# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_28858
_database_code_depnum_ccdc_archive 'CCDC 1541606'
_audit_update_record             
;
2017-04-01 deposited with the CCDC.
2017-06-14 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         'C41 H72 Co2 O20 P4, 2(Cl4 Co)'
_chemical_formula_sum            'C20.50 H36 Cl4 Co2 O10 P2'
_chemical_formula_weight         764.09

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_H-M_alt        'C c c a'
_space_group_name_Hall           '-C 2b 2bc'

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

_cell_length_a                   15.6558(5)
_cell_length_b                   25.4691(8)
_cell_length_c                   16.3904(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6535.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2485
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      28.50

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      1.55
_exptl_crystal_density_method    floatation
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             3128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.485
_shelx_estimated_absorpt_T_min   0.648
_shelx_estimated_absorpt_T_max   0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.893132
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            41875
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.917
_diffrn_reflns_theta_max         28.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4134
_reflns_number_gt                2485
_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       
;
CrysAlis CCD 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_cell_refinement       
;
CrysAlis Red 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction        
;
CrysAlis Red 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0291P)²+4.1493P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4134
_refine_ls_number_parameters     191
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0742
_refine_ls_wR_factor_gt          0.0567
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.027
_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
Co1 Co 0.5000 0.49679(2) 0.2500 0.03975(11) Uani 1 2 d S T P . .
Cl1 Cl 0.38011(3) 0.44656(2) 0.24525(3) 0.05154(15) Uani 1 1 d . . . . .
Cl2 Cl 0.50021(4) 0.54734(3) 0.13582(3) 0.05490(16) Uani 1 1 d . . . . .
Co2 Co 0.7500 0.5000 -0.00115(2) 0.02872(9) Uani 1 2 d S T P . .
O1W O 0.87980(10) 0.48284(7) -0.00990(9) 0.0531(4) Uani 1 1 d D . . . .
H1W1 H 0.9055(15) 0.5015(9) -0.0426(13) 0.080 Uiso 1 1 d D U . . .
H2W1 H 0.9063(15) 0.4802(11) 0.0332(9) 0.080 Uiso 1 1 d D U . . .
O2W O 0.7500 0.5000 0.12534(14) 0.0749(9) Uani 1 2 d DS T P . .
H1W2 H 0.7909(14) 0.5146(13) 0.1467(17) 0.112 Uiso 1 1 d D U . . .
