# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_FGP808
_audit_block_doi                 10.5517/ccdc.csd.cc23703h
_database_code_depnum_ccdc_archive 'CCDC 1943145'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.molstruc.2019.127139 2020
loop_
_audit_author_name
_audit_author_address
'Vincent DORCET'
;University of Rennes  ISCR 
France
;
_audit_update_record             
;
2019-09-13 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 17 novembre 2017                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H26 Br4 N4'
_chemical_formula_sum            'C44 H26 Br4 N4'
_chemical_formula_weight         930.33
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                            UNIT CELL INFORMATION                             #
#------------------------------------------------------------------------------#


_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'


_diffrn_orient_matrix_UB_11      -0.0125438
_diffrn_orient_matrix_UB_21      -0.0071298
_diffrn_orient_matrix_UB_31      -0.0383794
_diffrn_orient_matrix_UB_12      0.0249725
_diffrn_orient_matrix_UB_22      -0.1583445
_diffrn_orient_matrix_UB_32      0.0212541
_diffrn_orient_matrix_UB_13      -0.0412039
_diffrn_orient_matrix_UB_23      -0.0071086
_diffrn_orient_matrix_UB_33      -0.0045472

_cell_length_a                   27.018(3)
_cell_length_b                   6.1841(7)
_cell_length_c                   26.339(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.487(4)
_cell_angle_gamma                90
_cell_volume                     3972.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8029
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      27.47
_cell_measurement_wavelength     0.71073

#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1832
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_T_max  0.542

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_diffrn_reflns_av_r_equivalents  0.0574
_diffrn_reflns_av_uneti/neti     0.0396
_diffrn_reflns_number            23992
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.028
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             4528
_reflns_number_gt                3635
_reflns_threshold_expression     >2sigma(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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017_1 (Sheldrick, 2017)'
_computing_molecular_graphics    
'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2019)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_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)+(0.0224P)²+14.0139P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4528
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0700
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.088

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
N N 0.0061 0.0033 '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'

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
C1 C 0.56384(11) 0.1573(4) 0.43487(12) 0.0160(6) Uani 1 1 d . . . . .
C2 C 0.60768(12) 0.3031(5) 0.44041(13) 0.0216(6) Uani 1 1 d . . . . .
H2 H 0.625764 0.309913 0.416480 0.026 Uiso 1 1 calc R U . . .
C3 C 0.61811(12) 0.4277(5) 0.48599(13) 0.0210(6) Uani 1 1 d . . . . .
H3 H 0.644742 0.539417 0.500014 0.025 Uiso 1 1 calc R U . . .
C4 C 0.58118(11) 0.3593(4) 0.50938(12) 0.0156(6) Uani 1 1 d . . . . .
C5 C 0.58268(11) 0.4403(4) 0.55983(12) 0.0154(6) Uani 1 1 d . . . . .
C6 C 0.55113(11) 0.3657(4) 0.58668(12) 0.0151(6) Uani 1 1 d . . . . .
C7 C 0.55118(12) 0.4541(4) 0.63704(12) 0.0184(6) Uani 1 1 d . . . . .
H7 H 0.571706 0.575360 0.657450 0.022 Uiso 1 1 calc R U . . .
C8 C 0.51649(11) 0.3325(5) 0.65019(13) 0.0188(6) Uani 1 1 d . . . . .
H8 H 0.508702 0.352868 0.681770 0.023 Uiso 1 1 calc R U . . .
C9 C 0.49366(11) 0.1681(4) 0.60814(12) 0.0156(6) Uani 1 1 d . . . . .
C10 C 0.45633(11) 0.0069(5) 0.60596(11) 0.0159(5) Uani 1 1 d . . . . .
C11 C 0.62612(11) 0.6044(4) 0.59030(12) 0.0158(5) Uani 1 1 d . . . . .
C12 C 0.62532(12) 0.8089(5) 0.56782(13) 0.0216(6) Uani 1 1 d . . . . .
H12 H 0.595182 0.850011 0.533808 0.026 Uiso 1 1 calc R U . . .
C13 C 0.66813(13) 0.9537(4) 0.59459(14) 0.0239(7) Uani 1 1 d . . . . .
H13 H 0.667321 1.093418 0.579275 0.029 Uiso 1 1 calc R U . . .
C14 C 0.71170(11) 0.8911(5) 0.64366(13) 0.0204(6) Uani 1 1 d . . . . .
C15 C 0.71363(12) 0.6908(5) 0.66731(13) 0.0214(6) Uani 1 1 d . . . . .
H15 H 0.743926 0.650652 0.701312 0.026 Uiso 1 1 calc R U . . .
C16 C 0.67042(12) 0.5488(4) 0.64043(12) 0.0178(6) Uani 1 1 d . . . . .
H16 H 0.671088 0.410892 0.656590 0.021 Uiso 1 1 calc R U . . .
C17 C 0.43555(11) 0.0093(5) 0.65024(12) 0.0164(5) Uani 1 1 d . . . . .
C18 C 0.40720(12) 0.1869(5) 0.65713(13) 0.0224(6) Uani 1 1 d . . . . .
H18 H 0.402237 0.311279 0.634277 0.027 Uiso 1 1 calc R U . . .
C19 C 0.38614(12) 0.1852(5) 0.69670(14) 0.0229(6) Uani 1 1 d . . . . .
H19 H 0.367239 0.307792 0.701262 0.027 Uiso 1 1 calc R U . . .
C20 C 0.39299(11) 0.0032(5) 0.72941(12) 0.0181(6) Uani 1 1 d . . . . .
C21 C 0.42085(13) -0.1757(5) 0.72370(13) 0.0217(6) Uani 1 1 d . . . . .
H21 H 0.425483 -0.299991 0.746515 0.026 Uiso 1 1 calc R U . . .
C22 C 0.44198(12) -0.1708(5) 0.68405(12) 0.0204(6) Uani 1 1 d . . . . .
H22 H 0.461235 -0.293124 0.679980 0.024 Uiso 1 1 calc R U . . .
N1 N 0.54834(9) 0.1953(4) 0.47731(10) 0.0154(5) Uani 1 1 d . . . . .
N2 N 0.51543(9) 0.1940(4) 0.56997(10) 0.0159(5) Uani 1 1 d . . . . .
H2A H 0.507765 0.113984 0.539890 0.019 Uiso 1 1 calc R U . . .
Br1 Br 0.77021(2) 1.08935(5) 0.68142(2) 0.03399(10) Uani 1 1 d . . . . .
Br2 Br 0.36289(2) -0.00739(5) 0.78254(2) 0.02331(8) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
C1 N1 1.372(3) . ?
C1 C10 1.407(4) 5_656 ?
C1 C2 1.445(4) . ?
C2 C3 1.351(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.444(4) . ?
C3 H3 0.9500 . ?
C4 N1 1.372(4) . ?
C4 C5 1.404(4) . ?
C5 C6 1.399(4) . ?
C5 C11 1.497(4) . ?
C6 N2 1.374(3) . ?
C6 C7 1.434(4) . ?
C7 C8 1.358(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.433(4) . ?
C8 H8 0.9500 . ?
C9 N2 1.375(4) . ?
C9 C10 1.401(4) . ?
C10 C17 1.496(4) . ?
C11 C16 1.391(4) . ?
C11 C12 1.393(4) . ?
C12 C13 1.391(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.377(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(4) . ?
C14 Br1 1.907(3) . ?
C15 C16 1.387(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.389(4) . ?
C17 C18 1.395(4) . ?
C18 C19 1.386(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(4) . ?
C20 Br2 1.898(3) . ?
C21 C22 1.389(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
N2 H2A 0.8800 . ?

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
N1 C1 C10 126.4(2) . 5_656 ?
N1 C1 C2 109.6(2) . . ?
C10 C1 C2 123.9(3) 5_656 . ?
C3 C2 C1 107.1(3) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C2 C3 C4 107.1(3) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
N1 C4 C5 126.4(2) . . ?
N1 C4 C3 109.7(2) . . ?
C5 C4 C3 123.7(3) . . ?
C6 C5 C4 125.8(3) . . ?
C6 C5 C11 117.4(2) . . ?
C4 C5 C11 116.5(2) . . ?
N2 C6 C5 126.1(3) . . ?
N2 C6 C7 108.2(2) . . ?
C5 C6 C7 125.7(3) . . ?
C8 C7 C6 107.4(2) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 108.1(3) . . ?
C7 C8 H8 126.0 . . ?
C9 C8 H8 126.0 . . ?
N2 C9 C10 125.4(3) . . ?
N2 C9 C8 107.8(2) . . ?
C10 C9 C8 126.8(3) . . ?
C9 C10 C1 125.4(2) . 5_656 ?
C9 C10 C17 117.8(2) . . ?
C1 C10 C17 116.8(2) 5_656 . ?
C16 C11 C12 118.5(3) . . ?
C16 C11 C5 119.8(2) . . ?
C12 C11 C5 121.5(3) . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 118.9(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 121.9(3) . . ?
C13 C14 Br1 119.4(2) . . ?
C15 C14 Br1 118.7(2) . . ?
C14 C15 C16 118.6(3) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C15 C16 C11 121.3(3) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
C22 C17 C18 118.2(3) . . ?
C22 C17 C10 120.4(2) . . ?
C18 C17 C10 121.3(3) . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C20 C19 C18 119.1(3) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 121.2(3) . . ?
C19 C20 Br2 120.2(2) . . ?
C21 C20 Br2 118.6(2) . . ?
C20 C21 C22 118.9(3) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C17 C22 C21 121.4(3) . . ?
C17 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C1 N1 C4 106.6(2) . . ?
C6 N2 C9 108.6(2) . . ?
C6 N2 H2A 125.7 . . ?
C9 N2 H2A 125.7 . . ?

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
N1 C1 C2 C3 -0.1(3) . . . . ?
C10 C1 C2 C3 -176.1(3) 5_656 . . . ?
C1 C2 C3 C4 0.5(3) . . . . ?
C2 C3 C4 N1 -0.7(3) . . . . ?
C2 C3 C4 C5 174.8(3) . . . . ?
N1 C4 C5 C6 0.7(5) . . . . ?
C3 C4 C5 C6 -174.0(3) . . . . ?
N1 C4 C5 C11 173.8(3) . . . . ?
C3 C4 C5 C11 -0.9(4) . . . . ?
C4 C5 C6 N2 3.5(5) . . . . ?
C11 C5 C6 N2 -169.5(3) . . . . ?
C4 C5 C6 C7 -177.4(3) . . . . ?
C11 C5 C6 C7 9.5(4) . . . . ?
N2 C6 C7 C8 1.0(3) . . . . ?
C5 C6 C7 C8 -178.1(3) . . . . ?
C6 C7 C8 C9 -0.7(3) . . . . ?
C7 C8 C9 N2 0.1(3) . . . . ?
C7 C8 C9 C10 179.4(3) . . . . ?
N2 C9 C10 C1 1.6(5) . . . 5_656 ?
C8 C9 C10 C1 -177.6(3) . . . 5_656 ?
N2 C9 C10 C17 -177.8(2) . . . . ?
C8 C9 C10 C17 3.0(4) . . . . ?
C6 C5 C11 C16 64.8(3) . . . . ?
C4 C5 C11 C16 -108.9(3) . . . . ?
C6 C5 C11 C12 -119.5(3) . . . . ?
C4 C5 C11 C12 66.8(3) . . . . ?
C16 C11 C12 C13 0.7(4) . . . . ?
C5 C11 C12 C13 -175.1(3) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C12 C13 C14 C15 -1.0(5) . . . . ?
C12 C13 C14 Br1 -179.1(2) . . . . ?
C13 C14 C15 C16 0.4(4) . . . . ?
Br1 C14 C15 C16 178.5(2) . . . . ?
C14 C15 C16 C11 0.8(4) . . . . ?
C12 C11 C16 C15 -1.3(4) . . . . ?
C5 C11 C16 C15 174.6(3) . . . . ?
C9 C10 C17 C22 -123.3(3) . . . . ?
C1 C10 C17 C22 57.2(4) 5_656 . . . ?
C9 C10 C17 C18 59.7(4) . . . . ?
C1 C10 C17 C18 -119.8(3) 5_656 . . . ?
C22 C17 C18 C19 0.3(5) . . . . ?
C10 C17 C18 C19 177.4(3) . . . . ?
C17 C18 C19 C20 -0.7(5) . . . . ?
C18 C19 C20 C21 0.6(5) . . . . ?
C18 C19 C20 Br2 -178.3(2) . . . . ?
C19 C20 C21 C22 -0.3(5) . . . . ?
Br2 C20 C21 C22 178.6(2) . . . . ?
C18 C17 C22 C21 0.1(5) . . . . ?
C10 C17 C22 C21 -177.1(3) . . . . ?
C20 C21 C22 C17 -0.1(5) . . . . ?
C10 C1 N1 C4 175.5(3) 5_656 . . . ?
C2 C1 N1 C4 -0.3(3) . . . . ?
C5 C4 N1 C1 -174.8(3) . . . . ?
C3 C4 N1 C1 0.6(3) . . . . ?
C5 C6 N2 C9 178.2(3) . . . . ?
C7 C6 N2 C9 -1.0(3) . . . . ?
C10 C9 N2 C6 -178.8(3) . . . . ?
C8 C9 N2 C6 0.6(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
_geom_hbond_publ_flag
C19 H19 Br1 0.95 3.00 3.890(3) 156.7 3_445 yes
N2 H2A N1 0.88 2.39 2.935(3) 120.1 . yes
N2 H2A N1 0.88 2.36 2.910(3) 120.8 5_656 yes

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: sqz.res
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .FAB SHELXL file: sqz.fab
#...............................................................................



