# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_Lwk437s_new
_database_code_depnum_ccdc_archive 'CCDC 1421965'
_audit_update_record             
;
2015-09-02 deposited with the CCDC.
2016-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H14 O10 Os3 Te2'
_chemical_formula_weight         1288.15

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'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'

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

_cell_length_a                   14.1313(6)
_cell_length_b                   14.1313(6)
_cell_length_c                   28.8408(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5759.3(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9271
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      30.98

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.971
_exptl_crystal_F_000             4560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    15.242
_shelx_estimated_absorpt_T_min   0.121
_shelx_estimated_absorpt_T_max   0.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.121
_exptl_absorpt_correction_T_max  0.170
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35019
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.815
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2952
_reflns_number_gt                2864
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)] 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_abs_structure_details 
; 
 Flack x determined using 1253 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.000(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2952
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0168
_refine_ls_wR_factor_ref         0.0358
_refine_ls_wR_factor_gt          0.0355
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Os1 Os 0.57785(3) 0.7500 0.1250 0.01077(9) Uani 1 2 d S T P . .
Os2 Os 0.74163(2) 0.68739(2) 0.07050(2) 0.01170(7) Uani 1 1 d . . . . .
Te3 Te 0.80875(3) 0.86240(3) 0.09386(2) 0.01222(11) Uani 1 1 d . . . . .
C11 C 0.5838(5) 0.8720(6) 0.0935(3) 0.0165(16) Uani 1 1 d . . . . .
C12 C 0.4927(5) 0.7062(5) 0.0784(3) 0.0175(17) Uani 1 1 d . . . . .
C21 C 0.6752(5) 0.7413(6) 0.0200(3) 0.0170(17) Uani 1 1 d . . . . .
C22 C 0.6757(6) 0.5699(5) 0.0656(3) 0.0197(17) Uani 1 1 d . . . . .
C23 C 0.8463(6) 0.6442(6) 0.0343(3) 0.0242(19) Uani 1 1 d . . . . .
C31 C 0.9594(5) 0.8553(5) 0.0928(3) 0.0129(15) Uani 1 1 d . . . . .
C32 C 1.0052(5) 0.8352(5) 0.0513(3) 0.0174(17) Uani 1 1 d . . . . .
H32 H 0.9694 0.8211 0.0243 0.021 Uiso 1 1 calc R U . . .
C33 C 1.1027(5) 0.8358(5) 0.0495(3) 0.0165(17) Uani 1 1 d . . . . .
H33 H 1.1335 0.8211 0.0212 0.020 Uiso 1 1 calc R U . . .
C34 C 1.1577(5) 0.8578(5) 0.0887(3) 0.0132(16) Uani 1 1 d . . . . .
C35 C 1.2639(5) 0.8571(6) 0.0867(3) 0.0239(19) Uani 1 1 d . . . . .
H35A H 1.2894 0.8540 0.1183 0.036 Uiso 1 1 calc R U . . .
H35B H 1.2862 0.9151 0.0716 0.036 Uiso 1 1 calc R U . . .
H35C H 1.2853 0.8019 0.0691 0.036 Uiso 1 1 calc R U . . .
C36 C 1.1110(5) 0.8801(5) 0.1292(3) 0.0171(16) Uani 1 1 d . . . . .
H36 H 1.1464 0.8959 0.1561 0.021 Uiso 1 1 calc R U . . .
C37 C 1.0132(5) 0.8798(5) 0.1312(3) 0.0158(16) Uani 1 1 d . . . . .
H37 H 0.9824 0.8966 0.1593 0.019 Uiso 1 1 calc R U . . .
O11 O 0.5825(4) 0.9432(4) 0.0750(2) 0.0320(16) Uani 1 1 d . . . . .
O12 O 0.4408(4) 0.6841(4) 0.0494(2) 0.0260(13) Uani 1 1 d . . . . .
O21 O 0.6335(4) 0.7743(4) -0.0103(2) 0.0272(14) Uani 1 1 d . . . . .
O22 O 0.6339(5) 0.5010(4) 0.0637(2) 0.0356(15) Uani 1 1 d . . . . .
O23 O 0.9038(4) 0.6133(5) 0.0105(2) 0.0387(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C12 1.907(8) . ?
Os1 C12 1.907(8) 14_464 ?
Os1 C11 1.951(8) . ?
Os1 C11 1.951(8) 14_464 ?
Os1 Os2 2.9343(4) 14_464 ?
Os1 Os2 2.9343(4) . ?
Os2 C21 1.894(8) . ?
Os2 C22 1.909(8) . ?
Os2 C23 1.910(9) . ?
Os2 Te3 2.7330(6) . ?
Os2 Te3 2.7375(6) 14_464 ?
Te3 C31 2.131(7) . ?
Te3 Os2 2.7376(6) 14_464 ?
C11 O11 1.138(9) . ?
C12 O12 1.156(9) . ?
C21 O21 1.152(9) . ?
C22 O22 1.140(9) . ?
C23 O23 1.151(10) . ?
C31 C37 1.388(11) . ?
C31 C32 1.390(10) . ?
C32 C33 1.380(10) . ?
C33 C34 1.405(10) . ?
C34 C36 1.379(11) . ?
C34 C35 1.502(9) . ?
C36 C37 1.383(10) . ?

