# 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_njy1
_database_code_depnum_ccdc_archive 'CCDC 1817070'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H50 Mo4 N4 O29 Re4'
_chemical_formula_weight         2035.28

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'
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'
Mo Mo -1.6832 0.6857 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/acd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, x+1/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'y+5/4, x+3/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-y-3/4, -x-1/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
'-y-1/4, -x+1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                   16.777
_cell_length_b                   16.777
_cell_length_c                   39.340
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11072.9
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5584
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      23.62

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7568
_exptl_absorpt_coefficient_mu    9.665
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2146
_exptl_absorpt_correction_T_max  0.2361
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26531
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2436
_reflns_number_gt                1936
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0875P)²+96.5109P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2436
_refine_ls_number_parameters     76
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1387
_refine_ls_wR_factor_gt          0.1302
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.58732(3) 0.20142(3) 0.201790(9) 0.0510(2) Uani 1 1 d . . .
Mo1 Mo 0.44327(5) 0.14635(5) 0.14854(2) 0.0441(3) Uani 1 1 d . . .
O1 O 0.4857(5) 0.0550(5) 0.15018(18) 0.066(2) Uiso 1 1 d . . .
O2 O 0.4610(4) 0.1772(4) 0.10256(17) 0.0455(16) Uiso 1 1 d . . .
O3 O 0.3425(5) 0.1289(5) 0.14983(19) 0.064(2) Uiso 1 1 d . . .
O4 O 0.4623(4) 0.1820(4) 0.19393(19) 0.0495(16) Uiso 1 1 d . . .
O5 O 0.7616(7) 0.2479(7) 0.2080(3) 0.105(3) Uiso 1 1 d . . .
O6 O 0.6452(7) 0.0319(7) 0.2093(3) 0.108(3) Uiso 1 1 d . . .
O7 O 0.5742(7) 0.1971(7) 0.2788(3) 0.102(3) Uiso 1 1 d . . .
N1 N 0.6183(7) 0.8683(7) 0.1250 0.083(4) Uiso 1 2 d S . .
C1 C 0.6940(8) 0.2293(8) 0.2060(3) 0.067(3) Uiso 1 1 d . . .
C2 C 0.6221(8) 0.0971(8) 0.2060(3) 0.073(3) Uiso 1 1 d . . .
C3 C 0.5817(7) 0.2005(7) 0.2490(4) 0.069(3) Uiso 1 1 d . . .
C4 C 0.6685(11) 0.8946(11) 0.0955(4) 0.110(5) Uiso 1 1 d . . .
H4A H 0.7238 0.8869 0.1008 0.165 Uiso 1 1 calc R . .
H4B H 0.6589 0.9500 0.0909 0.165 Uiso 1 1 calc R . .
H4C H 0.6550 0.8636 0.0758 0.165 Uiso 1 1 calc R . .
C5 C 0.5355(10) 0.8810(11) 0.1159(5) 0.115(6) Uiso 1 1 d . . .
H5A H 0.5019 0.8646 0.1344 0.173 Uiso 1 1 calc R . .
H5B H 0.5229 0.8502 0.0960 0.173 Uiso 1 1 calc R . .
H5C H 0.5269 0.9365 0.1112 0.173 Uiso 1 1 calc R . .
N2 N 0.3708(6) 1.0000 0.2500 0.079(4) Uiso 1 2 d SGD . .
C6 C 0.3206(6) 0.9371(5) 0.2654(3) 0.104 Uiso 1 1 d GD . .
H6A H 0.2974 0.9051 0.2478 0.157 Uiso 1 1 calc R . .
H6B H 0.2790 0.9613 0.2786 0.157 Uiso 1 1 calc R . .
H6C H 0.3528 0.9040 0.2798 0.157 Uiso 1 1 calc R . .
C7 C 0.4237(7) 1.0359(6) 0.2765(2) 0.125 Uiso 1 1 d GD . .
H7A H 0.4561 1.0766 0.2663 0.188 Uiso 1 1 calc R . .
H7B H 0.4574 0.9953 0.2859 0.188 Uiso 1 1 calc R . .
H7C H 0.3916 1.0588 0.2942 0.188 Uiso 1 1 calc R . .
O1W O 0.3130(18) -0.0630(18) 0.1250 0.160 Uiso 0.50 2 d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.0487(3) 0.0714(3) 0.0329(3) 0.00777(17) -0.00747(16) -0.0039(2)
Mo1 0.0504(5) 0.0498(5) 0.0321(5) 0.0037(3) -0.0004(3) -0.0061(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C2 1.853(14) . ?