# ............... End of .FAB file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR FGP808                                                 #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/ccdc.csd.cc236zw6
_database_code_depnum_ccdc_archive 'CCDC 1943138'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.inorgchem.9b02697 2019
loop_
_audit_author_name
_audit_author_address
maweimin
;The CCDC
China
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_audit_creation_date             2019-08-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H21 N3 O9 Pb2'
_chemical_formula_sum            'C44 H40 N4 O4 Pb4'
_chemical_formula_weight         1517.56
_chemical_melting_point          ?
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'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3027(2)
_cell_length_b                   13.2085(3)
_cell_length_c                   13.4634(3)
_cell_angle_alpha                94.2432(18)
_cell_angle_beta                 94.4958(16)
_cell_angle_gamma                98.3760(18)
_cell_volume                     1800.24(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20923
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      30.2330
_cell_measurement_theta_min      1.9930
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47713
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.426
_diffrn_reflns_theta_min         2.006
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00  49.00   0.50   15.00    --   -9.20  73.00 -52.00  170
  2  ω     -1.00  79.00   0.50   15.00    --   10.30  73.00 -52.00  160
  3  ω    -13.00  14.00   0.50   15.00    --   -9.20 -57.00  60.00   54
  4  ω    -26.00  12.00   0.50   15.00    --   -9.20 -99.00  60.00   76
  5  ω    -36.00   8.00   0.50   15.00    --   -9.20 -57.00 -30.00   88
  6  ω    -22.00  18.00   0.50   15.00    --   -9.20 -99.00-120.00   80
  7  ω     20.00  67.00   0.50   15.00    --   10.30-130.00-134.52   94
  8  ω     26.00  72.00   0.50   15.00    --   10.30-140.00 -46.54   92
  9  ω    -22.00  23.00   0.50   15.00    --   -9.20 -99.00-180.00   90
 10  ω    -63.00  38.00   0.50   15.00    --   10.30 -77.00-120.00  202
 11  ω    -83.00 -35.00   0.50   15.00    --   -9.20 -57.00  60.00   96
 12  ω    -83.00 -57.00   0.50   15.00    --   -9.20 -57.00 -30.00   52
 13  ω    -22.00  50.00   0.50   15.00    --   10.30 -99.00 150.00  144
 14  ω     13.00  38.00   0.50   15.00    --   10.30 -73.00 178.00   50
 15  ω    -52.00 -24.00   0.50   15.00    --   10.30 -73.00 178.00   56
 16  ω    -83.00 -25.00   0.50   15.00    --   -9.20 -73.00 178.00  116
 17  ω    -37.00  65.00   0.50   15.00    --   -9.20  77.00   0.00  204
 18  ω    -53.00 -28.00   0.50   15.00    --   -9.20 106.00 -97.34   50
 19  ω    -57.00 -32.00   0.50   15.00    --   -9.20 113.00  -6.21   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073283000
_diffrn_orient_matrix_UB_12      0.0500234000
_diffrn_orient_matrix_UB_13      0.0194892000
_diffrn_orient_matrix_UB_21      -0.0356103000
_diffrn_orient_matrix_UB_22      -0.0213644000
_diffrn_orient_matrix_UB_23      0.0384279000
_diffrn_orient_matrix_UB_31      0.0596709000
_diffrn_orient_matrix_UB_32      0.0031139000
_diffrn_orient_matrix_UB_33      0.0309400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7615
_reflns_number_total             9401
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         3.737
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0543P)²+1.7612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0965
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C20(H20),
 C18(H18), C16(H16), C26(H26), C25(H25), C24(H24), C23(H23), C27(H27)
3.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 -0.51305(2) 0.94237(2) -0.33631(2) 0.02325(3) Uani 1 1 d . . . . .
O2 O -0.2583(2) 0.9354(2) -0.34157(18) 0.0279(6) Uani 1 1 d . . . . .
O1 O -0.3536(2) 0.9118(2) -0.20105(18) 0.0305(6) Uani 1 1 d . . . . .
O3 O 0.2115(2) 0.8928(2) -0.35693(18) 0.0307(7) Uani 1 1 d . . . . .
O4 O 0.3309(2) 0.8976(3) -0.2119(2) 0.0452(9) Uani 1 1 d . . . . .
O5 O -0.9695(2) 0.2399(2) -0.4732(2) 0.0310(7) Uani 1 1 d . . . . .
O6 O -0.8923(2) 0.09389(19) -0.45588(19) 0.0251(6) Uani 1 1 d . . . . .
O7 O -0.4116(2) 0.0999(2) -0.45713(19) 0.0265(6) Uani 1 1 d . . . . .
O8 O -0.2732(2) 0.2423(2) -0.40596(19) 0.0270(6) Uani 1 1 d . . . . .
O9 O -0.4858(3) 1.1157(3) -0.2246(2) 0.0523(9) Uani 1 1 d . . . . .
N1 N 0.0552(3) 0.8486(3) 0.2666(2) 0.0278(7) Uani 1 1 d . . . . .
N2 N -0.5370(2) 0.7469(2) -0.3495(2) 0.0194(6) Uani 1 1 d . . . . .
N3 N -0.4929(6) 1.1972(5) -0.0735(4) 0.098(2) Uani 1 1 d . . . . .
C1 C -0.2555(3) 0.9167(3) -0.2513(3) 0.0236(8) Uani 1 1 d . . . . .
C2 C -0.1284(3) 0.8947(3) -0.2021(3) 0.0237(8) Uani 1 1 d . . . . .
C3 C -0.0190(3) 0.8927(3) -0.2565(3) 0.0248(8) Uani 1 1 d . . . . .
H3 H -0.0268 0.8980 -0.3252 0.030 Uiso 1 1 calc R . . . .
C4 C 0.0999(3) 0.8828(3) -0.2085(3) 0.0266(9) Uani 1 1 d . . . . .
C5 C 0.1108(3) 0.8689(3) -0.1069(3) 0.0253(8) Uani 1 1 d . . . . .
H5 H 0.1921 0.8617 -0.0755 0.030 Uiso 1 1 calc R . . . .
C6 C 0.0032(3) 0.8657(3) -0.0522(3) 0.0254(9) Uani 1 1 d . . . . .
C7 C -0.1168(3) 0.8809(3) -0.1002(3) 0.0238(8) Uani 1 1 d . . . . .
H7 H -0.1897 0.8819 -0.0637 0.029 Uiso 1 1 calc R . . . .
C8 C 0.2221(3) 0.8905(3) -0.2638(3) 0.0273(9) Uani 1 1 d . . . . .
C9 C 0.0175(3) 0.8541(3) 0.0577(3) 0.0249(8) Uani 1 1 d . . . . .
C10 C 0.1338(4) 0.8346(4) 0.1037(3) 0.0428(11) Uani 1 1 d . . . . .
H10 H 0.2028 0.8229 0.0659 0.051 Uiso 1 1 calc R . . . .
C11 C 0.1483(4) 0.8324(4) 0.2078(3) 0.0412(11) Uani 1 1 d . . . . .
H11 H 0.2280 0.8187 0.2371 0.049 Uiso 1 1 calc R . . . .
C12 C -0.0591(4) 0.8632(3) 0.2206(3) 0.0326(10) Uani 1 1 d . . . . .
H12 H -0.1277 0.8721 0.2597 0.039 Uiso 1 1 calc R . . . .
C13 C -0.0820(4) 0.8657(3) 0.1188(3) 0.0313(10) Uani 1 1 d . . . . .
H13 H -0.1645 0.8753 0.0912 0.038 Uiso 1 1 calc R . . . .
C14 C -0.8758(3) 0.1906(3) -0.4578(3) 0.0232(8) Uani 1 1 d . . . . .
C15 C -0.7384(3) 0.2488(3) -0.4366(3) 0.0247(8) Uani 1 1 d . . . . .
C20 C -0.7186(3) 0.3543(3) -0.4166(3) 0.0269(9) Uani 1 1 d . . . . .
H20 H -0.7912 0.3887 -0.4176 0.032 Uiso 1 1 calc R . . . .
C19 C -0.5923(3) 0.4107(3) -0.3948(3) 0.0266(9) Uani 1 1 d . . . . .
C18 C -0.4860(3) 0.3559(3) -0.3967(3) 0.0266(9) Uani 1 1 d . . . . .
H18 H -0.4006 0.3911 -0.3833 0.032 Uiso 1 1 calc R . . . .
C17 C -0.5050(3) 0.2507(3) -0.4179(3) 0.0218(8) Uani 1 1 d . . . . .
C16 C -0.6310(3) 0.1961(3) -0.4381(2) 0.0221(8) Uani 1 1 d . . . . .
H16 H -0.6436 0.1253 -0.4525 0.027 Uiso 1 1 calc R . . . .
C21 C -0.3879(3) 0.1948(3) -0.4262(3) 0.0233(8) Uani 1 1 d . . . . .
C22 C -0.5741(4) 0.5237(3) -0.3756(3) 0.0315(9) Uani 1 1 d . . . . .
C26 C -0.6757(4) 0.5786(3) -0.3857(3) 0.0363(10) Uani 1 1 d . . . . .
H26 H -0.7608 0.5444 -0.4030 0.044 Uiso 1 1 calc R . . . .
C25 C -0.6538(4) 0.6857(3) -0.3704(3) 0.0379(11) Uani 1 1 d . . . . .
H25 H -0.7280 0.7182 -0.3752 0.045 Uiso 1 1 calc R . . . .
C24 C -0.4355(4) 0.6884(3) -0.3409(4) 0.0477(13) Uani 1 1 d . . . . .
H24 H -0.3507 0.7239 -0.3256 0.057 Uiso 1 1 calc R . . . .
C23 C -0.4492(4) 0.5822(4) -0.3530(4) 0.0508(14) Uani 1 1 d . . . . .
H23 H -0.3752 0.5497 -0.3460 0.061 Uiso 1 1 calc R . . . .
C27 C -0.4969(6) 1.1199(7) -0.1393(5) 0.088(2) Uani 1 1 d . . . . .
H27 H -0.5112 1.0562 -0.1136 0.105 Uiso 1 1 calc R . . . .
C28 C -0.4644(17) 1.3066(13) -0.1231(13) 0.270(3) Uani 1 1 d . U . . .
H28A H -0.4374 1.2950 -0.1891 0.404 Uiso 1 1 calc GR . . . .
H28B H -0.3959 1.3517 -0.0824 0.404 Uiso 1 1 calc GR . . . .
H28C H -0.5433 1.3375 -0.1269 0.404 Uiso 1 1 calc GR . . . .
C29 C -0.4930(7) 1.2106(7) 0.0294(4) 0.095(3) Uani 1 1 d . . . . .
H29A H -0.5822 1.2026 0.0470 0.142 Uiso 1 1 calc GR . . . .
H29B H -0.4490 1.2782 0.0530 0.142 Uiso 1 1 calc GR . . . .
H29C H -0.4478 1.1603 0.0594 0.142 Uiso 1 1 calc GR . . . .
Pb2 Pb -1.14601(2) 0.09332(2) -0.45287(2) 0.01875(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 2.645(2) . ?
Pb1 O1 2.452(2) . ?
Pb1 O4 2.456(3) 1_455 ?
Pb1 O9 2.611(3) . ?
Pb1 N2 2.549(3) . ?
O2 C1 1.257(4) . ?
O1 C1 1.256(4) . ?
O3 C8 1.253(4) . ?
O3 Pb2 2.623(2) 2_464 ?
O4 Pb1 2.456(3) 1_655 ?
O4 C8 1.261(4) . ?
O5 C14 1.254(4) . ?
O5 Pb2 2.503(2) . ?
O6 C14 1.266(4) . ?
O6 Pb2 2.617(2) . ?
O7 C21 1.274(4) . ?
O7 Pb2 2.746(2) 1_655 ?
O8 C21 1.255(4) . ?
O8 Pb2 2.586(3) 1_655 ?
O9 C27 1.160(7) . ?
N1 C11 1.322(5) . ?
N1 C12 1.334(5) . ?
N1 Pb2 2.624(3) 2_465 ?
N2 C25 1.345(5) . ?
N2 C24 1.390(5) . ?
N3 C27 1.295(9) . ?
N3 C28 1.635(17) . ?
N3 C29 1.383(8) . ?
C1 C2 1.497(5) . ?
C2 C3 1.394(5) . ?
C2 C7 1.396(5) . ?
C3 C4 1.368(5) . ?
C4 C5 1.391(5) . ?
C4 C8 1.507(5) . ?
C5 C6 1.375(5) . ?
C6 C7 1.397(5) . ?
C6 C9 1.497(5) . ?
C9 C10 1.372(5) . ?
C9 C13 1.382(5) . ?
C10 C11 1.400(6) . ?
C12 C13 1.375(5) . ?
C14 C15 1.505(4) . ?
C15 C20 1.382(5) . ?
C15 C16 1.390(5) . ?
C20 C19 1.401(5) . ?
C19 C18 1.399(5) . ?
C19 C22 1.477(5) . ?
C18 C17 1.380(5) . ?
C17 C16 1.387(4) . ?
C17 C21 1.510(5) . ?
C22 C26 1.362(5) . ?
C22 C23 1.400(5) . ?
C26 C25 1.396(6) . ?
C24 C23 1.385(6) . ?
Pb2 O3 2.623(2) 2_464 ?
Pb2 O7 2.746(2) 1_455 ?
Pb2 O8 2.586(3) 1_455 ?
Pb2 N1 2.624(3) 2_465 ?

