# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_f2-br
_database_code_depnum_ccdc_archive 'CCDC 2415233'
loop_
_audit_author_name
_audit_author_address
'zheng chunyang'
;Hubei Normal University
China
;
_audit_update_record             
;
2025-01-07 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_audit_creation_date             2024-09-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C21 H20 Br2 O4)'
_chemical_formula_sum            'C21 H20 Br2 O4'
_chemical_formula_weight         496.19
_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'
Br Br -0.6763 1.2805 '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           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                   26.8681(4)
_cell_length_b                   9.3502(2)
_cell_length_c                   33.4362(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.6710(10)
_cell_angle_gamma                90
_cell_volume                     8343.0(3)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    13165
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.2160
_cell_measurement_theta_min      3.7730
_shelx_estimated_absorpt_T_max   0.628
_shelx_estimated_absorpt_T_min   0.514
_exptl_absorpt_coefficient_mu    5.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            21059
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.307
_diffrn_reflns_theta_min         4.002
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  21.00   0.50    0.34    --  -41.86  32.00 -30.00  148
  2  ω    -51.00  -2.00   0.50    0.34    --  -41.86  33.00 -97.00   98
  3  ω    -63.00 -32.00   0.50    1.38    --  -94.76 117.00-150.00   62
  4  ω    -54.00 -26.00   0.50    0.34    --  -41.86 138.00-120.00   56
  5  ω    -94.00 -63.00   0.50    0.34    --  -41.86 138.00-120.00   62
  6  ω   -108.00 -76.00   0.50    1.38    --  -94.76  33.00 -97.00   64
  7  ω   -125.00-100.00   0.50    1.38    --  -94.76 -33.00-120.00   50
  8  ω   -154.00 -75.00   0.50    1.38    --  -94.76-117.00-180.00  158
  9  ω   -160.00-130.00   0.50    1.38    --  -94.76 -33.00-120.00   60
 10  ω     25.00  78.00   0.50    0.34    --   43.42  77.00   0.00  106
 11  ω     83.00 109.00   0.50    0.34    --   43.42  77.00   0.00   52
 12  ω     26.00 111.00   0.50    1.38    --   96.32 -25.00 -30.00  170
 13  ω     64.00  97.00   0.50    1.38    --   96.32 -33.00 -60.00   66
 14  ω     83.00 141.00   0.50    1.38    --   96.32  33.00 -97.00  116
 15  ω     41.00 108.00   0.50    1.38    --   96.32-117.00   0.00  134
 16  ω     64.00  89.00   0.50    1.38    --   96.32-117.00  30.00   50
 17  ω     33.00 107.00   0.50    1.38    --   96.32 -33.00 104.00  148
 18  ω     82.00 113.00   0.50    1.38    --   96.32-117.00 150.00   62
 19  ω     43.00  69.00   0.50    1.38    --   96.32-117.00 150.00   52
 20  ω     29.00 117.00   0.50    1.38    --   96.32 -59.00 120.00  176
 21  ω      3.00  29.00   0.50    0.34    --   43.42 -33.00 104.00   52
 22  ω    -23.00  25.00   0.50    0.34    --  -41.86  43.00 150.00   96
 23  ω    -63.00 -27.00   0.50    0.34    --  -41.86 -77.00  60.00   72
 24  ω    -55.00 -29.00   0.50    0.34    --  -41.86 -33.00 104.00   52
 25  ω     33.00  59.00   0.50    0.34    --   43.42  33.00 -97.00   52
 26  ω     27.00 109.00   0.50    1.38    --   96.32 -17.00-120.00  164
 27  ω   -108.00 -83.00   0.50    0.34    --  -41.86 -77.00  60.00   50
 28  ω   -146.00 -94.00   0.50    1.38    --  -94.76 -33.00 104.00  104
 29  ω    -79.00 -54.00   0.50    0.34    --  -41.86 -32.00 150.00   50
 30  ω   -115.00 -31.00   0.50    1.38    --  -94.76  59.00  90.00  168
 31  ω     84.00 109.00   0.50    0.34    --   43.42 138.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0510340000
_diffrn_orient_matrix_UB_12      0.0708375000
_diffrn_orient_matrix_UB_13      -0.0132751000
_diffrn_orient_matrix_UB_21      -0.0112705000
_diffrn_orient_matrix_UB_22      0.0032715000
_diffrn_orient_matrix_UB_23      0.0441395000
_diffrn_orient_matrix_UB_31      0.0245601000
_diffrn_orient_matrix_UB_32      0.1486120000
_diffrn_orient_matrix_UB_33      0.0053553000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_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                6598
_reflns_number_total             7479
_reflns_odcompleteness_completeness 99.40
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7479
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0550
_refine_ls_restrained_S_all      1.057
_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)+(0.0745P)²+16.0457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1539
_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. Rigid bond restraints
 C12A, C13A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C11A) \\sim Ueq,
Uanis(C10A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(Br2A)=Sof(Br1A)=Sof(Br3A)=Sof(Br4A)=Sof(C12A)=Sof(C11A)=Sof(H11A)=
 Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(C8A)=Sof(C13A)=Sof(H13A)=Sof(O1A\)=1-FVAR(1)
 Sof(Br1)=Sof(Br2)=Sof(Br3)=Sof(Br4)=Sof(C12)=Sof(C11)=Sof(H11)=Sof(C10)=
 Sof(H10)=Sof(C9)=Sof(C8)=Sof(C13)=Sof(H13)=Sof(O1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B), C35(H35A,
 H35B), C36(H36A,H36B), C39(H39A,H39B), C40(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C11(H11), C10(H10), C13(H13), C23(H23), C25(H25),
 C26(H26), C31(H31), C32(H32), C34(H34), C11A(H11A), C10A(H10A), C13A(H13A)
5.c Fitted hexagon refined as free rotating group:
 C12A(C11A,C10A,C9A,C8A,C13A)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C38(H38A,H38B,H38C), C42(H42A,H42B,
 H42C)
;
_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
Br1 Br 0.54749(11) 0.6649(2) 0.93874(9) 0.0770(6) Uani 0.556(10) 1 d . . P A 1
Br2 Br 0.19960(9) 0.3320(4) 0.78999(5) 0.0903(7) Uani 0.556(10) 1 d . . P A 5
Br3 Br 0.20434(15) 0.8996(4) 0.78491(9) 0.0977(7) Uani 0.556(10) 1 d . . P A 3
Br4 Br 0.0559(3) 0.5313(6) 1.04440(14) 0.0752(9) Uani 0.556(10) 1 d . . P A .
C1 C 0.41056(14) 0.5790(4) 0.87022(9) 0.0521(8) Uani 1 1 d . . . . .
C2 C 0.45289(13) 0.6468(4) 0.88801(10) 0.0527(7) Uani 1 1 d . . . . .
H2 H 0.459225 0.741759 0.882097 0.063 Uiso 1 1 calc R U . . .
C3 C 0.48587(15) 0.5706(4) 0.91490(12) 0.0644(9) Uani 1 1 d . . . . .
C4 C 0.47739(19) 0.4301(5) 0.92501(16) 0.0803(12) Uani 1 1 d . . . . .
H4 H 0.499557 0.382716 0.943968 0.096 Uiso 1 1 calc R U . . .
C5 C 0.4353(2) 0.3611(4) 0.90641(16) 0.0801(13) Uani 1 1 d . . . . .
H5 H 0.429465 0.265654 0.912139 0.096 Uiso 1 1 calc R U . . .
C6 C 0.40201(16) 0.4349(4) 0.87931(12) 0.0635(10) Uani 1 1 d . . . . .
C7 C 0.36795(13) 0.6404(4) 0.84124(10) 0.0540(8) Uani 1 1 d . . . . .
C12 C 0.2648(4) 0.3524(13) 0.8170(3) 0.053(2) Uani 0.556(10) 1 d . U P A 5
C11 C 0.2884(4) 0.2351(12) 0.8377(4) 0.066(3) Uani 0.556(10) 1 d . U P A 5
H11 H 0.272276 0.146988 0.836358 0.079 Uiso 0.556(10) 1 calc R U P A 5
C10 C 0.3341(4) 0.2467(11) 0.8597(4) 0.067(2) Uani 0.556(10) 1 d . U P A 5
H10 H 0.348682 0.169819 0.874258 0.080 Uiso 0.556(10) 1 calc R U P A 5
C9 C 0.3582(5) 0.3796(14) 0.8594(5) 0.054(2) Uani 0.556(10) 1 d . U P A 5
C8 C 0.3363(4) 0.4931(14) 0.8366(4) 0.044(2) Uani 0.556(10) 1 d . U P A 5
C13 C 0.2897(4) 0.4809(12) 0.8153(4) 0.057(2) Uani 0.556(10) 1 d . U P A 5
H13 H 0.275244 0.556890 0.800236 0.069 Uiso 0.556(10) 1 calc R U P A 5
C14 C 0.38605(14) 0.6921(5) 0.80115(10) 0.0608(9) Uani 1 1 d . . . . .
H14A H 0.357663 0.732095 0.784244 0.073 Uiso 1 1 calc R U . . .
H14B H 0.410290 0.768220 0.807172 0.073 Uiso 1 1 calc R U . . .
C15 C 0.40953(18) 0.5773(6) 0.77765(13) 0.0783(12) Uani 1 1 d . . . . .
H15A H 0.386058 0.499038 0.771990 0.094 Uiso 1 1 calc R U . . .
H15B H 0.439217 0.540108 0.793548 0.094 Uiso 1 1 calc R U . . .
C16 C 0.42368(18) 0.6382(7) 0.73831(14) 0.0796(14) Uani 1 1 d . . . . .
C17 C 0.4516(3) 0.5764(10) 0.67633(17) 0.139(3) Uani 1 1 d . . . . .
H17A H 0.423170 0.619168 0.660756 0.208 Uiso 1 1 calc R U . . .
H17B H 0.462215 0.494108 0.662379 0.208 Uiso 1 1 calc R U . . .
H17C H 0.478458 0.644455 0.680098 0.208 Uiso 1 1 calc R U . . .
C18 C 0.34313(13) 0.7708(4) 0.85952(10) 0.0583(8) Uani 1 1 d . . . . .
H18A H 0.368569 0.842066 0.867523 0.070 Uiso 1 1 calc R U . . .
H18B H 0.318946 0.813104 0.839118 0.070 Uiso 1 1 calc R U . . .
C19 C 0.31676(16) 0.7302(5) 0.89598(12) 0.0677(10) Uani 1 1 d . . . . .
H19A H 0.287242 0.674056 0.886903 0.081 Uiso 1 1 calc R U . . .
H19B H 0.339014 0.670566 0.913793 0.081 Uiso 1 1 calc R U . . .
C20 C 0.30139(14) 0.8557(5) 0.91907(11) 0.0610(9) Uani 1 1 d . . . . .
C21 C 0.2638(2) 0.9264(6) 0.97616(15) 0.0910(15) Uani 1 1 d . . . . .
H21A H 0.250231 1.006138 0.960403 0.136 Uiso 1 1 calc R U . . .
H21B H 0.293005 0.956313 0.993356 0.136 Uiso 1 1 calc R U . . .
H21C H 0.239106 0.891183 0.992320 0.136 Uiso 1 1 calc R U . . .
C22 C 0.13824(14) 0.7031(5) 0.87720(11) 0.0665(10) Uani 1 1 d . . . . .
C23 C 0.15597(15) 0.7205(6) 0.84007(12) 0.0794(13) Uani 1 1 d . . . . .
H23 H 0.154029 0.647689 0.821010 0.095 Uiso 1 1 calc R U . . .
C24 C 0.17711(17) 0.8551(8) 0.83291(16) 0.0908(17) Uani 1 1 d . . . . .
C25 C 0.17867(19) 0.9651(7) 0.8596(2) 0.101(2) Uani 1 1 d . . . . .
H25 H 0.192145 1.052672 0.853196 0.121 Uiso 1 1 calc R U . . .
C26 C 0.16042(17) 0.9475(6) 0.89599(15) 0.0797(12) Uani 1 1 d . . . . .
H26 H 0.161501 1.022104 0.914463 0.096 Uiso 1 1 calc R U . . .
C27 C 0.14037(14) 0.8162(4) 0.90455(11) 0.0606(9) Uani 1 1 d . . . . .
C28 C 0.11511(14) 0.5690(5) 0.89344(10) 0.0596(9) Uani 1 1 d . . . . .
C29 C 0.10590(12) 0.6238(4) 0.93516(10) 0.0522(8) Uani 1 1 d . . . . .
C30 C 0.12025(12) 0.7654(4) 0.94090(11) 0.0555(8) Uani 1 1 d . . . . .
C31 C 0.11533(15) 0.8349(4) 0.97726(12) 0.0635(9) Uani 1 1 d . . . . .
H31 H 0.125534 0.929382 0.981223 0.076 Uiso 1 1 calc R U . . .
C32 C 0.09503(14) 0.7606(5) 1.00717(11) 0.0622(9) Uani 1 1 d . . . . .
