# 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_Re-1
_database_code_depnum_ccdc_archive 'CCDC 2165137'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-04-07 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H58 N2 O4 P4 Re, I, 4.5(C6 H14)'
_chemical_formula_sum            'C91 H121 I N2 O4 P4 Re'
_chemical_formula_weight         1743.87

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   30.4077(5)
_cell_length_b                   30.4077(5)
_cell_length_c                   23.4090(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18744.8(8)
_cell_formula_units_Z            9
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5465
_cell_measurement_theta_min      2.7930
_cell_measurement_theta_max      28.2800

_exptl_crystal_description       blocks
_exptl_crystal_colour            Orange-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             8109
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.183
_exptl_absorpt_coefficient_mu    1.957
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            12109
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.610
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             8249
_reflns_number_gt                6695
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0391P)²+20.5407P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8249
_refine_ls_number_parameters     347
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.02356(6) Uani 1 2 d S . P . .
O1 O 0.53455(7) 0.47817(7) 0.54150(8) 0.0287(4) Uani 1 1 d . . . . .
N1 N 0.58857(9) 0.64761(9) 0.46434(10) 0.0301(6) Uani 1 1 d D . . . .
C2 C 0.54751(12) 0.63509(11) 0.50471(12) 0.0303(7) Uani 1 1 d . . . . .
H2A H 0.516435 0.626849 0.482880 0.036 Uiso 1 1 calc R U . . .
H2B H 0.556384 0.665583 0.528018 0.036 Uiso 1 1 calc R U . . .
P3 P 0.53276(3) 0.58141(3) 0.55370(3) 0.02446(17) Uani 1 1 d . . . . .
C4 C 0.57279(12) 0.61241(11) 0.41640(12) 0.0303(7) Uani 1 1 d . . . . .
H4A H 0.596226 0.629265 0.384018 0.036 Uiso 1 1 calc R U . . .
H4B H 0.538419 0.604462 0.404158 0.036 Uiso 1 1 calc R U . . .
P5 P 0.57163(3) 0.55233(3) 0.43265(3) 0.02428(17) Uani 1 1 d . . . . .
C6 C 0.6083(2) 0.69983(12) 0.4437(3) 0.0360(19) Uani 0.575(6) 1 d DG U P A 1
C7 C 0.65898(19) 0.73353(16) 0.4564(2) 0.0412(17) Uani 0.575(6) 1 d DG U P A 1
C8 C 0.68136(19) 0.78384(15) 0.4388(2) 0.061(2) Uani 0.575(6) 1 d G U P A 1
H8A H 0.715965 0.806871 0.447537 0.074 Uiso 0.575(6) 1 calc R U P A 1
C9 C 0.6531(3) 0.80046(13) 0.4085(2) 0.063(2) Uani 0.575(6) 1 d G U P A 1
H9A H 0.668393 0.834846 0.396472 0.076 Uiso 0.575(6) 1 calc R U P A 1
C10 C 0.6025(3) 0.76676(19) 0.3957(2) 0.075(3) Uani 0.575(6) 1 d G U P A 1
H10A H 0.583147 0.778122 0.375016 0.090 Uiso 0.575(6) 1 calc R U P A 1
C11 C 0.5801(2) 0.71645(17) 0.4133(3) 0.054(2) Uani 0.575(6) 1 d G U P A 1
H11A H 0.545471 0.693422 0.404624 0.065 Uiso 0.575(6) 1 calc R U P A 1
O12 O 0.68831(19) 0.7181(2) 0.4834(2) 0.0708(19) Uani 0.575(6) 1 d D U P A 1
H12 H 0.721250 0.741640 0.478981 0.106 Uiso 0.575(6) 1 calc R U P A 1
C6' C 0.6200(3) 0.7006(2) 0.4508(5) 0.037(3) Uiso 0.425(6) 1 d DG U P A 2
C7' C 0.5996(2) 0.7252(3) 0.4200(4) 0.049(3) Uiso 0.425(6) 1 d DG U P A 2
C8' C 0.6297(3) 0.7764(3) 0.4065(4) 0.056(3) Uiso 0.425(6) 1 d G U P A 2
H8'A H 0.615760 0.793213 0.385435 0.067 Uiso 0.425(6) 1 calc R U P A 2
C9' C 0.6801(3) 0.8029(2) 0.4239(4) 0.060(3) Uiso 0.425(6) 1 d G U P A 2
H9'A H 0.700678 0.837843 0.414737 0.072 Uiso 0.425(6) 1 calc R U P A 2
C10' C 0.7005(2) 0.7782(3) 0.4548(4) 0.065(3) Uiso 0.425(6) 1 d G U P A 2
H10B H 0.735002 0.796366 0.466692 0.078 Uiso 0.425(6) 1 calc R U P A 2
C11' C 0.6705(3) 0.7271(3) 0.4683(4) 0.043(3) Uiso 0.425(6) 1 d G U P A 2
H11B H 0.684408 0.710258 0.489346 0.052 Uiso 0.425(6) 1 calc R U P A 2
O12' O 0.5503(2) 0.6968(3) 0.4009(3) 0.059(2) Uiso 0.425(6) 1 d D U P A 2
H12' H 0.548504 0.674461 0.374477 0.088 Uiso 0.425(6) 1 calc R U P A 2
C13 C 0.48827(11) 0.58938(11) 0.59844(12) 0.0273(6) Uani 1 1 d . . . . .
C14 C 0.44417(12) 0.58417(12) 0.57344(14) 0.0356(7) Uani 1 1 d . . . . .
H14 H 0.436097 0.572913 0.535010 0.043 Uiso 1 1 calc R U . . .
C15 C 0.41235(13) 0.59528(13) 0.60427(16) 0.0454(9) Uani 1 1 d . . . . .
H15 H 0.382749 0.592261 0.586835 0.055 Uiso 1 1 calc R U . . .
C16 C 0.42342(14) 0.61083(13) 0.66056(16) 0.0468(9) Uani 1 1 d . . . . .
H16 H 0.401654 0.618968 0.681469 0.056 Uiso 1 1 calc R U . . .
C17 C 0.46604(13) 0.61458(12) 0.68655(15) 0.0427(9) Uani 1 1 d . . . . .
H17 H 0.472973 0.624415 0.725505 0.051 Uiso 1 1 calc R U . . .
C18 C 0.49882(12) 0.60393(11) 0.65564(13) 0.0321(7) Uani 1 1 d . . . . .
H18 H 0.528138 0.606565 0.673380 0.039 Uiso 1 1 calc R U . . .
C19 C 0.59020(11) 0.60210(12) 0.59551(12) 0.0298(7) Uani 1 1 d . . . . .
C20 C 0.62976(12) 0.65226(13) 0.59420(13) 0.0382(8) Uani 1 1 d . . . . .
H20 H 0.625850 0.677036 0.573656 0.046 Uiso 1 1 calc R U . . .
C21 C 0.67469(13) 0.66618(16) 0.62264(15) 0.0527(10) Uani 1 1 d . . . . .
H21 H 0.701663 0.700383 0.621259 0.063 Uiso 1 1 calc R U . . .
C22 C 0.68046(15) 0.63031(18) 0.65320(16) 0.0578(11) Uani 1 1 d . . . . .
H22 H 0.711775 0.639760 0.671668 0.069 Uiso 1 1 calc R U . . .
C23 C 0.64100(15) 0.58112(17) 0.65684(15) 0.0552(10) Uani 1 1 d . . . . .
H23 H 0.644416 0.557094 0.679531 0.066 Uiso 1 1 calc R U . . .
C24 C 0.59603(13) 0.56648(14) 0.62729(13) 0.0404(8) Uani 1 1 d . . . . .
H24 H 0.569248 0.532188 0.628753 0.048 Uiso 1 1 calc R U . . .
C25 C 0.63628(11) 0.57323(12) 0.45574(12) 0.0298(7) Uani 1 1 d . . . . .
C26 C 0.67707(12) 0.61383(13) 0.42954(14) 0.0407(8) Uani 1 1 d . . . . .
H26 H 0.671431 0.629350 0.397302 0.049 Uiso 1 1 calc R U . . .
C27 C 0.72593(13) 0.63221(15) 0.44947(15) 0.0502(10) Uani 1 1 d . . . . .
H27 H 0.753580 0.660519 0.431431 0.060 Uiso 1 1 calc R U . . .
C28 C 0.73438(13) 0.60939(16) 0.49549(15) 0.0532(10) Uani 1 1 d . . . . .
H28 H 0.767949 0.622060 0.509352 0.064 Uiso 1 1 calc R U . . .
C29 C 0.69449(14) 0.56828(17) 0.52160(15) 0.0555(11) Uani 1 1 d . . . . .
H29 H 0.700647 0.552504 0.553211 0.067 Uiso 1 1 calc R U . . .
C30 C 0.64506(13) 0.54969(14) 0.50187(14) 0.0428(8) Uani 1 1 d . . . . .
H30 H 0.617543 0.521146 0.519747 0.051 Uiso 1 1 calc R U . . .
C31 C 0.56826(11) 0.53121(10) 0.35877(11) 0.0258(6) Uani 1 1 d . . . . .
C32 C 0.60178(11) 0.51683(11) 0.33824(12) 0.0278(6) Uani 1 1 d . . . . .
H32 H 0.625946 0.516061 0.363320 0.033 Uiso 1 1 calc R U . . .
C33 C 0.60049(12) 0.50344(11) 0.28114(13) 0.0350(7) Uani 1 1 d . . . . .
H33 H 0.623337 0.493080 0.267503 0.042 Uiso 1 1 calc R U . . .
C34 C 0.56619(13) 0.50524(12) 0.24466(13) 0.0396(8) Uani 1 1 d . . . . .
H34 H 0.565915 0.496805 0.205534 0.048 Uiso 1 1 calc R U . . .
C35 C 0.53208(13) 0.51917(12) 0.26408(13) 0.0405(8) Uani 1 1 d . . . . .
H35 H 0.508214 0.519975 0.238532 0.049 Uiso 1 1 calc R U . . .
C36 C 0.53275(12) 0.53205(12) 0.32133(13) 0.0339(7) Uani 1 1 d . . . . .
H36 H 0.509134 0.541397 0.334964 0.041 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.7848(19) . ?
Re1 O1 1.7849(19) 10_666 ?
Re1 P3 2.4969(7) 10_666 ?
Re1 P3 2.4970(7) . ?
Re1 P5 2.5092(7) 10_666 ?
Re1 P5 2.5092(7) . ?
N1 C6' 1.438(6) . ?
N1 C2 1.457(4) . ?
N1 C4 1.457(4) . ?
N1 C6 1.471(4) . ?
C2 P3 1.857(3) . ?
P3 C19 1.818(3) . ?
P3 C13 1.821(3) . ?
C4 P5 1.849(3) . ?
P5 C25 1.820(3) . ?
P5 C31 1.830(3) . ?
C6 C7 1.3900 . ?
C6 C11 1.3900 . ?
C7 O12 1.355(8) . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C6' C7' 1.3900 . ?
C6' C11' 1.3900 . ?
C7' O12' 1.378(8) . ?
C7' C8' 1.3900 . ?
C8' C9' 1.3900 . ?
C9' C10' 1.3900 . ?
C10' C11' 1.3900 . ?
C13 C18 1.396(4) . ?
C13 C14 1.398(4) . ?
C14 C15 1.378(4) . ?
C15 C16 1.384(5) . ?
C16 C17 1.384(5) . ?
C17 C18 1.395(4) . ?
C19 C20 1.393(4) . ?
C19 C24 1.396(4) . ?
C20 C21 1.382(5) . ?
C21 C22 1.387(6) . ?
C22 C23 1.375(6) . ?
C23 C24 1.392(5) . ?
C25 C26 1.381(4) . ?
C25 C30 1.393(4) . ?
C26 C27 1.381(4) . ?
C27 C28 1.373(5) . ?
C28 C29 1.375(5) . ?
C29 C30 1.394(5) . ?
C31 C32 1.381(4) . ?
C31 C36 1.401(4) . ?
C32 C33 1.392(4) . ?
C33 C34 1.370(5) . ?
C34 C35 1.379(5) . ?
C35 C36 1.394(4) . ?