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 O2 51.47(8) . . ?
O1 Pb1 O4 81.99(8) . 1_455 ?
O1 Pb1 O9 78.78(10) . . ?
O1 Pb1 N2 77.83(9) . . ?
O4 Pb1 O2 132.91(8) 1_455 . ?
O4 Pb1 O9 79.14(11) 1_455 . ?
O4 Pb1 N2 77.79(10) 1_455 . ?
O9 Pb1 O2 96.13(10) . . ?
N2 Pb1 O2 84.85(8) . . ?
N2 Pb1 O9 149.06(10) . . ?
C1 O2 Pb1 87.67(19) . . ?
C1 O1 Pb1 96.7(2) . . ?
C8 O3 Pb2 169.4(2) . 2_464 ?
C8 O4 Pb1 101.3(2) . 1_655 ?
C14 O5 Pb2 95.2(2) . . ?
C14 O6 Pb2 89.60(19) . . ?
C21 O7 Pb2 90.12(18) . 1_655 ?
C21 O8 Pb2 98.2(2) . 1_655 ?
C27 O9 Pb1 122.9(5) . . ?
C11 N1 C12 115.8(3) . . ?
C11 N1 Pb2 113.4(2) . 2_465 ?
C12 N1 Pb2 127.4(2) . 2_465 ?
C25 N2 Pb1 123.0(2) . . ?
C25 N2 C24 110.4(3) . . ?
C24 N2 Pb1 126.5(2) . . ?
C27 N3 C28 111.6(8) . . ?
C27 N3 C29 135.9(8) . . ?
C29 N3 C28 112.0(8) . . ?
O2 C1 C2 117.7(3) . . ?
O1 C1 O2 124.1(3) . . ?
O1 C1 C2 118.1(3) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C7 119.4(3) . . ?
C7 C2 C1 120.2(3) . . ?
C4 C3 C2 119.7(3) . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 C8 120.6(3) . . ?
C5 C4 C8 118.9(3) . . ?
C6 C5 C4 121.1(3) . . ?
C5 C6 C7 118.4(3) . . ?
C5 C6 C9 120.5(3) . . ?
C7 C6 C9 121.0(3) . . ?
C2 C7 C6 120.7(3) . . ?
O3 C8 O4 123.7(3) . . ?
O3 C8 C4 119.3(3) . . ?
O4 C8 C4 117.0(3) . . ?
C10 C9 C6 120.8(3) . . ?
C10 C9 C13 116.4(3) . . ?
C13 C9 C6 122.8(3) . . ?
C9 C10 C11 119.8(4) . . ?
N1 C11 C10 123.7(4) . . ?
N1 C12 C13 124.1(4) . . ?
C12 C13 C9 120.0(3) . . ?
O5 C14 O6 122.8(3) . . ?
O5 C14 C15 118.8(3) . . ?
O6 C14 C15 118.4(3) . . ?
C20 C15 C14 120.2(3) . . ?
C20 C15 C16 120.0(3) . . ?
C16 C15 C14 119.8(3) . . ?
C15 C20 C19 121.8(3) . . ?
C20 C19 C22 120.6(3) . . ?
C18 C19 C20 117.0(3) . . ?
C18 C19 C22 122.3(3) . . ?
C17 C18 C19 121.4(3) . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 C21 120.0(3) . . ?
C16 C17 C21 119.3(3) . . ?
C17 C16 C15 119.2(3) . . ?
O7 C21 C17 117.1(3) . . ?
O8 C21 O7 122.6(3) . . ?
O8 C21 C17 120.2(3) . . ?
C26 C22 C19 122.6(3) . . ?
C26 C22 C23 115.3(4) . . ?
C23 C22 C19 122.0(4) . . ?
C22 C26 C25 120.9(4) . . ?
N2 C25 C26 127.1(4) . . ?
C23 C24 N2 126.0(4) . . ?
C24 C23 C22 120.2(4) . . ?
O9 C27 N3 131.7(8) . . ?
O3 Pb2 O7 77.52(8) 2_464 1_455 ?
O3 Pb2 N1 159.05(10) 2_464 2_465 ?
O5 Pb2 O3 83.97(8) . 2_464 ?
O5 Pb2 O6 51.15(8) . . ?
O5 Pb2 O7 126.46(8) . 1_455 ?
O5 Pb2 O8 81.68(8) . 1_455 ?
O5 Pb2 N1 78.12(9) . 2_465 ?
O6 Pb2 O3 100.10(8) . 2_464 ?
O6 Pb2 O7 177.03(8) . 1_455 ?
O6 Pb2 N1 76.99(9) . 2_465 ?
O8 Pb2 O3 90.08(8) 1_455 2_464 ?
O8 Pb2 O6 129.60(7) 1_455 . ?
O8 Pb2 O7 49.06(7) 1_455 1_455 ?
O8 Pb2 N1 76.75(9) 1_455 2_465 ?
N1 Pb2 O7 104.58(9) 2_465 1_455 ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.711
_oxdiff_exptl_absorpt_empirical_full_min 0.557
####################################################################### 
# 
# 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_3
_audit_block_doi                 10.5517/ccdc.csd.cc23701f
_database_code_depnum_ccdc_archive 'CCDC 1943143'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.inorgchem.9b02697 2019
loop_
_audit_author_name
_audit_author_address
maweimin
;The CCDC
China
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_audit_creation_date             2019-08-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C29 H21 N3 O9 Pb2, 0.5(C6 H15 N)'
_chemical_formula_sum            'C32 H28.50 N3.50 O9 Pb2'
_chemical_formula_weight         1020.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb C O N H'
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'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2850(3)
_cell_length_b                   13.3070(3)
_cell_length_c                   13.3260(3)
_cell_angle_alpha                102.181(2)
_cell_angle_beta                 97.698(2)
_cell_angle_gamma                94.222(2)
_cell_volume                     1756.90(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5140
_cell_measurement_theta_min      1.9870
_shelx_estimated_absorpt_T_max   0.249
_shelx_estimated_absorpt_T_min   0.160
_exptl_absorpt_coefficient_mu    9.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.967
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  19.00   0.50   12.00    --   -6.40  77.00 -30.00   82
  2  ω     29.00  55.00   0.50   12.00    --   -6.40  77.00 -30.00   52
  3  ω     37.00  67.00   0.50   12.00    --   -6.40  77.00-120.00   60
  4  ω     26.00  58.00   0.50   12.00    --    7.80  77.00-150.00   64
  5  ω      3.00  61.00   0.50   12.00    --    7.80  77.00 -60.00  116
  6  ω    -18.00  12.00   0.50   12.00    --    7.80  77.00-150.00   60
  7  ω    -31.00  22.00   0.50   12.00    --   -6.40  77.00-120.00  106
  8  ω    -21.00  73.00   0.50   12.00    --    7.80  77.00  60.00  188
  9  ω      4.00  74.00   0.50   12.00    --    7.80  77.00 150.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195265000
_diffrn_orient_matrix_UB_12      -0.0495548000
_diffrn_orient_matrix_UB_13      -0.0193035000
_diffrn_orient_matrix_UB_21      0.0150404000
_diffrn_orient_matrix_UB_22      -0.0067474000
_diffrn_orient_matrix_UB_23      0.0515280000
_diffrn_orient_matrix_UB_31      -0.0654953000
_diffrn_orient_matrix_UB_32      -0.0224854000
_diffrn_orient_matrix_UB_33      -0.0029502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5999
_reflns_number_total             6999
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         3.988
_refine_diff_density_min         -2.172
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²+10.7494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0987
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C30 = N4-C32 = N4-C34
 1.463 with sigma of 0.001
 N4-C31 = N4-C33 = N4-C35
 2.532 with sigma of 0.002
 C30-C32 = C32-C34 = C34-C30
 2.416 with sigma of 0.002
 C30-C31 = C32-C33 = C34-C35
 1.439 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) = Uanis(N4) = Uanis(C30) = Uanis(C32) = Uanis(C34) = Uanis(C31) =
Uanis(C33)
4. Others
 Fixed Sof: N4(0.5) C30(0.5) H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C16(H16), C12(H12), C20(H20), C13(H13), C5(H5), C11(H11),
 C18(H18), C25(H25), C23(H23), C24(H24), C26(H26), C10(H10), C27(H27)
5.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C31(H31A,H31B,
 H31C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 1.00873(2) 1.33726(2) 0.04530(2) 0.01219(2) Uani 1 1 d . . . . .
O6 O 1.38878(12) 1.44849(10) 0.90144(10) 0.0130(4) Uani 1 1 d . . . . .
O7 O 0.90867(12) 1.44737(10) 0.89718(10) 0.0130(4) Uani 1 1 d . . . . .
O2 O 0.75526(13) 1.34154(10) 0.05217(11) 0.0173(4) Uani 1 1 d . . . . .
O3 O 0.28189(13) 1.36170(10) 0.09384(11) 0.0179(4) Uani 1 1 d . . . . .
O8 O 0.76962(13) 1.38931(12) 0.75078(11) 0.0188(4) Uani 1 1 d . . . . .
O4 O 0.16492(14) 1.21216(11) 0.08158(13) 0.0247(4) Uani 1 1 d . . . . .
O1 O 0.84999(13) 1.19961(11) 0.06871(12) 0.0178(4) Uani 1 1 d . . . . .
O5 O 1.46920(13) 1.46084(12) 0.75806(11) 0.0197(4) Uani 1 1 d . . . . .
N2 N 1.03111(16) 1.35789(14) 0.24749(13) 0.0169(5) Uani 1 1 d . . . . .
C1 C 0.75176(18) 1.25238(15) 0.06991(15) 0.0146(5) Uani 1 1 d . . . . .
N1 N 0.45188(17) 0.74867(14) 0.16666(14) 0.0202(5) Uani 1 1 d . . . . .
O9 O 0.98416(18) 1.20651(13) -0.13315(14) 0.0357(5) Uani 1 1 d . . . . .
C3 C 0.51743(18) 1.26223(15) 0.09585(16) 0.0143(5) Uani 1 1 d . . . . .
H3 H 0.5246 1.3298 0.0870 0.017 Uiso 1 1 calc R . . . .
C8 C 0.27279(19) 1.26728(15) 0.09447(16) 0.0157(5) Uani 1 1 d . . . . .
C21 C 0.88599(19) 1.41251(14) 0.80063(15) 0.0131(5) Uani 1 1 d . . . . .
C15 C 1.23502(18) 1.42548(15) 0.74608(15) 0.0127(5) Uani 1 1 d . . . . .
C2 C 0.62727(18) 1.20762(15) 0.09633(15) 0.0138(5) Uani 1 1 d . . . . .
C14 C 1.37251(18) 1.44674(15) 0.80479(15) 0.0137(5) Uani 1 1 d . . . . .
C4 C 0.39588(19) 1.21605(15) 0.10861(16) 0.0149(5) Uani 1 1 d . . . . .
C7 C 0.61807(19) 1.10933(15) 0.11719(16) 0.0159(5) Uani 1 1 d . . . . .
H7 H 0.6924 1.0736 0.1189 0.019 Uiso 1 1 calc R . . . .
C17 C 1.00050(18) 1.40447(15) 0.74303(16) 0.0144(5) Uani 1 1 d . . . . .
C16 C 1.12876(19) 1.42413(15) 0.79800(16) 0.0154(5) Uani 1 1 d . . . . .
H16 H 1.1420 1.4363 0.8701 0.018 Uiso 1 1 calc R . . . .
C12 C 0.5668(2) 0.79096(16) 0.14895(17) 0.0200(6) Uani 1 1 d . . . . .
H12 H 0.6351 0.7494 0.1406 0.024 Uiso 1 1 calc R . . . .
C20 C 1.21650(19) 1.40804(16) 0.63804(16) 0.0179(6) Uani 1 1 d . . . . .
H20 H 1.2891 1.4097 0.6035 0.021 Uiso 1 1 calc R . . . .
C13 C 0.5888(2) 0.89187(15) 0.14247(16) 0.0173(5) Uani 1 1 d . . . . .
H13 H 0.6708 0.9172 0.1308 0.021 Uiso 1 1 calc R . . . .
C6 C 0.50005(19) 1.06315(15) 0.13562(16) 0.0143(5) Uani 1 1 d . . . . .
C5 C 0.38861(19) 1.11709(15) 0.12739(15) 0.0149(5) Uani 1 1 d . . . . .
H5 H 0.3076 1.0858 0.1347 0.018 Uiso 1 1 calc R . . . .
C19 C 1.08829(19) 1.38797(17) 0.58104(16) 0.0191(6) Uani 1 1 d . . . . .
C11 C 0.3577(2) 0.81128(17) 0.18413(19) 0.0247(6) Uani 1 1 d . . . . .
H11 H 0.2793 0.7846 0.2008 0.030 Uiso 1 1 calc R . . . .
C18 C 0.98143(19) 1.38476(16) 0.63489(16) 0.0156(5) Uani 1 1 d . . . . .
H18 H 0.8963 1.3693 0.5982 0.019 Uiso 1 1 calc R . . . .
C9 C 0.48834(19) 0.95749(15) 0.15335(16) 0.0160(5) Uani 1 1 d . . . . .
C25 C 1.1524(2) 1.37909(19) 0.30662(17) 0.0260(6) Uani 1 1 d . . . . .
H25 H 1.2252 1.3886 0.2738 0.031 Uiso 1 1 calc R . . . .
C23 C 0.9442(2) 1.35271(19) 0.40549(17) 0.0259(7) Uani 1 1 d . . . . .
H23 H 0.8699 1.3427 0.4365 0.031 Uiso 1 1 calc R . . . .
C24 C 0.9315(2) 1.34583(19) 0.30018(17) 0.0260(7) Uani 1 1 d . . . . .
H24 H 0.8467 1.3316 0.2626 0.031 Uiso 1 1 calc R . . . .
C22 C 1.0691(2) 1.37474(17) 0.46567(16) 0.0176(6) Uani 1 1 d . . . . .
C26 C 1.1736(2) 1.38735(19) 0.41307(16) 0.0231(6) Uani 1 1 d . . . . .
H26 H 1.2591 1.4015 0.4493 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3716(2) 0.91318(16) 0.17861(18) 0.0228(6) Uani 1 1 d . . . . .
H10 H 0.3031 0.9536 0.1917 0.027 Uiso 1 1 calc R . . . .
N3 N 0.9909(3) 1.0442(2) -0.2226(2) 0.0575(9) Uani 1 1 d . . . . .
C27 C 0.9931(3) 1.1154(2) -0.1362(2) 0.0451(9) Uani 1 1 d . . . . .
H27 H 1.0020 1.0943 -0.0737 0.054 Uiso 1 1 calc R . . . .
C29 C 0.9928(4) 0.9337(2) -0.2252(3) 0.0673(13) Uani 1 1 d . . . . .
H29A H 1.0096 0.9238 -0.1555 0.101 Uiso 1 1 calc GR . . . .
H29B H 1.0611 0.9074 -0.2627 0.101 Uiso 1 1 calc GR . . . .
H29C H 0.9090 0.8975 -0.2591 0.101 Uiso 1 1 calc GR . . . .
C28 C 0.9883(6) 1.0784(5) -0.3213(5) 0.1411(5) Uani 1 1 d . U . . .
H28A H 0.9016 1.0607 -0.3612 0.212 Uiso 1 1 calc GR . . . .
H28B H 1.0513 1.0448 -0.3600 0.212 Uiso 1 1 calc GR . . . .
H28C H 1.0101 1.1519 -0.3068 0.212 Uiso 1 1 calc GR . . . .
Pb2 Pb 1.64432(2) 1.44598(2) 0.90239(2) 0.01035(2) Uani 1 1 d . . . . .
N4 N 1.52765(3) 1.81688(3) 0.49726(2) 0.0873(12) Uani 0.5 1 d D . P . .
C30 C 1.43407(3) 1.72445(3) 0.45657(3) 0.0873(12) Uani 0.5 1 d D . P . .
H30A H 1.3738 1.7388 0.4000 0.105 Uiso 0.5 1 calc R . P . .
H30B H 1.4838 1.6699 0.4260 0.105 Uiso 0.5 1 calc R . P . .
C32 C 1.59105(4) 1.82039(4) 0.60312(2) 0.0873(12) Uani 0.5 1 d D . P . .
H32A H 1.5231 1.8296 0.6472 0.105 Uiso 0.5 1 calc R . P . .
H32B H 1.6196 1.7526 0.6037 0.105 Uiso 0.5 1 calc R . P . .
C33 C 1.70142(4) 1.89516(4) 0.65284(6) 0.0873(12) Uani 0.5 1 d D . P . .
H33A H 1.7791 1.8754 0.6244 0.131 Uiso 0.5 1 calc GR . P . .
H33B H 1.7152 1.8980 0.7261 0.131 Uiso 0.5 1 calc GR . P . .
H33C H 1.6836 1.9619 0.6412 0.131 Uiso 0.5 1 calc GR . P . .
C31 C 1.35476(4) 1.68230(4) 0.52200(3) 0.0873(12) Uani 0.5 1 d D . P . .
H31A H 1.2763 1.6437 0.4803 0.131 Uiso 0.5 1 calc GR . P . .
H31B H 1.3309 1.7376 0.5729 0.131 Uiso 0.5 1 calc GR . P . .
H31C H 1.4041 1.6375 0.5564 0.131 Uiso 0.5 1 calc GR . P . .
C34 C 1.62521(3) 1.82557(2) 0.42830(2) 0.0873(12) Uani 0.5 1 d D . P . .
H34A H 1.7039 1.7989 0.4567 0.105 Uiso 0.5 1 calc R . P . .
H34B H 1.5913 1.7789 0.3621 0.105 Uiso 0.5 1 calc R . P . .
C35 C 1.66676(8) 1.92334(2) 0.40648(4) 0.0873(12) Uani 0.5 1 d D . P . .
H35A H 1.6418 1.9207 0.3339 0.131 Uiso 0.5 1 calc GR . P . .
H35B H 1.7609 1.9375 0.4244 0.131 Uiso 0.5 1 calc GR . P . .
H35C H 1.6254 1.9770 0.4466 0.131 Uiso 0.5 1 calc GR . 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 O2 2.6251(14) . ?
Pb1 O4 2.4719(15) 1_655 ?
Pb1 O1 2.4607(14) . ?
Pb1 N2 2.6269(18) . ?
Pb1 O9 2.6027(16) . ?
O6 C14 1.271(2) . ?
O6 Pb2 2.6293(13) . ?
O7 C21 1.256(2) . ?
O7 Pb2 2.7278(13) 1_455 ?
O2 C1 1.257(3) . ?
O3 C8 1.255(3) . ?
O3 Pb2 2.6033(14) 2_786 ?
O8 C21 1.271(2) . ?
O8 Pb2 2.5513(14) 1_455 ?
O4 Pb1 2.4719(15) 1_455 ?
O4 C8 1.255(2) . ?
O1 C1 1.272(2) . ?
O5 C14 1.265(3) . ?
O5 Pb2 2.5035(14) . ?
N2 C25 1.359(3) . ?
N2 C24 1.336(3) . ?
C1 C2 1.488(3) . ?
N1 C12 1.342(3) . ?
N1 C11 1.335(3) . ?
N1 Pb2 2.6283(17) 2_776 ?
O9 C27 1.215(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.387(3) . ?
C3 C4 1.399(3) . ?
C8 C4 1.490(3) . ?
C21 C17 1.488(3) . ?
C15 C14 1.498(3) . ?
C15 C16 1.371(3) . ?
C15 C20 1.394(3) . ?
C2 C7 1.393(3) . ?
C4 C5 1.390(3) . ?
C7 H7 0.9300 . ?
C7 C6 1.395(3) . ?
C17 C16 1.398(3) . ?
C17 C18 1.393(3) . ?
C16 H16 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.368(3) . ?
C20 H20 0.9300 . ?
C20 C19 1.408(3) . ?
C13 H13 0.9300 . ?
C13 C9 1.403(3) . ?
C6 C5 1.401(3) . ?
C6 C9 1.473(3) . ?
C5 H5 0.9300 . ?
C19 C18 1.394(3) . ?
C19 C22 1.494(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.371(3) . ?
C18 H18 0.9300 . ?
C9 C10 1.411(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.386(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.375(3) . ?
C23 C22 1.396(3) . ?
C24 H24 0.9300 . ?
C22 C26 1.379(3) . ?
C26 H26 0.9300 . ?
C10 H10 0.9300 . ?
N3 C27 1.323(4) . ?
N3 C29 1.465(4) . ?
N3 C28 1.478(8) . ?
C27 H27 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Pb2 O7 2.7278(13) 1_655 ?
Pb2 O3 2.6034(14) 2_786 ?
Pb2 O8 2.5513(14) 1_655 ?
Pb2 N1 2.6283(17) 2_776 ?
N4 C30 1.4621(4) . ?
N4 C32 1.4625(4) . ?
N4 C34 1.4627(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.4386(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.4393(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.4391(5) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?