H32 H 0.090631 0.805589 1.031319 0.075 Uiso 1 1 calc R U . . .
C33 C 0.08147(13) 0.6212(4) 1.00114(10) 0.0577(8) Uani 1 1 d . . . . .
C34 C 0.08632(14) 0.5492(4) 0.96552(11) 0.0576(8) Uani 1 1 d . . . . .
H34 H 0.076735 0.453956 0.962148 0.069 Uiso 1 1 calc R U . . .
C35 C 0.06664(15) 0.5218(5) 0.86846(12) 0.0670(10) Uani 1 1 d . . . . .
H35A H 0.074632 0.487310 0.842610 0.080 Uiso 1 1 calc R U . . .
H35B H 0.052490 0.442548 0.882056 0.080 Uiso 1 1 calc R U . . .
C36 C 0.02746(18) 0.6382(6) 0.86130(19) 0.0922(15) Uani 1 1 d . . . . .
H36A H 0.019088 0.672590 0.887060 0.111 Uiso 1 1 calc R U . . .
H36B H 0.041346 0.717664 0.847616 0.111 Uiso 1 1 calc R U . . .
C37 C -0.01916(18) 0.5878(6) 0.83676(14) 0.0777(12) Uani 1 1 d . . . . .
C38 C -0.0740(4) 0.6252(10) 0.7760(2) 0.164(4) Uani 1 1 d . . . . .
H38A H -0.083966 0.705272 0.758996 0.245 Uiso 1 1 calc R U . . .
H38B H -0.101254 0.597725 0.790600 0.245 Uiso 1 1 calc R U . . .
H38C H -0.065236 0.546396 0.759818 0.245 Uiso 1 1 calc R U . . .
C39 C 0.15181(15) 0.4420(5) 0.89666(12) 0.0675(10) Uani 1 1 d . . . . .
H39A H 0.139553 0.369385 0.913768 0.081 Uiso 1 1 calc R U . . .
H39B H 0.152474 0.400719 0.870119 0.081 Uiso 1 1 calc R U . . .
C40 C 0.20536(16) 0.4829(5) 0.91372(14) 0.0739(11) Uani 1 1 d . . . . .
H40A H 0.222318 0.521546 0.892033 0.089 Uiso 1 1 calc R U . . .
H40B H 0.203637 0.558244 0.933436 0.089 Uiso 1 1 calc R U . . .
C41 C 0.23590(16) 0.3649(5) 0.93284(12) 0.0679(10) Uani 1 1 d . . . . .
C42 C 0.31748(18) 0.3029(6) 0.96307(17) 0.0909(14) Uani 1 1 d . . . . .
H42A H 0.313281 0.212716 0.949389 0.136 Uiso 1 1 calc R U . . .
H42B H 0.310711 0.291689 0.990456 0.136 Uiso 1 1 calc R U . . .
H42C H 0.351272 0.335788 0.962649 0.136 Uiso 1 1 calc R U . . .
O1 O 0.4166(5) 0.765(2) 0.7258(5) 0.096(4) Uani 0.556(10) 1 d . . P A 7
O2 O 0.43775(18) 0.5328(5) 0.71545(11) 0.1175(14) Uani 1 1 d . . . . .
O3 O 0.30999(16) 0.9768(4) 0.91255(13) 0.1033(12) Uani 1 1 d . . . . .
O4 O 0.27722(12) 0.8138(3) 0.94960(8) 0.0753(8) Uani 1 1 d . . . . .
O5 O 0.22099(14) 0.2488(4) 0.93921(15) 0.1051(12) Uani 1 1 d . . . . .
O6 O 0.28293(12) 0.4069(4) 0.94293(10) 0.0803(8) Uani 1 1 d . . . . .
O7 O -0.04380(17) 0.4910(5) 0.84464(15) 0.1298(18) Uani 1 1 d . . . . .
O8 O -0.03004(19) 0.6655(5) 0.80494(16) 0.1262(16) Uani 1 1 d . . . . .
Br2A Br 0.18989(17) 0.4060(12) 0.7786(3) 0.146(3) Uani 0.444(10) 1 d . . P A 6
Br1A Br 0.5378(2) 0.6468(6) 0.94269(17) 0.1259(17) Uani 0.444(10) 1 d . . P A 2
Br3A Br 0.20216(18) 0.8382(11) 0.7786(2) 0.131(2) Uani 0.444(10) 1 d . . P A 4
Br4A Br 0.0560(3) 0.5078(8) 1.04265(17) 0.0822(13) Uani 0.444(10) 1 d . . P A 4
C12A C 0.2539(4) 0.4108(14) 0.8079(4) 0.078(4) Uani 0.444(10) 1 d G U P A 6
C11A C 0.2724(5) 0.2882(12) 0.8279(4) 0.073(5) Uani 0.444(10) 1 d G U P A 6
H11A H 0.253538 0.204674 0.826206 0.087 Uiso 0.444(10) 1 calc R U P A 6
C10A C 0.3192(5) 0.2906(11) 0.8505(4) 0.087(4) Uani 0.444(10) 1 d G U P A 6
H10A H 0.331661 0.208538 0.863919 0.104 Uiso 0.444(10) 1 calc R U P A 6
C9A C 0.3475(4) 0.4155(13) 0.8531(4) 0.064(5) Uani 0.444(10) 1 d G U P A 6
C8A C 0.3289(4) 0.5381(11) 0.8331(5) 0.051(4) Uani 0.444(10) 1 d G U P A 6
C13A C 0.2821(4) 0.5357(12) 0.8106(4) 0.065(4) Uani 0.444(10) 1 d G U P A 6
H13A H 0.269702 0.617759 0.797172 0.078 Uiso 0.444(10) 1 calc R U P A 6
O1A\ O 0.4369(10) 0.743(3) 0.7342(7) 0.165(10) Uani 0.444(10) 1 d . . P A 8


_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
Br1 C3 1.962(5) . ?
Br2 C12 1.886(10) . ?
Br3 C24 1.886(5) . ?
Br4 C33 1.872(6) . ?
C1 C2 1.376(5) . ?
C1 C6 1.406(5) . ?
C1 C7 1.524(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.384(5) . ?
C3 C4 1.382(6) . ?
C3 Br1A 1.737(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.385(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.381(7) . ?
C6 C9 1.383(13) . ?
C6 C9A 1.627(11) . ?
C7 C8 1.617(11) . ?
C7 C14 1.555(4) . ?
C7 C18 1.549(5) . ?
C7 C8A 1.422(8) . ?
C12 C11 1.408(14) . ?
C12 C13 1.379(14) . ?
C11 H11 0.9300 . ?
C11 C10 1.358(14) . ?
C10 H10 0.9300 . ?
C10 C9 1.403(13) . ?
C9 C8 1.396(14) . ?
C8 C13 1.371(12) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.511(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.522(6) . ?
C16 O1 1.26(2) . ?
C16 O2 1.329(7) . ?
C16 O1A\ 1.06(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 O2 1.459(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.527(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.489(6) . ?
C20 O3 1.181(5) . ?
C20 O4 1.331(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 O4 1.450(5) . ?
C22 C23 1.390(5) . ?
C22 C27 1.395(6) . ?
C22 C28 1.526(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.412(8) . ?
C24 C25 1.359(9) . ?
C24 Br3A 2.016(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.374(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.384(6) . ?
C27 C30 1.466(5) . ?
C28 C29 1.533(5) . ?
C28 C35 1.528(5) . ?
C28 C39 1.539(6) . ?
C29 C30 1.386(5) . ?
C29 C34 1.385(5) . ?
C30 C31 1.398(5) . ?
C31 H31 0.9300 . ?
C31 C32 1.381(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.362(6) . ?
C33 C34 1.388(5) . ?
C33 Br4A 1.934(7) . ?
C34 H34 0.9300 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.513(7) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.492(7) . ?
C37 O7 1.170(6) . ?
C37 O8 1.294(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C38 O8 1.486(8) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.533(6) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.475(6) . ?
C41 O5 1.185(6) . ?
C41 O6 1.329(5) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C42 O6 1.454(6) . ?
Br2A C12A 1.879(9) . ?
C12A C11A 1.3900 . ?
C12A C13A 1.3900 . ?
C11A H11A 0.9300 . ?
C11A C10A 1.3900 . ?
C10A H10A 0.9300 . ?
C10A C9A 1.3900 . ?
C9A C8A 1.3900 . ?
C8A C13A 1.3900 . ?
C13A H13A 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 119.7(4) . . ?
C2 C1 C7 128.6(3) . . ?
C6 C1 C7 111.7(3) . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.6(3) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 Br1 118.6(3) . . ?
C2 C3 Br1A 123.4(4) . . ?
C4 C3 Br1 118.9(4) . . ?
C4 C3 C2 122.5(4) . . ?
C4 C3 Br1A 113.8(4) . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C9A 98.6(5) . . ?
C5 C6 C1 120.7(4) . . ?
C5 C6 C9 125.4(7) . . ?
C5 C6 C9A 140.5(6) . . ?
C9 C6 C1 113.9(7) . . ?
C1 C7 C8 95.0(5) . . ?
C1 C7 C14 112.2(3) . . ?
C1 C7 C18 111.8(3) . . ?
C14 C7 C8 113.3(5) . . ?
C18 C7 C8 117.5(5) . . ?
C18 C7 C14 106.7(3) . . ?
C8A C7 C1 110.5(6) . . ?
C8A C7 C14 110.0(7) . . ?
C8A C7 C18 105.2(6) . . ?
C11 C12 Br2 119.8(9) . . ?
C13 C12 Br2 119.7(8) . . ?
C13 C12 C11 120.4(9) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 C12 122.0(10) . . ?
C10 C11 H11 119.0 . . ?
C11 C10 H10 121.4 . . ?
C11 C10 C9 117.2(10) . . ?
C9 C10 H10 121.4 . . ?
C6 C9 C10 134.1(11) . . ?
C6 C9 C8 105.1(9) . . ?
C8 C9 C10 120.7(10) . . ?
C9 C8 C7 114.3(8) . . ?
C13 C8 C7 124.0(10) . . ?
C13 C8 C9 121.5(9) . . ?
C12 C13 H13 121.0 . . ?
C8 C13 C12 118.0(10) . . ?
C8 C13 H13 121.0 . . ?
C7 C14 H14A 108.6 . . ?
C7 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 C7 114.8(4) . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C14 C15 H15A 109.6 . . ?
C14 C15 H15B 109.6 . . ?
C14 C15 C16 110.2(4) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
O1 C16 C15 126.5(8) . . ?
O1 C16 O2 123.1(9) . . ?
O2 C16 C15 109.6(5) . . ?
O1A\ C16 C15 125.5(13) . . ?
O1A\ C16 O2 119.4(13) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
C7 C18 H18A 109.1 . . ?
C7 C18 H18B 109.1 . . ?
H18A C18 H18B 107.9 . . ?
C19 C18 C7 112.4(3) . . ?
C19 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.6(4) . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
O3 C20 C19 126.0(4) . . ?
O3 C20 O4 123.2(4) . . ?
O4 C20 C19 110.8(4) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
C23 C22 C27 120.3(4) . . ?
C23 C22 C28 127.6(4) . . ?
C27 C22 C28 112.1(3) . . ?
C22 C23 H23 121.9 . . ?
C22 C23 C24 116.2(5) . . ?
C24 C23 H23 121.9 . . ?
C23 C24 Br3 123.0(5) . . ?
C23 C24 Br3A 105.4(5) . . ?
C25 C24 Br3 114.0(4) . . ?
C25 C24 C23 123.1(4) . . ?
C25 C24 Br3A 131.5(5) . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.2(5) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.7 . . ?
C25 C26 C27 118.5(6) . . ?
C27 C26 H26 120.7 . . ?
C22 C27 C30 107.9(3) . . ?
C26 C27 C22 121.6(4) . . ?
C26 C27 C30 130.5(4) . . ?
C22 C28 C29 99.5(3) . . ?
C22 C28 C35 113.5(3) . . ?
C22 C28 C39 112.0(3) . . ?
C29 C28 C39 111.3(3) . . ?
C35 C28 C29 112.1(3) . . ?
C35 C28 C39 108.3(3) . . ?
C30 C29 C28 111.9(3) . . ?
C34 C29 C28 127.9(3) . . ?
C34 C29 C30 120.2(3) . . ?
C29 C30 C27 108.5(3) . . ?
C29 C30 C31 120.8(3) . . ?
C31 C30 C27 130.7(4) . . ?
C30 C31 H31 120.6 . . ?
C32 C31 C30 118.8(4) . . ?
C32 C31 H31 120.6 . . ?
C31 C32 H32 120.1 . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.1 . . ?
Br4 C33 Br4A 6.6(4) . . ?
C32 C33 Br4 115.6(3) . . ?
C32 C33 C34 122.8(3) . . ?
C32 C33 Br4A 122.0(4) . . ?
C34 C33 Br4 121.7(3) . . ?
C34 C33 Br4A 115.2(4) . . ?
