# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1812999'
_audit_update_record             
;
2017-12-21 deposited with the CCDC.
2018-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H14 O3 P Re'
_chemical_formula_weight         411.39

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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.3784(4)
_cell_length_b                   17.6786(7)
_cell_length_c                   10.3377(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.844(4)
_cell_angle_gamma                90
_cell_volume                     1348.30(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7344
_cell_measurement_theta_min      3.5420
_cell_measurement_theta_max      33.7600

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    9.120
_shelx_estimated_absorpt_T_min   0.143
_shelx_estimated_absorpt_T_max   0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.27397
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11837
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2632
_reflns_number_gt                2383
_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.
 
 _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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP-III (Farrugia 2012)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²+12.3405P] 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         2632
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_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 0.20666(5) 0.42384(2) 0.68875(4) 0.02339(16) Uani 1 1 d . . . . .
P1 P 0.2865(4) 0.32768(15) 0.8345(3) 0.0330(6) Uani 1 1 d . . . . .
O3 O 0.6632(10) 0.5144(5) 0.8534(7) 0.047(2) Uani 1 1 d . . . . .
O1 O -0.1515(12) 0.3437(5) 0.6365(9) 0.054(2) Uani 1 1 d . . . . .
O2 O 0.3752(13) 0.3352(5) 0.4680(8) 0.055(2) Uani 1 1 d . . . . .
C1 C -0.0130(14) 0.3726(6) 0.6572(11) 0.034(2) Uani 1 1 d . . . . .
C2 C 0.3113(16) 0.3678(6) 0.5529(10) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.5818(14) 0.5208(6) 0.7513(10) 0.033(2) Uani 1 1 d . . . . .
H8A H 0.650841 0.522223 0.674531 0.039 Uiso 1 1 calc R U . . .
C4 C 0.3856(13) 0.5265(5) 0.7383(9) 0.028(2) Uani 1 1 d . . . . .
C6 C 0.0995(15) 0.5437(6) 0.6535(11) 0.037(2) Uani 1 1 d . . . . .
H6A H -0.002149 0.557874 0.593130 0.045 Uiso 1 1 calc R U . . .
C7 C 0.0840(14) 0.5295(6) 0.7883(11) 0.035(2) Uani 1 1 d . . . . .
H7A H -0.030697 0.530771 0.838621 0.043 Uiso 1 1 calc R U . . .
C5 C 0.2842(14) 0.5414(5) 0.6222(9) 0.029(2) Uani 1 1 d . . . . .
H5A H 0.336371 0.554464 0.536298 0.035 Uiso 1 1 calc R U . . .
C3 C 0.2589(13) 0.5183(5) 0.8396(10) 0.029(2) Uani 1 1 d . . . . .
H3A H 0.290054 0.510254 0.933118 0.035 Uiso 1 1 calc R U . . .
C9 C 0.151(2) 0.3247(7) 0.9779(12) 0.053(3) Uani 1 1 d . . . . .
H9A H 0.151555 0.374646 1.019109 0.079 Uiso 1 1 calc R U . . .
H9B H 0.026418 0.310671 0.954389 0.079 Uiso 1 1 calc R U . . .
H9C H 0.201616 0.287240 1.038244 0.079 Uiso 1 1 calc R U . . .