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 N2 84.89(5) . . ?
O4 Pb1 O2 132.56(5) 1_655 . ?
O4 Pb1 N2 76.33(6) 1_655 . ?
O4 Pb1 O9 77.56(5) 1_655 . ?
O1 Pb1 O2 51.78(5) . . ?
O1 Pb1 O4 81.22(5) . 1_655 ?
O1 Pb1 N2 75.40(5) . . ?
O1 Pb1 O9 78.29(5) . . ?
O9 Pb1 O2 96.35(5) . . ?
O9 Pb1 N2 145.24(6) . . ?
C14 O6 Pb2 90.11(11) . . ?
C21 O7 Pb2 90.07(11) . 1_455 ?
C1 O2 Pb1 88.67(11) . . ?
C8 O3 Pb2 167.51(13) . 2_786 ?
C21 O8 Pb2 98.00(12) . 1_455 ?
C8 O4 Pb1 100.60(13) . 1_455 ?
C1 O1 Pb1 95.91(12) . . ?
C14 O5 Pb2 96.12(12) . . ?
C25 N2 Pb1 119.85(14) . . ?
C24 N2 Pb1 125.42(13) . . ?
C24 N2 C25 114.68(19) . . ?
O2 C1 O1 123.32(19) . . ?
O2 C1 C2 118.16(18) . . ?
O1 C1 C2 118.50(19) . . ?
C12 N1 Pb2 125.50(14) . 2_776 ?
C11 N1 C12 117.10(19) . . ?
C11 N1 Pb2 112.40(13) . 2_776 ?
C27 O9 Pb1 119.93(18) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.26(19) . . ?
C4 C3 H3 119.9 . . ?
O3 C8 C4 118.91(17) . . ?
O4 C8 O3 123.59(19) . . ?
O4 C8 C4 117.48(18) . . ?
O7 C21 O8 122.40(19) . . ?
O7 C21 C17 117.95(16) . . ?
O8 C21 C17 119.55(17) . . ?
C16 C15 C14 120.43(18) . . ?
C16 C15 C20 120.43(17) . . ?
C20 C15 C14 119.14(18) . . ?
C3 C2 C1 119.85(19) . . ?
C3 C2 C7 119.50(19) . . ?
C7 C2 C1 120.59(18) . . ?
O6 C14 C15 118.30(18) . . ?
O5 C14 O6 121.53(17) . . ?
O5 C14 C15 120.16(18) . . ?
C3 C4 C8 121.38(19) . . ?
C5 C4 C3 119.04(19) . . ?
C5 C4 C8 119.41(18) . . ?
C2 C7 H7 119.2 . . ?
C2 C7 C6 121.61(19) . . ?
C6 C7 H7 119.2 . . ?
C16 C17 C21 119.69(18) . . ?
C18 C17 C21 120.64(17) . . ?
C18 C17 C16 119.52(19) . . ?
C15 C16 C17 120.32(19) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
N1 C12 H12 118.2 . . ?
N1 C12 C13 123.6(2) . . ?
C13 C12 H12 118.2 . . ?
C15 C20 H20 119.9 . . ?
C15 C20 C19 120.26(19) . . ?
C19 C20 H20 119.9 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C9 120.4(2) . . ?
C9 C13 H13 119.8 . . ?
C7 C6 C5 117.56(19) . . ?
C7 C6 C9 121.82(18) . . ?
C5 C6 C9 120.37(18) . . ?
C4 C5 C6 121.78(19) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C20 C19 C22 119.87(19) . . ?
C18 C19 C20 118.58(19) . . ?
C18 C19 C22 121.50(17) . . ?
N1 C11 H11 118.5 . . ?
N1 C11 C10 122.9(2) . . ?
C10 C11 H11 118.5 . . ?
C17 C18 C19 120.86(17) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C13 C9 C6 123.26(19) . . ?
C13 C9 C10 114.86(19) . . ?
C10 C9 C6 121.83(19) . . ?
N2 C25 H25 118.2 . . ?
N2 C25 C26 123.7(2) . . ?
C26 C25 H25 118.2 . . ?
C24 C23 H23 120.2 . . ?
C24 C23 C22 119.7(2) . . ?
C22 C23 H23 120.2 . . ?
N2 C24 C23 125.25(19) . . ?
N2 C24 H24 117.4 . . ?
C23 C24 H24 117.4 . . ?
C23 C22 C19 122.03(19) . . ?
C26 C22 C19 121.73(17) . . ?
C26 C22 C23 116.20(19) . . ?
C25 C26 H26 119.7 . . ?
C22 C26 C25 120.51(19) . . ?
C22 C26 H26 119.7 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C27 N3 C29 123.5(3) . . ?
C27 N3 C28 118.1(3) . . ?
C29 N3 C28 118.3(3) . . ?
O9 C27 N3 124.5(3) . . ?
O9 C27 H27 117.8 . . ?
N3 C27 H27 117.8 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 Pb2 O7 177.75(4) . 1_655 ?
O3 Pb2 O6 101.72(4) 2_786 . ?
O3 Pb2 O7 76.81(4) 2_786 1_655 ?
O3 Pb2 N1 161.02(5) 2_786 2_776 ?
O8 Pb2 O6 129.12(4) 1_655 . ?
O8 Pb2 O7 49.45(4) 1_655 1_655 ?
O8 Pb2 O3 89.64(5) 1_655 2_786 ?
O8 Pb2 N1 78.23(5) 1_655 2_776 ?
O5 Pb2 O6 51.01(5) . . ?
O5 Pb2 O7 126.93(5) . 1_655 ?
O5 Pb2 O3 84.58(5) . 2_786 ?
O5 Pb2 O8 81.72(5) . 1_655 ?
O5 Pb2 N1 79.31(5) . 2_776 ?
N1 Pb2 O6 75.75(5) 2_776 . ?
N1 Pb2 O7 105.06(5) 2_776 1_655 ?
C30 N4 C32 111.60(3) . . ?
C30 N4 C34 111.44(2) . . ?
C32 N4 C34 111.40(3) . . ?
N4 C30 H30A 106.9 . . ?
N4 C30 H30B 106.9 . . ?
H30A C30 H30B 106.7 . . ?
C31 C30 N4 121.66(3) . . ?
C31 C30 H30A 106.9 . . ?
C31 C30 H30B 106.9 . . ?
N4 C32 H32A 107.0 . . ?
N4 C32 H32B 107.0 . . ?
H32A C32 H32B 106.7 . . ?
C33 C32 N4 121.33(5) . . ?
C33 C32 H32A 107.0 . . ?
C33 C32 H32B 107.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C34 H34A 107.0 . . ?
N4 C34 H34B 107.0 . . ?
H34A C34 H34B 106.7 . . ?
C35 C34 N4 121.44(4) . . ?
C35 C34 H34A 107.0 . . ?
C35 C34 H34B 107.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.998
_oxdiff_exptl_absorpt_empirical_full_min 0.462
####################################################################### 
# 
# 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_q1h
_audit_block_doi                 10.5517/ccdc.csd.cc236zx7
_database_code_depnum_ccdc_archive 'CCDC 1943139'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.molstruc.2019.127244 2020
loop_
_audit_author_name
_audit_author_address
'Akhileshwari P'
;University of Mysore
India
;
_audit_update_record             
;
2019-09-18 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H18 Cl N3 O3'
_chemical_formula_sum            'C23 H18 Cl N3 O3'
_chemical_formula_weight         419.85

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   11.171(2)
_cell_length_b                   21.929(5)
_cell_length_c                   9.307(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.257(14)
_cell_angle_gamma                90.00
_cell_volume                     2078.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4086
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      26.0

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         26028
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26028
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4086
_reflns_number_gt                2490
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  Mercury

_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)+(0.1087P)²+0.0000P] 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         4086
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1637
_refine_ls_wR_factor_gt          0.1246
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_restrained_S_all      0.931
_refine_ls_shift/su_max          0.000
_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
C1 C -0.0273(2) 0.68230(12) -0.1939(3) 0.0643(7) Uani 1 1 d . . .
H1 H 0.0588 0.6783 -0.1196 0.077 Uiso 1 1 calc R . .
C2 C -0.0664(3) 0.73177(12) -0.2910(4) 0.0728(8) Uani 1 1 d . . .
H2 H -0.0055 0.7622 -0.2816 0.087 Uiso 1 1 calc R . .
C3 C -0.1944(3) 0.73812(12) -0.4035(4) 0.0750(8) Uani 1 1 d . . .
H3 H -0.2169 0.7718 -0.4700 0.090 Uiso 1 1 calc R . .
C4 C -0.2878(2) 0.69536(12) -0.4175(3) 0.0675(7) Uani 1 1 d . . .
H4 H -0.3737 0.7002 -0.4919 0.081 Uiso 1 1 calc R . .
C5 C -0.2525(2) 0.64421(10) -0.3184(3) 0.0488(6) Uani 1 1 d . . .
C6 C -0.1212(2) 0.63791(10) -0.2102(3) 0.0490(6) Uani 1 1 d . . .
N7 N -0.11121(16) 0.58431(9) -0.1311(2) 0.0533(5) Uani 1 1 d . . .
H7 H -0.0401 0.5698 -0.0599 0.064 Uiso 1 1 calc R . .
C8 C -0.23269(18) 0.55738(10) -0.1832(2) 0.0437(5) Uani 1 1 d . . .
C9 C -0.3212(2) 0.59254(10) -0.2980(3) 0.0498(6) Uani 1 1 d . . .
H9 H -0.4103 0.5844 -0.3530 0.060 Uiso 1 1 calc R . .
C10 C -0.24714(19) 0.50157(10) -0.1047(3) 0.0445(5) Uani 1 1 d . . .
O11 O -0.14978(13) 0.47578(7) -0.00407(18) 0.0531(4) Uani 1 1 d . . .
N12 N -0.37043(15) 0.48173(8) -0.1422(2) 0.0465(5) Uani 1 1 d . . .
H12 H -0.4322 0.5013 -0.2155 0.056 Uiso 1 1 calc R . .
C13 C -0.40943(19) 0.43191(9) -0.0738(3) 0.0433(5) Uani 1 1 d . . .
C14 C -0.4966(2) 0.38991(10) -0.1725(3) 0.0536(6) Uani 1 1 d . . .
H14 H -0.5197 0.3922 -0.2804 0.064 Uiso 1 1 calc R . .
C15 C -0.5501(2) 0.34481(11) -0.1145(3) 0.0630(7) Uani 1 1 d . . .
H15 H -0.6103 0.3175 -0.1831 0.076 Uiso 1 1 calc R . .
C16 C -0.5143(2) 0.34026(10) 0.0450(3) 0.0601(7) Uani 1 1 d . . .
H16 H -0.5506 0.3099 0.0845 0.072 Uiso 1 1 calc R . .
C17 C -0.4251(2) 0.38040(10) 0.1466(3) 0.0538(6) Uani 1 1 d . . .
H17 H -0.3995 0.3764 0.2546 0.065 Uiso 1 1 calc R . .
C18 C -0.37254(18) 0.42708(9) 0.0883(3) 0.0434(5) Uani 1 1 d . . .
N19 N -0.28295(16) 0.46947(8) 0.1916(2) 0.0468(5) Uani 1 1 d . . .
H19 H -0.2181 0.4801 0.1700 0.056 Uiso 1 1 calc R . .
C20 C -0.28854(19) 0.49480(9) 0.3199(3) 0.0435(5) Uani 1 1 d . . .
O21 O -0.37447(14) 0.48529(7) 0.36844(18) 0.0537(4) Uani 1 1 d . . .
C22 C -0.1814(2) 0.53993(11) 0.4052(3) 0.0503(6) Uani 1 1 d . . .
H22A H -0.2183 0.5805 0.3957 0.060 Uiso 1 1 calc R . .
H22B H -0.1393 0.5296 0.5162 0.060 Uiso 1 1 calc R . .
O23 O -0.08740(15) 0.53869(8) 0.3383(2) 0.0651(5) Uani 1 1 d . . .
C24 C 0.0067(2) 0.58336(10) 0.3773(3) 0.0488(6) Uani 1 1 d . . .
C25 C 0.0305(2) 0.62469(11) 0.4945(3) 0.0598(7) Uani 1 1 d . . .
H25 H -0.0197 0.6249 0.5532 0.072 Uiso 1 1 calc R . .
C26 C 0.1316(2) 0.66686(12) 0.5256(3) 0.0666(7) Uani 1 1 d . . .
H26 H 0.1493 0.6952 0.6061 0.080 Uiso 1 1 calc R . .
C27 C 0.2045(2) 0.66677(12) 0.4388(3) 0.0634(7) Uani 1 1 d . . .
C28 C 0.1817(2) 0.62442(12) 0.3208(3) 0.0642(7) Uani 1 1 d . . .
H28 H 0.2323 0.6242 0.2625 0.077 Uiso 1 1 calc R . .
C29 C 0.0825(2) 0.58262(11) 0.2910(3) 0.0592(6) Uani 1 1 d . . .
H29 H 0.0662 0.5536 0.2123 0.071 Uiso 1 1 calc R . .
Cl30 Cl 0.32692(8) 0.72133(4) 0.47591(12) 0.1067(4) 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
C1 C2 1.364(4) . ?
C1 C6 1.393(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.390(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.405(3) . ?
C5 C9 1.424(3) . ?
C6 N7 1.367(3) . ?
N7 C8 1.373(3) . ?
N7 H7 0.8600 . ?
C8 C9 1.359(3) . ?
C8 C10 1.468(3) . ?
C9 H9 0.9300 . ?
C10 O11 1.242(2) . ?
C10 N12 1.346(2) . ?
N12 C13 1.420(3) . ?
N12 H12 0.8600 . ?
C13 C14 1.380(3) . ?
C13 C18 1.396(3) . ?
C14 C15 1.375(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.374(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.374(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(3) . ?
C17 H17 0.9300 . ?
C18 N19 1.414(3) . ?
N19 C20 1.341(3) . ?
N19 H19 0.8600 . ?
C20 O21 1.235(2) . ?
C20 C22 1.504(3) . ?
C22 O23 1.424(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
O23 C24 1.372(3) . ?
C24 C25 1.358(3) . ?
C24 C29 1.387(3) . ?
C25 C26 1.394(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.363(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.380(4) . ?
C27 Cl30 1.741(2) . ?
C28 C29 1.376(3) . ?
C28 H28 0.9300 . ?
C29 H29 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
C2 C1 C6 117.5(2) . . ?
C2 C1 H1 121.2 . . ?
C6 C1 H1 121.2 . . ?
C1 C2 C3 121.9(2) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.2(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 118.6(2) . . ?
C4 C5 C9 134.7(2) . . ?
C6 C5 C9 106.7(2) . . ?
N7 C6 C1 130.6(2) . . ?
N7 C6 C5 107.49(19) . . ?
C1 C6 C5 121.8(2) . . ?
C6 N7 C8 109.25(18) . . ?
C6 N7 H7 125.4 . . ?
C8 N7 H7 125.4 . . ?
C9 C8 N7 109.18(19) . . ?
C9 C8 C10 132.15(18) . . ?
N7 C8 C10 118.53(18) . . ?
C8 C9 C5 107.35(19) . . ?
C8 C9 H9 126.3 . . ?
C5 C9 H9 126.3 . . ?
O11 C10 N12 122.3(2) . . ?
O11 C10 C8 120.90(17) . . ?
N12 C10 C8 116.77(18) . . ?
C10 N12 C13 127.01(18) . . ?
C10 N12 H12 116.5 . . ?
C13 N12 H12 116.5 . . ?
C14 C13 C18 118.9(2) . . ?
C14 C13 N12 118.5(2) . . ?
C18 C13 N12 122.31(18) . . ?
C15 C14 C13 121.4(2) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C16 C15 C14 119.7(2) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 119.4(2) . . ?
C13 C18 N19 119.83(19) . . ?
C17 C18 N19 120.8(2) . . ?
C20 N19 C18 126.77(18) . . ?
C20 N19 H19 116.6 . . ?
C18 N19 H19 116.6 . . ?
O21 C20 N19 125.67(19) . . ?
O21 C20 C22 119.2(2) . . ?
N19 C20 C22 115.11(19) . . ?
O23 C22 C20 109.07(18) . . ?
O23 C22 H22A 109.9 . . ?
C20 C22 H22A 109.9 . . ?
O23 C22 H22B 109.9 . . ?
C20 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C24 O23 C22 119.53(17) . . ?
C25 C24 O23 124.4(2) . . ?
C25 C24 C29 120.5(2) . . ?
O23 C24 C29 115.0(2) . . ?
C24 C25 C26 119.0(2) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C27 C26 C25 120.4(2) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 120.9(2) . . ?
C26 C27 Cl30 119.6(2) . . ?
C28 C27 Cl30 119.5(2) . . ?
C29 C28 C27 118.6(2) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C28 C29 C24 120.6(2) . . ?
C28 C29 H29 119.7 . . ?
C24 C29 H29 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_lj-1
_audit_block_doi                 10.5517/ccdc.csd.cc236zy8
_database_code_depnum_ccdc_archive 'CCDC 1943140'
loop_
_audit_author_name
_audit_author_address
'Li Jie'
;tianjin university
China
;
_audit_update_record             
;
2019-07-25 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_audit_creation_date             2019-05-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Coronene-Fluoranil
_chemical_name_systematic        Coronene-Tetrafluoro-1,4-benzoquinone
_chemical_formula_moiety         'C6 F4 O2, C24 H12'
_chemical_formula_sum            'C30 H12 F4 O2'
_chemical_formula_weight         480.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7392(2)
_cell_length_b                   6.8776(2)
_cell_length_c                   16.1637(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.368(2)
_cell_angle_gamma                90
_cell_volume                     971.24(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3594
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      76.8170
_cell_measurement_theta_min      5.4530
_shelx_estimated_absorpt_T_max   0.947
_shelx_estimated_absorpt_T_min   0.947
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9648
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.115
_diffrn_reflns_theta_min         5.475
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00 -12.00   0.50    0.10    --  -46.12 113.00-130.00  152
  2  ω      6.00  89.00   0.50    0.10    --   46.12-113.00 138.00  166
  3  ω   -111.00 -27.00   0.50    0.39    -- -100.00 113.00-130.00  168
  4  ω     35.00 112.00   0.50    0.39    --  107.75-113.00 138.00  154
  5  ω     80.00 178.00   0.50    0.39    --  107.75 113.00-130.00  196
  6  ω   -118.00 -30.00   0.50    0.10    --  -46.12 -57.00  60.00  176
  7  ω     73.00 118.00   0.50    0.10    --   46.12 125.00 120.00   90
  8  ω     73.00 118.00   0.50    0.10    --   46.12 125.00  90.00   90
  9  ω     73.00 118.00   0.50    0.10    --   46.12 125.00-180.00   90
 10  ω     73.00 118.00   0.50    0.10    --   46.12 125.00  30.00   90
 11  ω   -173.00 -86.00   0.50    0.39    -- -100.00-113.00 138.00  174
 12  ω   -114.00 -27.00   0.50    0.39    -- -100.00  45.00  90.00  174
 13  ω     35.00 109.00   0.50    0.39    --  107.75 -94.00 -30.00  148
 14  ω     92.00 178.00   0.50    0.39    --  107.75  30.00 -30.00  172
 15  ω     33.00 122.00   0.50    0.39    --  107.75 -30.00 120.00  178
 16  ω     90.00 178.00   0.50    0.39    --  107.75  61.00 -60.00  176
 17  ω     35.00 117.00   0.50    0.39    --  107.75-125.00 120.00  164
 18  ω     23.00 110.00   0.50    0.10    --   46.12  77.00 150.00  174
 19  ω     23.00 118.00   0.50    0.10    --   46.12  77.00-120.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0059127000
_diffrn_orient_matrix_UB_12      0.2198054000
_diffrn_orient_matrix_UB_13      0.0181881000
_diffrn_orient_matrix_UB_21      0.1512596000
_diffrn_orient_matrix_UB_22      0.0155529000
_diffrn_orient_matrix_UB_23      -0.0465479000
_diffrn_orient_matrix_UB_31      -0.0904303000
_diffrn_orient_matrix_UB_32      0.0403114000
_diffrn_orient_matrix_UB_33      -0.0811841000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1575
_reflns_number_total             1961
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1961
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.053
_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)+(0.0480P)²+0.5063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1082
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C4(H4), C5(H5), C1(H1), C2(H2), C12(H12)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
F1 F 0.74069(11) 0.13397(15) 0.59639(6) 0.0280(3) Uani 1 1 d . . . . .
F2 F 0.76418(11) 0.12331(15) 0.42790(6) 0.0280(3) Uani 1 1 d . . . . .
O1 O 0.52268(14) -0.00846(19) 0.33566(7) 0.0281(3) Uani 1 1 d . . . . .
C7 C 0.47758(18) 0.4988(2) 0.58693(9) 0.0196(3) Uani 1 1 d . . . . .
C13 C 0.62730(18) 0.0697(2) 0.54734(10) 0.0202(3) Uani 1 1 d . . . . .
C9 C 0.35826(18) 0.4343(2) 0.53190(10) 0.0201(3) Uani 1 1 d . . . . .
C14 C 0.63833(18) 0.0647(2) 0.46539(10) 0.0203(3) Uani 1 1 d . . . . .
C15 C 0.51220(18) -0.0050(2) 0.41013(10) 0.0204(3) Uani 1 1 d . . . . .
C3 C 0.73854(19) 0.6259(2) 0.61009(10) 0.0238(4) Uani 1 1 d . . . . .
C8 C 0.61973(18) 0.5636(2) 0.55520(10) 0.0192(3) Uani 1 1 d . . . . .
C10 C 0.21752(19) 0.3701(2) 0.56371(11) 0.0238(4) Uani 1 1 d . . . . .
C6 C 0.4555(2) 0.4970(2) 0.67366(10) 0.0247(4) Uani 1 1 d . . . . .
C11 C 0.1976(2) 0.3751(3) 0.65042(12) 0.0296(4) Uani 1 1 d . . . . .
H11 H 0.104437 0.336578 0.671672 0.036 Uiso 1 1 calc R . . . .
C4 C 0.7138(2) 0.6184(3) 0.69690(11) 0.0286(4) Uani 1 1 d . . . . .
H4 H 0.791716 0.656019 0.733692 0.034 Uiso 1 1 calc R . . . .
C5 C 0.5776(2) 0.5568(3) 0.72666(10) 0.0285(4) Uani 1 1 d . . . . .
H5 H 0.564506 0.554002 0.783584 0.034 Uiso 1 1 calc R . . . .
C1 C 0.89824(19) 0.6951(3) 0.49294(12) 0.0292(4) Uani 1 1 d . . . . .
H1 H 0.990354 0.740418 0.472675 0.035 Uiso 1 1 calc R . . . .
C2 C 0.87757(19) 0.6930(3) 0.57645(12) 0.0285(4) Uani 1 1 d . . . . .
H2 H 0.955868 0.736081 0.611847 0.034 Uiso 1 1 calc R . . . .
C12 C 0.3117(2) 0.4348(3) 0.70344(11) 0.0292(4) Uani 1 1 d . . . . .
H12 H 0.295276 0.434930 0.760078 0.035 Uiso 1 1 calc R . . . .