O3W O 0.7500 0.5000 -0.12635(12) 0.0499(6) Uani 1 2 d DS T P . .
H1W3 H 0.7086(11) 0.5083(11) -0.1544(13) 0.075 Uiso 1 1 d D U . . .
P1 P 0.71527(4) 0.36454(2) -0.00496(4) 0.04637(15) Uani 1 1 d . . . . .
O1 O 0.71717(11) 0.42150(5) 0.00330(9) 0.0523(4) Uani 1 1 d . . . . .
O2 O 0.80257(12) 0.33648(7) -0.01180(11) 0.0683(5) Uani 1 1 d . . . . .
C8 C 0.8742(2) 0.35319(11) 0.03295(19) 0.0903(10) Uani 1 1 d . . . . .
H81 H 0.8552 0.3702 0.0827 0.135 Uiso 1 1 calc R U . . .
H82 H 0.9059 0.3787 0.0011 0.135 Uiso 1 1 calc R U . . .
C9 C 0.93195(19) 0.30794(12) 0.0543(2) 0.0864(9) Uani 1 1 d . . . . .
H91 H 0.9042 0.2858 0.0935 0.130 Uiso 1 1 calc R U . . .
H92 H 0.9842 0.3212 0.0770 0.130 Uiso 1 1 calc R U . . .
H93 H 0.9443 0.2880 0.0060 0.130 Uiso 1 1 calc R U . . .
O3 O 0.66985(13) 0.34520(7) -0.08698(10) 0.0737(5) Uani 1 1 d . . . . .
C10 C 0.6914(2) 0.36550(12) -0.16379(17) 0.0807(8) Uani 1 1 d . . . . .
H101 H 0.7530 0.3655 -0.1702 0.121 Uiso 1 1 calc R U . . .
H102 H 0.6716 0.4015 -0.1681 0.121 Uiso 1 1 calc R U . . .
C11 C 0.6526(3) 0.33387(19) -0.2279(2) 0.1446(18) Uani 1 1 d . . . . .
H111 H 0.6578 0.2973 -0.2143 0.217 Uiso 1 1 calc R U . . .
H112 H 0.6810 0.3406 -0.2787 0.217 Uiso 1 1 calc R U . . .
H113 H 0.5932 0.3428 -0.2328 0.217 Uiso 1 1 calc R U . . .
C1 C 0.5000 0.2500 0.2500 0.0298(8) Uani 1 4 d S T P . .
C2 C 0.55554(12) 0.28202(7) 0.19111(11) 0.0323(4) Uani 1 1 d . . . . .
C3 C 0.62809(14) 0.25892(7) 0.15781(13) 0.0427(5) Uani 1 1 d . . . . .
H3 H 0.6438 0.2256 0.1753 0.051 Uiso 1 1 calc R U . . .
C4 C 0.67712(14) 0.28344(8) 0.10024(13) 0.0451(5) Uani 1 1 d . . . . .
H4 H 0.7255 0.2669 0.0797 0.054 Uiso 1 1 calc R U . . .
C5 C 0.65471(13) 0.33302(7) 0.07253(12) 0.0370(5) Uani 1 1 d . . . . .
C6 C 0.58213(14) 0.35641(8) 0.10345(12) 0.0403(5) Uani 1 1 d . . . . .
H6 H 0.5662 0.3896 0.0852 0.048 Uiso 1 1 calc R U . . .
C7 C 0.53291(13) 0.33113(7) 0.16112(12) 0.0353(4) Uani 1 1 d . . . . .
H7 H 0.4836 0.3473 0.1803 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
Co1 Cl2 2.2716(6) 3_655 ?
Co1 Cl2 2.2716(6) . ?
Co1 Cl1 2.2727(6) 3_655 ?
Co1 Cl1 2.2728(6) . ?
Co2 O3W 2.052(2) . ?
Co2 O1 2.0657(13) . ?
Co2 O1 2.0658(13) 2_665 ?
Co2 O2W 2.073(2) . ?
Co2 O1W 2.0834(16) 2_665 ?
Co2 O1W 2.0835(16) . ?
O1W H1W1 0.822(5) . ?
O1W H2W1 0.822(5) . ?
O2W H1W2 0.820(5) . ?
O3W H1W3 0.823(5) . ?
P1 O1 1.4573(15) . ?
P1 O2 1.5464(19) . ?
P1 O3 1.5986(17) . ?
P1 C5 1.777(2) . ?
O2 C8 1.406(3) . ?
C8 C9 1.506(4) . ?
C8 H81 0.9700 . ?
C8 H82 0.9700 . ?
C9 H91 0.9600 . ?
C9 H92 0.9600 . ?
C9 H93 0.9600 . ?
O3 C10 1.402(3) . ?
C10 C11 1.457(4) . ?
C10 H101 0.9700 . ?
C10 H102 0.9700 . ?
C11 H111 0.9600 . ?
C11 H112 0.9600 . ?
C11 H113 0.9600 . ?
C1 C2 1.5339(18) 6 ?
C1 C2 1.5339(18) 8_455 ?
C1 C2 1.5339(18) 3_655 ?
C1 C2 1.5339(18) . ?