C29 C34 C33 117.8(4) . . ?
C29 C34 H34 121.1 . . ?
C33 C34 H34 121.1 . . ?
C28 C35 H35A 108.7 . . ?
C28 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C36 C35 C28 114.3(4) . . ?
C36 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
C35 C36 H36A 109.1 . . ?
C35 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C37 C36 C35 112.6(4) . . ?
C37 C36 H36A 109.1 . . ?
C37 C36 H36B 109.1 . . ?
O7 C37 C36 125.6(5) . . ?
O7 C37 O8 122.7(5) . . ?
O8 C37 C36 111.7(5) . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O8 C38 H38A 109.5 . . ?
O8 C38 H38B 109.5 . . ?
O8 C38 H38C 109.5 . . ?
C28 C39 H39A 108.9 . . ?
C28 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 C28 113.6(4) . . ?
C40 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C39 C40 H40A 108.5 . . ?
C39 C40 H40B 108.5 . . ?
H40A C40 H40B 107.5 . . ?
C41 C40 C39 115.2(4) . . ?
C41 C40 H40A 108.5 . . ?
C41 C40 H40B 108.5 . . ?
O5 C41 C40 125.5(4) . . ?
O5 C41 O6 123.8(5) . . ?
O6 C41 C40 110.7(4) . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O6 C42 H42A 109.5 . . ?
O6 C42 H42B 109.5 . . ?
O6 C42 H42C 109.5 . . ?
C16 O2 C17 115.4(6) . . ?
C20 O4 C21 115.8(4) . . ?
C41 O6 C42 117.2(4) . . ?
C37 O8 C38 118.6(5) . . ?
C11A C12A Br2A 119.1(7) . . ?
C11A C12A C13A 120.0 . . ?
C13A C12A Br2A 120.8(7) . . ?
C12A C11A H11A 120.0 . . ?
C10A C11A C12A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C11A C10A C9A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
C10A C9A C6 125.3(7) . . ?
C10A C9A C8A 120.0 . . ?
C8A C9A C6 114.7(7) . . ?
C9A C8A C7 104.4(8) . . ?
C13A C8A C7 135.6(8) . . ?
C13A C8A C9A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C8A C13A C12A 120.0 . . ?
C8A C13A H13A 120.0 . . ?

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
Br1 C3 C4 C5 -176.4(4) . . . . ?
Br2 C12 C11 C10 -176.0(9) . . . . ?
Br2 C12 C13 C8 177.7(8) . . . . ?
Br3 C24 C25 C26 -179.6(4) . . . . ?
Br4 C33 C34 C29 -179.6(4) . . . . ?
C1 C2 C3 Br1 177.7(3) . . . . ?
C1 C2 C3 C4 -1.1(6) . . . . ?
C1 C2 C3 Br1A -174.3(4) . . . . ?
C1 C6 C9 C10 -177.9(12) . . . . ?
C1 C6 C9 C8 -1.2(10) . . . . ?
C1 C6 C9A C10A -179.7(7) . . . . ?
C1 C6 C9A C8A -1.3(7) . . . . ?
C1 C7 C8 C9 0.8(8) . . . . ?
C1 C7 C8 C13 175.1(8) . . . . ?
C1 C7 C14 C15 59.7(4) . . . . ?
C1 C7 C18 C19 -65.3(4) . . . . ?
C1 C7 C8A C9A -4.5(7) . . . . ?
C1 C7 C8A C13A 178.2(9) . . . . ?
C2 C1 C6 C5 1.0(5) . . . . ?
C2 C1 C6 C9 -179.9(8) . . . . ?
C2 C1 C6 C9A 176.7(6) . . . . ?
C2 C1 C7 C8 -179.6(5) . . . . ?
C2 C1 C7 C14 62.7(5) . . . . ?
C2 C1 C7 C18 -57.2(4) . . . . ?
C2 C1 C7 C8A -174.1(7) . . . . ?
C2 C3 C4 C5 2.5(7) . . . . ?
C3 C4 C5 C6 -2.1(7) . . . . ?
C4 C5 C6 C1 0.4(6) . . . . ?
C4 C5 C6 C9 -178.7(9) . . . . ?
C4 C5 C6 C9A -173.0(10) . . . . ?
C5 C6 C9 C10 1.2(19) . . . . ?
C5 C6 C9 C8 177.9(6) . . . . ?
C5 C6 C9A C10A -5.5(15) . . . . ?
C5 C6 C9A C8A 172.9(7) . . . . ?
C6 C1 C2 C3 -0.6(5) . . . . ?
C6 C1 C7 C8 -1.4(5) . . . . ?
C6 C1 C7 C14 -119.2(3) . . . . ?
C6 C1 C7 C18 120.9(3) . . . . ?
C6 C1 C7 C8A 4.0(7) . . . . ?
C6 C9 C8 C7 0.2(11) . . . . ?
C6 C9 C8 C13 -174.3(10) . . . . ?
C6 C9A C8A C7 3.6(8) . . . . ?
C6 C9A C8A C13A -178.5(11) . . . . ?
C7 C1 C2 C3 177.4(3) . . . . ?
C7 C1 C6 C5 -177.3(3) . . . . ?
C7 C1 C6 C9 1.8(8) . . . . ?
C7 C1 C6 C9A -1.6(6) . . . . ?
C7 C8 C13 C12 -173.9(11) . . . . ?
C7 C14 C15 C16 177.5(3) . . . . ?
C7 C18 C19 C20 168.5(3) . . . . ?
C7 C8A C13A C12A 177.1(15) . . . . ?
C12 C11 C10 C9 -3.1(17) . . . . ?
C11 C12 C13 C8 -4.4(15) . . . . ?
C11 C10 C9 C6 174.9(15) . . . . ?
C11 C10 C9 C8 -1.4(14) . . . . ?
C10 C9 C8 C7 177.4(10) . . . . ?
C10 C9 C8 C13 2.9(14) . . . . ?
C9 C8 C13 C12 0.0(12) . . . . ?
C8 C7 C14 C15 -46.5(6) . . . . ?
C8 C7 C18 C19 43.1(7) . . . . ?
C13 C12 C11 C10 6.1(19) . . . . ?
C14 C7 C8 C9 117.6(8) . . . . ?
C14 C7 C8 C13 -68.0(9) . . . . ?
C14 C7 C18 C19 171.6(3) . . . . ?
C14 C7 C8A C9A 120.0(6) . . . . ?
C14 C7 C8A C13A -57.4(13) . . . . ?
C14 C15 C16 O1 -1.3(12) . . . . ?
C14 C15 C16 O2 -171.4(4) . . . . ?
C14 C15 C16 O1A\ 35(2) . . . . ?
C15 C16 O2 C17 179.0(5) . . . . ?
C18 C7 C8 C9 -117.1(8) . . . . ?
C18 C7 C8 C13 57.3(10) . . . . ?
C18 C7 C14 C15 -177.4(3) . . . . ?
C18 C7 C8A C9A -125.3(5) . . . . ?
C18 C7 C8A C13A 57.3(12) . . . . ?
C18 C19 C20 O3 -3.8(7) . . . . ?
C18 C19 C20 O4 177.9(3) . . . . ?
C19 C20 O4 C21 175.4(4) . . . . ?
C22 C23 C24 Br3 178.9(4) . . . . ?
C22 C23 C24 C25 -2.6(7) . . . . ?
C22 C23 C24 Br3A 176.7(3) . . . . ?
C22 C27 C30 C29 -0.5(4) . . . . ?
C22 C27 C30 C31 178.1(4) . . . . ?
C22 C28 C29 C30 1.3(4) . . . . ?
C22 C28 C29 C34 -178.1(4) . . . . ?
C22 C28 C35 C36 -52.7(5) . . . . ?
C22 C28 C39 C40 42.7(4) . . . . ?
C23 C22 C27 C26 -0.7(6) . . . . ?
C23 C22 C27 C30 -178.8(4) . . . . ?
C23 C22 C28 C29 178.5(4) . . . . ?
C23 C22 C28 C35 -62.2(5) . . . . ?
C23 C22 C28 C39 60.8(5) . . . . ?
C23 C24 C25 C26 1.8(8) . . . . ?
C24 C25 C26 C27 -0.3(8) . . . . ?
C25 C26 C27 C22 -0.2(7) . . . . ?
C25 C26 C27 C30 177.4(4) . . . . ?
C26 C27 C30 C29 -178.3(4) . . . . ?
C26 C27 C30 C31 0.3(7) . . . . ?
C27 C22 C23 C24 2.0(6) . . . . ?
C27 C22 C28 C29 -1.6(4) . . . . ?
C27 C22 C28 C35 117.7(4) . . . . ?
C27 C22 C28 C39 -119.3(4) . . . . ?
C27 C30 C31 C32 -179.6(4) . . . . ?
C28 C22 C23 C24 -178.1(4) . . . . ?
C28 C22 C27 C26 179.4(4) . . . . ?
C28 C22 C27 C30 1.4(4) . . . . ?
C28 C29 C30 C27 -0.6(4) . . . . ?
C28 C29 C30 C31 -179.4(3) . . . . ?
C28 C29 C34 C33 179.8(3) . . . . ?
C28 C35 C36 C37 179.9(4) . . . . ?
C28 C39 C40 C41 155.8(3) . . . . ?
C29 C28 C35 C36 59.1(5) . . . . ?
C29 C28 C39 C40 -67.7(4) . . . . ?
C29 C30 C31 C32 -1.2(6) . . . . ?
C30 C29 C34 C33 0.4(5) . . . . ?
C30 C31 C32 C33 1.6(6) . . . . ?
C31 C32 C33 Br4 178.6(4) . . . . ?
C31 C32 C33 C34 -1.1(6) . . . . ?
C31 C32 C33 Br4A 176.8(4) . . . . ?
C32 C33 C34 C29 0.1(6) . . . . ?
C34 C29 C30 C27 178.9(3) . . . . ?
C34 C29 C30 C31 0.1(5) . . . . ?
C35 C28 C29 C30 -119.0(4) . . . . ?
C35 C28 C29 C34 61.6(5) . . . . ?
C35 C28 C39 C40 168.6(3) . . . . ?
C35 C36 C37 O7 56.5(8) . . . . ?
C35 C36 C37 O8 -123.9(6) . . . . ?
C36 C37 O8 C38 176.9(7) . . . . ?
C39 C28 C29 C30 119.5(4) . . . . ?
C39 C28 C29 C34 -59.9(5) . . . . ?
C39 C28 C35 C36 -177.7(4) . . . . ?
C39 C40 C41 O5 -7.6(7) . . . . ?
C39 C40 C41 O6 173.6(3) . . . . ?
C40 C41 O6 C42 178.5(4) . . . . ?
O1 C16 O2 C17 8.5(12) . . . . ?
O3 C20 O4 C21 -2.9(6) . . . . ?
O5 C41 O6 C42 -0.2(6) . . . . ?
O7 C37 O8 C38 -3.6(11) . . . . ?
Br2A C12A C11A C10A -178.6(8) . . . . ?
Br2A C12A C13A C8A 178.6(8) . . . . ?
Br1A C3 C4 C5 176.3(4) . . . . ?
Br3A C24 C25 C26 -177.3(4) . . . . ?
Br4A C33 C34 C29 -177.9(4) . . . . ?
C12A C11A C10A C9A 0.0 . . . . ?
C11A C12A C13A C8A 0.0 . . . . ?
C11A C10A C9A C6 178.3(12) . . . . ?
C11A C10A C9A C8A 0.0 . . . . ?
C10A C9A C8A C7 -177.9(11) . . . . ?
C10A C9A C8A C13A 0.0 . . . . ?
C9A C8A C13A C12A 0.0 . . . . ?
C8A C7 C14 C15 -63.7(7) . . . . ?
C8A C7 C18 C19 54.7(7) . . . . ?
C13A C12A C11A C10A 0.0 . . . . ?