_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
F1 C13 1.3299(19) . ?
F2 C14 1.3309(17) . ?
O1 C15 1.2096(19) . ?
C7 C9 1.425(2) . ?
C7 C8 1.427(2) . ?
C7 C6 1.420(2) . ?
C13 C14 1.331(2) . ?
C13 C15 1.482(2) 3_656 ?
C9 C8 1.426(2) 3_666 ?
C9 C10 1.415(2) . ?
C14 C15 1.482(2) . ?
C3 C8 1.416(2) . ?
C3 C4 1.426(2) . ?
C3 C2 1.420(2) . ?
C10 C11 1.417(2) . ?
C10 C1 1.421(2) 3_666 ?
C6 C5 1.413(3) . ?
C6 C12 1.422(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.363(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.362(3) . ?
C5 H5 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.366(3) . ?
C2 H2 0.9300 . ?
C12 H12 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
C9 C7 C8 120.22(14) . . ?
C6 C7 C9 119.93(15) . . ?
C6 C7 C8 119.85(15) . . ?
F1 C13 C14 122.09(15) . . ?
F1 C13 C15 115.64(14) . 3_656 ?
C14 C13 C15 122.27(15) . 3_656 ?
C7 C9 C8 119.95(14) . 3_666 ?
C10 C9 C7 119.98(15) . . ?
C10 C9 C8 120.06(15) . 3_666 ?
F2 C14 C15 115.75(13) . . ?
C13 C14 F2 121.71(15) . . ?
C13 C14 C15 122.54(14) . . ?
O1 C15 C13 122.57(15) . 3_656 ?
O1 C15 C14 122.23(15) . . ?
C14 C15 C13 115.19(14) . 3_656 ?
C8 C3 C4 118.65(16) . . ?
C8 C3 C2 118.67(16) . . ?
C2 C3 C4 122.68(16) . . ?
C9 C8 C7 119.83(15) 3_666 . ?
C3 C8 C7 120.07(15) . . ?
C3 C8 C9 120.10(15) . 3_666 ?
C9 C10 C11 118.69(16) . . ?
C9 C10 C1 118.43(15) . 3_666 ?
C11 C10 C1 122.88(16) . 3_666 ?
C7 C6 C12 118.61(16) . . ?
C5 C6 C7 118.53(16) . . ?
C5 C6 C12 122.86(16) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 C10 121.63(16) . . ?
C12 C11 H11 119.2 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.88(16) . . ?
C5 C4 H4 119.6 . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 121.99(16) . . ?
C4 C5 H5 119.0 . . ?
C10 C1 H1 119.2 3_666 . ?
C2 C1 C10 121.62(16) . 3_666 ?
C2 C1 H1 119.2 . . ?
C3 C2 H2 119.5 . . ?
C1 C2 C3 121.10(16) . . ?
C1 C2 H2 119.5 . . ?
C6 C12 H12 119.4 . . ?
C11 C12 C6 121.13(16) . . ?
C11 C12 H12 119.4 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.810
_exptl_crystal_recrystallization_method ????
####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/ccdc.csd.cc236zz9
_database_code_depnum_ccdc_archive 'CCDC 1943141'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.inorgchem.9b02697 2019
loop_
_audit_author_name
_audit_author_address
maweimin
;The CCDC
China
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_audit_creation_date             2019-08-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H20 N3 O9 Pb2'
_chemical_formula_sum            'C30 H20 N3 O9 Pb2'
_chemical_formula_weight         980.87
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Pb'
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'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3203(2)
_cell_length_b                   13.2585(3)
_cell_length_c                   13.5030(3)
_cell_angle_alpha                93.919(2)
_cell_angle_beta                 94.862(2)
_cell_angle_gamma                98.199(2)
_cell_volume                     1816.10(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9477
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.4230
_cell_measurement_theta_min      2.0520
_shelx_estimated_absorpt_T_max   0.336
_shelx_estimated_absorpt_T_min   0.204
_exptl_absorpt_coefficient_mu    9.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.356
_diffrn_reflns_theta_min         2.003
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00 -26.00   0.50   25.00    --   10.30 -65.00 -97.00   56
  2  ω     -8.00  31.00   0.50   25.00    --   10.30 -65.00 -97.00   78
  3  ω    -18.00  23.00   0.50   25.00    --   -9.20 -99.00-120.00   82
  4  ω    -20.00  18.00   0.50   25.00    --   -9.20 -99.00-180.00   76
  5  ω    -65.00  33.00   0.50   25.00    --   10.30 -37.00-180.00  196
  6  ω    -32.00  59.00   0.50   25.00    --   -9.20  57.00 -60.00  182
  7  ω    -14.00  85.00   0.50   25.00    --   10.30  65.00  37.00  198
  8  ω    -22.00  18.00   0.50   25.00    --   -9.20 -99.00  90.00   80
  9  ω     22.00  49.00   0.50   25.00    --   10.30 -99.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0352911000
_diffrn_orient_matrix_UB_12      0.0251099000
_diffrn_orient_matrix_UB_13      0.0345356000
_diffrn_orient_matrix_UB_21      0.0199162000
_diffrn_orient_matrix_UB_22      0.0472193000
_diffrn_orient_matrix_UB_23      -0.0200180000
_diffrn_orient_matrix_UB_31      -0.0567812000
_diffrn_orient_matrix_UB_32      -0.0089907000
_diffrn_orient_matrix_UB_33      -0.0347053000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7350
_reflns_number_total             9057
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.465
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9057
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+2.8508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0742
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C13(H13), C12(H12), C11(H11), C10(H10), C20(H20),
 C18(H18), C16(H16), C26(H26), C25(H25), C24(H24), C23(H23)
3.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.48547(2) 0.93679(2) 0.16384(2) 0.01690(3) Uani 1 1 d . . . . .
Pb2 Pb -0.14720(2) 0.09199(2) 0.04884(2) 0.01317(3) Uani 1 1 d . . . . .
O1 O 0.6452(2) 0.9019(2) 0.29608(17) 0.0242(6) Uani 1 1 d . . . . .
O2 O 0.7392(2) 0.92993(19) 0.15635(16) 0.0215(6) Uani 1 1 d . . . . .
O3 O 1.2106(2) 0.88757(19) 0.14112(16) 0.0223(6) Uani 1 1 d . . . . .
O4 O 1.3305(2) 0.8832(2) 0.28458(18) 0.0314(7) Uani 1 1 d . . . . .
O5 O 0.0274(2) 0.23926(19) 0.03520(19) 0.0246(6) Uani 1 1 d . . . . .
O6 O 0.1060(2) 0.09286(18) 0.04712(17) 0.0188(5) Uani 1 1 d . . . . .
O8 O 0.7243(2) 0.23871(18) 0.09515(17) 0.0211(6) Uani 1 1 d . . . . .
O7 O 0.5852(2) 0.09846(18) 0.04351(17) 0.0209(6) Uani 1 1 d . . . . .
O9 O 0.5001(4) 1.0972(3) 0.2946(3) 0.0632(9) Uani 1 1 d . U . . .
N1 N 1.0637(3) 0.8563(2) 0.7646(2) 0.0257(8) Uani 1 1 d . . . . .
N2 N 0.4633(3) 0.7380(2) 0.1454(2) 0.0196(7) Uani 1 1 d . . . . .
N3 N 0.4765(12) 1.2152(10) 0.4298(10) 0.2300(14) Uani 1 1 d . U . . .
C2 C 0.8737(3) 0.8903(3) 0.2954(2) 0.0175(8) Uani 1 1 d . . . . .
C7 C 0.8853(3) 0.8782(3) 0.3981(2) 0.0192(8) Uani 1 1 d . . . . .
H7 H 0.8122 0.8783 0.4338 0.023 Uiso 1 1 calc R . . . .
C6 C 1.0067(3) 0.8658(3) 0.4472(2) 0.0179(8) Uani 1 1 d . . . . .
C5 C 1.1132(3) 0.8667(3) 0.3911(2) 0.0196(8) Uani 1 1 d . . . . .
H5 H 1.1948 0.8597 0.4226 0.024 Uiso 1 1 calc R . . . .
C4 C 1.1022(3) 0.8776(3) 0.2894(2) 0.0176(7) Uani 1 1 d . . . . .
C3 C 0.9802(3) 0.8891(3) 0.2418(2) 0.0171(7) Uani 1 1 d . . . . .
H3 H 0.9714 0.8961 0.1736 0.021 Uiso 1 1 calc R . . . .
C9 C 1.0228(3) 0.8575(3) 0.5566(2) 0.0181(8) Uani 1 1 d . . . . .
C13 C 0.9227(3) 0.8676(3) 0.6172(2) 0.0233(8) Uani 1 1 d . . . . .
H13 H 0.8394 0.8745 0.5888 0.028 Uiso 1 1 calc R . . . .
C12 C 0.9463(3) 0.8675(3) 0.7198(3) 0.0280(9) Uani 1 1 d . . . . .
H12 H 0.8781 0.8755 0.7591 0.034 Uiso 1 1 calc R . . . .
C11 C 1.1581(4) 0.8419(4) 0.7061(3) 0.0370(10) Uani 1 1 d . . . . .
H11 H 1.2391 0.8309 0.7356 0.044 Uiso 1 1 calc R . . . .
C10 C 1.1412(4) 0.8426(4) 0.6047(3) 0.0358(11) Uani 1 1 d . . . . .
H10 H 1.2107 0.8328 0.5674 0.043 Uiso 1 1 calc R . . . .
C1 C 0.7436(3) 0.9095(3) 0.2468(2) 0.0175(8) Uani 1 1 d . . . . .
C8 C 1.2222(3) 0.8824(3) 0.2342(2) 0.0201(8) Uani 1 1 d . . . . .
C15 C 0.2599(3) 0.2469(3) 0.0660(2) 0.0174(7) Uani 1 1 d . . . . .
C20 C 0.2790(3) 0.3534(3) 0.0842(2) 0.0200(8) Uani 1 1 d . . . . .
H20 H 0.2068 0.3882 0.0828 0.024 Uiso 1 1 calc R . . . .
C19 C 0.4060(3) 0.4080(3) 0.1045(2) 0.0190(8) Uani 1 1 d . . . . .
C18 C 0.5128(3) 0.3540(3) 0.1039(2) 0.0194(8) Uani 1 1 d . . . . .
H18 H 0.5978 0.3892 0.1174 0.023 Uiso 1 1 calc R . . . .
C17 C 0.4935(3) 0.2485(3) 0.0832(2) 0.0171(7) Uani 1 1 d . . . . .
C16 C 0.3661(3) 0.1941(3) 0.0650(2) 0.0165(7) Uani 1 1 d . . . . .
H16 H 0.3532 0.1233 0.0525 0.020 Uiso 1 1 calc R . . . .
C22 C 0.4256(3) 0.5216(3) 0.1212(2) 0.0207(8) Uani 1 1 d . . . . .
C26 C 0.3221(3) 0.5774(3) 0.1105(3) 0.0266(9) Uani 1 1 d . . . . .
H26 H 0.2368 0.5433 0.0951 0.032 Uiso 1 1 calc R . . . .
C25 C 0.3438(3) 0.6822(3) 0.1223(3) 0.0263(9) Uani 1 1 d . . . . .
H25 H 0.2717 0.7167 0.1138 0.032 Uiso 1 1 calc R . . . .
C24 C 0.5641(4) 0.6840(3) 0.1568(3) 0.0298(10) Uani 1 1 d . . . . .
H24 H 0.6483 0.7198 0.1729 0.036 Uiso 1 1 calc R . . . .
C23 C 0.5491(4) 0.5793(3) 0.1459(3) 0.0292(9) Uani 1 1 d . . . . .
H23 H 0.6225 0.5464 0.1551 0.035 Uiso 1 1 calc R . . . .
C14 C 0.1226(3) 0.1894(3) 0.0470(2) 0.0184(8) Uani 1 1 d . . . . .
C21 C 0.6095(3) 0.1912(3) 0.0744(2) 0.0156(7) Uani 1 1 d . . . . .
C27 C 0.4933(14) 1.1144(11) 0.3760(10) 0.1965(14) Uani 1 1 d . U . . .
C28 C 0.4956(11) 1.0304(8) 0.4599(7) 0.1352(14) Uani 1 1 d . U . . .
C29 C 0.4585(14) 1.2953(11) 0.3581(10) 0.226(3) Uani 1 1 d . U . . .
H29A H 0.5425 1.3231 0.3381 0.340 Uiso 1 1 calc GR . . . .
H29B H 0.4195 1.3489 0.3899 0.340 Uiso 1 1 calc GR . . . .
H29C H 0.4021 1.2648 0.3004 0.340 Uiso 1 1 calc GR . . . .
C30 C 0.5091(12) 1.2588(10) 0.5483(9) 0.195(3) Uani 1 1 d . U . . .
H30A H 0.4409 1.2286 0.5860 0.293 Uiso 1 1 calc GR . . . .
H30B H 0.5132 1.3318 0.5539 0.293 Uiso 1 1 calc GR . . . .
H30C H 0.5919 1.2412 0.5737 0.293 Uiso 1 1 calc GR . . . .


