# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1435068'
_audit_update_record             
;
2016-01-29 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_1                   
;
PROBLEM: Atom Pb1             has ADP max/min Ratio .....        5.1 oblate
RESPONSE: The ADP should be caused by the fact the atom weight of Pb and O is different too much. 
;

# Added during the CSD deposition process: Friday 29th of January 2016 05:46:10 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Br6 Cu2 H4 O4 Pb4'
_chemical_formula_weight         1503.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Br Br -0.2901 2.4595 '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'
Pb Pb -3.3944 10.1111 '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'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   14.1711(10)
_cell_length_b                   14.1711(10)
_cell_length_c                   15.8493(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3182.9(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2234
_cell_measurement_theta_min      2.866
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5056
_exptl_absorpt_coefficient_mu    59.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0403
_exptl_absorpt_correction_T_max  0.0867
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6046
_diffrn_reflns_av_R_equivalents  0.1204
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         25.01
_reflns_number_total             706
_reflns_number_gt                543
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0524P)²+730.1086P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         706
_refine_ls_number_parameters     38
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1315
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_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
Pb1 Pb 1.09747(6) 0.15431(6) 0.29241(5) 0.0106(4) Uani 1 1 d . . .
Cu1 Cu 0.3350(2) 0.9150(2) 0.1250 0.0153(9) Uani 1 2 d S . .
Br1 Br 0.2729(2) 1.0000 0.2500 0.0135(7) Uani 1 2 d S . .
Br2 Br 0.50286(15) 0.95328(15) 0.12229(15) 0.0108(5) Uani 1 1 d . . .
O1 O 0.9321(11) 0.1824(11) 0.3108(10) 0.010(3) Uani 1 1 d . . .
H1 H 0.9005 0.1492 0.2800 0.015 Uiso 1 1 d R . .

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
Pb1 0.0076(5) 0.0081(5) 0.0161(6) -0.0029(3) 0.0029(3) 0.0061(3)
Cu1 0.0121(13) 0.0121(13) 0.022(2) -0.0015(13) -0.0015(13) -0.0002(16)
Br1 0.0096(15) 0.0104(15) 0.0206(17) -0.0056(13) 0.000 0.000
Br2 0.0067(11) 0.0095(11) 0.0164(11) -0.0009(12) 0.0011(8) -0.0001(8)
O1 0.009(8) 0.009(8) 0.013(7) -0.001(7) 0.001(7) 0.003(6)

_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
Pb1 O1 2.370(16) 11_654 ?
Pb1 O1 2.394(16) . ?
Pb1 O1 2.398(15) 28_646 ?
Cu1 Br2 2.441(3) 8_665 ?
Cu1 Br2 2.441(3) . ?
Cu1 Br1 2.480(3) 4_464 ?
Cu1 Br1 2.480(3) . ?
Br1 Cu1 2.480(3) 2_655 ?
O1 Pb1 2.370(16) 11_654 ?
O1 Pb1 2.398(15) 18_676 ?
O1 H1 0.8128 . ?

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
O1 Pb1 O1 69.5(7) 11_654 . ?
O1 Pb1 O1 71.9(6) 11_654 28_646 ?
O1 Pb1 O1 71.5(6) . 28_646 ?
Br2 Cu1 Br2 115.7(2) 8_665 . ?
Br2 Cu1 Br1 104.59(9) 8_665 4_464 ?
Br2 Cu1 Br1 112.37(6) . 4_464 ?
Br2 Cu1 Br1 112.37(6) 8_665 . ?
Br2 Cu1 Br1 104.59(9) . . ?
Br1 Cu1 Br1 107.10(18) 4_464 . ?
Cu1 Br1 Cu1 138.46(17) 2_655 . ?
Pb1 O1 Pb1 108.7(6) 11_654 . ?
Pb1 O1 Pb1 105.2(6) 11_654 18_676 ?
Pb1 O1 Pb1 104.4(6) . 18_676 ?
Pb1 O1 H1 113.2 11_654 . ?
Pb1 O1 H1 111.8 . . ?
Pb1 O1 H1 112.9 18_676 . ?