O1A\ C16 O2 C17 -26(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.551
_oxdiff_exptl_absorpt_empirical_full_min 0.565
####################################################################### 
# 
# 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_cd1
_database_code_depnum_ccdc_archive 'CCDC 2415235'
loop_
_audit_author_name
_audit_author_address
'zheng chunyang'
;Hubei Normal University
China
;
_audit_update_record             
;
2025-01-07 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_audit_creation_date             2024-08-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H24 Cd N4 O4, 3(H2 O)'
_chemical_formula_sum            'C33 H30 Cd N4 O7'
_chemical_formula_weight         707.01
_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'
Cd Cd 0.1185 4.6533 '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'

_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                   11.4955(3)
_cell_length_b                   12.1086(3)
_cell_length_c                   12.9827(3)
_cell_angle_alpha                110.330(2)
_cell_angle_beta                 91.122(2)
_cell_angle_gamma                104.670(2)
_cell_volume                     1627.74(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11041
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9170
_cell_measurement_theta_min      3.6460
_shelx_estimated_absorpt_T_max   0.476
_shelx_estimated_absorpt_T_min   0.421
_exptl_absorpt_coefficient_mu    5.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15824
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.228
_diffrn_reflns_theta_min         3.656
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  61.00   0.50    0.20    --   43.99 -68.00 -53.00  168
  2  ω     24.00  56.00   0.50    0.20    --   43.99 -32.00 -60.00   64
  3  ω     39.00 117.00   0.50    0.20    --   96.32 -68.00 -53.00  156
  4  ω     62.00  88.00   0.50    0.20    --   96.32 -33.00-120.00   52
  5  ω     64.00 110.00   0.50    0.20    --   96.32 -96.00-150.00   92
  6  ω     79.00 105.00   0.50    0.20    --   96.32-117.00-150.00   52
  7  ω     43.00  69.00   0.50    0.20    --   96.32-117.00-150.00   52
  8  ω     28.00 127.00   0.50    0.20    --   96.32-145.00-180.00  198
  9  ω     35.00  84.00   0.50    0.20    --   96.32 -96.00 -60.00   98
 10  ω     30.00 109.00   0.50    0.20    --   96.32 -33.00 -60.00  158
 11  ω     30.00 113.00   0.50    0.20    --   96.32-117.00   0.00  166
 12  ω     52.00 117.00   0.50    0.20    --   96.32 -17.00  60.00  130
 13  ω     64.00 106.00   0.50    0.20    --   96.32 -96.00  90.00   84
 14  ω     31.00  81.00   0.50    0.20    --   96.32 -50.00  60.00  100
 15  ω     22.00  52.00   0.50    0.20    --   96.32 -96.00  90.00   60
 16  ω    -15.00  49.00   0.50    0.20    --   43.99 -32.00 120.00  128
 17  ω     20.00  46.00   0.50    0.20    --   43.99  68.00  80.00   52
 18  ω     51.00 110.00   0.50    0.20    --   43.99  68.00  80.00  118
 19  ω     80.00 161.00   0.50    0.20    --   96.32  68.00  80.00  162
 20  ω    114.00 142.00   0.50    0.20    --   96.32  77.00 120.00   56
 21  ω     86.00 111.00   0.50    0.20    --   96.32  77.00 120.00   50
 22  ω     78.00 158.00   0.50    0.20    --   96.32 117.00  30.00  160
 23  ω     84.00 163.00   0.50    0.20    --   96.32 117.00   0.00  158
 24  ω     77.00 159.00   0.50    0.20    --   96.32 117.00 -90.00  164
 25  ω     64.00 105.00   0.50    0.20    --   43.99 138.00-120.00   82
 26  ω    -28.00  -2.00   0.50    0.20    --  -42.11 104.00-150.00   52
 27  ω    -66.00 -41.00   0.50    0.20    --  -42.11 104.00-150.00   50
 28  ω    -69.00 -17.00   0.50    0.20    --  -42.11 138.00-180.00  104
 29  ω    -78.00 -53.00   0.50    0.20    --  -94.45 145.00-180.00   50
 30  ω   -117.00 -28.00   0.50    0.20    --  -94.45  77.00-150.00  178
 31  ω    -77.00 -21.00   0.50    0.20    --  -94.45  96.00 -90.00  112
 32  ω   -111.00 -85.00   0.50    0.20    --  -42.11 -21.00   0.00   52
 33  ω    -66.00 -33.00   0.50    0.20    --  -42.11 -21.00   0.00   66
 34  ω    -67.00 -38.00   0.50    0.20    --  -42.11 -68.00 -53.00   58
 35  ω    -18.00   7.00   0.50    0.20    --   43.99 -32.00 -60.00   50
 36  ω    -90.00 -65.00   0.50    0.20    --  -42.11-138.00-120.00   50
 37  ω   -106.00 -81.00   0.50    0.20    --  -42.11 -68.00 -53.00   50
 38  ω    -99.00 -73.00   0.50    0.20    --  -42.11 -32.00 -60.00   52
 39  ω   -115.00 -84.00   0.50    0.20    --  -94.45 -25.00-120.00   62
 40  ω   -143.00-117.00   0.50    0.20    --  -94.45 -25.00-120.00   52
 41  ω   -162.00-120.00   0.50    0.20    --  -94.45 -33.00-150.00   84
 42  ω   -140.00-115.00   0.50    0.20    --  -94.45 -68.00 -53.00   50
 43  ω   -132.00 -74.00   0.50    0.20    --  -94.45 -68.00   0.00  116
 44  ω   -160.00-108.00   0.50    0.20    --  -94.45 -96.00  30.00  104
 45  ω   -158.00 -81.00   0.50    0.20    --  -94.45 -96.00  60.00  154
 46  ω    -86.00 -61.00   0.50    0.20    --  -42.11-138.00 120.00   50
 47  ω     -3.00  23.00   0.50    0.20    --  -42.11  68.00  80.00   52
 48  ω    -51.00 -26.00   0.50    0.20    --  -42.11 138.00 120.00   50
 49  ω    -42.00  -7.00   0.50    0.20    --  -42.11  68.00  80.00   70
 50  ω    -96.00 -57.00   0.50    0.20    --  -42.11 138.00 120.00   78
 51  ω   -109.00 -75.00   0.50    0.20    --  -94.45  68.00  80.00   68
 52  ω   -104.00 -48.00   0.50    0.20    --  -94.45  96.00  60.00  112
 53  ω     28.00  54.00   0.50    0.20    --   43.99-104.00-180.00   52
 54  ω   -124.00 -89.00   0.50    0.20    --  -94.45 145.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0816093000
_diffrn_orient_matrix_UB_12      0.1098448000
_diffrn_orient_matrix_UB_13      0.0960223000
_diffrn_orient_matrix_UB_21      0.0684569000
_diffrn_orient_matrix_UB_22      -0.0849522000
_diffrn_orient_matrix_UB_23      0.0225495000
_diffrn_orient_matrix_UB_31      0.0901000000
_diffrn_orient_matrix_UB_32      0.0257084000
_diffrn_orient_matrix_UB_33      -0.0807057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_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                5459
_reflns_number_total             5916
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5916
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0490
_refine_ls_restrained_S_all      1.045
_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)+(0.1068P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1385
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O4W)
\\sim Ueq, Uanis(O2W) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3. Others
 Fixed Sof: O3W(0.5) H3WA(0.5) H3WB(0.5) O4W(0.5) H4WA(0.5) H4WB(0.5) O5W(0.5)
 H5WA(0.5) H5WB(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C18(H18), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
Cd1 Cd 0.30782(2) 0.24105(2) -0.14630(2) 0.04805(13) Uani 1 1 d . . . . .
O1 O 0.4876(3) 0.3622(3) 0.8223(3) 0.0755(9) Uani 1 1 d . . . . .
O2 O 0.3749(4) 0.2203(4) 0.6808(3) 0.1065(15) Uani 1 1 d . . . . .
O3 O 0.6988(7) -0.0414(4) 0.1816(4) 0.134(2) Uani 1 1 d . . . . .
O4 O 0.8527(4) -0.0551(4) 0.2624(5) 0.1125(17) Uani 1 1 d . . . . .
N1 N 1.1825(3) 0.3575(3) 0.8520(3) 0.0522(7) Uani 1 1 d . . . . .
N2 N 1.0539(3) 0.4267(3) 0.7807(3) 0.0502(7) Uani 1 1 d . . . . .
N3 N 0.3541(3) 0.2794(3) 0.0342(3) 0.0541(7) Uani 1 1 d . . . . .
N4 N 0.4474(3) 0.3147(3) 0.1983(3) 0.0542(7) Uani 1 1 d . . . . .
C1 C 1.1058(3) 0.3354(3) 0.7669(3) 0.0514(8) Uani 1 1 d . . . . .
H1 H 1.088954 0.264517 0.703952 0.062 Uiso 1 1 calc R U . . .
C2 C 1.1829(3) 0.4716(3) 0.9277(3) 0.0509(8) Uani 1 1 d . . . . .
C3 C 1.2474(4) 0.5396(4) 1.0321(3) 0.0621(10) Uani 1 1 d . . . . .
H3 H 1.303311 0.511700 1.061540 0.074 Uiso 1 1 calc R U . . .
C4 C 1.2252(5) 0.6490(4) 1.0895(4) 0.0757(12) Uani 1 1 d . . . . .
H4 H 1.268108 0.696910 1.158850 0.091 Uiso 1 1 calc R U . . .
C5 C 1.1395(5) 0.6910(5) 1.0466(4) 0.0771(13) Uani 1 1 d . . . . .
H5 H 1.125279 0.764821 1.089032 0.092 Uiso 1 1 calc R U . . .
C6 C 1.0759(4) 0.6251(4) 0.9430(4) 0.0658(10) Uani 1 1 d . . . . .
H6 H 1.018955 0.652606 0.914351 0.079 Uiso 1 1 calc R U . . .
C7 C 1.1009(3) 0.5168(3) 0.8843(3) 0.0504(8) Uani 1 1 d . . . . .
C8 C 0.9722(3) 0.4334(3) 0.6984(3) 0.0469(7) Uani 1 1 d . . . . .
C9 C 0.8769(3) 0.3319(3) 0.6408(3) 0.0438(7) Uani 1 1 d . . . . .
H9 H 0.863617 0.259646 0.654757 0.053 Uiso 1 1 calc R U . . .
C10 C 0.8021(3) 0.3420(3) 0.5613(3) 0.0404(6) Uani 1 1 d . . . . .
C11 C 0.8244(3) 0.4504(3) 0.5405(3) 0.0424(7) Uani 1 1 d . . . . .
C12 C 0.9189(3) 0.5509(3) 0.5985(3) 0.0503(8) Uani 1 1 d . . . . .
H12 H 0.932130 0.623006 0.584275 0.060 Uiso 1 1 calc R U . . .
C13 C 0.9944(3) 0.5424(3) 0.6788(3) 0.0528(8) Uani 1 1 d . . . . .
H13 H 1.059057 0.608987 0.719134 0.063 Uiso 1 1 calc R U . . .
C14 C 0.7328(3) 0.4328(3) 0.4517(3) 0.0438(7) Uani 1 1 d . . . . .
C15 C 0.7205(3) 0.5105(3) 0.3962(3) 0.0529(8) Uani 1 1 d . . . . .
H15 H 0.774021 0.588366 0.415814 0.063 Uiso 1 1 calc R U . . .
C16 C 0.6265(3) 0.4685(4) 0.3112(3) 0.0546(8) Uani 1 1 d . . . . .
H16 H 0.617960 0.517800 0.271886 0.066 Uiso 1 1 calc R U . . .
C17 C 0.5452(3) 0.3533(3) 0.2845(3) 0.0503(8) Uani 1 1 d . . . . .
C18 C 0.5566(3) 0.2755(3) 0.3391(3) 0.0477(7) Uani 1 1 d . . . . .
H18 H 0.501958 0.198314 0.320063 0.057 Uiso 1 1 calc R U . . .
C19 C 0.6518(3) 0.3159(3) 0.4228(3) 0.0423(7) Uani 1 1 d . . . . .
C20 C 0.6880(3) 0.2482(3) 0.4922(3) 0.0406(7) Uani 1 1 d . . . . .
C21 C 0.4578(3) 0.3239(4) 0.0978(3) 0.0552(9) Uani 1 1 d . . . . .
H21 H 0.530555 0.358197 0.076182 0.066 Uiso 1 1 calc R U . . .
C22 C 0.3275(3) 0.2583(4) 0.1989(3) 0.0519(8) Uani 1 1 d . . . . .
C23 C 0.2639(4) 0.2258(4) 0.2797(4) 0.0652(10) Uani 1 1 d . . . . .
H23 H 0.301195 0.242561 0.349719 0.078 Uiso 1 1 calc R U . . .
C24 C 0.1420(4) 0.1673(5) 0.2483(5) 0.0797(14) Uani 1 1 d . . . . .
H24 H 0.096763 0.142322 0.298907 0.096 Uiso 1 1 calc R U . . .
C25 C 0.0837(4) 0.1437(5) 0.1456(5) 0.0790(13) Uani 1 1 d . . . . .
H25 H 0.001232 0.104126 0.129481 0.095 Uiso 1 1 calc R U . . .
C26 C 0.1453(4) 0.1777(5) 0.0669(4) 0.0688(11) Uani 1 1 d . . . . .
H26 H 0.106294 0.162846 -0.001980 0.083 Uiso 1 1 calc R U . . .
C27 C 0.2699(3) 0.2359(4) 0.0952(3) 0.0539(8) Uani 1 1 d . . . . .
C28 C 0.7088(3) 0.1249(3) 0.4193(3) 0.0492(8) Uani 1 1 d . . . . .
H28A H 0.734320 0.087270 0.467377 0.059 Uiso 1 1 calc R U . . .
H28B H 0.632187 0.070923 0.377505 0.059 Uiso 1 1 calc R U . . .
C29 C 0.8023(5) 0.1336(4) 0.3384(4) 0.0743(13) Uani 1 1 d . . . . .
H29A H 0.788904 0.186317 0.300349 0.089 Uiso 1 1 calc R U . . .
