# 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_mo_170605e_0m
_database_code_depnum_ccdc_archive 'CCDC 1582224'
_audit_update_record             
;
2017-10-26 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Pb3SeO3Br4
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Br4 O3 Pb3 Se'
_chemical_formula_weight         1068.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   7.7290(15)
_cell_length_b                   8.4703(17)
_cell_length_c                   16.521(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1081.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2278
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      31.11

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    6.560
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   0.230
_exptl_transmission_factor_max   0.746
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    64.685
_shelx_estimated_absorpt_T_min   0.112
_shelx_estimated_absorpt_T_max   0.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            11056
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.466
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3138
_reflns_number_gt                2711
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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          
; 
 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)+(0.0124P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00323(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.371(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3138
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.002
_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
Pb1 Pb 0.55079(8) 1.00463(7) 0.92850(3) 0.01846(14) Uani 1 1 d . . . . .
Pb3 Pb 0.69502(7) 0.78452(6) 1.22839(4) 0.01961(15) Uani 1 1 d . . . . .
Pb2 Pb 0.54882(8) 0.49275(7) 0.93150(4) 0.02312(15) Uani 1 1 d . . . . .
Se1 Se 0.38523(17) 1.30184(15) 0.76954(9) 0.0140(3) Uani 1 1 d . . . . .
Br2 Br 0.74363(18) 0.7544(2) 1.03545(8) 0.0185(3) Uani 1 1 d . . . . .
Br4 Br 0.23851(18) 0.2494(2) 0.96529(9) 0.0216(3) Uani 1 1 d . . . . .
Br3 Br 0.9000(2) 0.99091(19) 0.85903(9) 0.0212(3) Uani 1 1 d . . . . .
Br1 Br 0.6224(2) 0.4939(2) 1.34491(10) 0.0284(4) Uani 1 1 d . . . . .
O1 O 0.5511(12) 1.2344(12) 0.8311(5) 0.017(2) Uani 1 1 d . . . . .
O3 O 0.3798(14) 1.4895(12) 0.8056(6) 0.018(2) Uani 1 1 d . . . . .
O2 O 0.5011(15) 1.3206(13) 0.6826(6) 0.026(3) 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
Pb1 O2 2.441(10) 3_646 ?
Pb1 O1 2.525(10) . ?
Pb1 Br3 2.9354(18) . ?
Pb1 Br4 3.0863(17) 4_567 ?
Pb1 Br2 3.1360(17) . ?
Pb1 Br4 3.2394(17) 1_565 ?
Pb3 O3 2.453(10) 4_577 ?
Pb3 O1 2.599(9) 2_675 ?
Pb3 O2 2.623(11) 2_675 ?
Pb3 Br3 2.9691(17) 2_675 ?
Pb3 Br1 3.1754(18) . ?
Pb3 Br2 3.2197(16) . ?
Pb2 O3 2.457(10) 1_545 ?
Pb2 O1 2.747(10) 1_545 ?
Pb2 Br1 2.9185(19) 2_664 ?
Pb2 Br4 3.0436(17) 4_557 ?
Pb2 Br2 3.1827(17) . ?
Pb2 Br4 3.2114(18) . ?
Pb2 Br2 3.2322(17) 4_467 ?
Se1 O3 1.698(10) . ?
Se1 O2 1.701(11) . ?
Se1 O1 1.733(9) . ?
Br2 Pb2 3.2322(17) 4_567 ?
Br4 Pb2 3.0436(18) 4_457 ?
Br4 Pb1 3.0863(17) 4_467 ?
Br4 Pb1 3.2394(17) 1_545 ?
Br3 Pb3 2.9692(17) 2_674 ?
Br1 Pb2 2.9185(19) 2_665 ?
O1 Pb3 2.599(9) 2_674 ?
O1 Pb2 2.747(10) 1_565 ?
O3 Pb3 2.453(10) 4_477 ?
O3 Pb2 2.457(10) 1_565 ?
O2 Pb1 2.441(10) 3_656 ?
O2 Pb3 2.623(11) 2_674 ?

