?
O12 S4 C84 F10 -175.1(15) . . . . ?
O12 S4 C84 F11 59.5(15) . . . . ?
O12 S4 C84 F12 -58.1(15) . . . . ?
O10A S4A C84A F10A 58(3) . . . . ?
O10A S4A C84A F11A -65(2) . . . . ?
O10A S4A C84A F12A 176(2) . . . . ?
O11A S4A C84A F10A -180(2) . . . . ?
O11A S4A C84A F11A 57(2) . . . . ?
O11A S4A C84A F12A -62(2) . . . . ?
O12A S4A C84A F10A -61(3) . . . . ?
O12A S4A C84A F11A 177(2) . . . . ?
O12A S4A C84A F12A 57(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-17
_olex2_date_sample_submission    2016-07-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id JV178
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.551(2)
2 0.449(2)
####################################################################### 
# 
# 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_eb17063
_database_code_depnum_ccdc_archive 'CCDC 1570740'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2022-04-03 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT221_eb17063             
;
PROBLEM: Solv./Anion  Resd 3  C   Ueq(max)/Ueq(min) Range       10.0 Ratio
RESPONSE: Discussed in _refine_special_details.
;
_vrf_PLAT041_eb17063             
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Discussed in _refine_special_details.
;
_vrf_PLAT077_eb17063             
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms ..     Please Check
RESPONSE: Discussed in _refine_special_details.
;
_vrf_PLAT202_eb17063             
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          5 Check
RESPONSE: Discussed in _refine_special_details.
;
_vrf_PLAT223_eb17063             
;
PROBLEM: Solv./Anion  Resd 3  H   Ueq(max)/Ueq(min) Range       10.0 Ratio
RESPONSE: Discussed in _refine_special_details.
;
# Added during the CSD deposition process: Sunday 03 April 2022 07:01 PM
# end Validation Reply Form

_audit_creation_date             2022-04-03
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6485)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Br6 Re, C82 H48 Cu2 F6 N8 O6 S2, 1.171(C4 H10 O), 1.658(C H3 N O2)'
_chemical_formula_sum            'C88.34 H64.69 Br6 Cu2 F6 N9.66 O10.48 Re S2'
_chemical_formula_weight         2400.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C90 H50 Br6 Cu2 F6 N10 O12 Re1 S2'
_chemical_oxdiff_usercomment     '@ 120 K JV484a'
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'
Cu Cu -1.9646 0.5888 '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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.25190(10)
_cell_length_b                   24.1742(2)
_cell_length_c                   12.27730(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.7300(10)
_cell_angle_gamma                90
_cell_volume                     4526.30(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    46662
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.8350
_cell_measurement_theta_min      4.0250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.278
_exptl_absorpt_correction_T_max  0.4717
_exptl_absorpt_correction_T_min  0.2481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1142 before and 0.0835 after correction.
The Ratio of minimum to maximum transmission is 0.5260.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2350
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 1 0.0279
0 5 -1 0.0279
-5 4 0 0.1515
5 -1 -1 0.1923
0 -5 -3 0.0295
0 5 3 0.0213
-3 3 5 0.0869
0 -2 -5 0.0239
0 2 5 0.0187
0 4 -5 0.0242

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of diethyl ether and nitromethane  by vapour diffusion'
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.043
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0126 -4.9884 0.9988 0.2897 -0.0190 0.1642
0.0126 4.9884 -0.9988 -0.2897 0.0190 -0.1642
-4.9888 4.0282 -0.0092 -0.5248 -0.0457 0.4245
4.9966 -1.0368 -0.9895 0.3424 0.0202 -0.5368
-0.0103 -5.0051 -2.9955 0.2043 -0.3884 0.0263
0.0103 5.0051 2.9955 -0.2043 0.3884 -0.0263
-2.9947 3.0368 4.9873 -0.2403 0.4477 0.4115
-0.0019 -2.0178 -4.9928 0.0005 -0.5063 -0.1205
0.0019 2.0178 4.9928 -0.0005 0.5063 0.1205
0.0125 3.9733 -4.9931 -0.3215 -0.3726 -0.2762

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            109104
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.342
_diffrn_reflns_theta_min         3.426
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -128.00 -35.00   1.00    5.00    --  -41.67-178.00 -60.00   93
  2  ω    -79.00  37.00   1.00    5.00    --  -41.67  19.00-150.00  116
  3  ω   -128.00 -35.00   1.00    5.00    --  -41.67-178.00 150.00   93
  4  ω   -114.00 -19.00   1.00    5.00    --  -41.67 -38.00  30.00   95
  5  ω     57.00 128.00   1.00    5.00    --   41.67 178.00  60.00   71
  6  ω     10.00 116.00   1.00    5.00    --   41.67  77.00 150.00  106
  7  ω     39.00 121.00   1.00   20.00    --  111.00-125.00 150.00   82
  8  ω     66.00 178.00   1.00   20.00    --  111.00  15.00 -60.00  112
  9  ω     40.00 135.00   1.00   20.00    --  111.00 -45.00-120.00   95
 10  ω     39.00 121.00   1.00   20.00    --  111.00-125.00  90.00   82
 11  ω     80.00 178.00   1.00   20.00    --  111.00  77.00-150.00   98
 12  ω     39.00 121.00   1.00   20.00    --  111.00-125.00  30.00   82
 13  ω     39.00 121.00   1.00   20.00    --  111.00-125.00 -60.00   82
 14  ω     39.00 121.00   1.00   20.00    --  111.00-125.00-120.00   82
 15  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00 -90.00   79
 16  ω     94.00 178.00   1.00   20.00    --  111.00 125.00 -30.00   84
 17  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00 120.00  105
 18  ω     39.00 121.00   1.00   20.00    --  111.00-125.00  60.00   82
 19  ω     39.00 121.00   1.00   20.00    --  111.00-125.00   0.00   82
 20  ω     39.00 121.00   1.00   20.00    --  111.00-125.00-150.00   82
 21  ω     66.00 178.00   1.00   20.00    --  111.00  15.00  60.00  112
 22  ω     80.00 178.00   1.00   20.00    --  111.00  77.00 -90.00   98
 23  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00  60.00  105
 24  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00-150.00   79
 25  ω     87.00 178.00   1.00   20.00    --  111.00  45.00  60.00   91
 26  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00 -30.00  105
 27  ω     39.00 121.00   1.00   20.00    --  111.00-125.00 -30.00   82
 28  ω     94.00 178.00   1.00   20.00    --  111.00 125.00 -90.00   84
 29  ω     94.00 178.00   1.00   20.00    --  111.00 125.00-150.00   84
 30  ω     87.00 178.00   1.00   20.00    --  111.00  45.00-150.00   91
 31  ω     87.00 178.00   1.00   20.00    --  111.00  45.00 -30.00   91
 32  ω     41.00 139.00   1.00   20.00    --  111.00 -61.00   0.00   98
 33  ω   -116.00 -10.00   1.00    5.00    --  -41.67 -77.00   0.00  106
 34  ω   -116.00 -10.00   1.00    5.00    --  -41.67 -77.00 150.00  106
 35  ω   -116.00 -10.00   1.00    5.00    --  -41.67 -77.00 -90.00  106
 36  ω   -112.00 -15.00   1.00    5.00    --  -41.67 -57.00  30.00   97
 37  ω   -116.00 -10.00   1.00    5.00    --  -41.67 -77.00-120.00  106
 38  ω   -112.00 -15.00   1.00    5.00    --  -41.67 -57.00 150.00   97
 39  ω     87.00 178.00   1.00   20.00    --  111.00  30.00 150.00   91
 40  ω     80.00 176.00   1.00   20.00    --  111.00  77.00   0.00   96
 41  ω     80.00 178.00   1.00   20.00    --  111.00  77.00 150.00   98
 42  ω     83.00 178.00   1.00   20.00    --  111.00  61.00  90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0616349000
_diffrn_orient_matrix_UB_12      -0.0538983000
_diffrn_orient_matrix_UB_13      0.0216520000
_diffrn_orient_matrix_UB_21      0.0269491000
_diffrn_orient_matrix_UB_22      0.0222475000
_diffrn_orient_matrix_UB_23      0.0924020000
_diffrn_orient_matrix_UB_31      -0.1059326000
_diffrn_orient_matrix_UB_32      -0.0257356000
_diffrn_orient_matrix_UB_33      0.0345726000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8666
_reflns_number_total             9438
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.603
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         9438
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0638
_refine_ls_restrained_S_all      1.192
_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)+(0.0682P)²+30.7700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1747
_refine_special_details          
;
A disorder model of the CF3 group resulted in no better refinement than the ordered model.  A region of solvent was modelled as a disordered mix of diethyl ether and nitromethane, consistent with molecular shape inferred from peaks in a difference electron density map.  The solvent molecules were refined using an isotropic model and geometric restraints based on average values obtained from a search of the Cambridge Structural Database.  While the solvent can be masked using the solvent mask routine in Olex2 to give a cleaner pattern it was felt prefereable to report the model which includes the solvent molecules.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
221_ALERT_2_B Solv./Anion Resd 3   C   Ueq(max)/Ueq(min) Range       10.0 Ratio
411_ALERT_2_B Short Inter H...H Contact   H20A   ..  H36     .       1.97 Ang.

Solvent disorder.  Discussed above.