H29B H 0.883326 0.167825 0.377834 0.089 Uiso 1 1 calc R U . . .
C30 C 0.7885(6) 0.0057(5) 0.2560(5) 0.0842(17) Uani 1 1 d . . . . .
C31 C 0.5904(3) 0.2197(3) 0.5661(3) 0.0475(7) Uani 1 1 d . . . . .
H31A H 0.516011 0.167428 0.519210 0.057 Uiso 1 1 calc R U . . .
H31B H 0.616290 0.174214 0.606341 0.057 Uiso 1 1 calc R U . . .
C32 C 0.5642(4) 0.3323(4) 0.6486(4) 0.0647(11) Uani 1 1 d . . . . .
H32A H 0.639048 0.386507 0.693742 0.078 Uiso 1 1 calc R U . . .
H32B H 0.534410 0.375931 0.608599 0.078 Uiso 1 1 calc R U . . .
C33 C 0.4726(4) 0.3018(4) 0.7230(4) 0.0600(10) Uani 1 1 d . . . . .
O1W O 0.7742(10) -0.1453(9) 0.5056(8) 0.230(4) Uani 1 1 d . U . . .
H1WA H 0.788201 -0.118225 0.453497 0.346 Uiso 1 1 d R U . . .
H1WB H 0.697231 -0.147605 0.495367 0.346 Uiso 1 1 d R U . . .
O3W O 0.5855(12) 0.0328(12) 0.8314(14) 0.166(5) Uani 0.5 1 d . U P . .
H3WA H 0.564334 -0.011166 0.870246 0.249 Uiso 0.5 1 d R U P . .
H3WB H 0.614154 0.105074 0.878426 0.249 Uiso 0.5 1 d R U P . .
O4W O 0.7235(14) 0.0548(12) 0.6903(12) 0.165(5) Uani 0.5 1 d . U P . .
H4WA H 0.702947 0.078750 0.755213 0.248 Uiso 0.5 1 d R U P . .
H4WB H 0.707797 -0.022600 0.671163 0.248 Uiso 0.5 1 d R U P . .
O5W O 0.6588(16) 0.1213(16) 1.0584(15) 0.204(7) Uani 0.5 1 d . U P . .
H5WA H 0.721082 0.122708 1.095823 0.305 Uiso 0.5 1 d R U P . .
H5WB H 0.616142 0.080498 1.092733 0.305 Uiso 0.5 1 d R U P . .
O2W O 0.9780(15) 0.0487(15) 0.5937(15) 0.198(6) Uani 0.5 1 d . U P . .
H2WA H 1.033393 0.037329 0.629911 0.297 Uiso 0.5 1 d R U P . .
H2WB H 0.914203 -0.004741 0.594641 0.297 Uiso 0.5 1 d R U 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
Cd1 O1 2.345(3) 1_554 ?
Cd1 O2 2.339(3) 1_554 ?
Cd1 O3 2.280(4) 2_655 ?
Cd1 O4 2.485(4) 2_655 ?
Cd1 N1 2.261(3) 1_454 ?
Cd1 N3 2.250(3) . ?
Cd1 C30 2.737(5) 2_655 ?
O1 C33 1.224(5) . ?
O2 C33 1.255(5) . ?
O3 C30 1.266(8) . ?
O4 C30 1.187(7) . ?
N1 C1 1.306(5) . ?
N1 C2 1.389(5) . ?
N2 C1 1.346(5) . ?
N2 C7 1.395(5) . ?
N2 C8 1.445(4) . ?
N3 C21 1.311(5) . ?
N3 C27 1.379(5) . ?
N4 C17 1.435(5) . ?
N4 C21 1.352(5) . ?
N4 C22 1.376(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.393(5) . ?
C2 C7 1.399(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.366(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.402(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.375(6) . ?
C8 C9 1.385(5) . ?
C8 C13 1.391(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.388(5) . ?
C10 C11 1.393(4) . ?
C10 C20 1.519(4) . ?
C11 C12 1.375(5) . ?
C11 C14 1.466(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.392(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.399(5) . ?
C14 C19 1.401(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.390(5) . ?
C17 C18 1.389(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.389(5) . ?
C19 C20 1.526(4) . ?
C20 C28 1.546(4) . ?
C20 C31 1.540(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.399(5) . ?
C22 C27 1.395(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.380(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.383(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.374(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.404(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.527(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.511(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.518(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.507(6) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8836 . ?
O3W H3WA 0.8502 . ?
O3W H3WB 0.8499 . ?
O4W H4WA 0.8498 . ?
O4W H4WB 0.8499 . ?
O5W H5WA 0.8500 . ?
O5W H5WB 0.8497 . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8499 . ?

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 Cd1 O4 135.30(13) 1_554 2_655 ?
O1 Cd1 C30 125.90(13) 1_554 2_655 ?
O2 Cd1 O1 54.43(11) 1_554 1_554 ?
O2 Cd1 O4 81.08(14) 1_554 2_655 ?
O2 Cd1 C30 79.87(14) 1_554 2_655 ?
O3 Cd1 O1 115.6(2) 2_655 1_554 ?
O3 Cd1 O2 88.67(18) 2_655 1_554 ?
O3 Cd1 O4 52.38(19) 2_655 2_655 ?
O3 Cd1 C30 27.34(19) 2_655 2_655 ?
O4 Cd1 C30 25.71(18) 2_655 2_655 ?
N1 Cd1 O1 99.79(12) 1_454 1_554 ?
N1 Cd1 O2 98.14(16) 1_454 1_554 ?
N1 Cd1 O3 140.0(2) 1_454 2_655 ?
N1 Cd1 O4 89.66(13) 1_454 2_655 ?
N1 Cd1 C30 115.32(17) 1_454 2_655 ?
N3 Cd1 O1 99.10(11) . 1_554 ?
N3 Cd1 O2 148.13(14) . 1_554 ?
N3 Cd1 O3 88.35(15) . 2_655 ?
N3 Cd1 O4 120.79(15) . 2_655 ?
N3 Cd1 N1 104.37(12) . 1_454 ?
N3 Cd1 C30 109.49(16) . 2_655 ?
C33 O1 Cd1 92.9(2) . 1_556 ?
C33 O2 Cd1 92.5(3) . 1_556 ?
C30 O3 Cd1 96.9(4) . 2_655 ?
C30 O4 Cd1 89.1(4) . 2_655 ?
C1 N1 Cd1 123.8(3) . 1_656 ?
C1 N1 C2 106.4(3) . . ?
C2 N1 Cd1 129.1(2) . 1_656 ?
C1 N2 C7 107.5(3) . . ?
C1 N2 C8 125.6(3) . . ?
C7 N2 C8 126.7(3) . . ?
C21 N3 Cd1 131.9(3) . . ?
C21 N3 C27 105.8(3) . . ?
C27 N3 Cd1 121.4(2) . . ?
C21 N4 C17 125.4(3) . . ?
C21 N4 C22 106.8(3) . . ?
C22 N4 C17 127.7(3) . . ?
N1 C1 N2 112.4(3) . . ?
N1 C1 H1 123.8 . . ?
N2 C1 H1 123.8 . . ?
N1 C2 C3 130.9(4) . . ?
N1 C2 C7 108.9(3) . . ?
C3 C2 C7 120.2(4) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 C2 117.4(4) . . ?
C4 C3 H3 121.3 . . ?
C3 C4 H4 119.1 . . ?
C3 C4 C5 121.7(4) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.4(5) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.6(4) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C2 104.7(3) . . ?
C6 C7 N2 132.6(4) . . ?
C6 C7 C2 122.5(4) . . ?
C9 C8 N2 119.5(3) . . ?
C9 C8 C13 122.4(3) . . ?
C13 C8 N2 118.0(3) . . ?
C8 C9 H9 121.3 . . ?
C8 C9 C10 117.4(3) . . ?
C10 C9 H9 121.3 . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 C20 128.0(3) . . ?
C11 C10 C20 111.5(3) . . ?
C10 C11 C14 108.0(3) . . ?
C12 C11 C10 121.6(3) . . ?
C12 C11 C14 130.4(3) . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.6(3) . . ?
C13 C12 H12 120.7 . . ?
C8 C13 C12 119.4(3) . . ?
C8 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C11 130.3(3) . . ?
C15 C14 C19 120.9(3) . . ?
C19 C14 C11 108.8(3) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 C14 118.4(3) . . ?
C16 C15 H15 120.8 . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.3(3) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 N4 118.7(3) . . ?
C18 C17 N4 119.6(3) . . ?
C18 C17 C16 121.7(3) . . ?
C17 C18 H18 120.9 . . ?
C17 C18 C19 118.3(3) . . ?
C19 C18 H18 120.9 . . ?
C14 C19 C20 110.4(3) . . ?
C18 C19 C14 120.4(3) . . ?
C18 C19 C20 129.1(3) . . ?
C10 C20 C19 101.1(2) . . ?
C10 C20 C28 113.7(3) . . ?
C10 C20 C31 111.1(3) . . ?
C19 C20 C28 111.9(3) . . ?
C19 C20 C31 111.9(3) . . ?
C31 C20 C28 107.2(3) . . ?
N3 C21 N4 112.6(3) . . ?
N3 C21 H21 123.7 . . ?
N4 C21 H21 123.7 . . ?
N4 C22 C23 132.5(4) . . ?
N4 C22 C27 105.7(3) . . ?
C27 C22 C23 121.8(4) . . ?
C22 C23 H23 122.3 . . ?
C24 C23 C22 115.5(4) . . ?
C24 C23 H23 122.3 . . ?
C23 C24 H24 118.3 . . ?
C23 C24 C25 123.4(4) . . ?
C25 C24 H24 118.3 . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.3(4) . . ?
C26 C25 H25 119.4 . . ?
C25 C26 H26 121.5 . . ?
C25 C26 C27 117.0(4) . . ?
C27 C26 H26 121.5 . . ?
N3 C27 C22 109.0(3) . . ?
N3 C27 C26 130.0(4) . . ?
C22 C27 C26 121.1(4) . . ?
C20 C28 H28A 108.4 . . ?
C20 C28 H28B 108.4 . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 C20 115.3(3) . . ?
C29 C28 H28A 108.4 . . ?
C29 C28 H28B 108.4 . . ?
C28 C29 H29A 110.1 . . ?
C28 C29 H29B 110.1 . . ?
H29A C29 H29B 108.4 . . ?
C30 C29 C28 107.9(3) . . ?
C30 C29 H29A 110.1 . . ?
C30 C29 H29B 110.1 . . ?
O3 C30 Cd1 55.8(3) . 2_655 ?
O3 C30 C29 117.9(6) . . ?
O4 C30 Cd1 65.2(3) . 2_655 ?
O4 C30 O3 118.7(5) . . ?
O4 C30 C29 123.2(7) . . ?
C29 C30 Cd1 159.2(3) . 2_655 ?
C20 C31 H31A 108.7 . . ?
C20 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C20 114.2(3) . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C31 C32 H32A 109.0 . . ?
C31 C32 H32B 109.0 . . ?
H32A C32 H32B 107.8 . . ?
C33 C32 C31 112.9(3) . . ?
C33 C32 H32A 109.0 . . ?
C33 C32 H32B 109.0 . . ?
O1 C33 Cd1 60.1(2) . 1_556 ?
O1 C33 O2 119.6(4) . . ?
O1 C33 C32 120.9(4) . . ?
O2 C33 Cd1 59.9(2) . 1_556 ?
O2 C33 C32 119.2(4) . . ?
C32 C33 Cd1 178.6(3) . 1_556 ?
H1WA O1W H1WB 89.3 . . ?
H3WA O3W H3WB 104.5 . . ?
H4WA O4W H4WB 104.5 . . ?
H5WA O5W H5WB 87.8 . . ?
H2WA O2W H2WB 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O1 C33 O2 7.5(5) 1_556 . . . ?
Cd1 O1 C33 C32 -178.9(4) 1_556 . . . ?
Cd1 O2 C33 O1 -7.5(5) 1_556 . . . ?
Cd1 O2 C33 C32 178.8(4) 1_556 . . . ?
Cd1 O3 C30 O4 18.2(6) 2_655 . . . ?
Cd1 O3 C30 C29 -156.8(3) 2_655 . . . ?
Cd1 O4 C30 O3 -16.5(5) 2_655 . . . ?
Cd1 O4 C30 C29 158.2(4) 2_655 . . . ?
Cd1 N1 C1 N2 -171.3(2) 1_656 . . . ?
Cd1 N1 C2 C3 -9.9(6) 1_656 . . . ?
Cd1 N1 C2 C7 170.9(3) 1_656 . . . ?
Cd1 N3 C21 N4 -170.4(3) . . . . ?
Cd1 N3 C27 C22 171.7(3) . . . . ?
Cd1 N3 C27 C26 -8.4(6) . . . . ?
N1 C2 C3 C4 -177.8(4) . . . . ?
N1 C2 C7 N2 -0.8(4) . . . . ?
N1 C2 C7 C6 176.1(4) . . . . ?