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 Re1 O1 180.00(10) . 10_666 ?
O1 Re1 P3 85.56(6) . 10_666 ?
O1 Re1 P3 94.44(6) 10_666 10_666 ?
O1 Re1 P3 94.44(6) . . ?
O1 Re1 P3 85.56(6) 10_666 . ?
P3 Re1 P3 180.0 10_666 . ?
O1 Re1 P5 84.72(6) . 10_666 ?
O1 Re1 P5 95.28(6) 10_666 10_666 ?
P3 Re1 P5 84.15(2) 10_666 10_666 ?
P3 Re1 P5 95.85(2) . 10_666 ?
O1 Re1 P5 95.28(6) . . ?
O1 Re1 P5 84.72(6) 10_666 . ?
P3 Re1 P5 95.85(2) 10_666 . ?
P3 Re1 P5 84.15(2) . . ?
P5 Re1 P5 180.00(2) 10_666 . ?
C6' N1 C2 116.0(5) . . ?
C6' N1 C4 116.4(5) . . ?
C2 N1 C4 112.5(2) . . ?
C2 N1 C6 109.3(3) . . ?
C4 N1 C6 110.3(3) . . ?
N1 C2 P3 115.4(2) . . ?
C19 P3 C13 107.06(13) . . ?
C19 P3 C2 105.09(14) . . ?
C13 P3 C2 96.16(13) . . ?
C19 P3 Re1 116.88(10) . . ?
C13 P3 Re1 117.83(10) . . ?
C2 P3 Re1 111.22(10) . . ?
N1 C4 P5 113.84(19) . . ?
C25 P5 C31 105.35(13) . . ?
C25 P5 C4 103.44(14) . . ?
C31 P5 C4 97.03(13) . . ?
C25 P5 Re1 118.59(10) . . ?
C31 P5 Re1 119.52(9) . . ?
C4 P5 Re1 109.71(10) . . ?
C7 C6 C11 120.0 . . ?
C7 C6 N1 115.4(3) . . ?
C11 C6 N1 124.6(3) . . ?
O12 C7 C8 118.4(4) . . ?
O12 C7 C6 121.5(4) . . ?
C8 C7 C6 120.0 . . ?
C7 C8 C9 120.0 . . ?
C10 C9 C8 120.0 . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C6 120.0 . . ?
C7' C6' C11' 120.0 . . ?
C7' C6' N1 119.4(6) . . ?
C11' C6' N1 120.6(6) . . ?
O12' C7' C8' 121.9(7) . . ?
O12' C7' C6' 118.0(7) . . ?
C8' C7' C6' 120.0 . . ?
C7' C8' C9' 120.0 . . ?
C8' C9' C10' 120.0 . . ?
C11' C10' C9' 120.0 . . ?
C10' C11' C6' 120.0 . . ?
C18 C13 C14 119.5(3) . . ?
C18 C13 P3 121.7(2) . . ?
C14 C13 P3 118.6(2) . . ?
C15 C14 C13 120.3(3) . . ?
C14 C15 C16 120.1(3) . . ?
C15 C16 C17 120.3(3) . . ?
C16 C17 C18 120.1(3) . . ?
C17 C18 C13 119.6(3) . . ?
C20 C19 C24 119.1(3) . . ?
C20 C19 P3 121.4(2) . . ?
C24 C19 P3 119.4(2) . . ?
C21 C20 C19 120.3(3) . . ?
C20 C21 C22 120.1(4) . . ?
C23 C22 C21 120.2(3) . . ?
C22 C23 C24 120.0(4) . . ?
C23 C24 C19 120.1(3) . . ?
C26 C25 C30 119.1(3) . . ?
C26 C25 P5 120.7(2) . . ?
C30 C25 P5 120.1(2) . . ?
C27 C26 C25 121.0(3) . . ?
C28 C27 C26 119.7(4) . . ?
C27 C28 C29 120.3(3) . . ?
C28 C29 C30 120.2(4) . . ?
C25 C30 C29 119.6(3) . . ?
C32 C31 C36 119.1(3) . . ?
C32 C31 P5 121.3(2) . . ?
C36 C31 P5 119.6(2) . . ?
C31 C32 C33 120.6(3) . . ?
C34 C33 C32 119.8(3) . . ?
C33 C34 C35 120.8(3) . . ?
C34 C35 C36 119.7(3) . . ?
C35 C36 C31 120.0(3) . . ?