#===============================================================================

077_ALERT_4_C Unitcell contains non-integer number of atoms ..     Please Check
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          5 Check
223_ALERT_4_C Solv./Anion Resd 3   H   Ueq(max)/Ueq(min) Range       10.0 Ratio
242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         S1 Check
342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0104 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      4.127 Check
971_ALERT_2_C Check Calcd Residual Density  0.50A From    O201       1.54 eA-3
972_ALERT_2_C Check Calcd Residual Density  0.83A From     Re1      -1.64 eA-3
976_ALERT_2_C Check Calcd Residual Density  0.68A From    O402      -0.55 eA-3
977_ALERT_2_C Check the Negative Difference Density on    H20A      -0.41 eA-3
977_ALERT_2_C Check the Negative Difference Density on    H20B      -0.32 eA-3
977_ALERT_2_C Check the Negative Difference Density on    H20I      -0.31 eA-3
977_ALERT_2_C Check the Negative Difference Density on    H20J      -0.59 eA-3
977_ALERT_2_C Check the Negative Difference Density on     H30      -0.32 eA-3

Solvent disorder.  Discussed above.  Pertains to all the above alerts.

978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note
#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         13 Note
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       0.50 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      30.77 Why ?
142_ALERT_4_G s.u. on b - Axis Small or Missing ..............    0.00020 Ang.
143_ALERT_4_G s.u. on c - Axis Small or Missing ..............    0.00010 Ang.
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          4 Report
173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          6 Report
174_ALERT_4_G The CIF-Embedded .res File Contains FLAT Records          2 Report
242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C41 Check
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3)..        100 % Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  4)..        100 % Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  5)..        100 % Note
304_ALERT_4_G Non-Integer Number of Atoms (   8.79) in Resd. #          3 Check
304_ALERT_4_G Non-Integer Number of Atoms (   2.90) in Resd. #          4 Check
304_ALERT_4_G Non-Integer Number of Atoms (   2.90) in Resd. #          5 Check
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C4     -   C6     ..       1.44 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C7     -   C8     ..       1.42 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C12    -   C20    ..       1.44 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C17    -   C19    ..       1.42 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C24    -   C26    ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C27    -   C28    ..       1.44 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C32    -   C40    ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C37    -   C39    ..       1.44 Ang.
398_ALERT_2_G Deviating  C-O-C  Angle from 120 Deg for >O201        106.6 Degree
432_ALERT_2_G Short Inter X...Y Contact  Br3    ..  C18     ..       3.33 Ang.
432_ALERT_2_G Short Inter X...Y Contact  O401   ..  C38     ..       3.01 Ang.
794_ALERT_5_G Tentative Bond Valency for Re1     (IV)    .....       3.91 Note
794_ALERT_5_G Tentative Bond Valency for Cu1     (II)    .....       2.19 Note
860_ALERT_3_G Number of Least-Squares Restraints .............         21 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         62 Note

Nothing here is significant, they mostly pertain to disorder (rounding errors in the formulae etc).