N2 C8 C9 C10 -178.9(3) . . . . ?
N2 C8 C13 C12 178.6(3) . . . . ?
N4 C17 C18 C19 -179.5(3) . . . . ?
N4 C22 C23 C24 -178.8(5) . . . . ?
N4 C22 C27 N3 -0.6(4) . . . . ?
N4 C22 C27 C26 179.5(4) . . . . ?
C1 N1 C2 C3 179.9(4) . . . . ?
C1 N1 C2 C7 0.8(4) . . . . ?
C1 N2 C7 C2 0.5(4) . . . . ?
C1 N2 C7 C6 -175.9(4) . . . . ?
C1 N2 C8 C9 47.3(5) . . . . ?
C1 N2 C8 C13 -131.4(4) . . . . ?
C2 N1 C1 N2 -0.4(4) . . . . ?
C2 C3 C4 C5 1.1(7) . . . . ?
C3 C2 C7 N2 180.0(3) . . . . ?
C3 C2 C7 C6 -3.2(6) . . . . ?
C3 C4 C5 C6 -1.8(8) . . . . ?
C4 C5 C6 C7 0.0(7) . . . . ?
C5 C6 C7 N2 178.4(4) . . . . ?
C5 C6 C7 C2 2.5(6) . . . . ?
C7 N2 C1 N1 -0.1(4) . . . . ?
C7 N2 C8 C9 -138.2(4) . . . . ?
C7 N2 C8 C13 43.0(5) . . . . ?
C7 C2 C3 C4 1.2(6) . . . . ?
C8 N2 C1 N1 175.3(3) . . . . ?
C8 N2 C7 C2 -174.7(3) . . . . ?
C8 N2 C7 C6 8.8(7) . . . . ?
C8 C9 C10 C11 0.8(5) . . . . ?
C8 C9 C10 C20 -175.8(3) . . . . ?
C9 C8 C13 C12 -0.1(6) . . . . ?
C9 C10 C11 C12 -1.1(5) . . . . ?
C9 C10 C11 C14 178.8(3) . . . . ?
C9 C10 C20 C19 -179.7(3) . . . . ?
C9 C10 C20 C28 -59.7(4) . . . . ?
C9 C10 C20 C31 61.4(4) . . . . ?
C10 C11 C12 C13 0.7(5) . . . . ?
C10 C11 C14 C15 -175.3(4) . . . . ?
C10 C11 C14 C19 2.9(4) . . . . ?
C10 C20 C28 C29 -57.5(4) . . . . ?
C10 C20 C31 C32 51.6(4) . . . . ?
C11 C10 C20 C19 3.4(3) . . . . ?
C11 C10 C20 C28 123.4(3) . . . . ?
C11 C10 C20 C31 -115.5(3) . . . . ?
C11 C12 C13 C8 -0.1(6) . . . . ?
C11 C14 C15 C16 177.5(4) . . . . ?
C11 C14 C19 C18 -179.2(3) . . . . ?
C11 C14 C19 C20 -0.7(4) . . . . ?
C12 C11 C14 C15 4.6(7) . . . . ?
C12 C11 C14 C19 -177.2(4) . . . . ?
C13 C8 C9 C10 -0.2(5) . . . . ?
C14 C11 C12 C13 -179.2(4) . . . . ?
C14 C15 C16 C17 1.7(6) . . . . ?
C14 C19 C20 C10 -1.5(3) . . . . ?
C14 C19 C20 C28 -122.8(3) . . . . ?
C14 C19 C20 C31 116.8(3) . . . . ?
C15 C14 C19 C18 -0.7(5) . . . . ?
C15 C14 C19 C20 177.7(3) . . . . ?
C15 C16 C17 N4 178.3(4) . . . . ?
C15 C16 C17 C18 -1.8(6) . . . . ?
C16 C17 C18 C19 0.5(6) . . . . ?
C17 N4 C21 N3 178.8(4) . . . . ?
C17 N4 C22 C23 2.5(7) . . . . ?
C17 N4 C22 C27 -178.1(4) . . . . ?
C17 C18 C19 C14 0.7(5) . . . . ?
C17 C18 C19 C20 -177.4(3) . . . . ?
C18 C19 C20 C10 176.7(3) . . . . ?
C18 C19 C20 C28 55.4(5) . . . . ?
C18 C19 C20 C31 -65.0(4) . . . . ?
C19 C14 C15 C16 -0.5(6) . . . . ?
C19 C20 C28 C29 56.2(4) . . . . ?
C19 C20 C31 C32 -60.5(4) . . . . ?
C20 C10 C11 C12 176.0(3) . . . . ?
C20 C10 C11 C14 -4.0(4) . . . . ?
C20 C28 C29 C30 -166.1(4) . . . . ?
C20 C31 C32 C33 -177.4(3) . . . . ?
C21 N3 C27 C22 1.0(4) . . . . ?
C21 N3 C27 C26 -179.1(5) . . . . ?
C21 N4 C17 C16 47.2(6) . . . . ?
C21 N4 C17 C18 -132.8(4) . . . . ?
C21 N4 C22 C23 -179.4(4) . . . . ?
C21 N4 C22 C27 -0.1(4) . . . . ?
C22 N4 C17 C16 -135.1(4) . . . . ?
C22 N4 C17 C18 44.9(6) . . . . ?
C22 N4 C21 N3 0.7(5) . . . . ?
C22 C23 C24 C25 -1.5(8) . . . . ?
C23 C22 C27 N3 178.9(4) . . . . ?
C23 C22 C27 C26 -1.0(6) . . . . ?
C23 C24 C25 C26 0.2(9) . . . . ?
C24 C25 C26 C27 0.7(8) . . . . ?
C25 C26 C27 N3 179.8(5) . . . . ?
C25 C26 C27 C22 -0.3(7) . . . . ?
C27 N3 C21 N4 -1.1(5) . . . . ?
C27 C22 C23 C24 1.9(7) . . . . ?
C28 C20 C31 C32 176.4(3) . . . . ?
C28 C29 C30 Cd1 8.3(16) . . . 2_655 ?
C28 C29 C30 O3 75.0(6) . . . . ?
C28 C29 C30 O4 -99.8(6) . . . . ?
C31 C20 C28 C29 179.3(4) . . . . ?
C31 C32 C33 O1 136.9(5) . . . . ?
C31 C32 C33 O2 -49.5(6) . . . . ?

_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 2.590
_oxdiff_exptl_absorpt_empirical_full_min 0.439
####################################################################### 
# 
# 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_f1
_database_code_depnum_ccdc_archive 'CCDC 2415234'
loop_
_audit_author_name
_audit_author_address
'zheng chunyang'
;Hubei Normal University
China
;
_audit_update_record             
;
2025-01-07 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_audit_creation_date             2024-08-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H26 N4 O4'
_chemical_formula_sum            'C33 H26 N4 O4'
_chemical_formula_weight         542.58
_chemical_absolute_configuration ?
_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'

_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           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   12.071(6)
_cell_length_b                   10.485(5)
_cell_length_c                   12.181(6)
_cell_angle_alpha                90
_cell_angle_beta                 118.789(9)
_cell_angle_gamma                90
_cell_volume                     1351.2(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1970
_cell_measurement_temperature    297.15
_cell_measurement_theta_max      20.90
_cell_measurement_theta_min      2.72
_shelx_estimated_absorpt_T_max   0.996
_shelx_estimated_absorpt_T_min   0.986
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10808
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.300
_diffrn_reflns_theta_min         1.925
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.873
_reflns_Friedel_fraction_max     0.784
_reflns_number_gt                2903
_reflns_number_total             4577
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 
;
 Flack x determined using 1020 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.7(10)
_refine_ls_extinction_coef       0.005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4577
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      1.012
_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)+(0.0593P)²+0.3572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1511
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C29(H29a,H29b), C31(H31a,H31b), C32(H32a,H32b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C14(H14), C16A(H16A),
 C19A(H19A), C18A(H18A), C17A(H17A), C21(H21), C24(H24), C25(H25), C26(H26),
 C27(H27)
2.c Fitted hexagon refined as free rotating group:
 C16A(C15,C20,C19A,C18A,C17A)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
C1 C 0.4113(7) 0.6622(5) 0.0653(7) 0.0404(14) Uani 1 1 d . . . . .
C2 C 0.3491(6) 0.7576(6) -0.0406(6) 0.0400(16) Uani 1 1 d . . . . .
C3 C 0.2839(6) 0.7350(6) -0.1668(6) 0.0470(18) Uani 1 1 d . . . . .
H3 H 0.276326 0.652726 -0.198162 0.056 Uiso 1 1 calc R U . . .
C4 C 0.2296(6) 0.8375(6) -0.2467(6) 0.0451(17) Uani 1 1 d . . . . .
C5 C 0.2380(6) 0.9592(6) -0.2013(6) 0.0488(18) Uani 1 1 d . . . . .
H5 H 0.200687 1.026639 -0.256683 0.059 Uiso 1 1 calc R U . . .
C6 C 0.3014(6) 0.9818(6) -0.0741(6) 0.0453(16) Uani 1 1 d . . . . .
H6 H 0.304930 1.063717 -0.043361 0.054 Uiso 1 1 calc R U . . .
C7 C 0.3598(6) 0.8814(6) 0.0076(6) 0.0424(16) Uani 1 1 d . . . . .
C8 C 0.4332(6) 0.8753(6) 0.1425(5) 0.0395(16) Uani 1 1 d . . . . .
C9 C 0.4653(6) 0.7484(6) 0.1767(6) 0.0403(16) Uani 1 1 d . . . . .
C10 C 0.5342(6) 0.7151(6) 0.3004(6) 0.0415(17) Uani 1 1 d . . . . .
H10 H 0.553452 0.630187 0.324150 0.050 Uiso 1 1 calc R U . . .
C11 C 0.5744(6) 0.8110(7) 0.3889(6) 0.0441(17) Uani 1 1 d . . . . .
C12 C 0.5441(6) 0.9362(6) 0.3568(6) 0.0480(18) Uani 1 1 d . . . . .
H12 H 0.572216 0.998636 0.418585 0.058 Uiso 1 1 calc R U . . .
C13 C 0.4713(6) 0.9696(6) 0.2320(6) 0.0448(17) Uani 1 1 d . . . . .
H13 H 0.448734 1.054130 0.209133 0.054 Uiso 1 1 calc R U . . .
C14 C 0.2113(7) 0.7418(7) -0.4398(7) 0.0521(18) Uani 1 1 d . . . . .
H14 H 0.286609 0.696238 -0.399833 0.062 Uiso 1 1 calc R U . . .
C16A C -0.0334(5) 0.9467(5) -0.4637(4) 0.078(2) Uani 1 1 d G . . . .
H16A H -0.020692 0.979860 -0.387722 0.094 Uiso 1 1 calc R U . . .
C15 C 0.0560(4) 0.8655(5) -0.4670(3) 0.0519(18) Uani 1 1 d G . . . .
C20 C 0.0370(5) 0.8159(5) -0.5806(4) 0.0552(19) Uani 1 1 d G . . . .
C19A C -0.0713(6) 0.8474(6) -0.6909(3) 0.080(3) Uani 1 1 d G . . . .
H19A H -0.084004 0.814244 -0.766858 0.096 Uiso 1 1 calc R U . . .
C18A C -0.1607(5) 0.9286(6) -0.6876(4) 0.099(3) Uani 1 1 d G . . . .
H18A H -0.233176 0.949746 -0.761328 0.119 Uiso 1 1 calc R U . . .
C17A C -0.1417(4) 0.9782(6) -0.5740(6) 0.097(3) Uani 1 1 d G . . . .
H17A H -0.201522 1.032555 -0.571761 0.117 Uiso 1 1 calc R U . . .
C21 C 0.6180(7) 0.8111(7) 0.6093(7) 0.062(2) Uani 1 1 d . . . . .
H21 H 0.551145 0.864720 0.595470 0.074 Uiso 1 1 calc R U . . .
C22 C 0.7504(7) 0.6961(7) 0.5756(6) 0.0514(18) Uani 1 1 d . . . . .
C23 C 0.7776(7) 0.6882(7) 0.6990(6) 0.058(2) Uani 1 1 d . . . . .
C24 C 0.8765(9) 0.6150(9) 0.7814(7) 0.087(3) Uani 1 1 d . . . . .
H24 H 0.895805 0.609396 0.864916 0.104 Uiso 1 1 calc R U . . .
C25 C 0.9455(9) 0.5513(10) 0.7394(9) 0.099(3) Uani 1 1 d . . . . .
H25 H 1.011302 0.498821 0.793667 0.119 Uiso 1 1 calc R U . . .
C26 C 0.9191(9) 0.5634(10) 0.6149(8) 0.103(3) Uani 1 1 d . . . . .
H26 H 0.970557 0.521864 0.589017 0.123 Uiso 1 1 calc R U . . .
C27 C 0.8200(8) 0.6342(8) 0.5304(7) 0.073(2) Uani 1 1 d . . . . .