C10 C 0.266(2) 0.2323(7) 0.7764(13) 0.059(4) Uani 1 1 d . . . . .
H10A H 0.335948 0.226775 0.696881 0.088 Uiso 1 1 calc R U . . .
H10B H 0.313867 0.197377 0.842214 0.088 Uiso 1 1 calc R U . . .
H10C H 0.138669 0.220808 0.758359 0.088 Uiso 1 1 calc R U . . .
C11 C 0.5140(19) 0.3309(9) 0.9008(15) 0.064(4) Uani 1 1 d . . . . .
H11A H 0.538438 0.381495 0.935556 0.097 Uiso 1 1 calc R U . . .
H11B H 0.526310 0.293440 0.970275 0.097 Uiso 1 1 calc R U . . .
H11C H 0.600648 0.319451 0.832595 0.097 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 C1 1.881(10) . ?
Re1 C2 1.893(11) . ?
Re1 C5 2.265(9) . ?
Re1 C6 2.290(10) . ?
Re1 C4 2.298(9) . ?
Re1 C3 2.313(9) . ?
Re1 C7 2.323(10) . ?
Re1 P1 2.341(3) . ?
P1 C10 1.795(13) . ?
P1 C9 1.801(13) . ?
P1 C11 1.804(14) . ?
O3 C8 1.212(12) . ?
O1 C1 1.159(13) . ?
O2 C2 1.155(13) . ?
C8 C4 1.455(14) . ?
C8 H8A 0.9500 . ?
C4 C3 1.422(14) . ?
C4 C5 1.429(13) . ?
C6 C5 1.406(16) . ?
C6 C7 1.423(16) . ?
C6 H6A 1.0000 . ?
C7 C3 1.403(14) . ?
C7 H7A 1.0000 . ?
C5 H5A 1.0000 . ?
C3 H3A 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
C1 Re1 C2 88.8(5) . . ?
C1 Re1 C5 127.6(4) . . ?
C2 Re1 C5 98.5(4) . . ?
C1 Re1 C6 97.1(4) . . ?
C2 Re1 C6 120.7(4) . . ?
C5 Re1 C6 36.0(4) . . ?
C1 Re1 C4 155.5(4) . . ?
C2 Re1 C4 109.9(4) . . ?
C5 Re1 C4 36.5(3) . . ?
C6 Re1 C4 60.0(4) . . ?
C1 Re1 C3 126.8(4) . . ?
C2 Re1 C3 144.3(4) . . ?
C5 Re1 C3 60.2(4) . . ?
C6 Re1 C3 59.5(4) . . ?
C4 Re1 C3 35.9(4) . . ?
C1 Re1 C7 97.1(4) . . ?
C2 Re1 C7 156.3(4) . . ?
C5 Re1 C7 59.9(4) . . ?
C6 Re1 C7 35.9(4) . . ?
C4 Re1 C7 59.5(4) . . ?
C3 Re1 C7 35.2(4) . . ?
C1 Re1 P1 88.3(3) . . ?
C2 Re1 P1 89.7(3) . . ?
C5 Re1 P1 143.1(3) . . ?
C6 Re1 P1 149.1(3) . . ?
C4 Re1 P1 107.0(3) . . ?
C3 Re1 P1 93.0(3) . . ?
C7 Re1 P1 113.3(3) . . ?
C10 P1 C9 101.8(6) . . ?
C10 P1 C11 103.2(8) . . ?
C9 P1 C11 102.2(7) . . ?
C10 P1 Re1 116.6(5) . . ?
C9 P1 Re1 114.4(4) . . ?
C11 P1 Re1 116.5(5) . . ?
O1 C1 Re1 177.3(10) . . ?
O2 C2 Re1 178.3(9) . . ?
O3 C8 C4 124.5(10) . . ?
O3 C8 H8A 117.7 . . ?
C4 C8 H8A 117.7 . . ?
C3 C4 C5 107.2(9) . . ?
C3 C4 C8 126.0(9) . . ?
C5 C4 C8 126.7(9) . . ?
C3 C4 Re1 72.6(5) . . ?
C5 C4 Re1 70.5(5) . . ?
C8 C4 Re1 122.2(7) . . ?
C5 C6 C7 108.2(9) . . ?
C5 C6 Re1 71.1(6) . . ?
C7 C6 Re1 73.3(6) . . ?
C5 C6 H6A 125.8 . . ?
C7 C6 H6A 125.8 . . ?
Re1 C6 H6A 125.8 . . ?
C3 C7 C6 108.0(10) . . ?
C3 C7 Re1 72.0(6) . . ?
C6 C7 Re1 70.8(6) . . ?
C3 C7 H7A 125.9 . . ?
C6 C7 H7A 125.9 . . ?
Re1 C7 H7A 125.9 . . ?
C6 C5 C4 108.0(9) . . ?
C6 C5 Re1 73.0(6) . . ?
C4 C5 Re1 73.0(5) . . ?
C6 C5 H5A 125.8 . . ?
C4 C5 H5A 125.8 . . ?
Re1 C5 H5A 125.8 . . ?
C7 C3 C4 108.5(9) . . ?
C7 C3 Re1 72.7(6) . . ?
C4 C3 Re1 71.4(5) . . ?
C7 C3 H3A 125.6 . . ?
C4 C3 H3A 125.6 . . ?
Re1 C3 H3A 125.6 . . ?
P1 C9 H9A 109.5 . . ?
P1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10A 109.5 . . ?
P1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_refine_diff_density_max         4.067
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.213