#===============================================================================
;
_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. Restrained distances
 O301-N301 = O302-N301 = O402-N401 = O401-N401
 1.22 with sigma of 0.02
 N301-C303 = N401-C401
 1.44 with sigma of 0.02
 O201-C203 = O201-C201
 1.41 with sigma of 0.02
 C204-C203 = C202-C201
 1.48 with sigma of 0.02
 O301-O302 = O401-O402
 2.12 with sigma of 0.04
 C303-O301 = C401-O402
 2.28 with sigma of 0.04
 C303-O302 = C401-O401
 2.28 with sigma of 0.04
 C203-C201
 2.36 with sigma of 0.04
 O201-C204
 2.36 with sigma of 0.04
 O201-C202
 2.36 with sigma of 0.04
3. Restrained planarity
 O301, O302, N301, C303
 with sigma of 0.1
 O401, O402, N401, C401
 with sigma of 0.1
4. Others
 Sof(O301)=Sof(O302)=Sof(N301)=Sof(C303)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(O401)=Sof(O402)=Sof(N401)=Sof(C401)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(1)
 Sof(O201)=Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(C202)=Sof(H20C)=Sof(H20D)=
 Sof(H20E)=Sof(C203)=Sof(H20F)=Sof(H20G)=Sof(C204)=Sof(H20H)=Sof(H20I)=
 Sof(H20J)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C203(H20F,H20G)
5.b Me refined with riding coordinates:
 C202(H20C,H20D,H20E), C204(H20H,H20I,H20J), C303(H30A,H30B,H30C), C401(H40A,
 H40B,H40C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C21(H21), C22(H22), C23(H23), C25(H25),
  C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38)
;
_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 0.500000 0.500000 0.03377(13) Uani 1 2 d S . P . .
Br1 Br 0.39618(5) 0.57343(3) 0.56539(6) 0.04516(19) Uani 1 1 d . . . . .
Br2 Br 0.57369(5) 0.57168(3) 0.38611(7) 0.0481(2) Uani 1 1 d . . . . .
Br3 Br 0.60453(5) 0.51853(4) 0.65488(7) 0.0506(2) Uani 1 1 d . . . . .
Cu1 Cu 0.73692(6) 0.39535(4) 0.84844(8) 0.0352(2) Uani 1 1 d . . . . .
S1 S 0.89417(12) 0.32874(8) 1.02293(17) 0.0479(4) Uani 1 1 d . . . . .
F1 F 0.8101(6) 0.3076(6) 1.1973(7) 0.160(5) Uani 1 1 d . . . . .
F2 F 0.9464(5) 0.3090(3) 1.2217(5) 0.102(2) Uani 1 1 d . . . . .
F3 F 0.8812(8) 0.3853(4) 1.1971(7) 0.145(4) Uani 1 1 d . . . . .
O1 O 0.8174(3) 0.3580(2) 0.9833(4) 0.0441(11) Uani 1 1 d . . . . .
O2 O 0.9748(4) 0.3558(3) 1.0019(7) 0.076(2) Uani 1 1 d . . . . .
O3 O 0.8940(5) 0.2711(3) 0.9959(6) 0.075(2) Uani 1 1 d . . . . .
N1 N 0.6734(4) 0.3252(2) 0.8071(5) 0.0385(12) Uani 1 1 d . . . . .
N2 N 0.2049(4) 0.5310(2) 0.1248(5) 0.0372(12) Uani 1 1 d . . . . .
N3 N 0.6384(4) 0.4151(2) 0.9487(5) 0.0365(12) Uani 1 1 d . . . . .
N4 N 0.1809(4) 0.6191(2) 0.2753(5) 0.0397(13) Uani 1 1 d . . . . .
C19 C 0.2612(5) 0.3845(3) 0.1759(6) 0.0437(16) Uani 1 1 d . . . . .
C1 C 0.6842(5) 0.2798(3) 0.8677(6) 0.0420(15) Uani 1 1 d . . . . .
H1 H 0.717899 0.282133 0.933126 0.050 Uiso 1 1 calc R U . . .
C2 C 0.6476(5) 0.2291(3) 0.8381(7) 0.0464(17) Uani 1 1 d . . . . .
H2 H 0.657526 0.197022 0.881160 0.056 Uiso 1 1 calc R U . . .
C3 C 0.5966(5) 0.2268(3) 0.7447(7) 0.0468(17) Uani 1 1 d . . . . .
H3 H 0.570733 0.192713 0.722988 0.056 Uiso 1 1 calc R U . . .
C4 C 0.5830(4) 0.2738(3) 0.6825(6) 0.0394(15) Uani 1 1 d . . . . .
C5 C 0.6239(4) 0.3230(3) 0.7157(6) 0.0379(14) Uani 1 1 d . . . . .
H5 H 0.616615 0.355417 0.672838 0.045 Uiso 1 1 calc R U . . .
C6 C 0.5283(5) 0.2724(3) 0.5861(6) 0.0424(16) Uani 1 1 d . . . . .
C7 C 0.4814(4) 0.2688(3) 0.5079(7) 0.0417(16) Uani 1 1 d . . . . .
C8 C 0.4270(4) 0.2617(3) 0.4138(6) 0.0388(14) Uani 1 1 d . . . . .
C9 C 0.4077(5) 0.2082(3) 0.3767(7) 0.0430(16) Uani 1 1 d . . . . .
H9 H 0.429735 0.176997 0.415130 0.052 Uiso 1 1 calc R U . . .
C10 C 0.3564(5) 0.2010(3) 0.2837(7) 0.0463(17) Uani 1 1 d . . . . .
H10 H 0.343896 0.164685 0.258178 0.056 Uiso 1 1 calc R U . . .
C11 C 0.3233(5) 0.2461(3) 0.2281(6) 0.0421(15) Uani 1 1 d . . . . .
H11 H 0.288354 0.240794 0.164344 0.051 Uiso 1 1 calc R U . . .
C12 C 0.3411(5) 0.2996(3) 0.2652(6) 0.0410(15) Uani 1 1 d . . . . .
C13 C 0.3931(4) 0.3076(3) 0.3569(6) 0.0402(15) Uani 1 1 d . . . . .
H13 H 0.405957 0.344021 0.381406 0.048 Uiso 1 1 calc R U . . .
C14 C 0.1175(5) 0.5266(3) 0.1076(7) 0.0439(16) Uani 1 1 d . . . . .
H14 H 0.084477 0.559346 0.095684 0.053 Uiso 1 1 calc R U . . .
C15 C 0.0742(5) 0.4763(3) 0.1068(7) 0.0494(18) Uani 1 1 d . . . . .
H15 H 0.012795 0.474668 0.093080 0.059 Uiso 1 1 calc R U . . .
C16 C 0.1214(5) 0.4286(3) 0.1261(7) 0.0498(18) Uani 1 1 d . . . . .
H16 H 0.092639 0.393706 0.126601 0.060 Uiso 1 1 calc R U . . .
C17 C 0.2111(5) 0.4318(3) 0.1447(6) 0.0388(14) Uani 1 1 d . . . . .
C18 C 0.2501(4) 0.4843(3) 0.1406(6) 0.0365(14) Uani 1 1 d . . . . .
H18 H 0.311924 0.486823 0.149596 0.044 Uiso 1 1 calc R U . . .
C20 C 0.3008(5) 0.3462(3) 0.2120(7) 0.0427(16) Uani 1 1 d . . . . .
C21 C 0.6521(5) 0.4161(3) 1.0572(6) 0.0406(15) Uani 1 1 d . . . . .
H21 H 0.710378 0.412216 1.084374 0.049 Uiso 1 1 calc R U . . .
C22 C 0.5856(5) 0.4223(3) 1.1301(6) 0.0432(16) Uani 1 1 d . . . . .
H22 H 0.597641 0.423232 1.206171 0.052 Uiso 1 1 calc R U . . .
C23 C 0.5007(5) 0.4273(3) 1.0908(6) 0.0409(15) Uani 1 1 d . . . . .
H23 H 0.453546 0.430276 1.140176 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4842(4) 0.4280(3) 0.9804(6) 0.0366(14) Uani 1 1 d . . . . .
C25 C 0.5551(4) 0.4213(3) 0.9108(6) 0.0360(14) Uani 1 1 d . . . . .
H25 H 0.544612 0.420950 0.834323 0.043 Uiso 1 1 calc R U . . .
C26 C 0.3980(4) 0.4341(3) 0.9343(6) 0.0389(14) Uani 1 1 d . . . . .
C27 C 0.3281(4) 0.4381(3) 0.8902(6) 0.0394(15) Uani 1 1 d . . . . .
C28 C 0.2439(4) 0.4436(3) 0.8366(6) 0.0395(15) Uani 1 1 d . . . . .
C29 C 0.1755(5) 0.4081(3) 0.8644(7) 0.0484(17) Uani 1 1 d . . . . .
H29 H 0.184479 0.380327 0.918174 0.058 Uiso 1 1 calc R U . . .
C30 C 0.0940(5) 0.4134(4) 0.8128(7) 0.0521(19) Uani 1 1 d . . . . .
H30 H 0.047141 0.389609 0.831957 0.062 Uiso 1 1 calc R U . . .
C31 C 0.0815(5) 0.4532(4) 0.7342(7) 0.0512(19) Uani 1 1 d . . . . .
H31 H 0.025630 0.457004 0.699892 0.061 Uiso 1 1 calc R U . . .
C32 C 0.1501(5) 0.4880(3) 0.7041(6) 0.0403(15) Uani 1 1 d . . . . .
C33 C 0.2318(4) 0.4826(3) 0.7554(6) 0.0389(14) Uani 1 1 d . . . . .
H33 H 0.279130 0.505749 0.734493 0.047 Uiso 1 1 calc R U . . .
C34 C 0.1235(5) 0.6616(3) 0.2724(6) 0.0425(15) Uani 1 1 d . . . . .
H34 H 0.123005 0.685231 0.210673 0.051 Uiso 1 1 calc R U . . .
C35 C 0.0661(5) 0.6720(3) 0.3543(7) 0.0491(18) Uani 1 1 d . . . . .
H35 H 0.025905 0.701896 0.348496 0.059 Uiso 1 1 calc R U . . .
C36 C 0.0672(5) 0.6387(3) 0.4456(7) 0.0475(17) Uani 1 1 d . . . . .
H36 H 0.027930 0.645186 0.503599 0.057 Uiso 1 1 calc R U . . .
C37 C 0.1266(5) 0.5956(3) 0.4508(6) 0.0435(16) Uani 1 1 d . . . . .
C38 C 0.1825(4) 0.5868(3) 0.3640(6) 0.0395(15) Uani 1 1 d . . . . .
H38 H 0.222921 0.556926 0.367611 0.047 Uiso 1 1 calc R U . . .
C39 C 0.1322(5) 0.5591(3) 0.5437(6) 0.0443(16) Uani 1 1 d . . . . .
C40 C 0.1392(5) 0.5272(3) 0.6174(6) 0.0459(17) Uani 1 1 d . . . . .
C41 C 0.8809(9) 0.3327(5) 1.1661(10) 0.080(3) Uani 1 1 d . . . . .
O201 O 0.2000(5) 0.3581(3) 0.5610(6) 0.0326(18) Uiso 0.585(10) 1 d D . P A 1
C201 C 0.146(2) 0.3126(10) 0.535(2) 0.134(11) Uiso 0.585(10) 1 d D . P A 1
H20A H 0.085262 0.325646 0.549079 0.161 Uiso 0.585(10) 1 calc R U P A 1
H20B H 0.158702 0.284675 0.591729 0.161 Uiso 0.585(10) 1 calc R U P A 1
C202 C 0.139(4) 0.281(3) 0.434(4) 0.33(4) Uiso 0.585(10) 1 d D . P A 1
H20C H 0.094582 0.252034 0.441402 0.498 Uiso 0.585(10) 1 calc R U P A 1
H20D H 0.121116 0.306048 0.374047 0.498 Uiso 0.585(10) 1 calc R U P A 1
H20E H 0.195524 0.264536 0.417259 0.498 Uiso 0.585(10) 1 calc R U P A 1
C203 C 0.1864(19) 0.3988(14) 0.475(3) 0.164(17) Uiso 0.585(10) 1 d D . P A 1
H20F H 0.219990 0.382262 0.414559 0.196 Uiso 0.585(10) 1 calc R U P A 1
H20G H 0.223474 0.429804 0.501198 0.196 Uiso 0.585(10) 1 calc R U P A 1
C204 C 0.1135(8) 0.4302(5) 0.4115(9) 0.018(2) Uiso 0.585(10) 1 d D . P A 1
H20H H 0.140143 0.454810 0.357814 0.028 Uiso 0.585(10) 1 calc R U P A 1
H20I H 0.075258 0.403519 0.373966 0.028 Uiso 0.585(10) 1 calc R U P A 1
H20J H 0.078817 0.452091 0.462480 0.028 Uiso 0.585(10) 1 calc R U P A 1
O301 O 0.1930(13) 0.2136(9) 0.4990(17) 0.097(7) Uiso 0.415(10) 1 d D . P A 2
O302 O 0.104(2) 0.2640(13) 0.565(2) 0.158(13) Uiso 0.415(10) 1 d D . P A 2
N301 N 0.1327(10) 0.2429(7) 0.4859(12) 0.057(4) Uiso 0.415(10) 1 d D . P A 2
C303 C 0.1001(11) 0.2487(7) 0.3767(12) 0.041(4) Uiso 0.415(10) 1 d D . P A 2
H30A H 0.049957 0.273987 0.375758 0.061 Uiso 0.415(10) 1 calc R U P A 2
H30B H 0.146498 0.263524 0.330539 0.061 Uiso 0.415(10) 1 calc R U P A 2
H30C H 0.081644 0.212423 0.348923 0.061 Uiso 0.415(10) 1 calc R U P A 2
O401 O 0.1207(19) 0.4686(9) 0.373(2) 0.147(11) Uiso 0.415(10) 1 d D . P A 2
O402 O 0.0891(16) 0.3820(9) 0.370(2) 0.119(9) Uiso 0.415(10) 1 d D . P A 2
N401 N 0.1290(9) 0.4224(6) 0.3981(11) 0.032(4) Uiso 0.415(10) 1 d D . P A 2
C401 C 0.2087(11) 0.4100(7) 0.4695(13) 0.033(3) Uiso 0.415(10) 1 d D . P A 2
H40A H 0.210474 0.370425 0.486289 0.050 Uiso 0.415(10) 1 calc R U P A 2
H40B H 0.262059 0.420526 0.430950 0.050 Uiso 0.415(10) 1 calc R U P A 2
H40C H 0.204992 0.431208 0.537394 0.050 Uiso 0.415(10) 1 calc R U P A 2