_refine_diff_density_max         0.627
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.070



####################################################################### 
# 
# 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_Re-3
_database_code_depnum_ccdc_archive 'CCDC 2165138'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-04-07 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H62 N2 O6 P4 Re, I, 1.75(CH2Cl2)'
_chemical_formula_sum            'C69.75 H65.50 Cl3.50 I N2 O6 P4 Re'
_chemical_formula_weight         1588.79

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   29.5291(7)
_cell_length_b                   29.5291(7)
_cell_length_c                   24.5448(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18534.9(9)
_cell_formula_units_Z            9
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5811
_cell_measurement_theta_min      2.7420
_cell_measurement_theta_max      28.1180

_exptl_crystal_description       blocks
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             7142
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.214
_exptl_absorpt_coefficient_mu    2.084
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            12034
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.265
_diffrn_reflns_theta_max         28.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             8080
_reflns_number_gt                6755
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0894P)²+150.4795P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8080
_refine_ls_number_parameters     419
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1396
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.02705(11) Uani 1 2 d S . P . .
O1 O 0.53750(13) 0.47782(13) 0.53612(13) 0.0323(7) Uani 1 1 d . . . . .
N1 N 0.40848(17) 0.34824(16) 0.53070(17) 0.0338(9) Uani 1 1 d D . . . .
C2 C 0.4277(2) 0.3823(2) 0.5785(2) 0.0340(11) Uani 1 1 d . . . . .
H2A H 0.463522 0.389671 0.587275 0.041 Uiso 1 1 calc R U . . .
H2B H 0.405022 0.364032 0.610150 0.041 Uiso 1 1 calc R U . . .
P3 P 0.42865(5) 0.44457(5) 0.56698(5) 0.0281(3) Uani 1 1 d . . . . .
C4 C 0.4491(2) 0.3599(2) 0.4907(2) 0.0333(11) Uani 1 1 d . . . . .
H4A H 0.438016 0.328799 0.467296 0.040 Uiso 1 1 calc R U . . .
H4B H 0.481342 0.366691 0.509955 0.040 Uiso 1 1 calc R U . . .
P5 P 0.46453(5) 0.41676(5) 0.44661(5) 0.0281(3) Uani 1 1 d . . . . .
C6 C 0.3817(3) 0.2933(2) 0.5476(4) 0.033(2) Uani 0.625(8) 1 d DG U P A 1
C7 C 0.3282(3) 0.2645(3) 0.5378(4) 0.044(2) Uani 0.625(8) 1 d G U P A 1
H7A H 0.310842 0.280823 0.521506 0.053 Uiso 0.625(8) 1 calc R U P A 1
C8 C 0.3002(3) 0.2119(2) 0.5518(4) 0.058(3) Uani 0.625(8) 1 d DG U P A 1
H8A H 0.263606 0.192225 0.545071 0.070 Uiso 0.625(8) 1 calc R U P A 1
C9 C 0.3256(3) 0.18800(19) 0.5756(3) 0.046(2) Uani 0.625(8) 1 d DG U P A 1
C10 C 0.3790(3) 0.2167(3) 0.5855(4) 0.052(3) Uani 0.625(8) 1 d DG U P A 1
H10A H 0.396421 0.200425 0.601764 0.063 Uiso 0.625(8) 1 calc R U P A 1
C11 C 0.4071(3) 0.2694(3) 0.5715(4) 0.050(3) Uani 0.625(8) 1 d G U P A 1
H11A H 0.443659 0.289024 0.578199 0.060 Uiso 0.625(8) 1 calc R U P A 1
C12 C 0.2935(6) 0.1305(4) 0.5914(7) 0.080(4) Uani 0.625(8) 1 d D U P A 1
H12A H 0.283722 0.109475 0.557541 0.096 Uiso 0.625(8) 1 calc R U P A 1
H12B H 0.316378 0.121355 0.612601 0.096 Uiso 0.625(8) 1 calc R U P A 1
C13 C 0.2466(7) 0.1146(5) 0.6225(7) 0.111(6) Uani 0.625(8) 1 d D U P A 1
O13 O 0.2137(6) 0.0703(5) 0.6337(6) 0.166(7) Uani 0.625(8) 1 d D U P A 1
O14 O 0.2378(6) 0.1485(6) 0.6456(6) 0.140(5) Uani 0.625(8) 1 d D U P A 1
H14 H 0.210676 0.132202 0.668687 0.210 Uiso 0.625(8) 1 d R U P A 1
C6' C 0.3734(6) 0.2934(4) 0.5403(8) 0.036(4) Uiso 0.375(8) 1 d DG U P A 2
C7' C 0.3210(6) 0.2684(5) 0.5253(7) 0.044(4) Uiso 0.375(8) 1 d G U P A 2
H7B H 0.307311 0.287290 0.507079 0.052 Uiso 0.375(8) 1 calc R U P A 2
C8' C 0.2886(4) 0.2156(5) 0.5371(7) 0.055(5) Uiso 0.375(8) 1 d DG U P A 2
H8B H 0.252789 0.198548 0.526856 0.067 Uiso 0.375(8) 1 calc R U P A 2
C9' C 0.3086(5) 0.1879(4) 0.5638(7) 0.051(5) Uiso 0.375(8) 1 d DG U P A 2
C10' C 0.3610(5) 0.2129(5) 0.5787(7) 0.042(4) Uiso 0.375(8) 1 d DG U P A 2
H10B H 0.374721 0.193995 0.596959 0.050 Uiso 0.375(8) 1 calc R U P A 2
C11' C 0.3934(4) 0.2656(5) 0.5670(8) 0.040(4) Uiso 0.375(8) 1 d G U P A 2
H11B H 0.429244 0.282737 0.577183 0.048 Uiso 0.375(8) 1 calc R U P A 2
C12' C 0.2734(8) 0.1317(6) 0.5805(11) 0.079(7) Uiso 0.375(8) 1 d D U P A 2
H12C H 0.291169 0.125201 0.611121 0.094 Uiso 0.375(8) 1 calc R U P A 2
H12D H 0.241483 0.129821 0.595831 0.094 Uiso 0.375(8) 1 calc R U P A 2
C13' C 0.2567(9) 0.0902(7) 0.5466(8) 0.079(6) Uiso 0.375(8) 1 d D U P A 2
O13' O 0.2581(7) 0.1048(7) 0.5022(7) 0.090(5) Uiso 0.375(8) 1 d D U P A 2
O14' O 0.2336(10) 0.0424(8) 0.5622(10) 0.141(7) Uiso 0.375(8) 1 d D U P A 2
H14B H 0.235494 0.040697 0.598709 0.211 Uiso 0.375(8) 1 d R U P A 2
C15 C 0.36144(19) 0.4226(2) 0.5476(2) 0.0324(10) Uani 1 1 d . . . . .
C16 C 0.3496(2) 0.4438(3) 0.5036(2) 0.0473(14) Uani 1 1 d . . . . .
H16A H 0.376719 0.472456 0.484458 0.057 Uiso 1 1 calc R U . . .
C17 C 0.2978(3) 0.4232(3) 0.4872(3) 0.0594(18) Uani 1 1 d . . . . .
H17A H 0.289850 0.438324 0.457173 0.071 Uiso 1 1 calc R U . . .
C18 C 0.2584(2) 0.3817(3) 0.5139(3) 0.0582(18) Uani 1 1 d . . . . .
H18A H 0.223359 0.367435 0.501638 0.070 Uiso 1 1 calc R U . . .
C19 C 0.2691(2) 0.3605(3) 0.5585(3) 0.0530(15) Uani 1 1 d . . . . .
H19A H 0.241506 0.331919 0.577300 0.064 Uiso 1 1 calc R U . . .
C20 C 0.3204(2) 0.3808(2) 0.5759(2) 0.0440(13) Uani 1 1 d . . . . .
H20A H 0.327739 0.366467 0.606974 0.053 Uiso 1 1 calc R U . . .
C21 C 0.4339(2) 0.46458(19) 0.63823(19) 0.0314(10) Uani 1 1 d . . . . .
C22 C 0.40058(19) 0.48028(19) 0.6596(2) 0.0328(11) Uani 1 1 d . . . . .
H22A H 0.375989 0.482571 0.636476 0.039 Uiso 1 1 calc R U . . .
C23 C 0.4027(2) 0.4927(2) 0.7142(2) 0.0412(13) Uani 1 1 d . . . . .
H23A H 0.380160 0.504090 0.728323 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4380(2) 0.4884(2) 0.7483(2) 0.0476(15) Uani 1 1 d . . . . .
H24A H 0.438949 0.496054 0.786027 0.057 Uiso 1 1 calc R U . . .
C25 C 0.4717(2) 0.4729(2) 0.7276(2) 0.0470(14) Uani 1 1 d . . . . .
H25A H 0.495777 0.470183 0.751019 0.056 Uiso 1 1 calc R U . . .
C26 C 0.4703(2) 0.4615(2) 0.6724(2) 0.0402(12) Uani 1 1 d . . . . .
H26A H 0.493944 0.451531 0.658004 0.048 Uiso 1 1 calc R U . . .
C27 C 0.50974(19) 0.40991(18) 0.40167(19) 0.0303(10) Uani 1 1 d . . . . .
C28 C 0.5558(2) 0.4154(2) 0.4244(2) 0.0366(11) Uani 1 1 d . . . . .
H28A H 0.564497 0.426287 0.461222 0.044 Uiso 1 1 calc R U . . .
C29 C 0.5889(2) 0.4049(2) 0.3930(3) 0.0449(13) Uani 1 1 d . . . . .
H29A H 0.619814 0.408046 0.408505 0.054 Uiso 1 1 calc R U . . .
C30 C 0.5765(2) 0.3900(2) 0.3392(3) 0.0485(15) Uani 1 1 d . . . . .
H30A H 0.598717 0.382234 0.317954 0.058 Uiso 1 1 calc R U . . .
C31 C 0.5324(2) 0.3862(2) 0.3162(2) 0.0433(13) Uani 1 1 d . . . . .
H31A H 0.524933 0.376974 0.278883 0.052 Uiso 1 1 calc R U . . .
C32 C 0.4984(2) 0.39583(19) 0.3472(2) 0.0343(11) Uani 1 1 d . . . . .
H32A H 0.467673 0.392774 0.331099 0.041 Uiso 1 1 calc R U . . .
C33 C 0.40547(19) 0.3968(2) 0.40723(19) 0.0331(11) Uani 1 1 d . . . . .
C34 C 0.4017(2) 0.4335(2) 0.3752(2) 0.0433(13) Uani 1 1 d . . . . .
H34A H 0.430190 0.468357 0.373601 0.052 Uiso 1 1 calc R U . . .
C35 C 0.3565(3) 0.4198(3) 0.3454(3) 0.0538(16) Uani 1 1 d . . . . .
H35A H 0.354469 0.445006 0.323133 0.065 Uiso 1 1 calc R U . . .
C36 C 0.3144(3) 0.3690(3) 0.3484(3) 0.0577(17) Uani 1 1 d . . . . .
H36A H 0.283317 0.359690 0.328621 0.069 Uiso 1 1 calc R U . . .
C37 C 0.3179(2) 0.3326(3) 0.3797(3) 0.0516(15) Uani 1 1 d . . . . .
H37A H 0.289113 0.297948 0.381601 0.062 Uiso 1 1 calc R U . . .
C38 C 0.3633(2) 0.3461(2) 0.4089(2) 0.0422(12) Uani 1 1 d . . . . .
H38A H 0.365493 0.320356 0.430155 0.051 Uiso 1 1 calc R U . . .
I1 I 0.666667 0.333333 0.4189(3) 0.096(2) Uiso 0.236(5) 3 d S U P B 1
I1' I 0.666667 0.333333 0.3868(3) 0.084(2) Uiso 0.217(5) 3 d S U P C 2
I1" I 0.666667 0.333333 0.333333 0.141(6) Uiso 0.094(5) 6 d S U P D 3
I2 I 0.55120(18) 0.28747(17) 0.50452(16) 0.0933(11) Uani 0.1667 1 d . . P . .
I3 I 0.5858(6) 0.4369(5) 0.5994(5) 0.153(5) Uani 0.0833 1 d . . P . .
I4 I 0.1594(6) 0.1239(7) 0.7114(7) 0.197(7) Uani 0.0833 1 d . . P . .