_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 2.440(2) . ?
Pb1 O2 2.643(2) . ?
Pb1 O4 2.449(2) 1_455 ?
Pb1 O9 2.648(4) . ?
Pb1 N2 2.605(3) . ?
Pb2 O3 2.635(2) 2_665 ?
Pb2 O5 2.489(2) . ?
Pb2 O6 2.613(2) . ?
Pb2 O8 2.578(2) 1_455 ?
Pb2 N1 2.605(3) 2_666 ?
O1 C1 1.256(4) . ?
O2 C1 1.268(4) . ?
O3 Pb2 2.635(2) 2_665 ?
O3 C8 1.260(4) . ?
O4 Pb1 2.449(2) 1_655 ?
O4 C8 1.257(4) . ?
O5 C14 1.266(4) . ?
O6 C14 1.267(4) . ?
O8 Pb2 2.578(2) 1_655 ?
O8 C21 1.259(4) . ?
O7 C21 1.255(4) . ?
O9 C27 1.118(14) . ?
N1 Pb2 2.604(3) 2_666 ?
N1 C12 1.340(5) . ?
N1 C11 1.331(5) . ?
N2 C25 1.345(4) . ?
N2 C24 1.348(5) . ?
N3 C27 1.516(18) . ?
N3 C29 1.506(17) . ?
N3 C30 1.653(16) . ?
C2 C7 1.403(4) . ?
C2 C3 1.369(5) . ?
C2 C1 1.506(4) . ?
C7 H7 0.9300 . ?
C7 C6 1.403(4) . ?
C6 C5 1.386(5) . ?
C6 C9 1.485(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.387(4) . ?
C4 C3 1.398(4) . ?
C4 C8 1.494(5) . ?
C3 H3 0.9300 . ?
C9 C13 1.386(5) . ?
C9 C10 1.380(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.387(5) . ?
C12 H12 0.9300 . ?
C11 H11 0.9300 . ?
C11 C10 1.367(5) . ?
C10 H10 0.9300 . ?
C15 C20 1.400(5) . ?
C15 C16 1.383(5) . ?
C15 C14 1.502(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.400(4) . ?
C19 C18 1.397(5) . ?
C19 C22 1.490(5) . ?
C18 H18 0.9300 . ?
C18 C17 1.390(5) . ?
C17 C16 1.400(4) . ?
C17 C21 1.515(5) . ?
C16 H16 0.9300 . ?
C22 C26 1.386(5) . ?
C22 C23 1.392(5) . ?
C26 H26 0.9300 . ?
C26 C25 1.372(5) . ?
C25 H25 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.371(5) . ?
C23 H23 0.9300 . ?
C27 C28 1.643(16) . ?
C28 C28 1.398(19) 2_676 ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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 O2 51.68(7) . . ?
O1 Pb1 O4 82.14(8) . 1_455 ?
O1 Pb1 O9 77.00(10) . . ?
O1 Pb1 N2 77.40(8) . . ?
O2 Pb1 O9 99.33(10) . . ?
O4 Pb1 O2 132.99(7) 1_455 . ?
O4 Pb1 O9 74.87(11) 1_455 . ?
O4 Pb1 N2 76.51(9) 1_455 . ?
N2 Pb1 O2 84.32(8) . . ?
N2 Pb1 O9 143.71(10) . . ?
O5 Pb2 O3 84.21(8) . 2_665 ?
O5 Pb2 O6 51.47(8) . . ?
O5 Pb2 O8 81.14(8) . 1_455 ?
O5 Pb2 N1 78.31(9) . 2_666 ?
O6 Pb2 O3 99.85(7) . 2_665 ?
O8 Pb2 O3 89.16(8) 1_455 2_665 ?
O8 Pb2 O6 129.87(7) 1_455 . ?
O8 Pb2 N1 76.82(9) 1_455 2_666 ?
N1 Pb2 O3 159.01(9) 2_666 2_665 ?
N1 Pb2 O6 78.25(8) 2_666 . ?
C1 O1 Pb1 97.29(19) . . ?
C1 O2 Pb1 87.57(18) . . ?
C8 O3 Pb2 170.2(2) . 2_665 ?
C8 O4 Pb1 101.2(2) . 1_655 ?
C14 O5 Pb2 95.6(2) . . ?
C14 O6 Pb2 89.82(18) . . ?
C21 O8 Pb2 98.4(2) . 1_655 ?
C27 O9 Pb1 139.2(8) . . ?
C12 N1 Pb2 126.2(2) . 2_666 ?
C11 N1 Pb2 114.4(2) . 2_666 ?
C11 N1 C12 117.2(3) . . ?
C25 N2 Pb1 119.4(2) . . ?
C25 N2 C24 115.5(3) . . ?
C24 N2 Pb1 125.1(2) . . ?
C27 N3 C30 131.3(12) . . ?
C29 N3 C27 111.6(12) . . ?
C29 N3 C30 115.2(11) . . ?
C7 C2 C1 118.7(3) . . ?
C3 C2 C7 120.4(3) . . ?
C3 C2 C1 120.8(3) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
C7 C6 C9 121.4(3) . . ?
C5 C6 C7 117.7(3) . . ?
C5 C6 C9 120.8(3) . . ?
C6 C5 H5 118.9 . . ?
C6 C5 C4 122.2(3) . . ?
C4 C5 H5 118.9 . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 C8 119.4(3) . . ?
C3 C4 C8 121.4(3) . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C13 C9 C6 122.7(3) . . ?
C10 C9 C6 121.5(3) . . ?
C10 C9 C13 115.8(3) . . ?
C9 C13 H13 119.9 . . ?
C9 C13 C12 120.2(3) . . ?
C12 C13 H13 119.9 . . ?
N1 C12 C13 122.5(3) . . ?
N1 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
N1 C11 H11 118.6 . . ?
N1 C11 C10 122.9(3) . . ?
C10 C11 H11 118.6 . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.3(3) . . ?
C11 C10 H10 119.4 . . ?
O1 C1 O2 123.5(3) . . ?
O1 C1 C2 119.1(3) . . ?
O2 C1 C2 117.4(3) . . ?
O3 C8 C4 119.1(3) . . ?
O4 C8 O3 123.6(3) . . ?
O4 C8 C4 117.3(3) . . ?
C20 C15 C14 119.7(3) . . ?
C16 C15 C20 120.6(3) . . ?
C16 C15 C14 119.7(3) . . ?
C15 C20 H20 119.8 . . ?
C19 C20 C15 120.5(3) . . ?
C19 C20 H20 119.8 . . ?
C20 C19 C22 120.1(3) . . ?
C18 C19 C20 118.5(3) . . ?
C18 C19 C22 121.3(3) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 C19 120.8(3) . . ?
C17 C18 H18 119.6 . . ?
C18 C17 C16 120.4(3) . . ?
C18 C17 C21 120.7(3) . . ?
C16 C17 C21 118.8(3) . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C26 C22 C19 122.2(3) . . ?
C26 C22 C23 115.3(3) . . ?
C23 C22 C19 122.4(3) . . ?
C22 C26 H26 119.6 . . ?
C25 C26 C22 120.9(3) . . ?
C25 C26 H26 119.6 . . ?
N2 C25 C26 123.8(3) . . ?
N2 C25 H25 118.1 . . ?
C26 C25 H25 118.1 . . ?
N2 C24 H24 118.2 . . ?
N2 C24 C23 123.6(3) . . ?
C23 C24 H24 118.2 . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.9(3) . . ?
C24 C23 H23 119.6 . . ?
O5 C14 O6 122.3(3) . . ?
O5 C14 C15 118.9(3) . . ?
O6 C14 C15 118.8(3) . . ?
O8 C21 C17 119.2(3) . . ?
O7 C21 O8 123.4(3) . . ?
O7 C21 C17 117.4(3) . . ?
O9 C27 N3 128.0(13) . . ?
O9 C27 C28 124.8(12) . . ?
N3 C27 C28 107.1(11) . . ?
C28 C28 C27 172.6(13) 2_676 . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.134
_oxdiff_exptl_absorpt_empirical_full_min 0.543
####################################################################### 
# 
# 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_sq
_database_code_depnum_ccdc_archive 'CCDC 1943144'
loop_
_audit_author_name
_audit_author_address
maweimin
;The CCDC
China
;
_audit_update_record             
;
2019-07-25 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_audit_creation_date             2019-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(C156 H84 N12 O54 Pb18)'
_chemical_formula_sum            'C276 H14 N2 O9 Pb3'
_chemical_formula_weight         4122.46
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb C O  H'
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'
Pb Pb -3.3944 10.1111 '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'

_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      hexagonal
_space_group_IT_number           180
_space_group_name_H-M_alt        'P 62 2 2'
_space_group_name_Hall           'P 62 2c (0 0 1)'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z'
'y, -x+y, z+2/3'
'x-y, x, z+1/3'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+2/3'
'-x+y, y, -z'
'x, x-y, -z+1/3'

_cell_length_a                   17.2929(4)
_cell_length_b                   17.2929(4)
_cell_length_c                   20.2996(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5257.2(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    27611
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.5810
_cell_measurement_theta_min      2.3400
_shelx_estimated_absorpt_T_max   0.216
_shelx_estimated_absorpt_T_min   0.156
_exptl_absorpt_coefficient_mu    14.747
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    7.813
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             12012
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48884
_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         25.984
_diffrn_reflns_theta_min         1.690
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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    -60.00  23.00   0.50   17.99    --   -6.48 -19.00  81.00  166
  2  ω      1.00  32.00   0.50   17.99    --   -6.48 -99.00 -30.00   62
  3  ω     20.00  62.00   0.50   17.99    --    7.96-125.00  20.00   84
  4  ω    -20.00  13.00   0.50   17.99    --   -6.48 -99.00-150.00   66
  5  ω    -22.00   4.00   0.50   17.99    --   -6.48 -99.00-120.00   52
  6  ω    -69.00  31.00   0.50   17.99    --    7.96 -37.00 -30.00  200
  7  ω    -56.00   0.00   0.50   17.99    --    7.96 -37.00  30.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0458782000
_diffrn_orient_matrix_UB_12      0.0235784000
_diffrn_orient_matrix_UB_13      0.0086354000
_diffrn_orient_matrix_UB_21      -0.0000629000
_diffrn_orient_matrix_UB_22      0.0409119000
_diffrn_orient_matrix_UB_23      -0.0021198000
_diffrn_orient_matrix_UB_31      -0.0117656000
_diffrn_orient_matrix_UB_32      -0.0034500000
_diffrn_orient_matrix_UB_33      0.0337872000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3369
_reflns_number_total             3460
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.337
_refine_ls_abs_structure_details 
;
 Flack x determined using 1335 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3460
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+12.4564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0764
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C11, C8, C7, C5, C6, C4, C3, C2
 with sigma of 0.1
 N1, C10, C9, C11, C4, C7, C5, C4, C3, C2, C1, C6
 with sigma of 0.1
 C4, C3, C2, C13, O4, O3
 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C4(H4), C11(H11), C2(H2), C10(H10), C8(H8)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.39432(3) 1.0000 0.5000 0.01391(14) Uani 1 2 d S T P . .
Pb2 Pb 0.57591(2) 1.18725(2) 0.41220(2) 0.01408(13) Uani 1 1 d . . . . .
O3 O 0.2725(5) 0.7170(5) 0.1791(3) 0.0207(16) Uani 1 1 d . . . . .
O2 O 0.3486(6) 0.9062(5) 0.3856(3) 0.0228(17) Uani 1 1 d . . . . .
O4 O 0.1851(6) 0.7486(5) 0.1192(3) 0.0232(17) Uani 1 1 d . . . . .
C1 C 0.3717(7) 0.9615(7) 0.2762(5) 0.019(2) Uani 1 1 d . . . . .
O1 O 0.4415(5) 1.0510(5) 0.3711(4) 0.0270(18) Uani 1 1 d . . . . .
C7 C 0.4276(8) 1.1016(7) 0.1180(4) 0.024(2) Uani 1 1 d . . . . .
C5 C 0.3860(7) 1.0218(7) 0.1657(5) 0.020(2) Uani 1 1 d . . . . .
C3 C 0.2999(6) 0.8658(7) 0.1858(5) 0.020(2) Uani 1 1 d . . . . .
C13 C 0.2481(7) 0.7707(7) 0.1603(5) 0.020(2) Uani 1 1 d . . . . .
C9 C 0.4173(9) 1.1778(8) 0.0253(5) 0.033(3) Uani 1 1 d . . . . .
H9 H 0.3848 1.1789 -0.0108 0.039 Uiso 1 1 calc R . . . .
N1 N 0.4965(7) 1.2401(7) 0.0318(5) 0.033(2) Uani 1 1 d . . . . .
C6 C 0.4084(7) 1.0348(7) 0.2323(5) 0.022(2) Uani 1 1 d . . . . .
H6 H 0.4476 1.0919 0.2479 0.026 Uiso 1 1 calc R . . . .
C4 C 0.3274(8) 0.9359(8) 0.1439(5) 0.023(2) Uani 1 1 d . . . . .
H4 H 0.3069 0.9264 0.1006 0.028 Uiso 1 1 calc R . . . .
C11 C 0.5091(8) 1.1652(8) 0.1255(6) 0.034(3) Uani 1 1 d . . . . .
H11 H 0.5438 1.1647 0.1604 0.041 Uiso 1 1 calc R . . . .
C2 C 0.3193(7) 0.8765(7) 0.2517(5) 0.018(2) Uani 1 1 d . . . . .
H2 H 0.2974 0.8272 0.2794 0.021 Uiso 1 1 calc R . . . .
C10 C 0.5443(9) 1.2363(9) 0.0789(6) 0.041(3) Uani 1 1 d . . . . .
H10 H 0.6036 1.2812 0.0825 0.049 Uiso 1 1 calc R . . . .
C8 C 0.3751(8) 1.1057(8) 0.0706(5) 0.030(3) Uani 1 1 d . . . . .
H8 H 0.3146 1.0636 0.0678 0.036 Uiso 1 1 calc R . . . .
C12 C 0.3901(7) 0.9759(7) 0.3491(4) 0.017(2) Uani 1 1 d . . . . .
O5 O 0.5477(3) 1.0955(7) 0.5000 0.015(2) Uani 1 2 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 Pb1 3.6550(12) 4_675 ?
Pb1 Pb2 3.6544(4) . ?
Pb1 Pb2 3.6543(4) 8_676 ?
Pb1 O2 2.714(7) . ?
Pb1 O2 2.714(7) 8_676 ?
Pb1 O1 2.751(8) . ?
Pb1 O1 2.751(8) 8_676 ?
Pb1 O5 2.320(6) . ?
Pb1 O5 2.320(6) 4_675 ?
Pb2 Pb2 3.6170(6) 11_556 ?
Pb2 O3 2.638(7) 6_665 ?
Pb2 O3 2.621(7) 7_565 ?
Pb2 O2 2.592(8) 4_675 ?
Pb2 O4 2.528(8) 6_665 ?
Pb2 O1 2.484(8) . ?
Pb2 O5 2.272(6) . ?
O3 Pb2 2.621(7) 7_455 ?
O3 Pb2 2.638(7) 5_454 ?
O3 C13 1.256(13) . ?
O2 Pb2 2.592(8) 4_675 ?
O2 C12 1.285(13) . ?
O4 Pb2 2.528(8) 5_454 ?
O4 C13 1.269(13) . ?
C1 C6 1.415(15) . ?
C1 C2 1.377(15) . ?
C1 C12 1.509(13) . ?
O1 C12 1.234(13) . ?
C7 C5 1.539(14) . ?
C7 C11 1.292(18) . ?
C7 C8 1.347(16) . ?
C5 C6 1.393(14) . ?
C5 C4 1.386(15) . ?
C3 C13 1.518(14) . ?
C3 C4 1.358(15) . ?
C3 C2 1.368(14) . ?
C9 H9 0.9300 . ?
C9 N1 1.257(16) . ?
C9 C8 1.424(16) . ?
N1 C10 1.285(17) . ?
C6 H6 0.9300 . ?
C4 H4 0.9300 . ?
C11 H11 0.9300 . ?
C11 C10 1.424(15) . ?
C2 H2 0.9300 . ?
C10 H10 0.9300 . ?
C8 H8 0.9300 . ?
O5 Pb1 2.320(6) 4_675 ?
O5 Pb2 2.272(6) 11_556 ?