_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 2.5171(7) 3_666 ?
Re1 Br1 2.5170(7) . ?
Re1 Br2 2.5022(8) . ?
Re1 Br2 2.5022(8) 3_666 ?
Re1 Br3 2.5062(8) 3_666 ?
Re1 Br3 2.5062(8) . ?
Cu1 O1 2.238(5) . ?
Cu1 N1 2.016(6) . ?
Cu1 N2 2.015(6) 3_666 ?
Cu1 N3 2.012(6) . ?
Cu1 N4 2.012(6) 3_666 ?
S1 O1 1.448(5) . ?
S1 O2 1.420(7) . ?
S1 O3 1.432(7) . ?
S1 C41 1.774(12) . ?
F1 C41 1.300(16) . ?
F2 C41 1.333(12) . ?
F3 C41 1.327(14) . ?
N1 C1 1.334(9) . ?
N1 C5 1.345(9) . ?
N2 C14 1.351(9) . ?
N2 C18 1.334(9) . ?
N3 C21 1.346(9) . ?
N3 C25 1.356(8) . ?
N4 C34 1.350(9) . ?
N4 C38 1.340(9) . ?
C19 C17 1.424(10) . ?
C19 C20 1.189(11) . ?
C1 H1 0.9500 . ?
C1 C2 1.392(10) . ?
C2 H2 0.9500 . ?
C2 C3 1.378(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(11) . ?
C4 C5 1.401(10) . ?
C4 C6 1.439(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.194(11) . ?
C7 C8 1.424(10) . ?
C8 C9 1.401(10) . ?
C8 C13 1.405(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(9) . ?
C12 C13 1.383(10) . ?
C12 C20 1.436(10) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.383(11) . ?
C15 H15 0.9500 . ?
C15 C16 1.379(11) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(10) . ?
C17 C18 1.404(9) . ?
C18 H18 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.369(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.381(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.375(11) . ?
C24 C25 1.396(10) . ?
C24 C26 1.432(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.194(10) . ?
C27 C28 1.440(9) . ?
C28 C29 1.397(10) . ?
C28 C33 1.384(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.394(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.373(12) . ?
C31 H31 0.9500 . ?
C31 C32 1.397(11) . ?
C32 C33 1.395(10) . ?
C32 C40 1.434(11) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C34 C35 1.364(11) . ?
C35 H35 0.9500 . ?
C35 C36 1.381(12) . ?
C36 H36 0.9500 . ?
C36 C37 1.380(11) . ?
C37 C38 1.389(11) . ?
C37 C39 1.445(11) . ?
C38 H38 0.9500 . ?
C39 C40 1.191(11) . ?
O201 C201 1.411(17) . ?
O201 C203 1.459(17) . ?
C201 H20A 0.9900 . ?
C201 H20B 0.9900 . ?
C201 C202 1.460(19) . ?
C202 H20C 0.9800 . ?
C202 H20D 0.9800 . ?
C202 H20E 0.9800 . ?
C203 H20F 0.9900 . ?
C203 H20G 0.9900 . ?
C203 C204 1.547(17) . ?
C204 H20H 0.9800 . ?
C204 H20I 0.9800 . ?
C204 H20J 0.9800 . ?
O301 N301 1.171(16) . ?
O302 N301 1.190(17) . ?
N301 C303 1.431(15) . ?
C303 H30A 0.9800 . ?
C303 H30B 0.9800 . ?
C303 H30C 0.9800 . ?
O401 N401 1.164(17) . ?
O402 N401 1.198(16) . ?
N401 C401 1.520(15) . ?
C401 H40A 0.9800 . ?
C401 H40B 0.9800 . ?
C401 H40C 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 180.0 . 3_666 ?
Br2 Re1 Br1 88.78(3) 3_666 3_666 ?
Br2 Re1 Br1 91.22(3) . 3_666 ?
Br2 Re1 Br1 91.22(3) 3_666 . ?
Br2 Re1 Br1 88.78(3) . . ?
Br2 Re1 Br2 180.0 3_666 . ?
Br2 Re1 Br3 89.18(3) 3_666 . ?
Br2 Re1 Br3 89.18(3) . 3_666 ?
Br2 Re1 Br3 90.82(3) . . ?
Br2 Re1 Br3 90.82(3) 3_666 3_666 ?
Br3 Re1 Br1 88.36(3) . 3_666 ?
Br3 Re1 Br1 88.36(3) 3_666 . ?
Br3 Re1 Br1 91.64(3) 3_666 3_666 ?
Br3 Re1 Br1 91.64(3) . . ?
Br3 Re1 Br3 180.0 3_666 . ?
N1 Cu1 O1 96.0(2) . . ?
N2 Cu1 O1 90.0(2) 3_666 . ?
N2 Cu1 N1 173.9(2) 3_666 . ?
N3 Cu1 O1 92.8(2) . . ?
N3 Cu1 N1 89.7(2) . . ?
N3 Cu1 N2 91.2(2) . 3_666 ?
N4 Cu1 O1 98.5(2) 3_666 . ?
N4 Cu1 N1 88.0(2) 3_666 . ?
N4 Cu1 N2 90.0(2) 3_666 3_666 ?
N4 Cu1 N3 168.6(2) 3_666 . ?
O1 S1 C41 101.8(4) . . ?
O2 S1 O1 114.3(4) . . ?
O2 S1 O3 113.9(5) . . ?
O2 S1 C41 105.4(6) . . ?
O3 S1 O1 113.5(4) . . ?
O3 S1 C41 106.4(5) . . ?
S1 O1 Cu1 151.6(4) . . ?
C1 N1 Cu1 119.7(5) . . ?
C1 N1 C5 119.8(6) . . ?
C5 N1 Cu1 120.4(5) . . ?
C14 N2 Cu1 121.8(5) . 3_666 ?
C18 N2 Cu1 119.9(5) . 3_666 ?
C18 N2 C14 117.6(6) . . ?
C21 N3 Cu1 120.1(5) . . ?
C21 N3 C25 118.1(6) . . ?
C25 N3 Cu1 121.3(5) . . ?
C34 N4 Cu1 121.5(5) . 3_666 ?
C38 N4 Cu1 120.5(5) . 3_666 ?
C38 N4 C34 118.0(6) . . ?
C20 C19 C17 173.6(9) . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.1(7) . . ?
C2 C1 H1 118.9 . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.3(7) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.3(7) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 118.3(7) . . ?
C3 C4 C6 121.1(7) . . ?
C5 C4 C6 120.7(7) . . ?
N1 C5 C4 121.2(6) . . ?
N1 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C7 C6 C4 176.7(8) . . ?
C6 C7 C8 177.2(8) . . ?
C9 C8 C7 119.5(7) . . ?
C9 C8 C13 119.5(7) . . ?
C13 C8 C7 121.0(6) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(7) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.4(6) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(7) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C20 119.9(7) . . ?
C13 C12 C11 120.2(7) . . ?
C13 C12 C20 119.9(6) . . ?
C8 C13 H13 120.1 . . ?
C12 C13 C8 119.9(6) . . ?
C12 C13 H13 120.1 . . ?
N2 C14 H14 118.6 . . ?
N2 C14 C15 122.7(7) . . ?
C15 C14 H14 118.6 . . ?
C14 C15 H15 120.5 . . ?
C16 C15 C14 119.0(7) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.2 . . ?
C15 C16 C17 119.6(7) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C19 121.6(6) . . ?
C16 C17 C18 117.6(6) . . ?
C18 C17 C19 120.6(6) . . ?
N2 C18 C17 123.5(6) . . ?
N2 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C19 C20 C12 173.4(8) . . ?
N3 C21 H21 118.6 . . ?
N3 C21 C22 122.8(7) . . ?
C22 C21 H21 118.6 . . ?
C21 C22 H22 120.7 . . ?
C21 C22 C23 118.7(7) . . ?
C23 C22 H22 120.7 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.3(7) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 117.9(6) . . ?
C23 C24 C26 123.1(7) . . ?
C25 C24 C26 119.0(6) . . ?
N3 C25 C24 122.1(7) . . ?
N3 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C27 C26 C24 176.1(8) . . ?
C26 C27 C28 179.4(8) . . ?
C29 C28 C27 119.8(7) . . ?
C33 C28 C27 120.1(6) . . ?
C33 C28 C29 120.1(7) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.8(7) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 C29 120.0(7) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.6(7) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C40 120.9(7) . . ?
C33 C32 C31 119.5(7) . . ?
C33 C32 C40 119.4(7) . . ?
C28 C33 C32 119.9(7) . . ?
C28 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
N4 C34 H34 118.5 . . ?
N4 C34 C35 123.0(7) . . ?
C35 C34 H34 118.5 . . ?
C34 C35 H35 120.4 . . ?
C34 C35 C36 119.2(7) . . ?
C36 C35 H35 120.4 . . ?
C35 C36 H36 120.7 . . ?
C37 C36 C35 118.6(8) . . ?
C37 C36 H36 120.7 . . ?
C36 C37 C38 119.3(7) . . ?
C36 C37 C39 121.9(7) . . ?
C38 C37 C39 118.8(7) . . ?
N4 C38 C37 121.9(7) . . ?
N4 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C40 C39 C37 176.8(8) . . ?
C39 C40 C32 178.0(9) . . ?
F1 C41 S1 111.9(9) . . ?
F1 C41 F2 105.5(11) . . ?
F1 C41 F3 111.3(12) . . ?
F2 C41 S1 113.0(9) . . ?
F3 C41 S1 109.6(9) . . ?
F3 C41 F2 105.4(10) . . ?
C201 O201 C203 106.4(18) . . ?
O201 C201 H20A 104.9 . . ?
O201 C201 H20B 104.9 . . ?
O201 C201 C202 129(3) . . ?
H20A C201 H20B 105.8 . . ?
C202 C201 H20A 104.9 . . ?
C202 C201 H20B 104.9 . . ?
C201 C202 H20C 109.5 . . ?
C201 C202 H20D 109.5 . . ?
C201 C202 H20E 109.5 . . ?
H20C C202 H20D 109.5 . . ?
H20C C202 H20E 109.5 . . ?
H20D C202 H20E 109.5 . . ?
O201 C203 H20F 101.4 . . ?
O201 C203 H20G 101.4 . . ?
O201 C203 C204 142(2) . . ?
H20F C203 H20G 104.6 . . ?
C204 C203 H20F 101.4 . . ?
C204 C203 H20G 101.4 . . ?
C203 C204 H20H 109.5 . . ?
C203 C204 H20I 109.5 . . ?
C203 C204 H20J 109.5 . . ?
H20H C204 H20I 109.5 . . ?
H20H C204 H20J 109.5 . . ?
H20I C204 H20J 109.5 . . ?
O301 N301 O302 116(2) . . ?
O301 N301 C303 116.8(17) . . ?
O302 N301 C303 127(2) . . ?
N301 C303 H30A 109.5 . . ?
N301 C303 H30B 109.5 . . ?
N301 C303 H30C 109.5 . . ?
H30A C303 H30B 109.5 . . ?
H30A C303 H30C 109.5 . . ?
H30B C303 H30C 109.5 . . ?
O401 N401 O402 131(2) . . ?
O401 N401 C401 115.0(18) . . ?
O402 N401 C401 113.8(17) . . ?
N401 C401 H40A 109.5 . . ?
N401 C401 H40B 109.5 . . ?
N401 C401 H40C 109.5 . . ?
H40A C401 H40B 109.5 . . ?
H40A C401 H40C 109.5 . . ?
H40B C401 H40C 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
Cu1 N1 C1 C2 -174.7(6) . . . . ?
Cu1 N1 C5 C4 176.6(5) . . . . ?
Cu1 N2 C14 C15 -169.2(6) 3_666 . . . ?
Cu1 N2 C18 C17 167.2(6) 3_666 . . . ?
Cu1 N3 C21 C22 -171.6(5) . . . . ?
Cu1 N3 C25 C24 171.7(5) . . . . ?
Cu1 N4 C34 C35 179.1(6) 3_666 . . . ?
Cu1 N4 C38 C37 180.0(5) 3_666 . . . ?
O1 S1 C41 F1 62.5(10) . . . . ?
O1 S1 C41 F2 -178.6(9) . . . . ?
O1 S1 C41 F3 -61.4(10) . . . . ?
O2 S1 O1 Cu1 60.3(8) . . . . ?
O2 S1 C41 F1 -177.9(9) . . . . ?
O2 S1 C41 F2 -58.9(10) . . . . ?
O2 S1 C41 F3 58.2(10) . . . . ?
O3 S1 O1 Cu1 -72.7(8) . . . . ?
O3 S1 C41 F1 -56.6(10) . . . . ?
O3 S1 C41 F2 62.3(11) . . . . ?
O3 S1 C41 F3 179.5(9) . . . . ?
N1 C1 C2 C3 -2.0(12) . . . . ?
N2 C14 C15 C16 1.2(13) . . . . ?
N3 C21 C22 C23 0.7(11) . . . . ?
N4 C34 C35 C36 1.3(12) . . . . ?
C19 C17 C18 N2 -171.7(7) . . . . ?
C1 N1 C5 C4 0.1(10) . . . . ?
C1 C2 C3 C4 0.3(12) . . . . ?
C2 C3 C4 C5 1.5(11) . . . . ?
C2 C3 C4 C6 -178.6(7) . . . . ?
C3 C4 C5 N1 -1.8(10) . . . . ?
C5 N1 C1 C2 1.8(11) . . . . ?
C6 C4 C5 N1 178.3(6) . . . . ?
C7 C8 C9 C10 -178.6(7) . . . . ?
C7 C8 C13 C12 179.5(7) . . . . ?
C8 C9 C10 C11 -0.7(12) . . . . ?
C9 C8 C13 C12 0.1(11) . . . . ?
C9 C10 C11 C12 -0.2(12) . . . . ?
C10 C11 C12 C13 1.1(11) . . . . ?
C10 C11 C12 C20 -175.1(7) . . . . ?
C11 C12 C13 C8 -1.0(11) . . . . ?
C13 C8 C9 C10 0.8(11) . . . . ?
C14 N2 C18 C17 -2.7(11) . . . . ?
C14 C15 C16 C17 -0.7(14) . . . . ?
C15 C16 C17 C19 173.5(8) . . . . ?
C15 C16 C17 C18 -1.3(12) . . . . ?
C16 C17 C18 N2 3.1(11) . . . . ?
C18 N2 C14 C15 0.5(12) . . . . ?
C20 C12 C13 C8 175.2(7) . . . . ?
C21 N3 C25 C24 -0.4(9) . . . . ?
C21 C22 C23 C24 -2.4(10) . . . . ?
C22 C23 C24 C25 2.6(10) . . . . ?
C22 C23 C24 C26 -178.8(6) . . . . ?
C23 C24 C25 N3 -1.2(10) . . . . ?
C25 N3 C21 C22 0.7(10) . . . . ?
C26 C24 C25 N3 -179.8(6) . . . . ?
C27 C28 C29 C30 179.9(8) . . . . ?
C27 C28 C33 C32 -179.7(7) . . . . ?
C28 C29 C30 C31 0.7(13) . . . . ?
C29 C28 C33 C32 2.6(11) . . . . ?
C29 C30 C31 C32 0.8(14) . . . . ?
C30 C31 C32 C33 -0.6(12) . . . . ?
C30 C31 C32 C40 176.0(8) . . . . ?
C31 C32 C33 C28 -1.1(11) . . . . ?
C33 C28 C29 C30 -2.4(12) . . . . ?
C34 N4 C38 C37 0.7(10) . . . . ?
C34 C35 C36 C37 -0.1(12) . . . . ?
C35 C36 C37 C38 -0.8(11) . . . . ?
C35 C36 C37 C39 179.7(7) . . . . ?
C36 C37 C38 N4 0.5(11) . . . . ?
C38 N4 C34 C35 -1.6(11) . . . . ?
C39 C37 C38 N4 -180.0(7) . . . . ?
C40 C32 C33 C28 -177.8(7) . . . . ?
C41 S1 O1 Cu1 173.4(8) . . . . ?
C201 O201 C203 C204 51(6) . . . . ?
C203 O201 C201 C202 52(6) . . . . ?