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1813001'
_audit_update_record             
;
2017-12-21 deposited with the CCDC.
2018-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H38 O3 P Re'
_chemical_formula_weight         615.73

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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.6645(6)
_cell_length_b                   10.3427(5)
_cell_length_c                   16.0747(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.819(4)
_cell_angle_gamma                90
_cell_volume                     2429.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9664
_cell_measurement_theta_min      3.4170
_cell_measurement_theta_max      33.9620

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.093
_shelx_estimated_absorpt_T_min   0.429
_shelx_estimated_absorpt_T_max   0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22794
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.217
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5300
_reflns_number_gt                4420
_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.
 
 _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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP-III (Farrugia 2012)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+2.4624P] 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         5300
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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 0.14418(2) 0.75949(2) 0.54339(2) 0.02241(8) Uani 1 1 d . . . . .
P1 P 0.28138(8) 0.64530(11) 0.51862(7) 0.0210(2) Uani 1 1 d . . . . .
O1 O 0.0304(3) 0.5953(4) 0.4161(2) 0.0438(10) Uani 1 1 d . . . . .
C1 C 0.0776(3) 0.6575(5) 0.4624(3) 0.0311(11) Uani 1 1 d . . . . .
O2 O 0.1649(3) 0.9643(4) 0.4102(3) 0.0474(10) Uani 1 1 d . . . . .
C2 C 0.1617(3) 0.8827(5) 0.4591(3) 0.0314(11) Uani 1 1 d . . . . .
O3 O 0.1956(3) 0.5328(4) 0.7487(3) 0.0515(11) Uani 1 1 d . . . . .
C3 C 0.1135(4) 0.6985(6) 0.6751(3) 0.0325(11) Uani 1 1 d . . . . .
C4 C 0.0311(4) 0.7455(5) 0.6299(4) 0.0387(14) Uani 1 1 d . . . . .
H4A H -0.027217 0.695899 0.618813 0.046 Uiso 1 1 calc R U . . .
C5 C 0.0428(4) 0.8779(6) 0.6145(3) 0.0436(14) Uani 1 1 d . . . . .
H5A H -0.005292 0.937338 0.588444 0.052 Uiso 1 1 calc R U . . .
C6 C 0.1313(4) 0.9154(5) 0.6479(3) 0.0372(13) Uani 1 1 d . . . . .
H6A H 0.156644 1.005171 0.647682 0.045 Uiso 1 1 calc R U . . .
C7 C 0.1761(4) 0.8061(5) 0.6851(3) 0.0289(10) Uani 1 1 d . . . . .
H7A H 0.237866 0.805202 0.716628 0.035 Uiso 1 1 calc R U . . .
C8 C 0.1296(5) 0.5682(6) 0.7045(3) 0.0427(14) Uani 1 1 d . . . . .
H8A H 0.084757 0.504977 0.687778 0.051 Uiso 1 1 calc R U . . .
C9 C 0.2779(3) 0.4688(4) 0.5479(3) 0.0255(10) Uani 1 1 d . . . . .
H9A H 0.281275 0.468169 0.610242 0.031 Uiso 1 1 calc R U . . .
C10 C 0.3628(3) 0.3908(5) 0.5254(3) 0.0319(11) Uani 1 1 d . . . . .
H10A H 0.360398 0.378536 0.464199 0.038 Uiso 1 1 calc R U . . .
H10B H 0.419198 0.439675 0.543130 0.038 Uiso 1 1 calc R U . . .
C11 C 0.3656(4) 0.2588(4) 0.5687(4) 0.0387(14) Uani 1 1 d . . . . .
H11A H 0.419129 0.209086 0.552610 0.046 Uiso 1 1 calc R U . . .
H11B H 0.372383 0.270915 0.630011 0.046 Uiso 1 1 calc R U . . .
C12 C 0.2782(4) 0.1837(5) 0.5440(4) 0.0433(14) Uani 1 1 d . . . . .
H12A H 0.279417 0.101033 0.575179 0.052 Uiso 1 1 calc R U . . .
H12B H 0.275346 0.163209 0.483717 0.052 Uiso 1 1 calc R U . . .
C13 C 0.1929(4) 0.2602(5) 0.5623(4) 0.0383(13) Uani 1 1 d . . . . .
H13A H 0.191520 0.270766 0.623367 0.046 Uiso 1 1 calc R U . . .
H13B H 0.137536 0.211508 0.541328 0.046 Uiso 1 1 calc R U . . .
C14 C 0.1917(4) 0.3942(5) 0.5207(3) 0.0331(11) Uani 1 1 d . . . . .
H14A H 0.186675 0.383857 0.459227 0.040 Uiso 1 1 calc R U . . .