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
Br2 Cu1 Br1 Cu1 114.39(14) 8_665 . . 2_655 ?
Br2 Cu1 Br1 Cu1 -11.86(9) . . . 2_655 ?
Br1 Cu1 Br1 Cu1 -131.30(4) 4_464 . . 2_655 ?
O1 Pb1 O1 Pb1 14.9(8) 11_654 . . 11_654 ?
O1 Pb1 O1 Pb1 91.9(6) 28_646 . . 11_654 ?
O1 Pb1 O1 Pb1 -97.1(5) 11_654 . . 18_676 ?
O1 Pb1 O1 Pb1 -20.0(6) 28_646 . . 18_676 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.648
_refine_diff_density_min         -4.850
_refine_diff_density_rms         0.626
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1534871'
_audit_update_record             
;
2017-02-26 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cl6 Cu2 H4 O4 Pb4'
_chemical_formula_weight         1236.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Cl Cl 0.1484 0.1585 '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'
Pb Pb -3.3944 10.1111 '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+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   13.7547(11)
_cell_length_b                   13.7547(11)
_cell_length_c                   15.3654(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2907.0(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1877
_cell_measurement_theta_min      2.962
_cell_measurement_theta_max      28.143

_exptl_crystal_description       block
_exptl_crystal_colour            gray
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4192
_exptl_absorpt_coefficient_mu    50.130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0652
_exptl_absorpt_correction_T_max  0.1272
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5483
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         24.92
_reflns_number_total             646
_reflns_number_gt                472
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0377P)²+20.6656P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         646
_refine_ls_number_parameters     38
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.140
_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
Pb1 Pb 0.40211(4) 0.34984(4) 0.03924(3) 0.0186(3) Uani 1 1 d . . .
Cu1 Cu 0.66593(15) 0.41593(15) 0.8750 0.0300(7) Uani 1 2 d S . .
Cl1 Cl 0.5006(2) 0.4538(3) 0.8796(3) 0.0209(8) Uani 1 1 d . . .
Cl2 Cl 0.7500 0.4719(4) 1.0000 0.0211(12) Uani 1 2 d S . .
O1 O 0.4309(7) 0.3178(7) 0.1922(6) 0.015(2) Uani 1 1 d . . .
H1 H 0.3960 0.3531 0.2252 0.017 Uiso 1 1 d R . .

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
Pb1 0.0186(4) 0.0180(4) 0.0192(4) 0.0029(3) -0.0035(2) 0.0072(2)
Cu1 0.0327(10) 0.0327(10) 0.0245(14) 0.0020(10) -0.0020(10) 0.0005(12)
Cl1 0.0194(19) 0.0227(19) 0.0206(19) 0.002(3) 0.0002(14) 0.0002(15)
Cl2 0.021(3) 0.017(3) 0.026(3) 0.000 -0.012(2) 0.000
O1 0.016(6) 0.017(6) 0.011(4) -0.003(4) 0.010(5) 0.006(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
Pb1 O1 2.336(10) 27_565 ?
Pb1 O1 2.377(10) 20_656 ?
Pb1 O1 2.424(9) . ?
Cu1 Cl1 2.334(4) 7_546 ?
Cu1 Cl1 2.334(4) . ?
Cu1 Cl2 2.370(2) . ?
Cu1 Cl2 2.370(2) 4_564 ?
Cl2 Cu1 2.370(2) 3_645 ?
O1 Pb1 2.336(10) 20_656 ?
O1 Pb1 2.377(10) 27_565 ?
O1 H1 0.8500 . ?

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
O1 Pb1 O1 68.8(4) 27_565 20_656 ?
O1 Pb1 O1 71.9(3) 27_565 . ?
O1 Pb1 O1 71.2(4) 20_656 . ?
Cl1 Cu1 Cl1 115.9(2) 7_546 . ?
Cl1 Cu1 Cl2 103.39(16) 7_546 . ?
Cl1 Cu1 Cl2 112.24(12) . . ?
Cl1 Cu1 Cl2 112.24(12) 7_546 4_564 ?
Cl1 Cu1 Cl2 103.39(16) . 4_564 ?
Cl2 Cu1 Cl2 109.9(2) . 4_564 ?
Cu1 Cl2 Cu1 142.1(2) . 3_645 ?
Pb1 O1 Pb1 109.4(4) 20_656 27_565 ?
Pb1 O1 Pb1 105.4(4) 20_656 . ?
Pb1 O1 Pb1 104.1(4) 27_565 . ?
Pb1 O1 H1 112.4 20_656 . ?
Pb1 O1 H1 112.4 27_565 . ?
Pb1 O1 H1 112.5 . . ?

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
Cl1 Cu1 Cl2 Cu1 -12.28(12) 7_546 . . 3_645 ?
Cl1 Cu1 Cl2 Cu1 113.30(15) . . . 3_645 ?
Cl2 Cu1 Cl2 Cu1 -132.26(6) 4_564 . . 3_645 ?
O1 Pb1 O1 Pb1 -94.24(14) 27_565 . . 20_656 ?
O1 Pb1 O1 Pb1 -21.1(4) 20_656 . . 20_656 ?
O1 Pb1 O1 Pb1 20.9(4) 27_565 . . 27_565 ?
O1 Pb1 O1 Pb1 94.02(13) 20_656 . . 27_565 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.92
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.910
_refine_diff_density_min         -2.941
_refine_diff_density_rms         0.499
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1435069'
_audit_update_record             
;
2016-01-29 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cu H2 I3 O2 Pb2'
_chemical_formula_weight         892.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
I I -0.4742 1.8119 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