_olex2_date_sample_data_collection 2017-05-05
_olex2_date_sample_submission    2017-05-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id JV484a
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.845
_oxdiff_exptl_absorpt_empirical_full_min 0.672
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1570741'
_audit_update_record             
;
2017-08-24 deposited with the CCDC.	2022-05-10 downloaded from the CCDC.
;
# eb17028
_audit_creation_date             2017-03-02
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Re, C80 H48 N8 Pd2, 2(F6 P), 6(C2 H3 N)'
_chemical_formula_sum            'C92 H66 Cl6 F12 N14 P2 Pd2 Re'
_chemical_formula_weight         2269.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C92 H66 Cl6 F12 N14 P2 Pd2 Re1'
_chemical_oxdiff_usercomment     '@ 120 K JV322-hexane'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1451(4)
_cell_length_b                   12.7786(4)
_cell_length_c                   17.3925(6)
_cell_angle_alpha                93.695(3)
_cell_angle_beta                 99.071(3)
_cell_angle_gamma                118.328(3)
_cell_volume                     2316.00(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11783
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.2390
_cell_measurement_theta_min      3.9660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.183
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1123
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -7 3 0.0317
0 7 -3 0.0228
-4 8 -4 0.0450
-5 -3 1 0.0503
6 1 0 0.0571
6 -7 4 0.0620
-1 0 11 0.0164
1 0 -11 0.0164
5 -6 -7 0.0410

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of hexane and dichloromethane by vapour diffusion'
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.033
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0003 -6.9910 3.0098 -0.1053 0.3434 0.8954
0.0003 6.9910 -3.0098 0.1053 -0.3434 -0.8954
-4.0007 7.9899 -3.9922 0.2463 -0.7892 -0.5871
-5.0012 -2.9960 1.0277 0.0737 -0.3448 0.9281
6.0014 0.9985 -0.0297 -0.1352 0.5421 -0.7813
6.0014 -6.9913 3.9813 -0.3072 0.9399 0.2407
-0.9928 -0.0013 11.0009 -0.9752 0.0055 0.0837
0.9928 0.0013 -11.0009 0.9752 -0.0055 -0.0837
4.9942 -5.9912 -7.0117 0.6815 0.6937 0.2456

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.222
_diffrn_reflns_theta_min         3.981
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  29.00   1.00   10.00    --  -41.42  57.00-150.00   97
  2  ω   -127.00 -34.00   1.00   10.00    --  -41.42 178.00-180.00   93
  3  ω   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00  60.00   97
  4  ω     19.00 114.00   1.00   10.00    --   41.42  38.00   0.00   95
  5  ω      1.00  81.00   1.00   10.00    --   41.42 -99.00   0.00   80
  6  ω     87.00 178.00   1.00   30.00    --  111.00  45.00  60.00   91
  7  ω     40.00 125.00   1.00   30.00    --  111.00-131.00 138.00   85
  8  ω     41.00 128.00   1.00   30.00    --  111.00-138.00 -36.00   87
  9  ω     80.00 178.00   1.00   30.00    --  111.00  77.00   0.00   98
 10  ω     94.00 178.00   1.00   30.00    --  111.00 125.00-120.00   84
 11  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 120.00   95
 12  ω     87.00 178.00   1.00   30.00    --  111.00  30.00 -30.00   91
 13  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00-150.00   79
 14  ω     39.00 121.00   1.00   30.00    --  111.00-125.00   0.00   82
 15  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00 150.00   79
 16  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00 -30.00   79
 17  ω     41.00 139.00   1.00   30.00    --  111.00 -61.00 -30.00   98
 18  ω     36.00 135.00   1.00   30.00    --  111.00 -30.00  90.00   99
 19  ω   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00 150.00   97
 20  ω   -115.00 -10.00   1.00   10.00    --  -41.42 -77.00 -30.00  105
 21  ω   -112.00 -15.00   1.00   10.00    --  -41.42 -57.00-150.00   97
 22  ω   -115.00 -10.00   1.00   10.00    --  -41.42 -77.00  60.00  105
 23  ω   -112.00 -65.00   1.00   10.00    --  -41.42-138.00 -36.00   47
 24  ω     87.00 178.00   1.00   30.00    --  111.00  30.00 -90.00   91
 25  ω     87.00 178.00   1.00   30.00    --  111.00  30.00-150.00   91
 26  ω     83.00 178.00   1.00   30.00    --  111.00  61.00-150.00   95
 27  ω     83.00 178.00   1.00   30.00    --  111.00  61.00  90.00   95
 28  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0190161000
_diffrn_orient_matrix_UB_12      -0.0238428000
_diffrn_orient_matrix_UB_13      -0.0903642000
_diffrn_orient_matrix_UB_21      0.0978849000
_diffrn_orient_matrix_UB_22      -0.0451046000
_diffrn_orient_matrix_UB_23      0.0093297000
_diffrn_orient_matrix_UB_31      -0.1087299000
_diffrn_orient_matrix_UB_32      -0.1290316000
_diffrn_orient_matrix_UB_33      -0.0022176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7713
_reflns_number_total             9485
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         2.080
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9485
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0550
_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)+(0.0830P)²+4.3337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1489
_refine_special_details          
;
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Re1 Check
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C41 Check
342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00951 Ang.
480_ALERT_4_C Long H...A H-Bond Reported H38    ..  CL1     ..       2.89 Ang.
480_ALERT_4_C Long H...A H-Bond Reported H25    ..  CL3     ..       2.96 Ang.
480_ALERT_4_C Long H...A H-Bond Reported H1     ..  F6      ..       2.57 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      4.863 Check
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          3 Report
971_ALERT_2_C Check Calcd Residual Density  1.05A From     Re1       2.23 eA-3
972_ALERT_2_C Check Calcd Residual Density  0.81A From     Re1      -2.04 eA-3
972_ALERT_2_C Check Calcd Residual Density  0.87A From     Re1      -1.90 eA-3
978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Nothing here is significant