_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 O1 1.779(3) . ?
Re1 O1 1.779(3) 10_666 ?
Re1 P5 2.5062(12) 10_666 ?
Re1 P5 2.5063(12) . ?
Re1 P3 2.5243(12) 10_666 ?
Re1 P3 2.5244(12) . ?
N1 C6' 1.441(10) . ?
N1 C4 1.453(6) . ?
N1 C2 1.463(6) . ?
N1 C6 1.467(6) . ?
C2 P3 1.848(5) . ?
P3 C15 1.816(5) . ?
P3 C21 1.828(5) . ?
C4 P5 1.851(5) . ?
P5 C33 1.816(5) . ?
P5 C27 1.819(5) . ?
C6 C7 1.3900 . ?
C6 C11 1.3900 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C9 C12 1.524(10) . ?
C10 C11 1.3900 . ?
C12 C13 1.44(2) . ?
C13 O13 1.209(15) . ?
C13 O14 1.286(18) . ?
C6' C7' 1.3900 . ?
C6' C11' 1.3900 . ?
C7' C8' 1.3900 . ?
C8' C9' 1.3900 . ?
C9' C10' 1.3900 . ?
C9' C12' 1.510(13) . ?
C10' C11' 1.3900 . ?
C12' C13' 1.35(2) . ?
C13' O13' 1.165(19) . ?
C13' O14' 1.28(2) . ?
C15 C16 1.378(8) . ?
C15 C20 1.407(8) . ?
C16 C17 1.392(8) . ?
C17 C18 1.363(10) . ?
C18 C19 1.375(10) . ?
C19 C20 1.387(8) . ?
C21 C22 1.382(7) . ?
C21 C26 1.404(7) . ?
C22 C23 1.382(7) . ?
C23 C24 1.393(9) . ?
C24 C25 1.380(9) . ?
C25 C26 1.391(8) . ?
C27 C32 1.391(7) . ?
C27 C28 1.403(7) . ?
C28 C29 1.396(7) . ?
C29 C30 1.383(9) . ?
C30 C31 1.372(9) . ?
C31 C32 1.398(7) . ?
C33 C34 1.388(8) . ?
C33 C38 1.390(8) . ?
C34 C35 1.391(8) . ?
C35 C36 1.390(10) . ?
C36 C37 1.367(10) . ?
C37 C38 1.392(8) . ?
I1' I1' 2.625(15) 16_655 ?
I3 I4 3.03(3) 15_556 ?