H14B H 0.137628 0.443285 0.536016 0.040 Uiso 1 1 calc R U . . .
C15 C 0.3899(3) 0.6992(5) 0.5782(3) 0.0249(10) Uani 1 1 d . . . . .
H15A H 0.440628 0.673945 0.543664 0.030 Uiso 1 1 calc R U . . .
C16 C 0.3947(3) 0.8475(5) 0.5869(3) 0.0292(11) Uani 1 1 d . . . . .
H16A H 0.381915 0.887729 0.531245 0.035 Uiso 1 1 calc R U . . .
H16B H 0.347350 0.877210 0.622924 0.035 Uiso 1 1 calc R U . . .
C17 C 0.4887(4) 0.8909(6) 0.6246(4) 0.0443(14) Uani 1 1 d . . . . .
H17A H 0.535400 0.869096 0.585757 0.053 Uiso 1 1 calc R U . . .
H17B H 0.488826 0.985928 0.632072 0.053 Uiso 1 1 calc R U . . .
C18 C 0.5134(4) 0.8259(7) 0.7085(4) 0.0546(17) Uani 1 1 d . . . . .
H18A H 0.576634 0.850151 0.729123 0.065 Uiso 1 1 calc R U . . .
H18B H 0.471697 0.857180 0.749474 0.065 Uiso 1 1 calc R U . . .
C19 C 0.5065(4) 0.6806(7) 0.7018(4) 0.0474(15) Uani 1 1 d . . . . .
H19A H 0.518473 0.642128 0.758096 0.057 Uiso 1 1 calc R U . . .
H19B H 0.553989 0.648393 0.666691 0.057 Uiso 1 1 calc R U . . .
C20 C 0.4118(4) 0.6367(5) 0.6638(3) 0.0341(12) Uani 1 1 d . . . . .
H20A H 0.410936 0.541435 0.658020 0.041 Uiso 1 1 calc R U . . .
H20B H 0.364650 0.661503 0.701449 0.041 Uiso 1 1 calc R U . . .
C21 C 0.3150(3) 0.6441(4) 0.4089(3) 0.0277(11) Uani 1 1 d . . . . .
H21A H 0.363623 0.576443 0.407973 0.033 Uiso 1 1 calc R U . . .
C22 C 0.2402(3) 0.6011(5) 0.3453(3) 0.0301(11) Uani 1 1 d . . . . .
H22A H 0.189736 0.664926 0.342956 0.036 Uiso 1 1 calc R U . . .
H22B H 0.215625 0.517104 0.362809 0.036 Uiso 1 1 calc R U . . .
C23 C 0.2742(4) 0.5869(5) 0.2585(3) 0.0307(11) Uani 1 1 d . . . . .
H23A H 0.321351 0.518251 0.259684 0.037 Uiso 1 1 calc R U . . .
H23B H 0.222678 0.560741 0.218303 0.037 Uiso 1 1 calc R U . . .
C24 C 0.3140(4) 0.7117(5) 0.2305(3) 0.0342(11) Uani 1 1 d . . . . .
H24A H 0.265470 0.778368 0.224296 0.041 Uiso 1 1 calc R U . . .
H24B H 0.338334 0.699234 0.175453 0.041 Uiso 1 1 calc R U . . .
C25 C 0.3908(4) 0.7576(5) 0.2937(3) 0.0373(15) Uani 1 1 d . . . . .
H25A H 0.442429 0.695876 0.294409 0.045 Uiso 1 1 calc R U . . .
H25B H 0.413030 0.842820 0.275991 0.045 Uiso 1 1 calc R U . . .
C26 C 0.3597(4) 0.7691(5) 0.3811(3) 0.0294(11) Uani 1 1 d . . . . .
H26A H 0.315405 0.841056 0.382574 0.035 Uiso 1 1 calc R U . . .
H26B H 0.413131 0.789736 0.420685 0.035 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 C1 1.883(5) . ?
Re1 C2 1.893(5) . ?
Re1 C4 2.257(6) . ?
Re1 C3 2.290(5) . ?
Re1 C5 2.303(5) . ?
Re1 C7 2.338(5) . ?
Re1 C6 2.348(5) . ?
Re1 P1 2.3951(12) . ?
P1 C15 1.871(5) . ?
P1 C21 1.871(4) . ?
P1 C9 1.887(5) . ?
O1 C1 1.167(6) . ?
O2 C2 1.157(6) . ?
O3 C8 1.208(7) . ?
C3 C8 1.441(8) . ?
C3 C7 1.443(8) . ?
C3 C4 1.442(8) . ?
C4 C5 1.404(7) . ?
C4 H4A 1.0000 . ?
C5 C6 1.416(8) . ?
C5 H5A 1.0000 . ?
C6 C7 1.416(7) . ?
C6 H6A 1.0000 . ?
C7 H7A 1.0000 . ?
C8 H8A 0.9500 . ?
C9 C14 1.514(7) . ?
C9 C10 1.552(6) . ?
C9 H9A 1.0000 . ?
C10 C11 1.532(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.523(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.530(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.538(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.530(7) . ?
C15 C16 1.542(7) . ?
C15 H15A 1.0000 . ?
C16 C17 1.526(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.524(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.510(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.538(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.503(7) . ?
C21 C26 1.532(6) . ?
C21 H21A 1.0000 . ?
C22 C23 1.527(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.502(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.527(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.518(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?

