# 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_mo_dtr26_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1455849'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-04-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H44 Cu F3 O3 P4 S'
_chemical_formula_weight         813.20

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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

_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+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'

_cell_length_a                   13.207(4)
_cell_length_b                   13.207(4)
_cell_length_c                   10.681(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1862.9(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1576
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      24.85

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_F_000             844
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.865
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3231
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.181
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             1536
_reflns_number_gt                1164
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.972

_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-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
;
 Refined as a 2-component inversion 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)+(0.1627P)²] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1536
_refine_ls_number_parameters     94
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0822
_refine_ls_wR_factor_ref         0.2337
_refine_ls_wR_factor_gt          0.2187
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.500 0.250 132.2 72.2
2 0.500 0.000 0.250 8.9 1.0
3 0.500 0.000 0.750 132.2 72.2
4 0.000 0.500 0.750 8.9 1.0
_platon_squeeze_details          
; 
Highly disordered anion CF3SO3 was treated by
SQUEEZE; correction is 146 electron/cell;
the required value is 134 electron/cell for two anions
in the full unit cell
;


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
Cu1 Cu 1.0000 1.0000 0.5000 0.0380(9) Uani 1 4 d S T P . .
P1 P 0.8571(2) 0.9590(2) 0.4022(3) 0.0389(9) Uani 1 1 d . . . . .
C1 C 0.8396(9) 0.8231(9) 0.3768(13) 0.045(3) Uani 1 1 d . . . . .
H1A H 0.7665 0.8093 0.3662 0.053 Uiso 1 1 calc R U . . .
H1B H 0.8740 0.8038 0.2980 0.053 Uiso 1 1 calc R U . . .
C2 C 0.8808(9) 0.7558(9) 0.4842(17) 0.054(4) Uani 1 1 d . . . . .
H2A H 0.8557 0.6860 0.4711 0.065 Uiso 1 1 calc R U . . .
H2B H 0.8516 0.7805 0.5640 0.065 Uiso 1 1 calc R U . . .
C3 C 0.9987(8) 0.7515(8) 0.4989(17) 0.047(3) Uani 1 1 d . . . . .
H3A H 1.0311 0.7561 0.4156 0.056 Uiso 1 1 calc R U . . .
H3B H 1.0187 0.6864 0.5376 0.056 Uiso 1 1 calc R U . . .
C4 C 0.8169(9) 1.0091(9) 0.2494(16) 0.049(3) Uani 1 1 d . . . . .
C5 C 0.7236(9) 0.9826(8) 0.1987(15) 0.047(4) Uani 1 1 d . . . . .
H5A H 0.6803 0.9374 0.2425 0.056 Uiso 1 1 calc R U . . .
C6 C 0.6950(12) 1.0203(11) 0.0887(19) 0.067(4) Uani 1 1 d . . . . .