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 Re1 O1 180.0 . 10_666 ?
O1 Re1 P5 93.94(11) . 10_666 ?
O1 Re1 P5 86.06(11) 10_666 10_666 ?
O1 Re1 P5 86.06(11) . . ?
O1 Re1 P5 93.94(11) 10_666 . ?
P5 Re1 P5 180.0 10_666 . ?
O1 Re1 P3 95.27(11) . 10_666 ?
O1 Re1 P3 84.73(11) 10_666 10_666 ?
P5 Re1 P3 84.30(4) 10_666 10_666 ?
P5 Re1 P3 95.70(4) . 10_666 ?
O1 Re1 P3 84.73(11) . . ?
O1 Re1 P3 95.27(11) 10_666 . ?
P5 Re1 P3 95.70(4) 10_666 . ?
P5 Re1 P3 84.30(4) . . ?
P3 Re1 P3 180.0 10_666 . ?
C6' N1 C4 114.9(10) . . ?
C6' N1 C2 117.1(9) . . ?
C4 N1 C2 112.9(4) . . ?
C4 N1 C6 112.3(5) . . ?
C2 N1 C6 110.0(5) . . ?
N1 C2 P3 111.6(3) . . ?
C15 P3 C21 105.5(2) . . ?
C15 P3 C2 102.4(2) . . ?
C21 P3 C2 97.6(2) . . ?
C15 P3 Re1 118.02(17) . . ?
C21 P3 Re1 120.36(16) . . ?
C2 P3 Re1 109.73(17) . . ?
N1 C4 P5 114.2(3) . . ?
C33 P5 C27 106.3(2) . . ?
C33 P5 C4 104.8(2) . . ?
C27 P5 C4 96.6(2) . . ?
C33 P5 Re1 117.31(17) . . ?
C27 P5 Re1 117.14(16) . . ?
C4 P5 Re1 112.11(16) . . ?
C7 C6 C11 120.0 . . ?
C7 C6 N1 116.5(5) . . ?
C11 C6 N1 123.5(5) . . ?
C8 C7 C6 120.0 . . ?
C7 C8 C9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 C12 118.7(6) . . ?
C10 C9 C12 121.3(6) . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C6 120.0 . . ?
C13 C12 C9 117.3(11) . . ?
O13 C13 O14 112.0(18) . . ?
O13 C13 C12 126.6(18) . . ?
O14 C13 C12 121.1(12) . . ?
C7' C6' C11' 120.0 . . ?
C7' C6' N1 122.5(10) . . ?
C11' C6' N1 117.4(10) . . ?
C6' C7' C8' 120.0 . . ?
C7' C8' C9' 120.0 . . ?
C10' C9' C8' 120.0 . . ?
C10' C9' C12' 119.0(7) . . ?
C8' C9' C12' 120.9(7) . . ?
C9' C10' C11' 120.0 . . ?
C10' C11' C6' 120.0 . . ?
C13' C12' C9' 125(2) . . ?
O13' C13' O14' 126(2) . . ?
O13' C13' C12' 108.1(18) . . ?
O14' C13' C12' 125(2) . . ?
C16 C15 C20 118.7(5) . . ?
C16 C15 P3 121.6(4) . . ?
C20 C15 P3 119.6(4) . . ?
C15 C16 C17 120.1(6) . . ?
C18 C17 C16 120.7(6) . . ?
C17 C18 C19 120.3(6) . . ?
C18 C19 C20 119.9(6) . . ?
C19 C20 C15 120.2(6) . . ?
C22 C21 C26 119.5(5) . . ?
C22 C21 P3 120.8(4) . . ?
C26 C21 P3 119.6(4) . . ?
C23 C22 C21 120.7(5) . . ?
C22 C23 C24 119.8(5) . . ?
C25 C24 C23 120.2(5) . . ?
C24 C25 C26 120.1(6) . . ?
C25 C26 C21 119.7(5) . . ?
C32 C27 C28 119.5(5) . . ?
C32 C27 P5 122.3(4) . . ?
C28 C27 P5 118.0(4) . . ?
C29 C28 C27 120.0(5) . . ?
C30 C29 C28 119.7(6) . . ?
C31 C30 C29 120.5(5) . . ?
C30 C31 C32 120.7(5) . . ?
C27 C32 C31 119.5(5) . . ?
C34 C33 C38 118.7(5) . . ?
C34 C33 P5 119.2(4) . . ?
C38 C33 P5 122.1(4) . . ?
C33 C34 C35 120.7(6) . . ?
C36 C35 C34 119.8(6) . . ?
C37 C36 C35 120.0(6) . . ?
C36 C37 C38 120.3(6) . . ?
C33 C38 C37 120.6(6) . . ?

_refine_diff_density_max         1.652
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.132



####################################################################### 
# 
# 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_Re-4
_database_code_depnum_ccdc_archive 'CCDC 2165139'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-04-07 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H56 N2 O8 P6 Re, Cl, 2(C6 H14)'
_chemical_formula_sum            'C66 H84 Cl N2 O8 P6 Re'
_chemical_formula_weight         1440.82

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9710(3)
_cell_length_b                   14.1823(3)
_cell_length_c                   18.7894(3)
_cell_angle_alpha                91.9605(16)
_cell_angle_beta                 101.2884(16)
_cell_angle_gamma                114.1629(19)
_cell_volume                     3067.26(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    13972
_cell_measurement_theta_min      2.5000
_cell_measurement_theta_max      28.1460