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
Pb2 Pb1 Pb1 65.402(10) 8_676 4_675 ?
Pb2 Pb1 Pb1 65.401(10) . 4_675 ?
Pb2 Pb1 Pb2 130.80(2) 8_676 . ?
O2 Pb1 Pb1 89.58(17) . 4_675 ?
O2 Pb1 Pb1 89.58(17) 8_676 4_675 ?
O2 Pb1 Pb2 88.68(17) . . ?
O2 Pb1 Pb2 88.68(17) 8_676 8_676 ?
O2 Pb1 Pb2 90.97(16) 8_676 . ?
O2 Pb1 Pb2 90.97(15) . 8_676 ?
O2 Pb1 O2 179.2(3) 8_676 . ?
O2 Pb1 O1 132.0(2) . 8_676 ?
O2 Pb1 O1 47.9(2) . . ?
O2 Pb1 O1 47.9(2) 8_676 8_676 ?
O2 Pb1 O1 132.0(2) 8_676 . ?
O1 Pb1 Pb1 82.16(17) . 4_675 ?
O1 Pb1 Pb1 82.16(17) 8_676 4_675 ?
O1 Pb1 Pb2 42.81(16) . . ?
O1 Pb1 Pb2 128.32(17) . 8_676 ?
O1 Pb1 Pb2 128.32(18) 8_676 . ?
O1 Pb1 Pb2 42.81(16) 8_676 8_676 ?
O1 Pb1 O1 164.3(4) . 8_676 ?
O5 Pb1 Pb1 38.04(19) 4_675 4_675 ?
O5 Pb1 Pb1 38.04(19) . 4_675 ?
O5 Pb1 Pb2 98.34(17) . 8_676 ?
O5 Pb1 Pb2 36.81(11) 4_675 8_676 ?
O5 Pb1 Pb2 98.34(17) 4_675 . ?
O5 Pb1 Pb2 36.80(11) . . ?
O5 Pb1 O2 108.25(19) 4_675 8_676 ?
O5 Pb1 O2 71.05(18) 4_675 . ?
O5 Pb1 O2 71.04(18) . 8_676 ?
O5 Pb1 O2 108.26(19) . . ?
O5 Pb1 O1 73.83(17) . . ?
O5 Pb1 O1 73.83(16) 4_675 8_676 ?
O5 Pb1 O1 93.65(19) . 8_676 ?
O5 Pb1 O1 93.65(19) 4_675 . ?
O5 Pb1 O5 76.1(4) 4_675 . ?
Pb2 Pb2 Pb1 65.784(8) 11_556 . ?
O3 Pb2 Pb1 79.80(16) 6_665 . ?
O3 Pb2 Pb1 111.07(15) 7_565 . ?
O3 Pb2 Pb2 46.35(16) 6_665 11_556 ?
O3 Pb2 Pb2 46.74(15) 7_565 11_556 ?
O3 Pb2 O3 65.3(3) 7_565 6_665 ?
O2 Pb2 Pb1 91.53(17) 4_675 . ?
O2 Pb2 Pb2 93.83(14) 4_675 11_556 ?
O2 Pb2 O3 139.4(2) 4_675 6_665 ?
O2 Pb2 O3 81.6(2) 4_675 7_565 ?
O4 Pb2 Pb1 55.83(19) 6_665 . ?
O4 Pb2 Pb2 80.86(15) 6_665 11_556 ?
O4 Pb2 O3 50.6(2) 6_665 6_665 ?
O4 Pb2 O3 115.6(2) 6_665 7_565 ?
O4 Pb2 O2 146.3(3) 6_665 4_675 ?
O1 Pb2 Pb1 48.81(18) . . ?
O1 Pb2 Pb2 114.13(18) . 11_556 ?
O1 Pb2 O3 117.8(3) . 6_665 ?
O1 Pb2 O3 153.6(2) . 7_565 ?
O1 Pb2 O2 82.1(3) . 4_675 ?
O1 Pb2 O4 70.2(3) . 6_665 ?
O5 Pb2 Pb1 37.73(12) . . ?
O5 Pb2 Pb2 37.2(2) . 11_556 ?
O5 Pb2 O3 75.1(2) . 6_665 ?
O5 Pb2 O3 75.5(2) . 7_565 ?
O5 Pb2 O2 74.13(18) . 4_675 ?
O5 Pb2 O4 82.28(17) . 6_665 ?
O5 Pb2 O1 80.1(3) . . ?
Pb2 O3 Pb2 86.9(2) 7_455 5_454 ?
C13 O3 Pb2 128.7(7) . 7_455 ?
C13 O3 Pb2 90.0(6) . 5_454 ?
Pb2 O2 Pb1 96.2(2) 4_675 . ?
C12 O2 Pb1 94.2(6) . . ?
C12 O2 Pb2 119.0(7) . 4_675 ?
C13 O4 Pb2 94.7(7) . 5_454 ?
C6 C1 C12 120.5(9) . . ?
C2 C1 C6 119.3(9) . . ?
C2 C1 C12 120.2(9) . . ?
Pb2 O1 Pb1 88.4(2) . . ?
C12 O1 Pb1 93.7(6) . . ?
C12 O1 Pb2 163.8(8) . . ?
C11 C7 C5 120.7(10) . . ?
C11 C7 C8 121.1(11) . . ?
C8 C7 C5 118.0(10) . . ?
C6 C5 C7 119.8(9) . . ?
C4 C5 C7 121.6(9) . . ?
C4 C5 C6 118.6(10) . . ?
C4 C3 C13 120.4(9) . . ?
C4 C3 C2 122.7(10) . . ?
C2 C3 C13 116.9(9) . . ?
O3 C13 O4 122.2(10) . . ?
O3 C13 C3 117.5(9) . . ?
O4 C13 C3 120.3(10) . . ?
N1 C9 H9 118.5 . . ?
N1 C9 C8 122.9(11) . . ?
C8 C9 H9 118.5 . . ?
C9 N1 C10 119.2(11) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.2(10) . . ?
C5 C6 H6 119.9 . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.8(9) . . ?
C3 C4 H4 120.1 . . ?
C7 C11 H11 121.0 . . ?
C7 C11 C10 117.9(12) . . ?
C10 C11 H11 121.0 . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 118.9(9) . . ?
C3 C2 H2 120.5 . . ?
N1 C10 C11 122.0(12) . . ?
N1 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C7 C8 C9 116.3(11) . . ?
C7 C8 H8 121.8 . . ?
C9 C8 H8 121.8 . . ?
O2 C12 C1 116.0(9) . . ?
O1 C12 O2 123.3(9) . . ?
O1 C12 C1 120.7(10) . . ?
Pb1 O5 Pb1 103.9(4) . 4_675 ?
Pb2 O5 Pb1 105.463(12) 11_556 4_675 ?
Pb2 O5 Pb1 118.625(12) 11_556 . ?
Pb2 O5 Pb1 118.623(12) . 4_675 ?
Pb2 O5 Pb1 105.465(12) . . ?
Pb2 O5 Pb2 105.5(4) 11_556 . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.945
_oxdiff_exptl_absorpt_empirical_full_min 0.430
####################################################################### 
# 
# 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_sq_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc23700d
_database_code_depnum_ccdc_archive 'CCDC 1943142'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C9CE01691K 2020
loop_
_audit_author_name
_audit_author_address
Mn
;SUST
China
;
_audit_update_record             
;
2019-12-02 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_audit_creation_date             2019-12-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H12 Mn3 O19, C4 H12 N'
_chemical_formula_sum            'C33 H24 Mn3 N O19'
_chemical_formula_weight         903.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   34.2808(8)
_cell_length_b                   19.8399(4)
_cell_length_c                   18.1612(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.818(2)
_cell_angle_gamma                90
_cell_volume                     12044.1(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8040
_cell_measurement_theta_min      2.6430
_shelx_estimated_absorpt_T_max   0.610
_shelx_estimated_absorpt_T_min   0.406
_exptl_absorpt_coefficient_mu    5.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.996
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34638
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.996
_diffrn_reflns_theta_min         2.644
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00  33.00   0.50   10.00    --  -43.80  42.00-105.00  180
  2  ω     48.00  73.00   0.50   10.00    --   43.80  42.00-105.00   50
  3  ω    105.00 138.00   0.50   20.00    --  111.75  42.00-105.00   66
  4  ω     88.00 177.00   0.50   20.00    --  111.75  30.00   0.00  178
  5  ω    103.00 135.00   0.50   20.00    --  111.75 -42.00 102.00   64
  6  ω     65.00  95.00   0.50   20.00    --  111.75 -94.00  30.00   60
  7  ω     82.00 115.00   0.50   20.00    --  111.75-125.00 -30.00   66
  8  ω     56.00 135.00   0.50   20.00    --  111.75 -30.00-120.00  158
  9  ω     38.00  78.00   0.50   20.00    --  111.75-125.00 -30.00   80
 10  ω     36.00  98.00   0.50   20.00    --  111.75 -42.00 102.00  124
 11  ω     31.00 152.00   0.50   20.00    --  111.75 -15.00 -30.00  242
 12  ω     60.00 106.00   0.50   10.00    --   43.80 178.00  30.00   92
 13  ω    -88.00 -63.00   0.50   20.00    --  -90.25  42.00-105.00   50
 14  ω    -94.00 -48.00   0.50   20.00    --  -90.25 125.00   0.00   92
 15  ω    -95.00 -41.00   0.50   20.00    --  -90.25 125.00 -90.00  108
 16  ω   -120.00 -27.00   0.50   10.00    --  -43.80 -42.00 102.00  186
 17  ω   -120.00 -80.00   0.50   20.00    --  -90.25 -42.00 102.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0234527000
_diffrn_orient_matrix_UB_12      0.0411461000
_diffrn_orient_matrix_UB_13      0.0477679000
_diffrn_orient_matrix_UB_21      0.0366255000
_diffrn_orient_matrix_UB_22      -0.0010315000
_diffrn_orient_matrix_UB_23      0.0667698000
_diffrn_orient_matrix_UB_31      0.0152121000
_diffrn_orient_matrix_UB_32      0.0658509000
_diffrn_orient_matrix_UB_33      -0.0288002000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9875
_reflns_number_total             12181
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         12181
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0984
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1847P)²+71.3239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3008
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-O15 = C26-O16 = C22-C26
 1.35 with sigma of 0.01
 O15-O16
 2.2 with sigma of 0.01
 C22-O15 = C22-O16
 2.33 with sigma of 0.01
 C32-C33
 1.4 with sigma of 0.01
3. Restrained planarity
 O15, O16, C22, C26
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C33) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(O19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C21(H21), C23(H23),
 C25(H25)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Mn1 Mn 0.74836(2) 0.69894(4) 0.33350(4) 0.0278(2) Uani 1 1 d . . . . .
Mn2 Mn 0.75001(2) 0.63345(4) 0.17014(4) 0.0269(2) Uani 1 1 d . . . . .
Mn3 Mn 0.53144(2) 0.90803(4) 0.33224(4) 0.0314(2) Uani 1 1 d . . . . .
O19 O 0.74962(18) 0.7295(2) 0.4437(2) 0.0611(13) Uani 1 1 d . U . . .
O1 O 0.81227(13) 0.6239(3) 0.2234(2) 0.0564(12) Uani 1 1 d . . . . .
O2 O 0.80843(12) 0.6681(2) 0.3355(2) 0.0502(10) Uani 1 1 d . . . . .
O3 O 0.93182(14) 0.4856(2) 0.2054(2) 0.0535(11) Uani 1 1 d . . . . .
O4 O 0.97890(13) 0.4724(3) 0.3095(3) 0.0614(13) Uani 1 1 d . . . . .
O5 O 0.96212(17) 0.5515(3) 0.5530(3) 0.0759(16) Uani 1 1 d . . . . .
O6 O 0.91970(16) 0.6271(3) 0.5614(3) 0.0721(15) Uani 1 1 d . . . . .
O7 O 0.74372(17) 0.5504(2) 0.2416(2) 0.0590(13) Uani 1 1 d . . . . .
O8 O 0.73687(16) 0.59365(18) 0.3511(3) 0.0530(11) Uani 1 1 d . . . . .
O9 O 0.74241(14) 0.30340(19) 0.2025(2) 0.0457(10) Uani 1 1 d . . . . .
O10 O 0.74283(15) 0.23816(18) 0.2984(3) 0.0525(11) Uani 1 1 d . . . . .
O11 O 0.74348(19) 0.4362(2) 0.5696(2) 0.0629(14) Uani 1 1 d . . . . .
O12 O 0.7525(2) 0.3309(2) 0.5536(2) 0.0723(17) Uani 1 1 d . . . . .
O13 O 0.68874(13) 0.6526(3) 0.1694(3) 0.0660(14) Uani 1 1 d . . . . .
O14 O 0.68674(12) 0.7108(2) 0.2744(3) 0.0530(11) Uani 1 1 d . . . . .
O15 O 0.5627(6) 0.5686(9) 0.0119(11) 0.315(11) Uani 1 1 d D U . . .
O16 O 0.5080(4) 0.6285(10) 0.0069(11) 0.303(10) Uani 1 1 d D U . . .
O17 O 0.50972(12) 0.8270(3) 0.1646(3) 0.0617(13) Uani 1 1 d . . . . .
O18 O 0.55951(13) 0.8401(3) 0.2666(2) 0.0547(11) Uani 1 1 d . . . . .
C1 C 0.82569(17) 0.6348(3) 0.2934(3) 0.0430(13) Uani 1 1 d . . . . .
C2 C 0.86472(15) 0.6035(3) 0.3285(3) 0.0376(12) Uani 1 1 d . . . . .
C3 C 0.88771(16) 0.5693(3) 0.2841(3) 0.0355(11) Uani 1 1 d . . . . .
H3 H 0.8791 0.5680 0.2318 0.043 Uiso 1 1 calc R . . . .
C4 C 0.92371(14) 0.5373(3) 0.3199(3) 0.0375(12) Uani 1 1 d . . . . .
C5 C 0.93775(17) 0.5457(3) 0.3964(3) 0.0473(14) Uani 1 1 d . . . . .
H5 H 0.9619 0.5260 0.4198 0.057 Uiso 1 1 calc R . . . .
C6 C 0.91698(18) 0.5824(3) 0.4388(3) 0.0431(13) Uani 1 1 d . . . . .
C7 C 0.88159(18) 0.6125(3) 0.4047(3) 0.0469(14) Uani 1 1 d . . . . .
H7 H 0.8685 0.6396 0.4333 0.056 Uiso 1 1 calc R . . . .
C8 C 0.94679(16) 0.4965(3) 0.2746(3) 0.0437(13) Uani 1 1 d . . . . .
C9 C 0.9340(2) 0.5885(4) 0.5237(4) 0.0536(17) Uani 1 1 d . . . . .
C10 C 0.7396(2) 0.5459(3) 0.3081(3) 0.0425(13) Uani 1 1 d . . . . .
C11 C 0.73968(19) 0.4755(3) 0.3394(3) 0.0396(12) Uani 1 1 d . . . . .
C12 C 0.73903(19) 0.4203(2) 0.2922(3) 0.0385(12) Uani 1 1 d . . . . .
H12 H 0.7373 0.4271 0.2409 0.046 Uiso 1 1 calc R . . . .
C13 C 0.74096(18) 0.3552(3) 0.3204(3) 0.0374(11) Uani 1 1 d . . . . .
C14 C 0.74319(19) 0.3457(3) 0.3968(3) 0.0422(13) Uani 1 1 d . . . . .
H14 H 0.7448 0.3022 0.4163 0.051 Uiso 1 1 calc R . . . .
C15 C 0.74306(19) 0.4000(3) 0.4446(3) 0.0393(12) Uani 1 1 d . . . . .
C16 C 0.7418(2) 0.4640(3) 0.4156(3) 0.0431(13) Uani 1 1 d . . . . .
H16 H 0.7423 0.5006 0.4477 0.052 Uiso 1 1 calc R . . . .
C17 C 0.74156(17) 0.2956(3) 0.2700(3) 0.0385(12) Uani 1 1 d . . . . .
C18 C 0.74622(19) 0.3891(3) 0.5275(3) 0.0415(13) Uani 1 1 d . . . . .
C19 C 0.67139(18) 0.6852(3) 0.2108(4) 0.0498(14) Uani 1 1 d . . . . .
C20 C 0.62698(19) 0.6958(4) 0.1819(4) 0.0569(18) Uani 1 1 d . . . . .
C21 C 0.6083(3) 0.6551(6) 0.1240(6) 0.096(3) Uani 1 1 d . U . . .
H21 H 0.6230 0.6244 0.1026 0.115 Uiso 1 1 calc R . . . .
C22 C 0.5656(4) 0.6597(7) 0.0962(7) 0.116(4) Uani 1 1 d D U . . .
C23 C 0.5464(4) 0.7175(6) 0.1200(7) 0.098(3) Uani 1 1 d . U . . .
H23 H 0.5200 0.7269 0.0971 0.117 Uiso 1 1 calc R . . . .
C24 C 0.56631(18) 0.7590(4) 0.1757(4) 0.062(2) Uani 1 1 d . . . . .
C25 C 0.60653(17) 0.7464(3) 0.2089(4) 0.0456(13) Uani 1 1 d . . . . .
H25 H 0.6195 0.7725 0.2495 0.055 Uiso 1 1 calc R . . . .
C26 C 0.5455(5) 0.6184(8) 0.0417(9) 0.264(13) Uani 1 1 d D U . . .
C27 C 0.54366(17) 0.8129(4) 0.2056(4) 0.0490(14) Uani 1 1 d . . . . .
N1 N 0.81939(17) 0.5855(3) 0.6209(4) 0.0548(14) Uani 1 1 d . . . . .
C28 C 0.8368(3) 0.5300(4) 0.5838(6) 0.084(3) Uani 1 1 d . . . . .
H28A H 0.8225 0.4890 0.5874 0.126 Uiso 1 1 calc GR . . . .
H28B H 0.8644 0.5241 0.6084 0.126 Uiso 1 1 calc GR . . . .
H28C H 0.8349 0.5409 0.5316 0.126 Uiso 1 1 calc GR . . . .
C29 C 0.7756(2) 0.5913(4) 0.5868(6) 0.083(3) Uani 1 1 d . . . . .
H29A H 0.7716 0.5963 0.5331 0.124 Uiso 1 1 calc GR . . . .
H29B H 0.7650 0.6300 0.6074 0.124 Uiso 1 1 calc GR . . . .
H29C H 0.7622 0.5514 0.5980 0.124 Uiso 1 1 calc GR . . . .
C30 C 0.8253(4) 0.5720(6) 0.7015(6) 0.107(4) Uani 1 1 d . . . . .
H30A H 0.8180 0.5262 0.7089 0.161 Uiso 1 1 calc GR . . . .
H30B H 0.8089 0.6020 0.7231 0.161 Uiso 1 1 calc GR . . . .
H30C H 0.8529 0.5790 0.7255 0.161 Uiso 1 1 calc GR . . . .
C31 C 0.8384(3) 0.6498(5) 0.6124(7) 0.092(3) Uani 1 1 d . . . . .
H31A H 0.8664 0.6472 0.6355 0.139 Uiso 1 1 calc GR . . . .
H31B H 0.8263 0.6847 0.6364 0.139 Uiso 1 1 calc GR . . . .
H31C H 0.8351 0.6600 0.5597 0.139 Uiso 1 1 calc GR . . . .
C32 C 0.7635(4) 0.7609(7) 0.5000(9) 0.111(4) Uani 1 1 d D . . . .
C33 C 0.7993(5) 0.7973(11) 0.4974(13) 0.214(9) Uani 1 1 d D U . . .
H33A H 0.8107 0.7794 0.4578 0.320 Uiso 1 1 calc GR . . . .
H33B H 0.8181 0.7927 0.5449 0.320 Uiso 1 1 calc GR . . . .
H33C H 0.7930 0.8441 0.4878 0.320 Uiso 1 1 calc GR . . . .