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
C12 Os1 C12 101.7(4) . 14_464 ?
C12 Os1 C11 89.2(3) . . ?
C12 Os1 C11 93.9(3) 14_464 . ?
C12 Os1 C11 93.9(3) . 14_464 ?
C12 Os1 C11 89.2(3) 14_464 14_464 ?
C11 Os1 C11 175.1(4) . 14_464 ?
C12 Os1 Os2 166.7(2) . 14_464 ?
C12 Os1 Os2 91.3(2) 14_464 14_464 ?
C11 Os1 Os2 87.1(2) . 14_464 ?
C11 Os1 Os2 89.0(2) 14_464 14_464 ?
C12 Os1 Os2 91.3(2) . . ?
C12 Os1 Os2 166.7(2) 14_464 . ?
C11 Os1 Os2 89.0(2) . . ?
C11 Os1 Os2 87.1(2) 14_464 . ?
Os2 Os1 Os2 75.859(14) 14_464 . ?
C21 Os2 C22 92.9(3) . . ?
C21 Os2 C23 95.3(3) . . ?
C22 Os2 C23 93.4(3) . . ?
C21 Os2 Te3 89.9(2) . . ?
C22 Os2 Te3 167.0(2) . . ?
C23 Os2 Te3 98.9(3) . . ?
C21 Os2 Te3 165.8(2) . 14_464 ?
C22 Os2 Te3 90.7(2) . 14_464 ?
C23 Os2 Te3 98.2(2) . 14_464 ?
Te3 Os2 Te3 83.682(17) . 14_464 ?
C21 Os2 Os1 84.2(2) . . ?
C22 Os2 Os1 85.2(2) . . ?
C23 Os2 Os1 178.5(3) . . ?
Te3 Os2 Os1 82.463(12) . . ?
Te3 Os2 Os1 82.386(13) 14_464 . ?
C31 Te3 Os2 107.47(19) . . ?
C31 Te3 Os2 110.3(2) . 14_464 ?
Os2 Te3 Os2 82.509(15) . 14_464 ?
O11 C11 Os1 176.6(7) . . ?
O12 C12 Os1 176.7(7) . . ?
O21 C21 Os2 178.9(7) . . ?
O22 C22 Os2 177.6(7) . . ?
O23 C23 Os2 174.0(8) . . ?
C37 C31 C32 118.9(6) . . ?
C37 C31 Te3 121.6(5) . . ?
C32 C31 Te3 119.1(5) . . ?
C33 C32 C31 119.7(7) . . ?
C32 C33 C34 121.6(7) . . ?
C36 C34 C33 117.9(6) . . ?
C36 C34 C35 120.8(7) . . ?
C33 C34 C35 121.4(7) . . ?
C34 C36 C37 120.9(7) . . ?
C36 C37 C31 121.0(7) . . ?

_refine_diff_density_max         0.982
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.116