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

_cell_length_a                   16.6743(15)
_cell_length_b                   20.8855(18)
_cell_length_c                   20.8865(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7273.7(11)
_cell_formula_units_Z            32
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3424
_cell_measurement_theta_min      2.759
_cell_measurement_theta_max      27.964

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             11840
_exptl_absorpt_coefficient_mu    49.377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0602
_exptl_absorpt_correction_T_max  0.1101
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8811
_diffrn_reflns_av_R_equivalents  0.1096
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1610
_reflns_number_gt                1320
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0590P)²+71.7119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1610
_refine_ls_number_parameters     74
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.095
_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
Pb1 Pb 0.54372(4) 0.37321(3) 0.78057(3) 0.0185(2) Uani 1 1 d . . .
Pb2 Pb 0.69893(4) 0.46743(3) 0.87193(3) 0.0205(2) Uani 1 1 d . . .
Cu1 Cu 0.3750 0.68117(15) 0.8750 0.0244(7) Uani 1 2 d S . .
Cu2 Cu 0.3750 0.54855(16) 0.8750 0.0253(7) Uani 1 2 d S . .
I1 I 0.37693(6) 0.47500(5) 0.97796(5) 0.0165(3) Uani 1 1 d . . .
I2 I 0.37730(6) 0.76547(6) 0.97161(5) 0.0175(3) Uani 1 1 d . . .
I3 I 0.50719(6) 0.61470(5) 0.86279(5) 0.0154(3) Uani 1 1 d . . .
O1 O 0.5601(6) 0.4405(6) 0.8741(4) 0.014(2) Uani 1 1 d U . .
H1 H 0.5297 0.4731 0.8735 0.016 Uiso 1 1 d R . .
O2 O 0.6848(6) 0.3738(4) 0.8095(6) 0.017(3) Uani 1 1 d . . .
H2 H 0.7160 0.3729 0.7773 0.020 Uiso 1 1 d R . .

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
Pb1 0.0186(4) 0.0196(4) 0.0172(4) 0.0008(2) -0.0038(2) -0.0021(3)
Pb2 0.0199(4) 0.0105(4) 0.0311(4) 0.0000(2) -0.0004(3) -0.0069(3)
Cu1 0.0196(15) 0.0148(17) 0.0389(18) 0.000 0.0024(13) 0.000
Cu2 0.0201(15) 0.0181(17) 0.0378(17) 0.000 0.0014(13) 0.000
I1 0.0151(6) 0.0100(6) 0.0243(6) 0.0020(4) 0.0000(4) 0.0015(4)
I2 0.0185(6) 0.0144(6) 0.0195(6) -0.0018(4) -0.0007(4) -0.0009(4)
I3 0.0116(5) 0.0099(5) 0.0248(5) -0.0005(4) 0.0026(4) -0.0001(4)
O1 0.011(4) 0.013(4) 0.017(4) -0.001(3) -0.002(3) 0.007(3)
O2 0.016(5) 0.010(6) 0.025(6) 0.004(4) -0.007(5) 0.000(5)

_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
Pb1 O1 2.410(9) 4_556 ?
Pb1 O1 2.421(10) . ?
Pb1 O2 2.429(10) . ?
Pb2 O2 2.362(10) . ?
Pb2 O1 2.383(10) . ?
Pb2 O2 2.396(10) 4_556 ?
Cu1 I3 2.617(2) 3_556 ?
Cu1 I3 2.617(2) . ?
Cu1 I2 2.678(2) . ?
Cu1 I2 2.678(2) 3_556 ?
Cu1 Cu2 2.770(5) . ?
Cu2 I3 2.614(2) . ?
Cu2 I3 2.614(2) 3_556 ?
Cu2 I1 2.643(2) 3_556 ?
Cu2 I1 2.643(2) . ?
O1 Pb1 2.410(9) 4_556 ?
O1 H1 0.8500 . ?
O2 Pb2 2.396(10) 4_556 ?
O2 H2 0.8500 . ?