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
C1 Re1 C2 88.6(2) . . ?
C1 Re1 C4 91.4(2) . . ?
C2 Re1 C4 129.4(2) . . ?
C1 Re1 C3 110.7(2) . . ?
C2 Re1 C3 153.7(2) . . ?
C4 Re1 C3 37.0(2) . . ?
C1 Re1 C5 108.8(2) . . ?
C2 Re1 C5 97.4(2) . . ?
C4 Re1 C5 35.86(19) . . ?
C3 Re1 C5 60.2(2) . . ?
C1 Re1 C7 147.02(19) . . ?
C2 Re1 C7 122.1(2) . . ?
C4 Re1 C7 60.6(2) . . ?
C3 Re1 C7 36.32(19) . . ?
C5 Re1 C7 59.43(19) . . ?
C1 Re1 C6 144.2(2) . . ?
C2 Re1 C6 94.2(2) . . ?
C4 Re1 C6 59.7(2) . . ?
C3 Re1 C6 59.61(19) . . ?
C5 Re1 C6 35.4(2) . . ?
C7 Re1 C6 35.18(18) . . ?
C1 Re1 P1 90.17(15) . . ?
C2 Re1 P1 92.68(15) . . ?
C4 Re1 P1 137.91(15) . . ?
C3 Re1 P1 104.52(14) . . ?
C5 Re1 P1 158.64(15) . . ?
C7 Re1 P1 99.30(13) . . ?
C6 Re1 P1 125.25(15) . . ?
C15 P1 C21 101.8(2) . . ?
C15 P1 C9 101.6(2) . . ?
C21 P1 C9 104.1(2) . . ?
C15 P1 Re1 117.25(15) . . ?
C21 P1 Re1 116.85(17) . . ?
C9 P1 Re1 113.26(15) . . ?
O1 C1 Re1 174.5(4) . . ?
O2 C2 Re1 173.2(4) . . ?
C8 C3 C7 126.8(5) . . ?
C8 C3 C4 126.1(5) . . ?
C7 C3 C4 107.1(5) . . ?
C8 C3 Re1 121.4(4) . . ?
C7 C3 Re1 73.6(3) . . ?
C4 C3 Re1 70.3(3) . . ?
C5 C4 C3 108.0(5) . . ?
C5 C4 Re1 73.9(3) . . ?
C3 C4 Re1 72.7(3) . . ?
C5 C4 H4A 125.8 . . ?
C3 C4 H4A 125.8 . . ?
Re1 C4 H4A 125.8 . . ?
C4 C5 C6 108.8(5) . . ?
C4 C5 Re1 70.3(3) . . ?
C6 C5 Re1 74.0(3) . . ?
C4 C5 H5A 125.5 . . ?
C6 C5 H5A 125.5 . . ?
Re1 C5 H5A 125.5 . . ?
C7 C6 C5 108.6(5) . . ?
C7 C6 Re1 72.0(3) . . ?
C5 C6 Re1 70.5(3) . . ?
C7 C6 H6A 125.7 . . ?
C5 C6 H6A 125.7 . . ?
Re1 C6 H6A 125.7 . . ?
C6 C7 C3 107.5(5) . . ?
C6 C7 Re1 72.8(3) . . ?
C3 C7 Re1 70.0(3) . . ?
C6 C7 H7A 126.2 . . ?
C3 C7 H7A 126.2 . . ?
Re1 C7 H7A 126.2 . . ?
O3 C8 C3 125.3(6) . . ?
O3 C8 H8A 117.4 . . ?
C3 C8 H8A 117.4 . . ?
C14 C9 C10 109.6(4) . . ?
C14 C9 P1 117.4(3) . . ?
C10 C9 P1 114.0(3) . . ?
C14 C9 H9A 104.8 . . ?
C10 C9 H9A 104.8 . . ?
P1 C9 H9A 104.8 . . ?
C11 C10 C9 110.5(4) . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 110.3(5) . . ?
C12 C11 H11A 109.6 . . ?
C10 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 111.8(5) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 C14 111.3(5) . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C9 C14 C13 110.8(4) . . ?
C9 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C20 C15 C16 109.5(4) . . ?
C20 C15 P1 116.1(3) . . ?
C16 C15 P1 111.9(3) . . ?
C20 C15 H15A 106.2 . . ?
C16 C15 H15A 106.2 . . ?
P1 C15 H15A 106.2 . . ?
C17 C16 C15 111.2(4) . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 111.2(5) . . ?
C18 C17 H17A 109.4 . . ?
C16 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C16 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C19 C18 C17 111.5(5) . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
C17 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 C20 112.0(5) . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C15 C20 C19 110.4(5) . . ?
C15 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
C15 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C22 C21 C26 110.9(4) . . ?
C22 C21 P1 114.0(3) . . ?
C26 C21 P1 115.0(3) . . ?
C22 C21 H21A 105.3 . . ?
C26 C21 H21A 105.3 . . ?
P1 C21 H21A 105.3 . . ?
C21 C22 C23 111.9(4) . . ?
C21 C22 H22A 109.2 . . ?
C23 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C24 C23 C22 110.9(4) . . ?
C24 C23 H23A 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C25 110.6(4) . . ?
C23 C24 H24A 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C26 C25 C24 112.2(4) . . ?
C26 C25 H25A 109.2 . . ?
C24 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
C24 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 C21 111.9(4) . . ?
C25 C26 H26A 109.2 . . ?
C21 C26 H26A 109.2 . . ?
C25 C26 H26B 109.2 . . ?
C21 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?

