# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_pb(of)cu3(seo3)2(no3)
_database_code_depnum_ccdc_archive 'CCDC 1894159'
_audit_update_record             
;
2019-01-28 deposited with the CCDC.	2020-08-25 downloaded from the CCDC.
;
_audit_creation_date             2019-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.67(Cu4.5 F1.5 N1.5 O15 Pb1.5 Se3)'
_chemical_formula_sum            'Cu3 F N O10 Pb Se2'
_chemical_formula_weight         748.74
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 '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'
Pb Pb -3.3944 10.1111 '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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_H-M_alt        'R 3 m'
_space_group_name_Hall           'R 3 -2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   6.69730(10)
_cell_length_b                   6.69730(10)
_cell_length_c                   18.5548(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     720.75(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    2844
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1680
_cell_measurement_theta_min      3.2790
_shelx_estimated_absorpt_T_max   0.364
_shelx_estimated_absorpt_T_min   0.330
_exptl_absorpt_coefficient_mu    31.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    5.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             999
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3679
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.540
_diffrn_reflns_theta_min         3.294
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00  62.00   0.50    5.00    --  -28.00  45.00 270.00  360
  2  ω   -118.00  62.00   0.50    5.00    --  -28.00  45.00 180.00  360
  3  ω   -118.00  62.00   0.50    5.00    --  -28.00  45.00  90.00  360
  4  ω   -118.00 -93.00   0.50    5.00    --  -28.00  45.00   0.00   50
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0220887000
_diffrn_orient_matrix_UB_12      -0.0671880000
_diffrn_orient_matrix_UB_13      0.0248215000
_diffrn_orient_matrix_UB_21      -0.0743640000
_diffrn_orient_matrix_UB_22      -0.1009954000
_diffrn_orient_matrix_UB_23      -0.0197506000
_diffrn_orient_matrix_UB_31      0.0945704000
_diffrn_orient_matrix_UB_32      0.0153437000
_diffrn_orient_matrix_UB_33      -0.0213315000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.986
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                705
_reflns_number_total             708
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.488(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         708
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0146
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+1.8800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0355
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.512(9)
 0.488(9)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.6667 0.3333 0.35012(2) 0.01185(10) Uani 1 6 d S T P . .
Se1 Se 0.3333 0.6667 0.36690(7) 0.0110(3) Uani 1 6 d S T P . .
Se2 Se 0.6667 0.3333 0.64972(7) 0.0114(3) Uani 1 6 d S T P . .
Cu1 Cu 0.50713(9) 0.49287(9) 0.50825(5) 0.01226(18) Uani 1 2 d S T P . .
F1 F 0.3333 0.6667 0.5313(5) 0.0131(14) Uani 1 6 d S T P . .
O1 O 0.6667 0.3333 0.4800(5) 0.0090(16) Uani 1 6 d S T P . .
O2 O 0.4665(5) 0.5335(5) 0.4052(3) 0.0182(11) Uani 1 2 d S T P . .
O3 O 0.5348(5) 0.4652(5) 0.6112(3) 0.0221(13) Uani 1 2 d S T P . .
O4 O 0.1059(5) 0.2118(11) 0.5130(4) 0.0370(17) Uani 1 2 d S T P . .
N1 N 0.0000 0.0000 0.5120(8) 0.0135(17) Uani 1 6 d S T P . .


_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 F1 2.823(8) 13_544 ?
Pb1 O1 2.409(9) . ?
Pb1 O2 2.537(6) 3_665 ?
Pb1 O2 2.537(6) 2_655 ?
Pb1 O2 2.537(6) . ?
Pb1 O3 2.694(6) 15_554 ?
Pb1 O3 2.694(6) 14_654 ?
Pb1 O3 2.694(6) 13_544 ?
Se1 O2 1.700(6) 2_665 ?
Se1 O2 1.700(6) 3_565 ?
Se1 O2 1.700(6) . ?
Se2 O3 1.689(6) 3_665 ?
Se2 O3 1.689(6) . ?
Se2 O3 1.689(6) 2_655 ?
Cu1 F1 2.061(2) . ?
Cu1 O1 1.924(3) . ?
Cu1 O2 1.970(6) . ?
Cu1 O3 1.937(5) . ?
Cu1 O4 2.391(4) . ?
Cu1 O4 2.391(4) 2_665 ?
F1 Cu1 2.061(2) 2_665 ?
F1 Cu1 2.061(2) 3_565 ?
O1 Cu1 1.924(3) 2_655 ?
O1 Cu1 1.924(3) 3_665 ?
O3 Pb1 2.694(6) 7_455 ?
O4 Cu1 2.391(4) 3_565 ?
O4 N1 1.228(6) . ?