#===============================================================================
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.003 Degree
233_ALERT_4_G Hirshfeld (M-X Solvent)    Re1    --  Cl1     ..        5.8 s.u.
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of         P1 Check
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C4     -   C6     ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C7     -   C8     ..       1.42 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C12    -   C20    ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C17    -   C19    ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C24    -   C26    ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C27    -   C28    ..       1.43 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C32    -   C40    ..       1.44 Ang.
371_ALERT_2_G Long    C(sp2)-C(sp1) Bond  C37    -   C39    ..       1.43 Ang.
484_ALERT_4_G Round D-H..A Angle Rep for C5     ..  CL2     to        167 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C38    ..  CL1     to        152 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C21    ..  F6      to        154 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C21    ..  F1      to        151 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C25    ..  CL3     to        152 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C1     ..  F6      to        152 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C1     ..  F4      to        153 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C34    ..  F6      to        152 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C14    ..  F6      to        155 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C2     ..  N5      to        172 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C35    ..  F5      to        149 Degree
484_ALERT_4_G Round D-H..A Angle Rep for C15    ..  N6      to        149 Degree
794_ALERT_5_G Tentative Bond Valency for Re1     (IV)    .....       4.24 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        204 Note
933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          4 Note


Nothing here is significant

#===============================================================================
;
_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:
 C5(H5), C18(H18), C38(H38), C11(H11), C21(H21), C25(H25), C31(H31), C33(H33),
 C13(H13), C9(H9), C1(H1), C34(H34), C30(H30), C29(H29), C14(H14), C10(H10),
 C2(H2), C36(H36), C35(H35), C23(H23), C15(H15), C22(H22), C16(H16), C3(H3)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C)
;
_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 0.000000 0.500000 0.500000 0.02609(11) Uani 1 2 d S T P . .
Pd1 Pd 0.09807(4) 0.33638(3) 0.79642(2) 0.02257(11) Uani 1 1 d . . . . .
P1 P 0.78218(17) 0.76070(16) 0.95270(9) 0.0360(3) Uani 1 1 d . . . . .
Cl2 Cl 0.15091(17) 0.44181(17) 0.54956(11) 0.0474(4) Uani 1 1 d . . . . .
Cl1 Cl -0.15914(17) 0.33401(16) 0.54325(11) 0.0490(4) Uani 1 1 d . . . . .
Cl3 Cl 0.0521(2) 0.61878(17) 0.62392(10) 0.0505(4) Uani 1 1 d . . . . .
F6 F 0.8673(4) 0.7516(4) 1.0306(2) 0.0478(10) Uani 1 1 d . . . . .
F5 F 0.6930(5) 0.7676(4) 0.8767(2) 0.0543(11) Uani 1 1 d . . . . .
N4 N 0.0368(5) 0.8329(4) 0.2475(3) 0.0275(10) Uani 1 1 d . . . . .
N3 N 0.2368(4) 0.5043(4) 0.8421(3) 0.0264(9) Uani 1 1 d . . . . .
N1 N 0.2297(5) 0.2981(4) 0.7672(3) 0.0250(9) Uani 1 1 d . . . . .
F1 F 0.6741(5) 0.6253(5) 0.9511(4) 0.0742(16) Uani 1 1 d . . . . .
N2 N 0.0317(4) 0.6238(4) 0.1716(3) 0.0263(9) Uani 1 1 d . . . . .
F3 F 0.8872(6) 0.8914(5) 0.9524(4) 0.089(2) Uani 1 1 d . . . . .
F4 F 0.7116(6) 0.8021(6) 1.0063(3) 0.0763(17) Uani 1 1 d . . . . .
C5 C 0.2605(5) 0.3144(5) 0.6972(3) 0.0255(11) Uani 1 1 d . . . . .
H5 H 0.218665 0.343905 0.661223 0.031 Uiso 1 1 calc R . . . .
C18 C 0.0891(5) 0.5770(5) 0.2188(3) 0.0262(11) Uani 1 1 d . . . . .
H18 H 0.069123 0.563478 0.269126 0.031 Uiso 1 1 calc R . . . .
F2 F 0.8436(6) 0.7109(7) 0.8985(3) 0.0841(19) Uani 1 1 d . . . . .
C8 C 0.4188(6) 0.3510(5) 0.4565(3) 0.0260(11) Uani 1 1 d . . . . .
C38 C 0.1039(6) 0.8635(5) 0.3233(3) 0.0273(11) Uani 1 1 d . . . . .
H38 H 0.084962 0.802364 0.355449 0.033 Uiso 1 1 calc R . . . .
C28 C 0.4658(6) 0.9715(5) 0.6939(3) 0.0292(12) Uani 1 1 d . . . . .
C12 C 0.3635(5) 0.4110(5) 0.3332(3) 0.0277(11) Uani 1 1 d . . . . .
C11 C 0.4573(5) 0.3950(5) 0.3048(3) 0.0275(11) Uani 1 1 d . . . . .
H11 H 0.468433 0.406985 0.252589 0.033 Uiso 1 1 calc R . . . .
C21 C 0.3010(6) 0.5257(6) 0.9173(4) 0.0328(12) Uani 1 1 d . . . . .
H21 H 0.277225 0.461281 0.946990 0.039 Uiso 1 1 calc R . . . .
C32 C 0.4196(5) 1.0373(5) 0.5711(3) 0.0259(11) Uani 1 1 d . . . . .
C4 C 0.3523(6) 0.2897(5) 0.6746(3) 0.0297(12) Uani 1 1 d . . . . .
C25 C 0.2673(5) 0.5949(5) 0.8000(3) 0.0256(11) Uani 1 1 d . . . . .
H25 H 0.220420 0.579723 0.747581 0.031 Uiso 1 1 calc R . . . .
C17 C 0.1773(6) 0.5475(5) 0.1960(4) 0.0308(12) Uani 1 1 d . . . . .
C31 C 0.5415(6) 1.1401(5) 0.5915(3) 0.0278(11) Uani 1 1 d . . . . .
H31 H 0.567953 1.197286 0.556569 0.033 Uiso 1 1 calc R . . . .
C33 C 0.3827(6) 0.9524(5) 0.6221(3) 0.0286(11) Uani 1 1 d . . . . .
H33 H 0.301172 0.881609 0.608090 0.034 Uiso 1 1 calc R . . . .
C13 C 0.3433(6) 0.3880(5) 0.4083(3) 0.0284(11) Uani 1 1 d . . . . .
H13 H 0.278506 0.397105 0.427049 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5166(6) 0.3423(5) 0.4289(3) 0.0282(11) Uani 1 1 d . . . . .
H9 H 0.572010 0.322873 0.462125 0.034 Uiso 1 1 calc R . . . .
C39 C 0.2701(6) 1.0038(5) 0.4348(3) 0.0292(11) Uani 1 1 d . . . . .
C37 C 0.1991(6) 0.9802(5) 0.3558(3) 0.0277(11) Uani 1 1 d . . . . .
C1 C 0.2883(6) 0.2562(6) 0.8191(3) 0.0310(12) Uani 1 1 d . . . . .
H1 H 0.265838 0.244478 0.868991 0.037 Uiso 1 1 calc R . . . .
C34 C 0.0632(6) 0.9207(6) 0.2025(4) 0.0321(12) Uani 1 1 d . . . . .
H34 H 0.017332 0.900593 0.149374 0.038 Uiso 1 1 calc R . . . .
C30 C 0.6233(5) 1.1583(5) 0.6624(3) 0.0278(11) Uani 1 1 d . . . . .
H30 H 0.705837 1.227812 0.675710 0.033 Uiso 1 1 calc R . . . .
C40 C 0.3355(6) 1.0180(5) 0.4969(3) 0.0289(11) Uani 1 1 d . . . . .
C29 C 0.5856(5) 1.0760(5) 0.7138(3) 0.0277(11) Uani 1 1 d . . . . .
H29 H 0.641308 1.090384 0.762938 0.033 Uiso 1 1 calc R . . . .
C24 C 0.3680(6) 0.7127(5) 0.8324(3) 0.0289(11) Uani 1 1 d . . . . .
C14 C 0.0578(6) 0.6404(6) 0.0994(4) 0.0327(12) Uani 1 1 d . . . . .
H14 H 0.015465 0.672033 0.065838 0.039 Uiso 1 1 calc R . . . .
C10 C 0.5325(6) 0.3621(5) 0.3526(3) 0.0282(11) Uani 1 1 d . . . . .
H10 H 0.596744 0.352556 0.333332 0.034 Uiso 1 1 calc R . . . .
C2 C 0.3802(7) 0.2299(7) 0.8011(4) 0.0402(15) Uani 1 1 d . . . . .
H2 H 0.419623 0.199326 0.837817 0.048 Uiso 1 1 calc R . . . .
C6 C 0.3800(6) 0.3089(5) 0.5981(3) 0.0290(11) Uani 1 1 d . . . . .
C7 C 0.3979(6) 0.3281(5) 0.5335(3) 0.0298(12) Uani 1 1 d . . . . .
C36 C 0.2250(6) 1.0705(5) 0.3088(4) 0.0317(12) Uani 1 1 d . . . . .
H36 H 0.289030 1.151402 0.329266 0.038 Uiso 1 1 calc R . . . .
C19 C 0.2392(6) 0.4992(6) 0.2475(4) 0.0320(12) Uani 1 1 d . . . . .
C20 C 0.2936(6) 0.4573(5) 0.2865(3) 0.0289(11) Uani 1 1 d . . . . .
C35 C 0.1557(6) 1.0399(5) 0.2318(4) 0.0345(13) Uani 1 1 d . . . . .
H35 H 0.171275 1.100005 0.199120 0.041 Uiso 1 1 calc R . . . .
C23 C 0.4340(6) 0.7328(6) 0.9098(4) 0.0366(13) Uani 1 1 d . . . . .
H23 H 0.501880 0.810862 0.933342 0.044 Uiso 1 1 calc R . . . .
N6 N 0.1153(7) 0.6947(7) 0.8938(4) 0.0540(16) Uani 1 1 d . . . . .
C27 C 0.4288(6) 0.8834(5) 0.7453(4) 0.0296(12) Uani 1 1 d . . . . .
C15 C 0.1436(7) 0.6132(6) 0.0722(4) 0.0366(14) Uani 1 1 d . . . . .
H15 H 0.159997 0.625992 0.021006 0.044 Uiso 1 1 calc R . . . .
C22 C 0.3997(6) 0.6380(6) 0.9522(4) 0.0361(13) Uani 1 1 d . . . . .
H22 H 0.444108 0.650471 1.005011 0.043 Uiso 1 1 calc R . . . .
N7 N 0.0951(8) 1.0163(7) 0.6620(5) 0.067(2) Uani 1 1 d . . . . .
C16 C 0.2054(6) 0.5667(6) 0.1213(4) 0.0365(13) Uani 1 1 d . . . . .
H16 H 0.265816 0.548119 0.104503 0.044 Uiso 1 1 calc R . . . .
C26 C 0.3999(6) 0.8067(5) 0.7854(4) 0.0309(12) Uani 1 1 d . . . . .
C3 C 0.4143(6) 0.2488(6) 0.7287(4) 0.0357(14) Uani 1 1 d . . . . .
H3 H 0.479415 0.233978 0.716047 0.043 Uiso 1 1 calc R . . . .
C43 C 0.0967(9) 0.7496(8) 0.8516(5) 0.0536(19) Uani 1 1 d . . . . .
C41 C 0.6219(10) 1.0866(8) 0.9388(5) 0.062(2) Uani 1 1 d . . . . .
C45 C 0.0517(9) 0.9487(8) 0.6104(6) 0.056(2) Uani 1 1 d . . . . .
N5 N 0.5422(11) 1.1127(10) 0.9222(5) 0.087(3) Uani 1 1 d . . . . .
C46 C -0.0081(10) 0.8564(8) 0.5395(6) 0.067(2) Uani 1 1 d . . . . .
H46A H 0.052931 0.873681 0.504995 0.101 Uiso 1 1 calc GR . . . .
H46B H -0.084370 0.856894 0.511381 0.101 Uiso 1 1 calc GR . . . .
H46C H -0.032752 0.777077 0.554825 0.101 Uiso 1 1 calc GR . . . .
C44 C 0.0711(12) 0.8202(10) 0.7953(6) 0.081(3) Uani 1 1 d . . . . .
H44A H -0.014338 0.770364 0.761502 0.121 Uiso 1 1 calc GR . . . .
H44B H 0.135399 0.846405 0.762629 0.121 Uiso 1 1 calc GR . . . .
H44C H 0.075281 0.890847 0.824125 0.121 Uiso 1 1 calc GR . . . .
C42 C 0.7197(10) 1.0515(9) 0.9577(8) 0.080(3) Uani 1 1 d . . . . .
H42A H 0.704796 0.987675 0.916244 0.120 Uiso 1 1 calc GR . . . .
H42B H 0.715799 1.021936 1.008326 0.120 Uiso 1 1 calc GR . . . .
H42C H 0.804421 1.121371 0.961152 0.120 Uiso 1 1 calc GR . . . .