_refine_diff_density_max         2.398
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.155


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1813000'
_audit_update_record             
;
2017-12-21 deposited with the CCDC.
2018-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H20 O3 P Re'
_chemical_formula_weight         597.59

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'
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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.4865(6)
_cell_length_b                   15.5796(6)
_cell_length_c                   18.0757(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4361.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11696
_cell_measurement_theta_min      2.9410
_cell_measurement_theta_max      34.5430

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_F_000             2320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.672
_shelx_estimated_absorpt_T_min   0.397
_shelx_estimated_absorpt_T_max   0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34093
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.919
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3844
_reflns_number_gt                3168
_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.
 
 _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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP-III (Farrugia 2012)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+9.2045P] 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         3844
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.002
_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 0.51970(2) 0.57151(2) 0.77595(2) 0.02058(9) Uani 1 1 d . . . . .
P1 P 0.55555(8) 0.65620(8) 0.67223(7) 0.0204(3) Uani 1 1 d . . . . .
O1 O 0.7109(3) 0.5479(3) 0.8124(2) 0.0376(10) Uani 1 1 d . . . . .
C1 C 0.6389(4) 0.5565(3) 0.7963(3) 0.0250(12) Uani 1 1 d . . . . .
O2 O 0.5202(2) 0.4073(2) 0.6828(2) 0.0367(10) Uani 1 1 d . . . . .
C2 C 0.5206(3) 0.4710(4) 0.7155(3) 0.0229(12) Uani 1 1 d . . . . .
C3 C 0.4570(4) 0.5421(4) 0.8886(3) 0.0347(14) Uani 1 1 d . . . . .
H3A H 0.475258 0.496353 0.924111 0.042 Uiso 1 1 calc R U . . .
O3 O 0.5962(3) 0.6220(4) 0.9801(3) 0.0764(17) Uani 1 1 d . . . . .
C4 C 0.3929(4) 0.5344(4) 0.8337(4) 0.0472(17) Uani 1 1 d . . . . .
H4A H 0.358191 0.481671 0.823289 0.057 Uiso 1 1 calc R U . . .
C5 C 0.3796(4) 0.6170(5) 0.8003(4) 0.0461(17) Uani 1 1 d . . . . .
H5A H 0.334643 0.631499 0.762581 0.055 Uiso 1 1 calc R U . . .
C6 C 0.4374(4) 0.6755(4) 0.8341(3) 0.0382(14) Uani 1 1 d . . . . .
H6A H 0.440270 0.738730 0.825089 0.046 Uiso 1 1 calc R U . . .
C7 C 0.4847(4) 0.6289(4) 0.8890(3) 0.0361(14) Uani 1 1 d . . . . .
C8 C 0.5560(5) 0.6630(5) 0.9366(4) 0.0516(18) Uani 1 1 d . . . . .
H8A H 0.570227 0.722043 0.931648 0.062 Uiso 1 1 calc R U . . .
C9 C 0.4649(3) 0.8020(3) 0.6163(3) 0.0285(12) Uani 1 1 d . . . . .
H9A H 0.513340 0.835579 0.630435 0.034 Uiso 1 1 calc R U . . .
C10 C 0.4639(3) 0.7144(3) 0.6312(3) 0.0244(11) Uani 1 1 d . . . . .
C11 C 0.3916(3) 0.6667(3) 0.6108(3) 0.0340(14) Uani 1 1 d . . . . .
H11A H 0.389066 0.607245 0.622256 0.041 Uiso 1 1 calc R U . . .