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
O1 Pb1 O1 68.9(5) 4_556 . ?
O1 Pb1 O2 71.8(4) 4_556 . ?
O1 Pb1 O2 71.8(4) . . ?
O2 Pb2 O1 73.6(4) . . ?
O2 Pb2 O2 70.3(5) . 4_556 ?
O1 Pb2 O2 72.9(4) . 4_556 ?
I3 Cu1 I3 115.93(13) 3_556 . ?
I3 Cu1 I2 106.70(3) 3_556 . ?
I3 Cu1 I2 114.21(3) . . ?
I3 Cu1 I2 114.21(3) 3_556 3_556 ?
I3 Cu1 I2 106.70(3) . 3_556 ?
I2 Cu1 I2 97.80(11) . 3_556 ?
I3 Cu1 Cu2 57.97(6) 3_556 . ?
I3 Cu1 Cu2 57.97(6) . . ?
I2 Cu1 Cu2 131.10(6) . . ?
I2 Cu1 Cu2 131.10(6) 3_556 . ?
I3 Cu2 I3 116.18(13) . 3_556 ?
I3 Cu2 I1 103.77(3) . 3_556 ?
I3 Cu2 I1 112.11(3) 3_556 3_556 ?
I3 Cu2 I1 112.11(3) . . ?
I3 Cu2 I1 103.77(3) 3_556 . ?
I1 Cu2 I1 108.93(12) 3_556 . ?
I3 Cu2 Cu1 58.09(7) . . ?
I3 Cu2 Cu1 58.09(7) 3_556 . ?
I1 Cu2 Cu1 125.53(6) 3_556 . ?
I1 Cu2 Cu1 125.53(6) . . ?
Cu2 I3 Cu1 63.94(9) . . ?
Pb2 O1 Pb1 104.8(3) . 4_556 ?
Pb2 O1 Pb1 103.4(3) . . ?
Pb1 O1 Pb1 109.5(5) 4_556 . ?
Pb2 O1 H1 112.9 . . ?
Pb1 O1 H1 112.8 4_556 . ?
Pb1 O1 H1 112.8 . . ?
Pb2 O2 Pb2 108.5(5) . 4_556 ?
Pb2 O2 Pb1 103.8(4) . . ?
Pb2 O2 Pb1 103.8(4) 4_556 . ?
Pb2 O2 H2 113.3 . . ?
Pb2 O2 H2 113.2 4_556 . ?
Pb1 O2 H2 113.3 . . ?

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
I3 Cu1 Cu2 I3 180.0 3_556 . . . ?
I2 Cu1 Cu2 I3 -95.51(4) . . . . ?
I2 Cu1 Cu2 I3 84.49(4) 3_556 . . . ?
I3 Cu1 Cu2 I3 180.0 . . . 3_556 ?
I2 Cu1 Cu2 I3 84.49(4) . . . 3_556 ?
I2 Cu1 Cu2 I3 -95.51(4) 3_556 . . 3_556 ?
I3 Cu1 Cu2 I1 95.74(4) 3_556 . . 3_556 ?
I3 Cu1 Cu2 I1 -84.26(4) . . . 3_556 ?
I2 Cu1 Cu2 I1 -179.77(4) . . . 3_556 ?
I2 Cu1 Cu2 I1 0.23(4) 3_556 . . 3_556 ?
I3 Cu1 Cu2 I1 -84.26(4) 3_556 . . . ?
I3 Cu1 Cu2 I1 95.74(4) . . . . ?
I2 Cu1 Cu2 I1 0.23(4) . . . . ?
I2 Cu1 Cu2 I1 -179.77(4) 3_556 . . . ?
I3 Cu2 I3 Cu1 0.0 3_556 . . . ?
I1 Cu2 I3 Cu1 123.52(7) 3_556 . . . ?
I1 Cu2 I3 Cu1 -119.08(8) . . . . ?
I3 Cu1 I3 Cu2 0.0 3_556 . . . ?
I2 Cu1 I3 Cu2 124.68(8) . . . . ?
I2 Cu1 I3 Cu2 -128.46(7) 3_556 . . . ?
O2 Pb2 O1 Pb1 93.8(4) . . . 4_556 ?
O2 Pb2 O1 Pb1 19.9(4) 4_556 . . 4_556 ?
O2 Pb2 O1 Pb1 -20.9(4) . . . . ?
O2 Pb2 O1 Pb1 -94.8(4) 4_556 . . . ?
O1 Pb1 O1 Pb2 97.5(3) 4_556 . . . ?
O2 Pb1 O1 Pb2 20.6(4) . . . . ?
O1 Pb1 O1 Pb1 -13.8(5) 4_556 . . 4_556 ?
O2 Pb1 O1 Pb1 -90.7(4) . . . 4_556 ?
O1 Pb2 O2 Pb2 -89.1(4) . . . 4_556 ?
O2 Pb2 O2 Pb2 -11.9(5) 4_556 . . 4_556 ?
O1 Pb2 O2 Pb1 20.9(4) . . . . ?
O2 Pb2 O2 Pb1 98.1(3) 4_556 . . . ?
O1 Pb1 O2 Pb2 -93.9(4) 4_556 . . . ?
O1 Pb1 O2 Pb2 -20.8(4) . . . . ?
O1 Pb1 O2 Pb2 19.5(4) 4_556 . . 4_556 ?
O1 Pb1 O2 Pb2 92.7(4) . . . 4_556 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.214
_refine_diff_density_min         -4.063
_refine_diff_density_rms         0.765