_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 Cl2 2.3522(15) 2_566 ?
Re1 Cl2 2.3522(15) . ?
Re1 Cl1 2.3610(16) . ?
Re1 Cl1 2.3610(16) 2_566 ?
Re1 Cl3 2.3635(17) 2_566 ?
Re1 Cl3 2.3635(17) . ?
Pd1 N4 1.994(5) 2_566 ?
Pd1 N3 2.000(5) . ?
Pd1 N1 2.004(5) . ?
Pd1 N2 2.013(5) 2_566 ?
P1 F6 1.616(4) . ?
P1 F5 1.607(4) . ?
P1 F1 1.595(5) . ?
P1 F3 1.548(5) . ?
P1 F4 1.582(5) . ?
P1 F2 1.564(5) . ?
N4 C38 1.360(7) . ?
N4 C34 1.350(7) . ?
N3 C21 1.350(8) . ?
N3 C25 1.342(7) . ?
N1 C5 1.331(7) . ?
N1 C1 1.353(7) . ?
N2 C18 1.340(7) . ?
N2 C14 1.349(7) . ?
C5 H5 0.9500 . ?
C5 C4 1.397(8) . ?
C18 H18 0.9500 . ?
C18 C17 1.394(8) . ?
C8 C13 1.409(8) . ?
C8 C9 1.397(8) . ?
C8 C7 1.426(8) . ?
C38 H38 0.9500 . ?
C38 C37 1.389(8) . ?
C28 C33 1.402(8) . ?
C28 C29 1.399(9) . ?
C28 C27 1.430(8) . ?
C12 C11 1.403(8) . ?
C12 C13 1.390(8) . ?
C12 C20 1.433(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.369(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.375(9) . ?
C32 C31 1.404(8) . ?
C32 C33 1.398(8) . ?
C32 C40 1.439(8) . ?
C4 C6 1.431(8) . ?
C4 C3 1.391(8) . ?
C25 H25 0.9500 . ?
C25 C24 1.416(8) . ?
C17 C19 1.431(8) . ?
C17 C16 1.403(9) . ?
C31 H31 0.9500 . ?
C31 C30 1.385(8) . ?
C33 H33 0.9500 . ?
C13 H13 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.394(8) . ?
C39 C37 1.432(8) . ?
C39 C40 1.183(9) . ?
C37 C36 1.399(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.391(9) . ?
C30 H30 0.9500 . ?
C30 C29 1.382(8) . ?
C29 H29 0.9500 . ?
C24 C23 1.394(9) . ?
C24 C26 1.430(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(8) . ?
C10 H10 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.387(9) . ?
C6 C7 1.196(8) . ?
C36 H36 0.9500 . ?
C36 C35 1.385(9) . ?
C19 C20 1.193(8) . ?
C35 H35 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.385(9) . ?
N6 C43 1.117(11) . ?
C27 C26 1.187(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(8) . ?
C22 H22 0.9500 . ?
N7 C45 1.072(12) . ?
C16 H16 0.9500 . ?
C3 H3 0.9500 . ?
C43 C44 1.467(12) . ?
C41 N5 1.169(13) . ?
C41 C42 1.456(13) . ?
C45 C46 1.468(13) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 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
Cl2 Re1 Cl2 180.0 2_566 . ?
Cl2 Re1 Cl1 90.47(6) . 2_566 ?
Cl2 Re1 Cl1 90.47(6) 2_566 . ?
Cl2 Re1 Cl1 89.53(6) . . ?
Cl2 Re1 Cl1 89.53(6) 2_566 2_566 ?
Cl2 Re1 Cl3 91.06(7) . 2_566 ?
Cl2 Re1 Cl3 91.06(7) 2_566 . ?
Cl2 Re1 Cl3 88.94(7) 2_566 2_566 ?
Cl2 Re1 Cl3 88.94(7) . . ?
Cl1 Re1 Cl1 180.00(9) . 2_566 ?
Cl1 Re1 Cl3 90.11(7) . 2_566 ?
Cl1 Re1 Cl3 89.89(7) . . ?
Cl1 Re1 Cl3 89.89(7) 2_566 2_566 ?
Cl1 Re1 Cl3 90.11(7) 2_566 . ?
Cl3 Re1 Cl3 180.0 2_566 . ?
N4 Pd1 N3 178.21(18) 2_566 . ?
N4 Pd1 N1 89.21(19) 2_566 . ?
N4 Pd1 N2 91.57(19) 2_566 2_566 ?
N3 Pd1 N1 89.52(19) . . ?
N3 Pd1 N2 89.67(19) . 2_566 ?
N1 Pd1 N2 178.65(18) . 2_566 ?
F5 P1 F6 177.9(3) . . ?
F1 P1 F6 89.6(3) . . ?
F1 P1 F5 89.0(3) . . ?
F3 P1 F6 91.1(3) . . ?
F3 P1 F5 90.4(3) . . ?
F3 P1 F1 178.8(4) . . ?
F3 P1 F4 93.4(4) . . ?
F3 P1 F2 90.5(4) . . ?
F4 P1 F6 90.0(2) . . ?
F4 P1 F5 88.4(3) . . ?
F4 P1 F1 87.6(4) . . ?
F2 P1 F6 90.8(3) . . ?
F2 P1 F5 90.7(3) . . ?
F2 P1 F1 88.5(4) . . ?
F2 P1 F4 176.0(4) . . ?
C38 N4 Pd1 121.2(4) . 2_566 ?
C34 N4 Pd1 120.6(4) . 2_566 ?
C34 N4 C38 118.1(5) . . ?
C21 N3 Pd1 118.5(4) . . ?
C25 N3 Pd1 121.8(4) . . ?
C25 N3 C21 119.8(5) . . ?
C5 N1 Pd1 120.4(4) . . ?
C5 N1 C1 119.6(5) . . ?
C1 N1 Pd1 120.0(4) . . ?
C18 N2 Pd1 121.9(4) . 2_566 ?
C18 N2 C14 119.0(5) . . ?
C14 N2 Pd1 119.0(4) . 2_566 ?
N1 C5 H5 118.9 . . ?
N1 C5 C4 122.3(5) . . ?
C4 C5 H5 118.9 . . ?
N2 C18 H18 119.1 . . ?
N2 C18 C17 121.9(5) . . ?
C17 C18 H18 119.1 . . ?
C13 C8 C7 119.8(5) . . ?
C9 C8 C13 119.2(5) . . ?
C9 C8 C7 121.0(5) . . ?
N4 C38 H38 118.6 . . ?
N4 C38 C37 122.9(5) . . ?
C37 C38 H38 118.6 . . ?
C33 C28 C27 120.0(6) . . ?
C29 C28 C33 119.4(5) . . ?
C29 C28 C27 120.5(5) . . ?
C11 C12 C20 119.8(5) . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 C20 120.1(5) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 C12 119.7(5) . . ?
C10 C11 H11 120.2 . . ?
N3 C21 H21 119.1 . . ?
N3 C21 C22 121.9(6) . . ?
C22 C21 H21 119.1 . . ?
C31 C32 C40 120.1(5) . . ?
C33 C32 C31 119.4(5) . . ?
C33 C32 C40 120.5(5) . . ?
C5 C4 C6 119.2(5) . . ?
C3 C4 C5 118.0(5) . . ?
C3 C4 C6 122.9(5) . . ?
N3 C25 H25 119.4 . . ?
N3 C25 C24 121.2(5) . . ?
C24 C25 H25 119.4 . . ?
C18 C17 C19 121.3(6) . . ?
C18 C17 C16 118.8(5) . . ?
C16 C17 C19 120.0(5) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 C32 120.2(5) . . ?
C30 C31 H31 119.9 . . ?
C28 C33 H33 120.0 . . ?
C32 C33 C28 120.1(5) . . ?
C32 C33 H33 120.0 . . ?
C8 C13 H13 120.0 . . ?
C12 C13 C8 120.0(5) . . ?
C12 C13 H13 120.0 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.8(5) . . ?
C10 C9 H9 120.1 . . ?
C40 C39 C37 173.0(6) . . ?
C38 C37 C39 119.4(5) . . ?
C38 C37 C36 118.4(5) . . ?
C36 C37 C39 122.1(6) . . ?
N1 C1 H1 119.3 . . ?
N1 C1 C2 121.5(5) . . ?
C2 C1 H1 119.3 . . ?
N4 C34 H34 119.0 . . ?
N4 C34 C35 121.9(6) . . ?
C35 C34 H34 119.0 . . ?
C31 C30 H30 119.8 . . ?
C29 C30 C31 120.4(5) . . ?
C29 C30 H30 119.8 . . ?
C39 C40 C32 177.7(7) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(5) . . ?
C30 C29 H29 119.8 . . ?
C25 C24 C26 119.8(5) . . ?
C23 C24 C25 118.2(5) . . ?
C23 C24 C26 122.0(6) . . ?
N2 C14 H14 118.6 . . ?
N2 C14 C15 122.7(5) . . ?
C15 C14 H14 118.6 . . ?
C11 C10 C9 121.2(5) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 119.1(5) . . ?
C3 C2 H2 120.5 . . ?
C7 C6 C4 175.7(6) . . ?
C6 C7 C8 179.7(6) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 C37 118.8(6) . . ?
C35 C36 H36 120.6 . . ?
C20 C19 C17 176.0(7) . . ?
C19 C20 C12 177.8(7) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.8(6) . . ?
C36 C35 H35 120.1 . . ?
C24 C23 H23 120.3 . . ?
C22 C23 C24 119.4(6) . . ?
C22 C23 H23 120.3 . . ?
C26 C27 C28 176.4(6) . . ?
C14 C15 H15 120.7 . . ?
C14 C15 C16 118.6(6) . . ?
C16 C15 H15 120.7 . . ?
C21 C22 C23 119.5(6) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 119.0(6) . . ?
C15 C16 H16 120.5 . . ?
C27 C26 C24 177.8(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 C4 119.6(5) . . ?
C2 C3 H3 120.2 . . ?
N6 C43 C44 179.2(11) . . ?
N5 C41 C42 178.5(11) . . ?
N7 C45 C46 179.7(12) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5 Cl2 0.95 2.61 3.540(6) 166.9 .
C38 H38 Cl1 0.95 2.89 3.752(6) 151.9 2_566
C21 H21 F6 0.95 2.54 3.416(8) 153.5 2_667
C21 H21 F1 0.95 2.29 3.155(8) 150.5 2_667
C25 H25 Cl3 0.95 2.96 3.829(6) 152.3 .
C1 H1 F6 0.95 2.57 3.439(7) 151.7 2_667
C1 H1 F4 0.95 2.30 3.173(8) 153.3 2_667
C34 H34 F6 0.95 2.50 3.364(8) 152.1 1_454
C14 H14 F6 0.95 2.47 3.357(7) 154.9 1_454
C2 H2 N5 0.95 2.58 3.527(10) 171.9 1_545
C35 H35 F5 0.95 2.38 3.224(7) 148.5 2_676
C15 H15 N6 0.95 2.51 3.354(9) 148.5 1_554