C12 C 0.3231(4) 0.7054(4) 0.5736(4) 0.0390(15) Uani 1 1 d . . . . .
H12A H 0.274602 0.672121 0.558977 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3256(4) 0.7918(4) 0.5582(3) 0.0390(14) Uani 1 1 d . . . . .
H13A H 0.279493 0.817977 0.531919 0.047 Uiso 1 1 calc R U . . .
C14 C 0.3953(4) 0.8405(4) 0.5809(4) 0.0407(15) Uani 1 1 d . . . . .
H14A H 0.395652 0.900641 0.572329 0.049 Uiso 1 1 calc R U . . .
C15 C 0.6020(3) 0.6007(3) 0.5920(3) 0.0220(11) Uani 1 1 d . . . . .
C16 C 0.5701(4) 0.6068(3) 0.5208(3) 0.0319(13) Uani 1 1 d . . . . .
H16A H 0.518399 0.637974 0.511983 0.038 Uiso 1 1 calc R U . . .
C17 C 0.6124(4) 0.5681(4) 0.4620(3) 0.0385(15) Uani 1 1 d . . . . .
H17A H 0.589027 0.572611 0.413529 0.046 Uiso 1 1 calc R U . . .
C18 C 0.6881(4) 0.5230(4) 0.4731(3) 0.0328(13) Uani 1 1 d . . . . .
H18A H 0.717523 0.497610 0.432516 0.039 Uiso 1 1 calc R U . . .
C19 C 0.7206(4) 0.5154(3) 0.5441(3) 0.0318(13) Uani 1 1 d . . . . .
H19A H 0.772162 0.483723 0.552373 0.038 Uiso 1 1 calc R U . . .
C20 C 0.6788(3) 0.5534(3) 0.6028(3) 0.0286(12) Uani 1 1 d . . . . .
H20A H 0.701947 0.547711 0.651243 0.034 Uiso 1 1 calc R U . . .
C21 C 0.6377(3) 0.7396(3) 0.6878(3) 0.0225(11) Uani 1 1 d . . . . .
C22 C 0.6936(3) 0.7659(3) 0.6321(3) 0.0307(12) Uani 1 1 d . . . . .
H22A H 0.686562 0.744275 0.583328 0.037 Uiso 1 1 calc R U . . .
C23 C 0.7598(3) 0.8235(3) 0.6472(4) 0.0371(15) Uani 1 1 d . . . . .
H23A H 0.799145 0.839325 0.609266 0.045 Uiso 1 1 calc R U . . .
C24 C 0.7683(4) 0.8577(4) 0.7171(4) 0.0372(15) Uani 1 1 d . . . . .
H24A H 0.813403 0.897266 0.727411 0.045 Uiso 1 1 calc R U . . .
C25 C 0.7113(4) 0.8344(4) 0.7721(3) 0.0394(15) Uani 1 1 d . . . . .
H25A H 0.715960 0.859336 0.819930 0.047 Uiso 1 1 calc R U . . .
C26 C 0.6475(4) 0.7751(4) 0.7578(3) 0.0349(14) Uani 1 1 d . . . . .
H26A H 0.609504 0.758126 0.796400 0.042 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 C1 1.896(6) . ?
Re1 C2 1.910(6) . ?
Re1 C7 2.296(6) . ?
Re1 C4 2.298(6) . ?
Re1 C3 2.302(5) . ?
Re1 C6 2.314(6) . ?
Re1 C5 2.325(6) . ?
Re1 P1 2.3588(13) . ?
P1 C15 1.836(5) . ?
P1 C21 1.840(5) . ?
P1 C10 1.841(5) . ?
O1 C1 1.160(6) . ?
O2 C2 1.155(7) . ?
C3 C4 1.409(9) . ?
C3 C7 1.418(8) . ?
C3 H3A 1.0000 . ?
O3 C8 1.188(9) . ?
C4 C5 1.435(10) . ?
C4 H4A 1.0000 . ?
C5 C6 1.417(9) . ?
C5 H5A 1.0000 . ?
C6 C7 1.430(9) . ?
C6 H6A 1.0000 . ?
C7 C8 1.498(9) . ?
C8 H8A 0.9500 . ?
C9 C14 1.389(7) . ?
C9 C10 1.390(7) . ?
C9 H9A 0.9500 . ?
C10 C11 1.394(7) . ?
C11 C12 1.393(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.375(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.382(8) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.382(7) . ?
C15 C20 1.413(7) . ?
C16 C17 1.386(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.382(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.383(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.377(7) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C22 1.389(7) . ?
C21 C26 1.390(8) . ?
C22 C23 1.389(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.379(9) . ?
C23 H23A 0.9500 . ?
C24 C25 1.378(9) . ?
C24 H24A 0.9500 . ?
C25 C26 1.378(8) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Re1 C2 90.2(2) . . ?