C2 C7 1.390(2) . ?
C2 C3 1.391(3) . ?
C3 C4 1.367(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(3) . ?
C6 C7 1.379(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Co1 Cl2 110.95(4) 3_655 . ?
Cl2 Co1 Cl1 106.97(2) 3_655 3_655 ?
Cl2 Co1 Cl1 110.25(2) . 3_655 ?
Cl2 Co1 Cl1 110.25(2) 3_655 . ?
Cl2 Co1 Cl1 106.97(2) . . ?
Cl1 Co1 Cl1 111.49(3) 3_655 . ?
O3W Co2 O1 92.03(4) . . ?
O3W Co2 O1 92.03(4) . 2_665 ?
O1 Co2 O1 175.95(8) . 2_665 ?
O3W Co2 O2W 180.0 . . ?
O1 Co2 O2W 87.97(4) . . ?
O1 Co2 O2W 87.97(4) 2_665 . ?
O3W Co2 O1W 86.06(4) . 2_665 ?
O1 Co2 O1W 87.87(7) . 2_665 ?
O1 Co2 O1W 92.41(7) 2_665 2_665 ?
O2W Co2 O1W 93.94(4) . 2_665 ?
O3W Co2 O1W 86.06(4) . . ?
O1 Co2 O1W 92.41(7) . . ?
O1 Co2 O1W 87.87(7) 2_665 . ?
O2W Co2 O1W 93.94(4) . . ?
O1W Co2 O1W 172.11(9) 2_665 . ?
Co2 O1W H1W1 114(2) . . ?
Co2 O1W H2W1 116.8(19) . . ?
H1W1 O1W H2W1 111(3) . . ?
Co2 O2W H1W2 115(2) . . ?
Co2 O3W H1W3 124.0(18) . . ?
O1 P1 O2 116.66(10) . . ?
O1 P1 O3 113.21(10) . . ?
O2 P1 O3 100.94(11) . . ?
O1 P1 C5 113.21(9) . . ?
O2 P1 C5 108.34(10) . . ?
O3 P1 C5 102.98(9) . . ?
P1 O1 Co2 164.86(11) . . ?
C8 O2 P1 121.81(19) . . ?
O2 C8 C9 111.6(2) . . ?
O2 C8 H81 109.3 . . ?
C9 C8 H81 109.3 . . ?
O2 C8 H82 109.3 . . ?
C9 C8 H82 109.3 . . ?
H81 C8 H82 108.0 . . ?
C8 C9 H91 109.5 . . ?
C8 C9 H92 109.5 . . ?
H91 C9 H92 109.5 . . ?
C8 C9 H93 109.5 . . ?
H91 C9 H93 109.5 . . ?
H92 C9 H93 109.5 . . ?
C10 O3 P1 122.29(17) . . ?
O3 C10 C11 110.0(3) . . ?
O3 C10 H101 109.7 . . ?
C11 C10 H101 109.7 . . ?
O3 C10 H102 109.7 . . ?
C11 C10 H102 109.7 . . ?
H101 C10 H102 108.2 . . ?
C10 C11 H111 109.5 . . ?
C10 C11 H112 109.5 . . ?
H111 C11 H112 109.5 . . ?
C10 C11 H113 109.5 . . ?
H111 C11 H113 109.5 . . ?
H112 C11 H113 109.5 . . ?
C2 C1 C2 115.76(13) 6 8_455 ?
C2 C1 C2 110.94(14) 6 3_655 ?
C2 C1 C2 102.00(13) 8_455 3_655 ?
C2 C1 C2 102.00(13) 6 . ?
C2 C1 C2 110.94(14) 8_455 . ?
C2 C1 C2 115.76(13) 3_655 . ?
C7 C2 C3 116.75(17) . . ?
C7 C2 C1 123.82(16) . . ?
C3 C2 C1 119.01(15) . . ?
C4 C3 C2 122.41(18) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C3 C4 C5 119.98(19) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 118.77(18) . . ?
C6 C5 P1 120.47(15) . . ?
C4 C5 P1 120.69(16) . . ?
C7 C6 C5 120.69(19) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 121.35(19) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 Cl2 0.822(5) 2.428(7) 3.2422(16) 171(3) 10_655
O1W H2W1 Cl2 0.822(5) 2.337(10) 3.1344(16) 164(3) 2_665
O2W H1W2 Cl1 0.820(5) 2.462(12) 3.2405(17) 159(3) 4_565
O3W H1W3 Cl1 0.823(5) 2.338(10) 3.1304(13) 162(3) 9_665

_refine_diff_density_max         0.427
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.052


_exptl_crystal_preparation       
', Magnetic properties,third harmonic generation'