_exptl_crystal_description       blocks
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.099
_exptl_absorpt_coefficient_mu    2.240
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            41145
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.506
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13231
_reflns_number_gt                10719
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0250P)²+4.5192P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13231
_refine_ls_number_parameters     643
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0761
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Re1A Re 0.000000 0.000000 0.500000 0.01933(5) Uani 1 2 d S . P . .
O1A O 0.03040(19) 0.07985(17) 0.58339(13) 0.0252(5) Uani 1 1 d . . . . .
N1A N 0.2086(2) 0.2841(2) 0.48021(16) 0.0246(6) Uani 1 1 d . . . . .
C2A C 0.0955(3) 0.2743(2) 0.4864(2) 0.0253(8) Uani 1 1 d . . . . .
H2A H 0.081112 0.331458 0.464353 0.030 Uiso 1 1 calc R U . . .
H2B H 0.094513 0.281684 0.538858 0.030 Uiso 1 1 calc R U . . .
P3A P -0.02222(7) 0.14805(7) 0.44091(5) 0.02270(19) Uani 1 1 d . . . . .
C4A C 0.2607(3) 0.2364(2) 0.53455(19) 0.0231(7) Uani 1 1 d . . . . .
H4A H 0.238550 0.244062 0.581193 0.028 Uiso 1 1 calc R U . . .
H4B H 0.346347 0.272993 0.543434 0.028 Uiso 1 1 calc R U . . .
P5A P 0.21367(7) 0.09710(6) 0.50448(5) 0.02136(19) Uani 1 1 d . . . . .
C6A C 0.2866(3) 0.3842(3) 0.4638(2) 0.0288(8) Uani 1 1 d . . . . .
H6A H 0.246605 0.399158 0.418008 0.035 Uiso 1 1 calc R U . . .
H6B H 0.355222 0.377042 0.453565 0.035 Uiso 1 1 calc R U . . .
P7A P 0.33822(8) 0.49667(7) 0.53160(6) 0.0321(2) Uani 1 1 d . . . . .
O8A O 0.4250(2) 0.58773(18) 0.50326(14) 0.0352(6) Uani 1 1 d . . . . .
O9A O 0.3848(3) 0.4760(2) 0.60553(15) 0.0464(7) Uani 1 1 d . . . . .
O10A O 0.2281(2) 0.5158(2) 0.53646(19) 0.0533(8) Uani 1 1 d . . . . .
C11A C -0.0243(3) 0.1542(3) 0.3446(2) 0.0318(9) Uani 1 1 d . . . . .
C12A C -0.0520(4) 0.0657(3) 0.2976(2) 0.0406(10) Uani 1 1 d . . . . .
H12A H -0.064625 0.001682 0.316661 0.049 Uiso 1 1 calc R U . . .
C13A C -0.0614(5) 0.0692(4) 0.2231(3) 0.0616(14) Uani 1 1 d . . . . .
H13A H -0.081184 0.007449 0.191686 0.074 Uiso 1 1 calc R U . . .
C14A C -0.0429(6) 0.1596(5) 0.1946(3) 0.0758(17) Uani 1 1 d . . . . .
H14A H -0.049727 0.161551 0.143429 0.091 Uiso 1 1 calc R U . . .
C15A C -0.0138(5) 0.2490(4) 0.2408(3) 0.0726(16) Uani 1 1 d . . . . .
H15A H -0.000314 0.312653 0.220976 0.087 Uiso 1 1 calc R U . . .
C16A C -0.0040(4) 0.2475(4) 0.3153(2) 0.0527(12) Uani 1 1 d . . . . .
H16A H 0.016524 0.309742 0.346402 0.063 Uiso 1 1 calc R U . . .
C17A C -0.1436(3) 0.1740(3) 0.4551(2) 0.0270(8) Uani 1 1 d . . . . .
C18A C -0.2219(3) 0.1851(3) 0.3980(2) 0.0406(10) Uani 1 1 d . . . . .
H18A H -0.216175 0.175636 0.348880 0.049 Uiso 1 1 calc R U . . .
C19A C -0.3087(4) 0.2104(4) 0.4134(3) 0.0564(13) Uani 1 1 d . . . . .
H19A H -0.361989 0.218658 0.374392 0.068 Uiso 1 1 calc R U . . .
C20A C -0.3186(4) 0.2234(3) 0.4835(3) 0.0547(13) Uani 1 1 d . . . . .
H20A H -0.378366 0.240859 0.492994 0.066 Uiso 1 1 calc R U . . .
C21A C -0.2428(4) 0.2114(3) 0.5402(3) 0.0478(11) Uani 1 1 d . . . . .
H21A H -0.250354 0.219579 0.589032 0.057 Uiso 1 1 calc R U . . .
C22A C -0.1547(3) 0.1871(3) 0.5259(2) 0.0376(9) Uani 1 1 d . . . . .
H22A H -0.101522 0.179432 0.565351 0.045 Uiso 1 1 calc R U . . .
C23A C 0.3164(3) 0.0750(2) 0.5760(2) 0.0248(8) Uani 1 1 d . . . . .
C24A C 0.3043(3) 0.0853(3) 0.6475(2) 0.0327(9) Uani 1 1 d . . . . .
H24A H 0.241445 0.097923 0.656936 0.039 Uiso 1 1 calc R U . . .
C25A C 0.3846(4) 0.0770(3) 0.7049(2) 0.0419(10) Uani 1 1 d . . . . .
H25A H 0.376912 0.084126 0.753791 0.050 Uiso 1 1 calc R U . . .
C26A C 0.4754(4) 0.0586(3) 0.6908(3) 0.0509(12) Uani 1 1 d . . . . .
H26A H 0.530077 0.052935 0.730155 0.061 Uiso 1 1 calc R U . . .
C27A C 0.4875(3) 0.0484(3) 0.6209(3) 0.0473(11) Uani 1 1 d . . . . .
H27A H 0.550714 0.035921 0.611910 0.057 Uiso 1 1 calc R U . . .
C28A C 0.4081(3) 0.0561(3) 0.5629(2) 0.0347(9) Uani 1 1 d . . . . .
H28A H 0.416529 0.048372 0.514202 0.042 Uiso 1 1 calc R U . . .
C29A C 0.2639(3) 0.0975(3) 0.4207(2) 0.0274(8) Uani 1 1 d . . . . .
C30A C 0.2022(3) 0.0173(3) 0.3637(2) 0.0413(10) Uani 1 1 d . . . . .
H30A H 0.133044 -0.038980 0.368584 0.050 Uiso 1 1 calc R U . . .
C31A C 0.2397(4) 0.0181(4) 0.3003(2) 0.0561(13) Uani 1 1 d . . . . .
H31A H 0.197037 -0.038235 0.262152 0.067 Uiso 1 1 calc R U . . .
C32A C 0.3376(4) 0.0991(4) 0.2914(3) 0.0544(13) Uani 1 1 d . . . . .
H32A H 0.363113 0.099192 0.247304 0.065 Uiso 1 1 calc R U . . .
C33A C 0.3995(3) 0.1810(4) 0.3471(3) 0.0478(11) Uani 1 1 d . . . . .
H33A H 0.466698 0.238494 0.340831 0.057 Uiso 1 1 calc R U . . .
C34A C 0.3641(3) 0.1794(3) 0.4114(2) 0.0354(9) Uani 1 1 d . . . . .
H34A H 0.408440 0.234779 0.449968 0.042 Uiso 1 1 calc R U . . .
Re1B Re 0.500000 0.500000 0.000000 0.03290(7) Uani 1 2 d S . P . .
O1B O 0.3793(2) 0.3951(2) 0.02011(14) 0.0407(7) Uani 1 1 d . . . . .
N1B N 0.4642(3) 0.5918(2) 0.18708(16) 0.0380(8) Uani 1 1 d . . . . .
C2B C 0.4942(4) 0.5034(3) 0.1898(2) 0.0358(9) Uani 1 1 d . . . . .
H2C H 0.422413 0.438187 0.173783 0.043 Uiso 1 1 calc R U . . .
H2D H 0.530329 0.501555 0.240965 0.043 Uiso 1 1 calc R U . . .
P3B P 0.59431(9) 0.50959(8) 0.13180(5) 0.0328(2) Uani 1 1 d . . . . .
C4B C 0.3646(4) 0.5751(3) 0.1284(2) 0.0422(10) Uani 1 1 d . . . . .
H4C H 0.324782 0.616823 0.142517 0.051 Uiso 1 1 calc R U . . .
H4D H 0.308992 0.500672 0.120856 0.051 Uiso 1 1 calc R U . . .