H27 H 0.800750 0.640190 0.446888 0.088 Uiso 1 1 calc R U . . .
C28 C 0.5121(7) 0.5786(6) 0.0590(6) 0.0490(17) Uani 1 1 d . . . . .
H28A H 0.546747 0.521546 0.130512 0.059 Uiso 1 1 calc R U . . .
H28B H 0.471665 0.526451 -0.015907 0.059 Uiso 1 1 calc R U . . .
C29 C 0.6194(7) 0.6504(7) 0.0576(6) 0.057(2) Uani 1 1 d . . . . .
H29A H 0.627254 0.732547 0.097424 0.068 Uiso 1 1 calc R U . . .
H29B H 0.697085 0.603765 0.107854 0.068 Uiso 1 1 calc R U . . .
C30 C 0.6069(7) 0.6722(7) -0.0679(7) 0.0514(19) Uani 1 1 d . . . . .
C31 C 0.3095(7) 0.5715(6) 0.0667(6) 0.0505(18) Uani 1 1 d . . . . .
H31A H 0.273090 0.521139 -0.009461 0.061 Uiso 1 1 calc R U . . .
H31B H 0.351147 0.513072 0.136650 0.061 Uiso 1 1 calc R U . . .
C32 C 0.2013(7) 0.6387(8) 0.0773(6) 0.060(2) Uani 1 1 d . . . . .
H32A H 0.194168 0.725451 0.047054 0.073 Uiso 1 1 calc R U . . .
H32B H 0.122611 0.595289 0.023153 0.073 Uiso 1 1 calc R U . . .
C33 C 0.2179(7) 0.6422(7) 0.2058(7) 0.0556(19) Uani 1 1 d . . . . .
N1 N 0.1365(6) 0.7393(6) -0.5610(6) 0.0595(17) Uani 1 1 d . . . . .
N2 N 0.1685(5) 0.8167(5) -0.3786(5) 0.0452(14) Uani 1 1 d . . . . .
N3 N 0.6938(7) 0.7614(7) 0.7178(5) 0.0665(19) Uani 1 1 d . . . . .
N4 N 0.6466(5) 0.7767(5) 0.5183(5) 0.0486(15) Uani 1 1 d . . . . .
O1 O 0.5353(6) 0.6188(6) -0.1633(5) 0.090(2) Uani 1 1 d . . . . .
O2 O 0.6837(6) 0.7601(5) -0.0675(5) 0.0790(17) Uani 1 1 d . . . . .
H2 H 0.677096 0.765645 -0.137542 0.118 Uiso 1 1 calc R U . . .
O3 O 0.2838(7) 0.5772(7) 0.2893(6) 0.103(2) Uani 1 1 d . . . . .
O4 O 0.1430(7) 0.7262(6) 0.2179(6) 0.0873(19) Uani 1 1 d . . . . .
H4 H 0.158019 0.728187 0.291086 0.131 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.515(9) . ?
C1 C9 1.494(9) . ?
C1 C28 1.531(9) . ?
C1 C31 1.561(9) . ?
C2 C3 1.369(9) . ?
C2 C7 1.405(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(9) . ?
C4 C5 1.375(9) . ?
C4 N2 1.426(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(9) . ?
C7 C8 1.445(8) . ?
C8 C9 1.392(8) . ?
C8 C13 1.377(8) . ?
C9 C10 1.370(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.380(9) . ?
C11 C12 1.368(9) . ?
C11 N4 1.432(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.385(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 N1 1.309(9) . ?
C14 N2 1.345(9) . ?
C16A H16A 0.9300 . ?
C16A C15 1.3900 . ?
C16A C17A 1.3900 . ?
C15 C20 1.3900 . ?
C15 N2 1.363(6) . ?
C20 C19A 1.3900 . ?
C20 N1 1.367(7) . ?
C19A H19A 0.9300 . ?
C19A C18A 1.3900 . ?
C18A H18A 0.9300 . ?
C18A C17A 1.3900 . ?
C17A H17A 0.9300 . ?
C21 H21 0.9300 . ?
C21 N3 1.300(9) . ?
C21 N4 1.360(8) . ?
C22 C23 1.378(9) . ?
C22 C27 1.369(10) . ?
C22 N4 1.389(8) . ?
C23 C24 1.366(10) . ?
C23 N3 1.374(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.347(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.396(12) . ?
C26 H26 0.9300 . ?
C26 C27 1.362(10) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.505(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.481(10) . ?
C30 O1 1.202(8) . ?
C30 O2 1.305(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.543(10) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.480(10) . ?
C33 O3 1.163(8) . ?
C33 O4 1.321(9) . ?
O2 H2 0.8200 . ?
O4 H4 0.8200 . ?

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 C28 114.6(6) . . ?
C2 C1 C31 110.0(6) . . ?
C9 C1 C2 101.2(4) . . ?
C9 C1 C28 112.5(6) . . ?
C9 C1 C31 111.0(6) . . ?
C28 C1 C31 107.5(4) . . ?
C3 C2 C1 128.5(6) . . ?
C3 C2 C7 121.1(6) . . ?
C7 C2 C1 110.3(6) . . ?
C2 C3 H3 120.8 . . ?
C2 C3 C4 118.5(6) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 N2 119.1(6) . . ?
C5 C4 C3 121.3(6) . . ?
C5 C4 N2 119.5(6) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.3(6) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 120.3 . . ?
C5 C6 C7 119.5(6) . . ?
C7 C6 H6 120.3 . . ?
C2 C7 C8 108.5(6) . . ?
C6 C7 C2 119.3(6) . . ?
C6 C7 C8 132.2(6) . . ?
C9 C8 C7 108.3(6) . . ?
C13 C8 C7 131.1(6) . . ?
C13 C8 C9 120.7(6) . . ?
C8 C9 C1 111.7(6) . . ?
C10 C9 C1 127.8(6) . . ?
C10 C9 C8 120.5(6) . . ?
C9 C10 H10 120.9 . . ?
C9 C10 C11 118.2(6) . . ?
C11 C10 H10 120.9 . . ?
C10 C11 N4 118.4(6) . . ?
C12 C11 C10 122.1(6) . . ?
C12 C11 N4 119.5(6) . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.8(6) . . ?
C13 C12 H12 120.1 . . ?
C8 C13 C12 118.7(6) . . ?
C8 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
N1 C14 H14 123.3 . . ?
N1 C14 N2 113.4(6) . . ?
N2 C14 H14 123.3 . . ?
C15 C16A H16A 120.0 . . ?
C15 C16A C17A 120.0 . . ?
C17A C16A H16A 120.0 . . ?
C16A C15 C20 120.0 . . ?
N2 C15 C16A 134.4(4) . . ?
N2 C15 C20 105.6(4) . . ?
C19A C20 C15 120.0 . . ?
N1 C20 C15 109.7(4) . . ?
N1 C20 C19A 130.3(4) . . ?
C20 C19A H19A 120.0 . . ?
C20 C19A C18A 120.0 . . ?
C18A C19A H19A 120.0 . . ?
C19A C18A H18A 120.0 . . ?
C19A C18A C17A 120.0 . . ?
C17A C18A H18A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C18A C17A C16A 120.0 . . ?
C18A C17A H17A 120.0 . . ?
N3 C21 H21 123.5 . . ?
N3 C21 N4 113.1(7) . . ?
N4 C21 H21 123.5 . . ?
C23 C22 N4 105.5(6) . . ?
C27 C22 C23 122.7(7) . . ?
C27 C22 N4 131.7(6) . . ?
C24 C23 C22 120.0(8) . . ?
C24 C23 N3 130.1(7) . . ?
N3 C23 C22 109.9(6) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 C23 118.8(8) . . ?
C25 C24 H24 120.6 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.5(8) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.0 . . ?
C27 C26 C25 121.9(9) . . ?
C27 C26 H26 119.0 . . ?
C22 C27 H27 122.0 . . ?
C26 C27 C22 116.1(7) . . ?
C26 C27 H27 122.0 . . ?
C1 C28 H28A 108.5 . . ?
C1 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 C1 115.0(5) . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C28 C29 H29A 108.4 . . ?
C28 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C30 C29 C28 115.4(6) . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
O1 C30 C29 126.5(7) . . ?
O1 C30 O2 120.8(7) . . ?
O2 C30 C29 112.7(7) . . ?
C1 C31 H31A 108.5 . . ?
C1 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 C1 115.2(6) . . ?
C32 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
C31 C32 H32A 108.7 . . ?
C31 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
C33 C32 C31 114.3(6) . . ?
C33 C32 H32A 108.7 . . ?
C33 C32 H32B 108.7 . . ?
O3 C33 C32 126.7(7) . . ?
O3 C33 O4 120.6(8) . . ?
O4 C33 C32 112.6(7) . . ?
C14 N1 C20 104.8(6) . . ?
C14 N2 C4 125.9(6) . . ?
C14 N2 C15 106.5(5) . . ?
C15 N2 C4 127.6(5) . . ?
C21 N3 C23 105.6(6) . . ?
C21 N4 C11 124.9(6) . . ?
C21 N4 C22 105.9(6) . . ?
C22 N4 C11 129.0(5) . . ?
C30 O2 H2 109.5 . . ?
C33 O4 H4 109.5 . . ?

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
C3 H3 O3 0.93 2.42 3.317(10) 161.9 2_564 yes
C10 H10 O1 0.93 2.63 3.527(9) 162.3 2_565 yes
O2 H2 N3 0.82 1.87 2.676(8) 168.3 1_554 yes
O4 H4 N1 0.82 1.94 2.735(9) 162.0 1_556 yes

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
C1 C2 C3 C4 177.0(7) . . . . ?
C1 C2 C7 C6 -175.7(6) . . . . ?
C1 C2 C7 C8 3.1(7) . . . . ?
C1 C9 C10 C11 -179.6(7) . . . . ?
C1 C28 C29 C30 -96.6(8) . . . . ?
C1 C31 C32 C33 -98.1(7) . . . . ?
C2 C1 C9 C8 3.2(8) . . . . ?
C2 C1 C9 C10 -179.3(6) . . . . ?
C2 C1 C28 C29 57.8(8) . . . . ?
C2 C1 C31 C32 -56.5(7) . . . . ?
C2 C3 C4 C5 -1.3(10) . . . . ?
C2 C3 C4 N2 175.9(6) . . . . ?
C2 C7 C8 C9 -1.0(7) . . . . ?
C2 C7 C8 C13 179.0(6) . . . . ?
C3 C2 C7 C6 1.2(10) . . . . ?
C3 C2 C7 C8 180.0(6) . . . . ?
C3 C4 C5 C6 0.0(10) . . . . ?
C3 C4 N2 C14 -41.9(9) . . . . ?
C3 C4 N2 C15 136.8(7) . . . . ?
C4 C5 C6 C7 1.9(9) . . . . ?
C5 C4 N2 C14 135.4(7) . . . . ?
C5 C4 N2 C15 -45.9(9) . . . . ?
C5 C6 C7 C2 -2.5(9) . . . . ?
C5 C6 C7 C8 179.1(6) . . . . ?
C6 C7 C8 C9 177.6(7) . . . . ?
C6 C7 C8 C13 -2.5(12) . . . . ?
C7 C2 C3 C4 0.7(10) . . . . ?
C7 C8 C9 C1 -1.6(7) . . . . ?
C7 C8 C9 C10 -179.2(6) . . . . ?
C7 C8 C13 C12 -178.9(6) . . . . ?
C8 C9 C10 C11 -2.3(9) . . . . ?
C9 C1 C2 C3 179.6(6) . . . . ?
C9 C1 C2 C7 -3.8(8) . . . . ?
C9 C1 C28 C29 -57.1(8) . . . . ?
C9 C1 C31 C32 54.7(7) . . . . ?
C9 C8 C13 C12 1.0(9) . . . . ?
C9 C10 C11 C12 2.1(9) . . . . ?
C9 C10 C11 N4 -179.9(6) . . . . ?
C10 C11 C12 C13 -0.3(9) . . . . ?
C10 C11 N4 C21 -126.3(7) . . . . ?
C10 C11 N4 C22 47.9(9) . . . . ?
C11 C12 C13 C8 -1.3(9) . . . . ?
C12 C11 N4 C21 51.8(9) . . . . ?
C12 C11 N4 C22 -134.0(7) . . . . ?
C13 C8 C9 C1 178.5(6) . . . . ?
C13 C8 C9 C10 0.8(9) . . . . ?
C16A C15 C20 C19A 0.0 . . . . ?
C16A C15 C20 N1 179.9(5) . . . . ?
C16A C15 N2 C4 0.5(9) . . . . ?
C16A C15 N2 C14 179.4(5) . . . . ?
C15 C16A C17A C18A 0.0 . . . . ?
C15 C20 C19A C18A 0.0 . . . . ?
C15 C20 N1 C14 0.8(6) . . . . ?
C20 C15 N2 C4 -179.2(5) . . . . ?
C20 C15 N2 C14 -0.3(6) . . . . ?
C20 C19A C18A C17A 0.0 . . . . ?