C1 Re1 C7 96.1(2) . . ?
C2 Re1 C7 146.1(2) . . ?
C1 Re1 C4 135.5(2) . . ?
C2 Re1 C4 93.4(2) . . ?
C7 Re1 C4 59.4(2) . . ?
C1 Re1 C3 102.4(2) . . ?
C2 Re1 C3 110.2(2) . . ?
C7 Re1 C3 35.9(2) . . ?
C4 Re1 C3 35.7(2) . . ?
C1 Re1 C6 122.3(2) . . ?
C2 Re1 C6 146.9(2) . . ?
C7 Re1 C6 36.2(2) . . ?
C4 Re1 C6 59.9(2) . . ?
C3 Re1 C6 60.3(2) . . ?
C1 Re1 C5 155.4(2) . . ?
C2 Re1 C5 111.4(2) . . ?
C7 Re1 C5 59.5(2) . . ?
C4 Re1 C5 36.2(2) . . ?
C3 Re1 C5 60.0(2) . . ?
C6 Re1 C5 35.6(2) . . ?
C1 Re1 P1 89.66(16) . . ?
C2 Re1 P1 90.12(15) . . ?
C7 Re1 P1 123.06(16) . . ?
C4 Re1 P1 134.64(19) . . ?
C3 Re1 P1 156.02(15) . . ?
C6 Re1 P1 95.70(16) . . ?
C5 Re1 P1 101.52(17) . . ?
C15 P1 C21 100.5(2) . . ?
C15 P1 C10 102.5(2) . . ?
C21 P1 C10 104.3(2) . . ?
C15 P1 Re1 117.19(16) . . ?
C21 P1 Re1 115.87(17) . . ?
C10 P1 Re1 114.46(17) . . ?
O1 C1 Re1 176.6(5) . . ?
O2 C2 Re1 175.8(5) . . ?
C4 C3 C7 107.3(5) . . ?
C4 C3 Re1 72.0(3) . . ?
C7 C3 Re1 71.8(3) . . ?
C4 C3 H3A 126.2 . . ?
C7 C3 H3A 126.2 . . ?
Re1 C3 H3A 126.2 . . ?
C3 C4 C5 108.8(6) . . ?
C3 C4 Re1 72.3(3) . . ?
C5 C4 Re1 73.0(3) . . ?
C3 C4 H4A 125.5 . . ?
C5 C4 H4A 125.5 . . ?
Re1 C4 H4A 125.5 . . ?
C6 C5 C4 107.7(6) . . ?
C6 C5 Re1 71.8(3) . . ?
C4 C5 Re1 70.9(3) . . ?
C6 C5 H5A 126.1 . . ?
C4 C5 H5A 126.1 . . ?
Re1 C5 H5A 126.1 . . ?
C5 C6 C7 107.2(5) . . ?
C5 C6 Re1 72.7(3) . . ?
C7 C6 Re1 71.2(3) . . ?
C5 C6 H6A 126.2 . . ?
C7 C6 H6A 126.2 . . ?
Re1 C6 H6A 126.2 . . ?
C3 C7 C6 109.0(5) . . ?
C3 C7 C8 124.3(6) . . ?
C6 C7 C8 126.5(6) . . ?
C3 C7 Re1 72.3(3) . . ?
C6 C7 Re1 72.6(3) . . ?
C8 C7 Re1 118.4(4) . . ?
O3 C8 C7 125.1(7) . . ?
O3 C8 H8A 117.4 . . ?
C7 C8 H8A 117.4 . . ?
C14 C9 C10 120.3(5) . . ?
C14 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C9 C10 C11 118.8(5) . . ?
C9 C10 P1 123.6(4) . . ?
C11 C10 P1 117.6(4) . . ?
C12 C11 C10 120.6(5) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C13 C12 C11 120.0(5) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C14 120.0(5) . . ?
C12 C13 H13A 120.0 . . ?
C14 C13 H13A 120.0 . . ?
C13 C14 C9 120.4(5) . . ?
C13 C14 H14A 119.8 . . ?
C9 C14 H14A 119.8 . . ?
C16 C15 C20 117.8(5) . . ?
C16 C15 P1 124.3(4) . . ?
C20 C15 P1 117.8(4) . . ?
C15 C16 C17 121.0(5) . . ?
C15 C16 H16A 119.5 . . ?
C17 C16 H16A 119.5 . . ?
C18 C17 C16 120.7(5) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C17 C18 C19 119.2(5) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
C20 C19 C18 120.5(5) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C15 120.9(5) . . ?
C19 C20 H20A 119.6 . . ?
C15 C20 H20A 119.6 . . ?
C22 C21 C26 118.3(5) . . ?
C22 C21 P1 121.9(4) . . ?
C26 C21 P1 119.7(4) . . ?
C21 C22 C23 120.5(5) . . ?
C21 C22 H22A 119.7 . . ?
C23 C22 H22A 119.7 . . ?
C24 C23 C22 120.0(6) . . ?
C24 C23 H23A 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
C24 C25 C26 120.0(6) . . ?
C24 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C25 C26 C21 121.1(5) . . ?
C25 C26 H26A 119.5 . . ?
C21 C26 H26A 119.5 . . ?

_refine_diff_density_max         2.224
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.129


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