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
O2 Pb1 O1 90.8(4) 3_646 . ?
O2 Pb1 Br3 80.3(3) 3_646 . ?
O1 Pb1 Br3 77.3(2) . . ?
O2 Pb1 Br4 159.4(3) 3_646 4_567 ?
O1 Pb1 Br4 80.9(2) . 4_567 ?
Br3 Pb1 Br4 79.44(5) . 4_567 ?
O2 Pb1 Br2 94.0(3) 3_646 . ?
O1 Pb1 Br2 151.6(2) . . ?
Br3 Pb1 Br2 75.91(4) . . ?
Br4 Pb1 Br2 84.98(4) 4_567 . ?
O2 Pb1 Br4 115.3(3) 3_646 1_565 ?
O1 Pb1 Br4 68.1(2) . 1_565 ?
Br3 Pb1 Br4 141.61(5) . 1_565 ?
Br4 Pb1 Br4 79.13(2) 4_567 1_565 ?
Br2 Pb1 Br4 132.91(4) . 1_565 ?
O3 Pb3 O1 76.0(3) 4_577 2_675 ?
O3 Pb3 O2 71.2(3) 4_577 2_675 ?
O1 Pb3 O2 59.4(3) 2_675 2_675 ?
O3 Pb3 Br3 79.1(2) 4_577 2_675 ?
O1 Pb3 Br3 75.6(2) 2_675 2_675 ?
O2 Pb3 Br3 130.4(2) 2_675 2_675 ?
O3 Pb3 Br1 147.8(3) 4_577 . ?
O1 Pb3 Br1 71.9(2) 2_675 . ?
O2 Pb3 Br1 94.0(3) 2_675 . ?
Br3 Pb3 Br1 90.70(5) 2_675 . ?
O3 Pb3 Br2 76.6(2) 4_577 . ?
O1 Pb3 Br2 123.6(2) 2_675 . ?
O2 Pb3 Br2 65.4(2) 2_675 . ?
Br3 Pb3 Br2 143.05(5) 2_675 . ?
Br1 Pb3 Br2 124.02(5) . . ?
O3 Pb2 O1 58.9(3) 1_545 1_545 ?
O3 Pb2 Br1 92.8(3) 1_545 2_664 ?
O1 Pb2 Br1 74.3(2) 1_545 2_664 ?
O3 Pb2 Br4 136.3(2) 1_545 4_557 ?
O1 Pb2 Br4 78.4(2) 1_545 4_557 ?
Br1 Pb2 Br4 83.19(5) 2_664 4_557 ?
O3 Pb2 Br2 135.8(2) 1_545 . ?
O1 Pb2 Br2 151.4(2) 1_545 . ?
Br1 Pb2 Br2 79.95(5) 2_664 . ?
Br4 Pb2 Br2 86.51(4) 4_557 . ?
O3 Pb2 Br4 75.1(3) 1_545 . ?
O1 Pb2 Br4 66.3(2) 1_545 . ?
Br1 Pb2 Br4 139.50(5) 2_664 . ?
Br4 Pb2 Br4 80.20(2) 4_557 . ?
Br2 Pb2 Br4 134.96(4) . . ?
O3 Pb2 Br2 76.3(2) 1_545 4_467 ?
O1 Pb2 Br2 129.4(2) 1_545 4_467 ?
Br1 Pb2 Br2 133.83(5) 2_664 4_467 ?
Br4 Pb2 Br2 134.70(5) 4_557 4_467 ?
Br2 Pb2 Br2 78.04(2) . 4_467 ?
Br4 Pb2 Br2 81.42(4) . 4_467 ?
O3 Se1 O2 102.8(5) . . ?
O3 Se1 O1 97.0(5) . . ?
O2 Se1 O1 97.9(5) . . ?
Pb1 Br2 Pb2 86.66(4) . . ?
Pb1 Br2 Pb3 116.67(5) . . ?
Pb2 Br2 Pb3 122.28(5) . . ?
Pb1 Br2 Pb2 89.67(5) . 4_567 ?
Pb2 Br2 Pb2 153.87(5) . 4_567 ?
Pb3 Br2 Pb2 82.27(4) . 4_567 ?
Pb2 Br4 Pb1 84.84(4) 4_457 4_467 ?
Pb2 Br4 Pb2 152.84(6) 4_457 . ?
Pb1 Br4 Pb2 90.95(5) 4_467 . ?
Pb2 Br4 Pb1 91.88(5) 4_457 1_545 ?
Pb1 Br4 Pb1 152.75(5) 4_467 1_545 ?
Pb2 Br4 Pb1 79.73(4) . 1_545 ?
Pb1 Br3 Pb3 91.80(5) . 2_674 ?
Pb2 Br1 Pb3 96.49(5) 2_665 . ?
Se1 O1 Pb1 128.8(5) . . ?
Se1 O1 Pb3 101.3(4) . 2_674 ?
Pb1 O1 Pb3 111.7(4) . 2_674 ?
Se1 O1 Pb2 95.0(4) . 1_565 ?
Pb1 O1 Pb2 103.2(3) . 1_565 ?
Pb3 O1 Pb2 116.6(4) 2_674 1_565 ?
Se1 O3 Pb3 131.7(5) . 4_477 ?
Se1 O3 Pb2 107.1(5) . 1_565 ?
Pb3 O3 Pb2 119.6(4) 4_477 1_565 ?
Se1 O2 Pb1 127.5(5) . 3_656 ?
Se1 O2 Pb3 101.3(4) . 2_674 ?
Pb1 O2 Pb3 125.5(4) 3_656 2_674 ?

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
O3 Se1 O1 Pb1 123.1(7) . . . . ?
O2 Se1 O1 Pb1 -132.9(7) . . . . ?
O3 Se1 O1 Pb3 -106.8(5) . . . 2_674 ?
O2 Se1 O1 Pb3 -2.8(5) . . . 2_674 ?
O3 Se1 O1 Pb2 11.6(4) . . . 1_565 ?
O2 Se1 O1 Pb2 115.7(4) . . . 1_565 ?
O2 Se1 O3 Pb3 81.5(8) . . . 4_477 ?
O1 Se1 O3 Pb3 -178.7(7) . . . 4_477 ?
O2 Se1 O3 Pb2 -113.3(5) . . . 1_565 ?
O1 Se1 O3 Pb2 -13.6(5) . . . 1_565 ?
O3 Se1 O2 Pb1 -52.3(8) . . . 3_656 ?
O1 Se1 O2 Pb1 -151.3(7) . . . 3_656 ?
O3 Se1 O2 Pb3 101.8(5) . . . 2_674 ?
O1 Se1 O2 Pb3 2.7(5) . . . 2_674 ?

_refine_diff_density_max         2.620
_refine_diff_density_min         -2.547
_refine_diff_density_rms         0.416