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
Pd1 N4 C38 C37 179.6(4) 2_566 . . . ?
Pd1 N4 C34 C35 179.3(5) 2_566 . . . ?
Pd1 N3 C21 C22 178.3(5) . . . . ?
Pd1 N3 C25 C24 -178.3(4) . . . . ?
Pd1 N1 C5 C4 179.5(4) . . . . ?
Pd1 N1 C1 C2 -179.4(5) . . . . ?
Pd1 N2 C18 C17 178.9(4) 2_566 . . . ?
Pd1 N2 C14 C15 -178.7(5) 2_566 . . . ?
N4 C38 C37 C39 -176.7(5) . . . . ?
N4 C38 C37 C36 1.3(8) . . . . ?
N4 C34 C35 C36 1.1(10) . . . . ?
N3 C21 C22 C23 0.8(10) . . . . ?
N3 C25 C24 C23 -0.8(8) . . . . ?
N3 C25 C24 C26 178.6(5) . . . . ?
N1 C5 C4 C6 179.7(6) . . . . ?
N1 C5 C4 C3 -1.2(9) . . . . ?
N1 C1 C2 C3 1.0(11) . . . . ?
N2 C18 C17 C19 179.1(6) . . . . ?
N2 C18 C17 C16 -0.6(9) . . . . ?
N2 C14 C15 C16 0.1(11) . . . . ?
C5 N1 C1 C2 0.2(10) . . . . ?
C5 C4 C3 C2 2.3(10) . . . . ?
C18 N2 C14 C15 -1.3(9) . . . . ?
C18 C17 C16 C15 -0.6(10) . . . . ?
C8 C9 C10 C11 2.7(9) . . . . ?
C38 N4 C34 C35 -0.3(9) . . . . ?
C38 C37 C36 C35 -0.5(9) . . . . ?
C12 C11 C10 C9 1.0(9) . . . . ?
C11 C12 C13 C8 1.4(9) . . . . ?
C21 N3 C25 C24 1.5(8) . . . . ?
C32 C31 C30 C29 -0.3(8) . . . . ?
C25 N3 C21 C22 -1.5(9) . . . . ?
C25 C24 C23 C22 0.2(9) . . . . ?
C31 C32 C33 C28 1.6(8) . . . . ?
C31 C30 C29 C28 1.9(8) . . . . ?
C33 C28 C29 C30 -1.7(8) . . . . ?
C33 C32 C31 C30 -1.4(8) . . . . ?
C13 C8 C9 C10 -4.3(9) . . . . ?
C13 C12 C11 C10 -3.0(9) . . . . ?
C9 C8 C13 C12 2.3(9) . . . . ?
C39 C37 C36 C35 177.4(6) . . . . ?
C37 C36 C35 C34 -0.6(9) . . . . ?
C1 N1 C5 C4 0.0(9) . . . . ?
C1 C2 C3 C4 -2.2(11) . . . . ?
C34 N4 C38 C37 -0.9(8) . . . . ?
C40 C32 C31 C30 -179.2(5) . . . . ?
C40 C32 C33 C28 179.4(5) . . . . ?
C29 C28 C33 C32 -0.1(8) . . . . ?
C24 C23 C22 C21 -0.2(10) . . . . ?
C14 N2 C18 C17 1.5(9) . . . . ?
C14 C15 C16 C17 0.9(11) . . . . ?
C6 C4 C3 C2 -178.6(7) . . . . ?
C7 C8 C13 C12 179.7(6) . . . . ?
C7 C8 C9 C10 178.3(6) . . . . ?
C19 C17 C16 C15 179.7(6) . . . . ?
C20 C12 C11 C10 173.6(6) . . . . ?
C20 C12 C13 C8 -175.3(5) . . . . ?
C27 C28 C33 C32 -178.9(5) . . . . ?
C27 C28 C29 C30 177.1(5) . . . . ?
C26 C24 C23 C22 -179.3(6) . . . . ?

_olex2_date_sample_data_collection 2017-03-28
_olex2_date_sample_submission    2017-01-19
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id JV322-hexane
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.669