H6A H 0.6316 1.0014 0.0538 0.080 Uiso 1 1 calc R U . . .
C7 C 0.7584(11) 1.0886(11) 0.0236(17) 0.059(4) Uani 1 1 d . . . . .
H7A H 0.7364 1.1160 -0.0540 0.071 Uiso 1 1 calc R U . . .
C8 C 0.8475(11) 1.1148(11) 0.0686(14) 0.054(4) Uani 1 1 d . . . . .
H8A H 0.8904 1.1588 0.0223 0.064 Uiso 1 1 calc R U . . .
C9 C 0.8791(10) 1.0767(8) 0.1870(15) 0.048(3) Uani 1 1 d . . . . .
H9A H 0.9417 1.0973 0.2225 0.058 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
Cu1 P1 2.224(3) . ?
Cu1 P1 2.224(3) 3_576 ?
Cu1 P1 2.224(3) 2_775 ?
Cu1 P1 2.224(3) 4_756 ?
P1 C3 1.836(13) 3_576 ?
P1 C1 1.830(12) . ?
P1 C4 1.839(17) . ?
C1 C2 1.55(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.566(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 P1 1.836(13) 4_756 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.384(18) . ?
C4 C5 1.392(18) . ?
C5 C6 1.33(2) . ?
C5 H5A 0.9500 . ?
C6 C7 1.41(2) . ?
C6 H6A 0.9500 . ?
C7 C8 1.32(2) . ?
C7 H7A 0.9500 . ?
C8 C9 1.42(2) . ?
C8 H8A 0.9500 . ?
C9 H9A 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
P1 Cu1 P1 102.75(8) . 3_576 ?
P1 Cu1 P1 123.97(19) . 2_775 ?
P1 Cu1 P1 102.75(8) 3_576 2_775 ?
P1 Cu1 P1 102.75(8) . 4_756 ?
P1 Cu1 P1 123.97(19) 3_576 4_756 ?
P1 Cu1 P1 102.75(8) 2_775 4_756 ?
C3 P1 C1 106.7(5) 3_576 . ?
C3 P1 C4 100.5(7) 3_576 . ?
C1 P1 C4 100.7(6) . . ?
C3 P1 Cu1 107.5(5) 3_576 . ?
C1 P1 Cu1 114.5(4) . . ?
C4 P1 Cu1 125.0(4) . . ?
C2 C1 P1 114.1(10) . . ?
C2 C1 H1A 108.7 . . ?
P1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
P1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 C3 116.3(12) . . ?
C1 C2 H2A 108.2 . . ?
C3 C2 H2A 108.2 . . ?
C1 C2 H2B 108.2 . . ?
C3 C2 H2B 108.2 . . ?
H2A C2 H2B 107.4 . . ?
C2 C3 P1 109.4(9) . 4_756 ?
C2 C3 H3A 109.8 . . ?
P1 C3 H3A 109.8 4_756 . ?
C2 C3 H3B 109.8 . . ?
P1 C3 H3B 109.8 4_756 . ?
H3A C3 H3B 108.2 . . ?
C9 C4 C5 120.0(15) . . ?
C9 C4 P1 119.3(10) . . ?
C5 C4 P1 120.7(11) . . ?
C6 C5 C4 120.0(13) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
C5 C6 C7 120.4(15) . . ?
C5 C6 H6A 119.8 . . ?
C7 C6 H6A 119.8 . . ?
C8 C7 C6 121.1(16) . . ?
C8 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C7 C8 C9 119.5(14) . . ?
C7 C8 H8A 120.2 . . ?
C9 C8 H8A 120.2 . . ?
C4 C9 C8 118.9(14) . . ?
C4 C9 H9A 120.6 . . ?
C8 C9 H9A 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 P1 C1 C2 -83.2(11) 3_576 . . . ?
C4 P1 C1 C2 172.3(9) . . . . ?
Cu1 P1 C1 C2 35.6(11) . . . . ?
P1 C1 C2 C3 -69.6(15) . . . . ?
C1 C2 C3 P1 86.6(15) . . . 4_756 ?
C3 P1 C4 C9 121.1(10) 3_576 . . . ?
C1 P1 C4 C9 -129.5(10) . . . . ?
Cu1 P1 C4 C9 0.9(13) . . . . ?
C3 P1 C4 C5 -56.7(11) 3_576 . . . ?
C1 P1 C4 C5 52.8(11) . . . . ?
Cu1 P1 C4 C5 -176.8(8) . . . . ?
C9 C4 C5 C6 1.5(19) . . . . ?
P1 C4 C5 C6 179.2(11) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?
C5 C6 C7 C8 1(2) . . . . ?
C6 C7 C8 C9 -2(2) . . . . ?
C5 C4 C9 C8 -2.5(18) . . . . ?
P1 C4 C9 C8 179.8(10) . . . . ?
C7 C8 C9 C4 3(2) . . . . ?

_refine_diff_density_max         2.147
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.132

_shelxl_version_number           2013-4