_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
Mn1 O19 2.083(4) . ?
Mn1 O2 2.141(4) . ?
Mn1 O8 2.163(4) . ?
Mn1 O9 2.217(4) 4_655 ?
Mn1 O14 2.160(4) . ?
Mn2 O1 2.147(4) . ?
Mn2 O7 2.138(4) . ?
Mn2 O10 2.154(4) 4_655 ?
Mn2 O11 2.262(4) 6_565 ?
Mn2 O12 2.251(4) 6_565 ?
Mn2 O13 2.132(4) . ?
Mn2 C18 2.604(5) 6_565 ?
Mn3 O3 2.191(4) 4_655 ?
Mn3 O4 2.172(4) 3_455 ?
Mn3 O5 2.198(5) 7_666 ?
Mn3 O6 2.363(5) 7_666 ?
Mn3 O17 2.148(4) 2_655 ?
Mn3 O18 2.161(4) . ?
Mn3 C9 2.622(7) 7_666 ?
O19 C32 1.201(17) . ?
O19 C32 1.218(16) 7_666 ?
O1 C1 1.271(7) . ?
O2 C1 1.255(7) . ?
O3 Mn3 2.191(4) 4_645 ?
O3 C8 1.267(7) . ?
O4 Mn3 2.172(4) 3_545 ?
O4 C8 1.238(7) . ?
O5 Mn3 2.198(5) 7_666 ?
O5 C9 1.235(9) . ?
O6 Mn3 2.363(5) 7_666 ?
O6 C9 1.201(8) . ?
O7 C10 1.250(7) . ?
O8 C10 1.244(7) . ?
O9 Mn1 2.217(4) 4_645 ?
O9 C17 1.242(7) . ?
O10 Mn2 2.154(4) 4_645 ?
O10 C17 1.247(6) . ?
O11 Mn2 2.262(4) 6_566 ?
O11 C18 1.224(7) . ?
O12 Mn2 2.251(4) 6_566 ?
O12 C18 1.251(7) . ?
O13 C19 1.239(8) . ?
O14 C19 1.264(8) . ?
O15 C26 1.326(9) . ?
O16 C26 1.319(9) . ?
O17 Mn3 2.148(4) 2_655 ?
O17 C27 1.266(7) . ?
O18 C27 1.243(7) . ?
C1 C2 1.485(7) . ?
C2 C3 1.418(7) . ?
C2 C7 1.388(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.411(7) . ?
C4 C5 1.376(7) . ?
C4 C8 1.499(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.368(8) . ?
C6 C7 1.370(8) . ?
C6 C9 1.528(8) . ?
C7 H7 0.9300 . ?
C9 Mn3 2.622(7) 7_666 ?
C10 C11 1.507(7) . ?
C11 C12 1.389(7) . ?
C11 C16 1.388(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.387(7) . ?
C13 C14 1.385(7) . ?
C13 C17 1.499(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.384(8) . ?
C15 C16 1.372(7) . ?
C15 C18 1.501(7) . ?
C16 H16 0.9300 . ?
C18 Mn2 2.604(5) 6_566 ?
C19 C20 1.511(8) . ?
C20 C21 1.368(12) . ?
C20 C25 1.376(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.440(15) . ?
C22 C23 1.435(16) . ?
C22 C26 1.350(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.362(13) . ?
C24 C25 1.399(8) . ?
C24 C27 1.494(8) . ?
C25 H25 0.9300 . ?
N1 C28 1.485(9) . ?
N1 C29 1.496(10) . ?
N1 C30 1.458(12) . ?
N1 C31 1.456(10) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 O19 1.218(16) 7_666 ?
C32 C32 1.02(2) 7_666 ?
C32 C33 1.433(9) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

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
O19 Mn1 O2 104.6(2) . . ?
O19 Mn1 O8 96.03(19) . . ?
O19 Mn1 O9 92.13(17) . 4_655 ?
O19 Mn1 O14 104.8(2) . . ?
O2 Mn1 O8 85.84(19) . . ?
O2 Mn1 O9 94.15(18) . 4_655 ?
O2 Mn1 O14 150.55(17) . . ?
O8 Mn1 O9 171.57(17) . 4_655 ?
O14 Mn1 O8 89.3(2) . . ?
O14 Mn1 O9 86.53(18) . 4_655 ?
O1 Mn2 O10 85.5(2) . 4_655 ?
O1 Mn2 O11 102.7(2) . 6_565 ?
O1 Mn2 O12 102.1(2) . 6_565 ?
O1 Mn2 C18 104.95(18) . 6_565 ?
O7 Mn2 O1 83.3(2) . . ?
O7 Mn2 O10 127.12(17) . 4_655 ?
O7 Mn2 O11 90.76(16) . 6_565 ?
O7 Mn2 O12 147.46(16) . 6_565 ?
O7 Mn2 C18 118.78(18) . 6_565 ?
O10 Mn2 O11 142.07(17) 4_655 6_565 ?
O10 Mn2 O12 85.42(17) 4_655 6_565 ?
O10 Mn2 C18 114.05(18) 4_655 6_565 ?
O11 Mn2 C18 28.03(17) 6_565 6_565 ?
O12 Mn2 O11 56.70(16) 6_565 6_565 ?
O12 Mn2 C18 28.69(17) 6_565 6_565 ?
O13 Mn2 O1 153.9(2) . . ?
O13 Mn2 O7 84.8(2) . . ?
O13 Mn2 O10 83.3(2) . 4_655 ?
O13 Mn2 O11 100.6(2) . 6_565 ?
O13 Mn2 O12 100.5(2) . 6_565 ?
O13 Mn2 C18 101.1(2) . 6_565 ?
O3 Mn3 O5 95.5(2) 4_655 7_666 ?
O3 Mn3 O6 96.3(2) 4_655 7_666 ?
O3 Mn3 C9 97.41(19) 4_655 7_666 ?
O4 Mn3 O3 92.1(2) 3_455 4_655 ?
O4 Mn3 O5 82.53(19) 3_455 7_666 ?
O4 Mn3 O6 137.42(17) 3_455 7_666 ?
O4 Mn3 C9 110.3(2) 3_455 7_666 ?
O5 Mn3 O6 55.18(19) 7_666 7_666 ?
O5 Mn3 C9 27.9(2) 7_666 7_666 ?
O6 Mn3 C9 27.3(2) 7_666 7_666 ?
O17 Mn3 O3 163.76(18) 2_655 4_655 ?
O17 Mn3 O4 85.6(2) 2_655 3_455 ?
O17 Mn3 O5 100.2(2) 2_655 7_666 ?
O17 Mn3 O6 96.2(2) 2_655 7_666 ?
O17 Mn3 O18 85.6(2) 2_655 . ?
O17 Mn3 C9 98.5(2) 2_655 7_666 ?
O18 Mn3 O3 84.8(2) . 4_655 ?
O18 Mn3 O4 135.54(17) . 3_455 ?
O18 Mn3 O5 141.92(19) . 7_666 ?
O18 Mn3 O6 86.87(17) . 7_666 ?
O18 Mn3 C9 114.1(2) . 7_666 ?
C32 O19 Mn1 156.7(8) 7_666 . ?
C32 O19 Mn1 152.7(7) . . ?
C32 O19 C32 49.9(10) . 7_666 ?
C1 O1 Mn2 122.6(4) . . ?
C1 O2 Mn1 136.2(4) . . ?
C8 O3 Mn3 107.2(4) . 4_645 ?
C8 O4 Mn3 158.5(5) . 3_545 ?
C9 O5 Mn3 95.5(4) . 7_666 ?
C9 O6 Mn3 88.5(4) . 7_666 ?
C10 O7 Mn2 133.6(4) . . ?
C10 O8 Mn1 127.0(4) . . ?
C17 O9 Mn1 102.1(3) . 4_645 ?
C17 O10 Mn2 169.1(4) . 4_645 ?
C18 O11 Mn2 91.7(3) . 6_566 ?
C18 O12 Mn2 91.5(4) . 6_566 ?
C19 O13 Mn2 134.0(5) . . ?
C19 O14 Mn1 125.0(4) . . ?
C27 O17 Mn3 132.3(4) . 2_655 ?
C27 O18 Mn3 127.0(4) . . ?
O1 C1 C2 116.8(5) . . ?
O2 C1 O1 125.8(5) . . ?
O2 C1 C2 117.4(5) . . ?
C3 C2 C1 121.1(5) . . ?
C7 C2 C1 120.8(5) . . ?
C7 C2 C3 117.8(5) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C8 120.3(5) . . ?
C5 C4 C3 118.9(5) . . ?
C5 C4 C8 120.7(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.6(5) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C7 119.7(5) . . ?
C5 C6 C9 118.8(5) . . ?
C7 C6 C9 121.5(6) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 C2 121.8(5) . . ?
C6 C7 H7 119.1 . . ?
O3 C8 C4 119.4(5) . . ?
O4 C8 O3 124.1(5) . . ?
O4 C8 C4 116.4(5) . . ?
O5 C9 Mn3 56.5(3) . 7_666 ?
O5 C9 C6 118.3(6) . . ?
O6 C9 Mn3 64.3(4) . 7_666 ?
O6 C9 O5 120.7(6) . . ?
O6 C9 C6 120.9(6) . . ?
C6 C9 Mn3 174.8(5) . 7_666 ?
O7 C10 C11 116.1(5) . . ?
O8 C10 O7 126.3(5) . . ?
O8 C10 C11 117.5(5) . . ?
C12 C11 C10 119.9(5) . . ?
C16 C11 C10 121.6(5) . . ?
C16 C11 C12 118.4(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 120.9(5) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C17 121.0(5) . . ?
C14 C13 C12 118.9(5) . . ?
C14 C13 C17 120.0(5) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.1(5) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C18 120.5(5) . . ?
C16 C15 C14 118.9(5) . . ?
C16 C15 C18 120.5(5) . . ?
C11 C16 H16 119.2 . . ?
C15 C16 C11 121.7(5) . . ?
C15 C16 H16 119.2 . . ?
O9 C17 O10 121.1(5) . . ?
O9 C17 C13 120.7(5) . . ?
O10 C17 C13 118.1(5) . . ?
O11 C18 Mn2 60.3(3) . 6_566 ?
O11 C18 O12 120.0(5) . . ?
O11 C18 C15 121.2(5) . . ?
O12 C18 Mn2 59.8(3) . 6_566 ?
O12 C18 C15 118.8(5) . . ?
C15 C18 Mn2 178.0(4) . 6_566 ?
O13 C19 O14 127.2(6) . . ?
O13 C19 C20 116.3(6) . . ?
O14 C19 C20 116.4(5) . . ?
C21 C20 C19 116.7(7) . . ?
C21 C20 C25 121.0(7) . . ?
C25 C20 C19 122.1(6) . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.9(10) . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 116.3(10) . . ?
C26 C22 C21 122.1(11) . . ?
C26 C22 C23 120.9(11) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.3(10) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 119.6(7) . . ?
C23 C24 C27 119.2(7) . . ?
C25 C24 C27 120.9(6) . . ?
C20 C25 C24 120.5(6) . . ?
C20 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
O15 C26 C22 123.4(10) . . ?
O16 C26 O15 113.1(9) . . ?
O16 C26 C22 123.0(10) . . ?
O17 C27 C24 115.3(6) . . ?
O18 C27 O17 126.2(6) . . ?
O18 C27 C24 118.4(5) . . ?
C28 N1 C29 109.7(6) . . ?
C30 N1 C28 109.8(7) . . ?
C30 N1 C29 109.4(8) . . ?
C31 N1 C28 111.6(7) . . ?
C31 N1 C29 108.7(7) . . ?
C31 N1 C30 107.6(8) . . ?
N1 C28 H28A 109.5 . . ?
N1 C28 H28B 109.5 . . ?
N1 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 C29 H29A 109.5 . . ?
N1 C29 H29B 109.5 . . ?
N1 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N1 C30 H30A 109.5 . . ?
N1 C30 H30B 109.5 . . ?
N1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C31 H31A 109.5 . . ?
N1 C31 H31B 109.5 . . ?
N1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O19 C32 O19 130.1(10) . 7_666 ?
O19 C32 C33 114.4(15) . . ?
O19 C32 C33 115.3(16) 7_666 . ?
C32 C32 O19 65.9(18) 7_666 . ?
C32 C32 O19 64.2(16) 7_666 7_666 ?
C32 C32 C33 175(2) 7_666 . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.853