N1 O4 1.228(6) 3 ?
N1 O4 1.228(6) 2 ?

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 F1 180.0 . 13_544 ?
O1 Pb1 O2 66.25(12) . 3_665 ?
O1 Pb1 O2 66.25(12) . 2_655 ?
O1 Pb1 O2 66.25(12) . . ?
O1 Pb1 O3 119.85(11) . 14_654 ?
O1 Pb1 O3 119.85(11) . 13_544 ?
O1 Pb1 O3 119.85(11) . 15_554 ?
O2 Pb1 F1 113.75(12) . 13_544 ?
O2 Pb1 F1 113.75(12) 3_665 13_544 ?
O2 Pb1 F1 113.75(12) 2_655 13_544 ?
O2 Pb1 O2 104.88(14) 2_655 . ?
O2 Pb1 O2 104.88(14) 3_665 . ?
O2 Pb1 O2 104.88(14) 3_665 2_655 ?
O2 Pb1 O3 78.67(10) 2_655 13_544 ?
O2 Pb1 O3 78.67(10) 3_665 13_544 ?
O2 Pb1 O3 78.67(10) 2_655 15_554 ?
O2 Pb1 O3 173.89(17) . 13_544 ?
O2 Pb1 O3 173.89(17) 3_665 15_554 ?
O2 Pb1 O3 78.67(10) 3_665 14_654 ?
O2 Pb1 O3 173.89(17) 2_655 14_654 ?
O2 Pb1 O3 78.67(10) . 15_554 ?
O2 Pb1 O3 78.67(10) . 14_654 ?
O3 Pb1 F1 60.15(11) 13_544 13_544 ?
O3 Pb1 F1 60.15(11) 14_654 13_544 ?
O3 Pb1 F1 60.15(11) 15_554 13_544 ?
O3 Pb1 O3 97.37(15) 13_544 15_554 ?
O3 Pb1 O3 97.37(15) 13_544 14_654 ?
O3 Pb1 O3 97.37(15) 15_554 14_654 ?
O2 Se1 O2 103.8(2) 3_565 . ?
O2 Se1 O2 103.8(2) 2_665 3_565 ?
O2 Se1 O2 103.8(2) 2_665 . ?
O3 Se2 O3 103.4(2) 2_655 3_665 ?
O3 Se2 O3 103.4(2) 2_655 . ?
O3 Se2 O3 103.4(2) 3_665 . ?
F1 Cu1 O4 72.97(12) . 2_665 ?
F1 Cu1 O4 72.97(12) . . ?
O1 Cu1 F1 176.1(3) . . ?
O1 Cu1 O2 88.0(3) . . ?
O1 Cu1 O3 96.3(3) . . ?
O1 Cu1 O4 106.89(12) . 2_665 ?
O1 Cu1 O4 106.89(12) . . ?
O2 Cu1 F1 88.1(3) . . ?
O2 Cu1 O4 88.1(2) . 2_665 ?
O2 Cu1 O4 88.1(2) . . ?
O3 Cu1 F1 87.6(3) . . ?
O3 Cu1 O2 175.7(3) . . ?
O3 Cu1 O4 90.7(2) . . ?
O3 Cu1 O4 90.7(2) . 2_665 ?
O4 Cu1 O4 145.8(2) . 2_665 ?
Cu1 F1 Cu1 115.80(16) 3_565 . ?
Cu1 F1 Cu1 115.80(16) 2_665 . ?
Cu1 F1 Cu1 115.81(16) 3_565 2_665 ?
Cu1 O1 Pb1 105.8(2) 3_665 . ?
Cu1 O1 Pb1 105.8(2) 2_655 . ?
Cu1 O1 Pb1 105.8(2) . . ?
Cu1 O1 Cu1 112.8(2) 3_665 2_655 ?
Cu1 O1 Cu1 112.9(2) 3_665 . ?
Cu1 O1 Cu1 112.9(2) 2_655 . ?
Se1 O2 Pb1 131.6(3) . . ?
Se1 O2 Cu1 128.5(3) . . ?
Cu1 O2 Pb1 99.9(2) . . ?
Se2 O3 Pb1 125.1(2) . 7_455 ?
Se2 O3 Cu1 124.6(3) . . ?
Cu1 O3 Pb1 110.3(2) . 7_455 ?
Cu1 O4 Cu1 93.8(2) . 3_565 ?
N1 O4 Cu1 132.95(12) . 3_565 ?
N1 O4 Cu1 132.95(12) . . ?
O4 N1 O4 119.98(5) 2 3 ?
O4 N1 O4 119.98(5) . 3 ?
O4 N1 O4 119.98(5) 2 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.778
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.512(9)
2 0.488(9)