Re1 C1 1.857(14) . ?
Re1 C3 1.859(16) . ?
Re1 O4 2.145(7) . ?
Re1 O4 2.148(7) 2_655 ?
Re1 O2 2.158(7) 23_656 ?
Mo1 O1 1.691(8) . ?
Mo1 O3 1.716(8) . ?
Mo1 O2 1.905(7) . ?
Mo1 O4 1.910(7) . ?
Mo1 O2 2.410(7) 32_565 ?
Mo1 O2 2.428(7) 23_656 ?
O2 Re1 2.158(7) 32_565 ?
O2 Mo1 2.410(7) 23_656 ?
O2 Mo1 2.428(7) 32_565 ?
O4 Re1 2.149(7) 2_655 ?
O5 C1 1.179(16) . ?
O6 C2 1.168(16) . ?
O7 C3 1.179(19) . ?
N1 C5 1.450(19) . ?
N1 C5 1.450(19) 6_455 ?
N1 C4 1.502(19) 6_455 ?
N1 C4 1.502(19) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
N2 C6 1.481(6) . ?
N2 C6 1.481(8) 3_575 ?
N2 C7 1.495(6) . ?
N2 C7 1.495(8) 3_575 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Re1 C1 85.8(6) . . ?
C2 Re1 C3 85.4(5) . . ?
C1 Re1 C3 87.8(5) . . ?
C2 Re1 O4 100.2(5) . . ?
C1 Re1 O4 173.4(4) . . ?
C3 Re1 O4 95.4(4) . . ?
C2 Re1 O4 174.4(5) . 2_655 ?
C1 Re1 O4 99.0(5) . 2_655 ?
C3 Re1 O4 97.6(4) . 2_655 ?
O4 Re1 O4 74.9(3) . 2_655 ?
C2 Re1 O2 101.2(4) . 23_656 ?
C1 Re1 O2 100.3(4) . 23_656 ?
C3 Re1 O2 169.9(4) . 23_656 ?
O4 Re1 O2 76.0(3) . 23_656 ?
O4 Re1 O2 75.3(3) 2_655 23_656 ?
O1 Mo1 O3 105.0(4) . . ?
O1 Mo1 O2 102.5(3) . . ?
O3 Mo1 O2 103.2(3) . . ?
O1 Mo1 O4 100.2(3) . . ?
O3 Mo1 O4 101.0(3) . . ?
O2 Mo1 O4 141.0(3) . . ?
O1 Mo1 O2 161.4(3) . 32_565 ?
O3 Mo1 O2 93.5(3) . 32_565 ?
O2 Mo1 O2 74.3(3) . 32_565 ?
O4 Mo1 O2 74.0(3) . 32_565 ?
O1 Mo1 O2 91.6(3) . 23_656 ?
O3 Mo1 O2 163.3(3) . 23_656 ?
O2 Mo1 O2 73.9(3) . 23_656 ?
O4 Mo1 O2 74.2(3) . 23_656 ?
O2 Mo1 O2 69.9(3) 32_565 23_656 ?
Mo1 O2 Re1 154.0(4) . 32_565 ?
Mo1 O2 Mo1 101.7(3) . 23_656 ?
Re1 O2 Mo1 93.9(2) 32_565 23_656 ?
Mo1 O2 Mo1 101.0(3) . 32_565 ?
Re1 O2 Mo1 92.9(2) 32_565 32_565 ?
Mo1 O2 Mo1 110.1(3) 23_656 32_565 ?
Mo1 O4 Re1 110.2(3) . . ?
Mo1 O4 Re1 110.8(3) . 2_655 ?
Re1 O4 Re1 102.7(3) . 2_655 ?
C5 N1 C5 110.0(18) . 6_455 ?
C5 N1 C4 113.0(10) . 6_455 ?
C5 N1 C4 107.6(10) 6_455 6_455 ?
C5 N1 C4 107.6(10) . . ?
C5 N1 C4 113.0(10) 6_455 . ?
C4 N1 C4 105.6(17) 6_455 . ?
O5 C1 Re1 178.5(12) . . ?
O6 C2 Re1 178.2(13) . . ?
O7 C3 Re1 176.0(12) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 N2 C6 110.6(3) . 3_575 ?
C6 N2 C7 109.9 . . ?
C6 N2 C7 109.6(6) 3_575 . ?
C6 N2 C7 109.6(6) . 3_575 ?
C6 N2 C7 109.9(4) 3_575 3_575 ?
C7 N2 C7 107.2(3) . 3_575 ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.548
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.195