P5B P 0.40909(10) 0.61236(8) 0.04234(5) 0.0392(3) Uani 1 1 d . . . . .
C6B C 0.4691(4) 0.6421(3) 0.2576(2) 0.0431(10) Uani 1 1 d . . . . .
H6C H 0.450561 0.702374 0.248511 0.052 Uiso 1 1 calc R U . . .
H6D H 0.549976 0.669784 0.286817 0.052 Uiso 1 1 calc R U . . .
P7B P 0.37476(11) 0.56285(11) 0.31224(7) 0.0522(3) Uani 1 1 d . . . . .
O8B O 0.3898(5) 0.6337(4) 0.3783(2) 0.1140(19) Uani 1 1 d . . . . .
O9B O 0.2515(3) 0.5106(4) 0.2649(3) 0.1100(17) Uani 1 1 d . . . . .
O10B O 0.4107(3) 0.4756(2) 0.33357(15) 0.0469(7) Uani 1 1 d . . . . .
C11B C 0.7259(3) 0.6240(3) 0.1755(2) 0.0351(9) Uani 1 1 d . . . . .
C12B C 0.7898(4) 0.6921(3) 0.1336(2) 0.0466(11) Uani 1 1 d . . . . .
H12B H 0.765879 0.678496 0.081725 0.056 Uiso 1 1 calc R U . . .
C13B C 0.8889(4) 0.7806(4) 0.1665(3) 0.0595(13) Uani 1 1 d . . . . .
H13B H 0.933385 0.827063 0.137425 0.071 Uiso 1 1 calc R U . . .
C14B C 0.9222(4) 0.8006(4) 0.2418(3) 0.0571(13) Uani 1 1 d . . . . .
H14B H 0.989314 0.861750 0.264507 0.069 Uiso 1 1 calc R U . . .
C15B C 0.8605(4) 0.7341(4) 0.2837(2) 0.0526(12) Uani 1 1 d . . . . .
H15B H 0.884963 0.748801 0.335527 0.063 Uiso 1 1 calc R U . . .
C16B C 0.7617(4) 0.6445(3) 0.2518(2) 0.0476(11) Uani 1 1 d . . . . .
H16B H 0.718964 0.597795 0.281443 0.057 Uiso 1 1 calc R U . . .
C17B C 0.6177(4) 0.3961(3) 0.1580(2) 0.0362(9) Uani 1 1 d . . . . .
C18B C 0.7199(4) 0.4033(4) 0.2031(2) 0.0521(12) Uani 1 1 d . . . . .
H18B H 0.784219 0.469126 0.218767 0.063 Uiso 1 1 calc R U . . .
C19B C 0.7272(5) 0.3127(4) 0.2252(3) 0.0649(15) Uani 1 1 d . . . . .
H19B H 0.796215 0.317625 0.257078 0.078 Uiso 1 1 calc R U . . .
C20B C 0.6366(5) 0.2173(4) 0.2016(3) 0.0597(14) Uani 1 1 d . . . . .
H20B H 0.643027 0.156313 0.216631 0.072 Uiso 1 1 calc R U . . .
C21B C 0.5369(4) 0.2099(3) 0.1563(2) 0.0520(12) Uani 1 1 d . . . . .
H21B H 0.474157 0.143331 0.139627 0.062 Uiso 1 1 calc R U . . .
C22B C 0.5261(4) 0.2977(3) 0.1344(2) 0.0412(10) Uani 1 1 d . . . . .
H22B H 0.455909 0.291351 0.103078 0.049 Uiso 1 1 calc R U . . .
C23B C 0.2679(4) 0.5904(4) -0.0134(2) 0.0464(11) Uani 1 1 d . . . . .
C24B C 0.1802(4) 0.4899(4) -0.0249(3) 0.0611(14) Uani 1 1 d . . . . .
H24B H 0.195779 0.435310 -0.004804 0.073 Uiso 1 1 calc R U . . .
C25B C 0.0685(5) 0.4685(6) -0.0661(3) 0.0818(18) Uani 1 1 d . . . . .
H25B H 0.009248 0.399316 -0.075158 0.098 Uiso 1 1 calc R U . . .
C26B C 0.0458(6) 0.5476(7) -0.0930(3) 0.085(2) Uani 1 1 d . . . . .
H26B H -0.030087 0.533437 -0.120108 0.102 Uiso 1 1 calc R U . . .
C27B C 0.1308(6) 0.6470(6) -0.0815(3) 0.0838(19) Uani 1 1 d . . . . .
H27B H 0.113431 0.701361 -0.100590 0.101 Uiso 1 1 calc R U . . .
C28B C 0.2429(5) 0.6698(4) -0.0422(2) 0.0609(14) Uani 1 1 d . . . . .
H28B H 0.301738 0.739045 -0.034988 0.073 Uiso 1 1 calc R U . . .
C29B C 0.4929(5) 0.7540(3) 0.0625(2) 0.0482(12) Uani 1 1 d . . . . .
C30B C 0.6013(5) 0.8024(4) 0.0495(3) 0.0600(14) Uani 1 1 d . . . . .
H30B H 0.635476 0.761836 0.031051 0.072 Uiso 1 1 calc R U . . .
C31B C 0.6621(6) 0.9099(4) 0.0627(3) 0.0775(18) Uani 1 1 d . . . . .
H31B H 0.738338 0.942297 0.054780 0.093 Uiso 1 1 calc R U . . .
C32B C 0.6125(7) 0.9698(4) 0.0874(3) 0.086(2) Uani 1 1 d . . . . .
H32B H 0.652834 1.043622 0.094752 0.103 Uiso 1 1 calc R U . . .
C33B C 0.5053(7) 0.9221(4) 0.1010(3) 0.080(2) Uani 1 1 d . . . . .
H33B H 0.471618 0.963554 0.118771 0.095 Uiso 1 1 calc R U . . .
C34B C 0.4432(5) 0.8142(4) 0.0896(3) 0.0646(15) Uani 1 1 d . . . . .
H34B H 0.368539 0.782144 0.100053 0.077 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1A O1A 1.779(2) . ?
Re1A O1A 1.779(2) 2_556 ?
Re1A P3A 2.5008(9) 2_556 ?
Re1A P3A 2.5008(9) . ?
Re1A P5A 2.5221(8) . ?
Re1A P5A 2.5221(8) 2_556 ?
N1A C2A 1.445(4) . ?
N1A C4A 1.451(4) . ?
N1A C6A 1.453(4) . ?
C2A P3A 1.848(3) . ?
P3A C11A 1.810(4) . ?
P3A C17A 1.821(3) . ?
C4A P5A 1.843(3) . ?
P5A C29A 1.818(4) . ?
P5A C23A 1.830(3) . ?
C6A P7A 1.808(4) . ?
P7A O9A 1.492(3) . ?
P7A O8A 1.520(3) . ?
P7A O10A 1.578(3) . ?
C11A C12A 1.384(5) . ?
C11A C16A 1.395(5) . ?
C12A C13A 1.385(6) . ?
C13A C14A 1.355(7) . ?
C14A C15A 1.381(7) . ?
C15A C16A 1.383(6) . ?
C17A C22A 1.380(5) . ?
C17A C18A 1.387(5) . ?
C18A C19A 1.389(6) . ?
C19A C20A 1.361(7) . ?
C20A C21A 1.368(6) . ?
C21A C22A 1.391(5) . ?
C23A C28A 1.384(5) . ?
C23A C24A 1.392(5) . ?
C24A C25A 1.390(5) . ?
C25A C26A 1.376(6) . ?
C26A C27A 1.362(6) . ?
C27A C28A 1.387(5) . ?
C29A C30A 1.384(5) . ?
C29A C34A 1.391(5) . ?
C30A C31A 1.370(6) . ?
C31A C32A 1.365(6) . ?
C32A C33A 1.384(6) . ?
C33A C34A 1.371(6) . ?
Re1B O1B 1.781(3) . ?
Re1B O1B 1.781(3) 2_665 ?
Re1B P3B 2.5104(9) . ?
Re1B P3B 2.5104(9) 2_665 ?
Re1B P5B 2.5261(11) . ?
Re1B P5B 2.5261(11) 2_665 ?
N1B C4B 1.454(5) . ?
N1B C2B 1.456(5) . ?
N1B C6B 1.460(5) . ?
C2B P3B 1.830(4) . ?
P3B C11B 1.820(4) . ?
P3B C17B 1.822(4) . ?
C4B P5B 1.845(4) . ?
P5B C23B 1.819(4) . ?
P5B C29B 1.833(4) . ?
C6B P7B 1.805(4) . ?
P7B O8B 1.499(4) . ?
P7B O9B 1.524(4) . ?
P7B O10B 1.530(3) . ?
C11B C12B 1.375(6) . ?
C11B C16B 1.399(5) . ?
C12B C13B 1.387(6) . ?
C13B C14B 1.379(7) . ?
C14B C15B 1.353(7) . ?
C15B C16B 1.389(6) . ?
C17B C18B 1.389(6) . ?
C17B C22B 1.397(5) . ?
C18B C19B 1.397(6) . ?
C19B C20B 1.364(7) . ?
C20B C21B 1.364(7) . ?
C21B C22B 1.377(6) . ?
C23B C24B 1.388(7) . ?
C23B C28B 1.391(6) . ?
C24B C25B 1.406(7) . ?
C25B C26B 1.360(9) . ?
C26B C27B 1.366(9) . ?
C27B C28B 1.393(7) . ?
C29B C30B 1.366(7) . ?
C29B C34B 1.397(6) . ?
C30B C31B 1.387(6) . ?
C31B C32B 1.372(9) . ?
C32B C33B 1.356(9) . ?
C33B C34B 1.392(7) . ?

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
O1A Re1A O1A 180.0 . 2_556 ?
O1A Re1A P3A 95.46(8) . 2_556 ?
O1A Re1A P3A 84.54(8) 2_556 2_556 ?
O1A Re1A P3A 84.54(8) . . ?
O1A Re1A P3A 95.46(8) 2_556 . ?
P3A Re1A P3A 180.0 2_556 . ?
O1A Re1A P5A 85.61(7) . . ?
O1A Re1A P5A 94.39(7) 2_556 . ?
P3A Re1A P5A 93.94(3) 2_556 . ?
P3A Re1A P5A 86.06(3) . . ?
O1A Re1A P5A 94.39(7) . 2_556 ?
O1A Re1A P5A 85.61(7) 2_556 2_556 ?
P3A Re1A P5A 86.07(3) 2_556 2_556 ?
P3A Re1A P5A 93.93(3) . 2_556 ?
P5A Re1A P5A 180.0 . 2_556 ?
C2A N1A C4A 114.2(3) . . ?
C2A N1A C6A 116.1(3) . . ?
C4A N1A C6A 116.0(3) . . ?
N1A C2A P3A 112.4(2) . . ?
C11A P3A C17A 105.54(17) . . ?
C11A P3A C2A 104.10(17) . . ?
C17A P3A C2A 97.44(15) . . ?
C11A P3A Re1A 119.93(13) . . ?
C17A P3A Re1A 115.95(12) . . ?
C2A P3A Re1A 111.00(11) . . ?
N1A C4A P5A 111.4(2) . . ?
C29A P5A C23A 106.52(16) . . ?
C29A P5A C4A 103.59(17) . . ?
C23A P5A C4A 97.48(15) . . ?
C29A P5A Re1A 119.02(11) . . ?
C23A P5A Re1A 118.01(11) . . ?
C4A P5A Re1A 109.16(11) . . ?
N1A C6A P7A 118.2(3) . . ?
O9A P7A O8A 114.30(16) . . ?
O9A P7A O10A 107.03(19) . . ?
O8A P7A O10A 110.59(16) . . ?
O9A P7A C6A 111.71(17) . . ?
O8A P7A C6A 107.09(16) . . ?
O10A P7A C6A 105.82(16) . . ?
C12A C11A C16A 118.4(4) . . ?
C12A C11A P3A 121.0(3) . . ?
C16A C11A P3A 120.5(3) . . ?
C11A C12A C13A 120.9(4) . . ?
C14A C13A C12A 120.7(5) . . ?
C13A C14A C15A 119.2(5) . . ?
C14A C15A C16A 121.2(5) . . ?
C15A C16A C11A 119.6(4) . . ?
C22A C17A C18A 119.1(3) . . ?
C22A C17A P3A 118.3(3) . . ?
C18A C17A P3A 122.6(3) . . ?
C17A C18A C19A 119.4(4) . . ?
C20A C19A C18A 121.0(4) . . ?
C19A C20A C21A 120.2(4) . . ?
C20A C21A C22A 119.6(5) . . ?
C17A C22A C21A 120.7(4) . . ?
C28A C23A C24A 119.6(3) . . ?
C28A C23A P5A 123.5(3) . . ?
C24A C23A P5A 116.8(3) . . ?
C25A C24A C23A 119.7(4) . . ?
C26A C25A C24A 119.9(4) . . ?
C27A C26A C25A 120.7(4) . . ?
C26A C27A C28A 120.3(4) . . ?
C23A C28A C27A 119.9(4) . . ?
C30A C29A C34A 118.1(4) . . ?
C30A C29A P5A 120.9(3) . . ?
C34A C29A P5A 121.0(3) . . ?
C31A C30A C29A 120.9(4) . . ?
C32A C31A C30A 120.7(4) . . ?
C31A C32A C33A 119.5(4) . . ?
C34A C33A C32A 120.1(4) . . ?
C33A C34A C29A 120.8(4) . . ?
O1B Re1B O1B 180.00(15) . 2_665 ?
O1B Re1B P3B 84.31(8) . . ?
O1B Re1B P3B 95.69(8) 2_665 . ?
O1B Re1B P3B 95.69(8) . 2_665 ?
O1B Re1B P3B 84.31(8) 2_665 2_665 ?
P3B Re1B P3B 180.0 . 2_665 ?
O1B Re1B P5B 84.51(9) . . ?
O1B Re1B P5B 95.49(9) 2_665 . ?
P3B Re1B P5B 87.70(3) . . ?
P3B Re1B P5B 92.30(3) 2_665 . ?
O1B Re1B P5B 95.49(9) . 2_665 ?
O1B Re1B P5B 84.51(9) 2_665 2_665 ?
P3B Re1B P5B 92.30(3) . 2_665 ?
P3B Re1B P5B 87.70(3) 2_665 2_665 ?
P5B Re1B P5B 180.0 . 2_665 ?
C4B N1B C2B 113.3(3) . . ?
C4B N1B C6B 116.3(3) . . ?
C2B N1B C6B 115.9(3) . . ?
N1B C2B P3B 112.4(3) . . ?
C11B P3B C17B 106.85(18) . . ?
C11B P3B C2B 103.08(18) . . ?
C17B P3B C2B 97.59(18) . . ?
C11B P3B Re1B 119.77(13) . . ?
C17B P3B Re1B 116.33(12) . . ?
C2B P3B Re1B 110.19(12) . . ?
N1B C4B P5B 111.2(3) . . ?
C23B P5B C29B 106.2(2) . . ?
C23B P5B C4B 98.3(2) . . ?
C29B P5B C4B 103.2(2) . . ?
C23B P5B Re1B 115.58(14) . . ?
C29B P5B Re1B 120.15(18) . . ?
C4B P5B Re1B 110.55(13) . . ?
N1B C6B P7B 117.1(3) . . ?
O8B P7B O9B 114.8(3) . . ?
O8B P7B O10B 111.43(19) . . ?
O9B P7B O10B 106.8(2) . . ?
O8B P7B C6B 106.5(2) . . ?
O9B P7B C6B 108.4(2) . . ?
O10B P7B C6B 108.74(19) . . ?
C12B C11B C16B 119.5(4) . . ?
C12B C11B P3B 120.1(3) . . ?
C16B C11B P3B 120.4(3) . . ?
C11B C12B C13B 120.5(4) . . ?
C14B C13B C12B 119.5(5) . . ?
C15B C14B C13B 120.7(4) . . ?
C14B C15B C16B 120.7(4) . . ?
C15B C16B C11B 119.2(4) . . ?
C18B C17B C22B 118.7(4) . . ?
C18B C17B P3B 123.1(3) . . ?
C22B C17B P3B 118.1(3) . . ?
C17B C18B C19B 119.4(4) . . ?
C20B C19B C18B 121.0(4) . . ?
C19B C20B C21B 119.8(4) . . ?
C20B C21B C22B 120.8(4) . . ?
C21B C22B C17B 120.4(4) . . ?
C24B C23B C28B 119.0(4) . . ?
C24B C23B P5B 117.7(3) . . ?
C28B C23B P5B 123.2(4) . . ?
C23B C24B C25B 120.4(5) . . ?
C26B C25B C24B 119.5(6) . . ?
C25B C26B C27B 120.7(6) . . ?
C26B C27B C28B 120.8(6) . . ?
C23B C28B C27B 119.6(6) . . ?
C30B C29B C34B 119.2(5) . . ?
C30B C29B P5B 121.5(3) . . ?
C34B C29B P5B 119.2(4) . . ?
C29B C30B C31B 120.8(5) . . ?
C32B C31B C30B 120.3(6) . . ?
C33B C32B C31B 119.1(6) . . ?
C32B C33B C34B 121.9(6) . . ?
C33B C34B C29B 118.6(6) . . ?

_refine_diff_density_max         1.029
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.088




#===END

# start Validation Reply Form
_vrf_PLAT420_Re-1                
;
PROBLEM: D-H Bond Without Acceptor  O12      --H12      .     Please Check 
RESPONSE: ...
The O12-H hydrogen atom could not be located for either partial-occupancy
orientation of the disordered N1-bound -C6H4OH group, and so they were added
in idealised positions with O-H distances of 0.90 A. See the supporting
information for more details.
;
_vrf_PLAT420_Re-3                
;
PROBLEM: D-H Bond Without Acceptor  O14      --H14      .     Please Check 
RESPONSE: ...
The O14-H hydrogen atom could not be located for either partial-occupancy
orientation of the disordered N1-bound -C6H4CH2COOH group, and so they were
added in idealised positions with O-H distances of 0.90 A. See the supporting
information for more details.
;
_vrf_PLAT430_Re-4                
;
PROBLEM: Short Inter D...A Contact  O8A      ..O8B      .       2.46 Ang.  
RESPONSE: ...
The presumed two OH hydrogen atoms of the P7-based PO3 unit of each
independent molecule could not be reliably located and so were omitted. These
O...O contacts show where some of them would be. See the supporting
information for more details.
;
# end Validation Reply Form