C19A C20 N1 C14 -179.2(5) . . . . ?
C19A C18A C17A C16A 0.0 . . . . ?
C17A C16A C15 C20 0.0 . . . . ?
C17A C16A C15 N2 -179.7(6) . . . . ?
C22 C23 C24 C25 -0.3(13) . . . . ?
C22 C23 N3 C21 0.4(9) . . . . ?
C23 C22 C27 C26 0.0(12) . . . . ?
C23 C22 N4 C11 -175.3(7) . . . . ?
C23 C22 N4 C21 -0.3(8) . . . . ?
C23 C24 C25 C26 2.2(15) . . . . ?
C24 C23 N3 C21 -179.8(9) . . . . ?
C24 C25 C26 C27 -3.2(17) . . . . ?
C25 C26 C27 C22 2.0(15) . . . . ?
C27 C22 C23 C24 -0.9(12) . . . . ?
C27 C22 C23 N3 178.9(7) . . . . ?
C27 C22 N4 C11 5.8(12) . . . . ?
C27 C22 N4 C21 -179.2(8) . . . . ?
C28 C1 C2 C3 58.3(9) . . . . ?
C28 C1 C2 C7 -125.1(6) . . . . ?
C28 C1 C9 C8 126.0(6) . . . . ?
C28 C1 C9 C10 -56.6(9) . . . . ?
C28 C1 C31 C32 178.1(5) . . . . ?
C28 C29 C30 O1 -15.6(11) . . . . ?
C28 C29 C30 O2 164.0(6) . . . . ?
C31 C1 C2 C3 -62.9(9) . . . . ?
C31 C1 C2 C7 113.7(6) . . . . ?
C31 C1 C9 C8 -113.5(6) . . . . ?
C31 C1 C9 C10 63.9(9) . . . . ?
C31 C1 C28 C29 -179.6(5) . . . . ?
C31 C32 C33 O3 -19.3(12) . . . . ?
C31 C32 C33 O4 163.9(7) . . . . ?
N1 C14 N2 C4 179.8(6) . . . . ?
N1 C14 N2 C15 0.9(8) . . . . ?
N1 C20 C19A C18A -179.9(6) . . . . ?
N2 C4 C5 C6 -177.2(6) . . . . ?
N2 C14 N1 C20 -1.1(8) . . . . ?
N2 C15 C20 C19A 179.7(4) . . . . ?
N2 C15 C20 N1 -0.3(5) . . . . ?
N3 C21 N4 C11 175.9(6) . . . . ?
N3 C21 N4 C22 0.6(8) . . . . ?
N3 C23 C24 C25 180.0(9) . . . . ?
N4 C11 C12 C13 -178.3(5) . . . . ?
N4 C21 N3 C23 -0.6(9) . . . . ?
N4 C22 C23 C24 -179.9(7) . . . . ?
N4 C22 C23 N3 0.0(8) . . . . ?
N4 C22 C27 C26 178.7(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_pb2
_database_code_depnum_ccdc_archive 'CCDC 2415236'
loop_
_audit_author_name
_audit_author_address
'zheng chunyang'
;Hubei Normal University
China
;
_audit_update_record             
;
2025-01-07 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_audit_creation_date             2025-01-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H24 N4 O4 Pb, H2 O'
_chemical_formula_sum            'C33 H26 N4 O5 Pb'
_chemical_formula_weight         765.77
_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                   11.2015(15)
_cell_length_b                   11.4714(16)
_cell_length_c                   12.5314(17)
_cell_angle_alpha                72.283(2)
_cell_angle_beta                 76.741(2)
_cell_angle_gamma                65.449(2)
_cell_volume                     1385.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      20.17
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.404
_shelx_estimated_absorpt_T_min   0.373
_exptl_absorpt_coefficient_mu    6.141
_exptl_absorpt_correction_T_max  0.7541
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction'
_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    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13551
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.009
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3742
_reflns_number_total             4847
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4847
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.043
_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)+(0.0392P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0829
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O2 \\sim O2A \\sim O1 \\sim O1A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O3 \\sim O4 \\sim O4A \\sim O3A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O2) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O3A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(O4A)=Sof(O3A)=1-FVAR(1)
 Sof(O3)=Sof(O4)=FVAR(1)
 Sof(O2A)=Sof(O1A)=1-FVAR(2)
 Sof(O1)=Sof(O2)=FVAR(2)
4.a Riding coordinates:
 O5(H5A,H5B)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.95591(3) -0.26813(3) 0.72745(2) 0.04760(11) Uani 1 1 d . . . . .
N1 N 0.1487(6) 0.4020(6) 0.3608(5) 0.0561(15) Uani 1 1 d . . . . .
N2 N 0.2117(5) 0.4743(5) 0.4748(4) 0.0429(13) Uani 1 1 d . . . . .
N3 N 0.7169(5) 0.2662(5) 1.0810(4) 0.0424(13) Uani 1 1 d . . . . .
N4 N 0.8649(5) 0.2261(6) 1.1903(5) 0.0529(15) Uani 1 1 d . . . . .
O1 O 0.7296(8) -0.1116(9) 0.7110(10) 0.075(3) Uani 0.713(12) 1 d . U P A 1
O3 O 0.1252(8) 0.2386(9) 1.0872(6) 0.086(2) Uani 0.738(8) 1 d . U P B 1
O4 O 0.1297(9) 0.4141(9) 1.1064(7) 0.092(3) Uani 0.738(8) 1 d . U P B 1
O5 O 0.1206(8) 0.0150(7) 1.0241(7) 0.153(3) Uani 1 1 d . . . . .
H5A H 0.070295 -0.025897 1.061392 0.229 Uiso 1 1 d R U . . .
H5B H 0.112955 0.066763 1.063752 0.229 Uiso 1 1 d R U . . .
C1 C 0.4522(5) 0.2435(5) 0.8197(5) 0.0303(13) Uani 1 1 d . . . . .
C2 C 0.4021(5) 0.3505(6) 0.7165(5) 0.0330(14) Uani 1 1 d . . . . .
C3 C 0.3228(6) 0.3577(6) 0.6434(5) 0.0362(14) Uani 1 1 d . . . . .
H3 H 0.293424 0.289797 0.653666 0.043 Uiso 1 1 calc R U . . .
C4 C 0.2876(6) 0.4676(6) 0.5546(5) 0.0367(15) Uani 1 1 d . . . . .
C5 C 0.3298(6) 0.5699(6) 0.5422(5) 0.0420(16) Uani 1 1 d . . . . .
H5 H 0.305700 0.643471 0.482411 0.050 Uiso 1 1 calc R U . . .
C6 C 0.4057(6) 0.5642(6) 0.6157(5) 0.0378(15) Uani 1 1 d . . . . .
H6 H 0.431768 0.634123 0.606840 0.045 Uiso 1 1 calc R U . . .
C7 C 0.4435(5) 0.4556(6) 0.7027(5) 0.0332(14) Uani 1 1 d . . . . .
C8 C 0.5233(5) 0.4218(6) 0.7929(5) 0.0320(14) Uani 1 1 d . . . . .
C9 C 0.5288(5) 0.3004(6) 0.8618(5) 0.0306(13) Uani 1 1 d . . . . .
C10 C 0.5951(5) 0.2463(6) 0.9554(5) 0.0369(15) Uani 1 1 d . . . . .
H10 H 0.600169 0.163787 1.000730 0.044 Uiso 1 1 calc R U . . .
C11 C 0.6539(6) 0.3178(6) 0.9804(5) 0.0377(15) Uani 1 1 d . . . . .
C12 C 0.6527(6) 0.4360(6) 0.9100(5) 0.0436(16) Uani 1 1 d . . . . .
H12 H 0.696207 0.480759 0.926592 0.052 Uiso 1 1 calc R U . . .
C13 C 0.5886(6) 0.4892(6) 0.8155(5) 0.0394(15) Uani 1 1 d . . . . .
H13 H 0.588996 0.568968 0.767647 0.047 Uiso 1 1 calc R U . . .
C14 C 0.2178(7) 0.3703(7) 0.4415(6) 0.0528(18) Uani 1 1 d . . . . .
H14 H 0.267669 0.283510 0.473939 0.063 Uiso 1 1 calc R U . . .
C15 C 0.0919(6) 0.5380(7) 0.3353(6) 0.0504(18) Uani 1 1 d . . . . .
C16 C 0.1301(6) 0.5861(7) 0.4053(5) 0.0431(16) Uani 1 1 d . . . . .
C17 C 0.0826(7) 0.7216(7) 0.3992(6) 0.059(2) Uani 1 1 d . . . . .
H17 H 0.103750 0.753888 0.448969 0.071 Uiso 1 1 calc R U . . .
C18 C 0.0046(8) 0.8034(8) 0.3178(8) 0.078(3) Uani 1 1 d . . . . .
H18 H -0.027006 0.893929 0.310834 0.093 Uiso 1 1 calc R U . . .
C19 C -0.0297(8) 0.7560(8) 0.2445(7) 0.076(3) Uani 1 1 d . . . . .
H19 H -0.082054 0.815753 0.188709 0.091 Uiso 1 1 calc R U . . .
C20 C 0.0114(7) 0.6239(8) 0.2520(6) 0.063(2) Uani 1 1 d . . . . .
H20 H -0.013258 0.592800 0.203472 0.075 Uiso 1 1 calc R U . . .
C21 C 0.8288(6) 0.2783(7) 1.0918(6) 0.0478(17) Uani 1 1 d . . . . .
H21 H 0.874844 0.320817 1.032779 0.057 Uiso 1 1 calc R U . . .
C22 C 0.6774(6) 0.1996(6) 1.1853(5) 0.0413(15) Uani 1 1 d . . . . .
C23 C 0.5689(7) 0.1628(7) 1.2277(6) 0.0529(18) Uani 1 1 d . . . . .
H23 H 0.505133 0.181045 1.182472 0.063 Uiso 1 1 calc R U . . .
C24 C 0.5604(8) 0.0987(8) 1.3388(7) 0.069(2) Uani 1 1 d . . . . .
H24 H 0.488148 0.074229 1.370576 0.083 Uiso 1 1 calc R U . . .
C25 C 0.6584(9) 0.0688(8) 1.4059(6) 0.069(2) Uani 1 1 d . . . . .
H25 H 0.651617 0.021326 1.480300 0.082 Uiso 1 1 calc R U . . .
C26 C 0.7637(7) 0.1075(7) 1.3652(6) 0.0543(18) Uani 1 1 d . . . . .
H26 H 0.826740 0.089803 1.410982 0.065 Uiso 1 1 calc R U . . .
C27 C 0.7727(6) 0.1739(7) 1.2534(5) 0.0444(16) Uani 1 1 d . . . . .
C28 C 0.5419(6) 0.1114(6) 0.7916(5) 0.0394(15) Uani 1 1 d . . . . .
H28A H 0.489316 0.077948 0.766374 0.047 Uiso 1 1 calc R U . . .
H28B H 0.576250 0.049236 0.859853 0.047 Uiso 1 1 calc R U . . .
C29 C 0.6586(6) 0.1175(6) 0.7006(5) 0.0449(16) Uani 1 1 d . . . . .
H29A H 0.625321 0.161080 0.628007 0.054 Uiso 1 1 calc R U . . .
H29B H 0.697855 0.170872 0.716032 0.054 Uiso 1 1 calc R U . . .
C30 C 0.7623(7) -0.0127(7) 0.6935(6) 0.0494(17) Uani 1 1 d . . . . .
C31 C 0.3376(6) 0.2268(6) 0.9084(5) 0.0403(15) Uani 1 1 d . . . . .
H31A H 0.291193 0.189072 0.880544 0.048 Uiso 1 1 calc R U . . .
H31B H 0.373171 0.164929 0.976373 0.048 Uiso 1 1 calc R U . . .
C32 C 0.2397(6) 0.3548(6) 0.9380(5) 0.0430(16) Uani 1 1 d . . . . .
H32A H 0.287879 0.408891 0.936252 0.052 Uiso 1 1 calc R U . . .
H32B H 0.180142 0.402067 0.880470 0.052 Uiso 1 1 calc R U . . .
C33 C 0.1608(7) 0.3384(8) 1.0487(6) 0.0527(18) Uani 1 1 d . . . . .
O2 O 0.8800(7) -0.0269(7) 0.6695(9) 0.071(2) Uani 0.713(12) 1 d . U P A 1
O4A O 0.051(3) 0.357(3) 1.061(2) 0.098(4) Uani 0.262(8) 1 d . U P B 2
O3A O 0.217(3) 0.297(3) 1.129(2) 0.099(4) Uani 0.262(8) 1 d . U P B 2
O2A O 0.854(2) -0.054(2) 0.757(2) 0.083(5) Uani 0.287(12) 1 d . U P A 2
O1A O 0.756(2) -0.082(2) 0.644(2) 0.062(4) Uani 0.287(12) 1 d . U P A 2


_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 N4 2.716(5) 2_757 ?
Pb1 O1 2.434(8) . ?
Pb1 O3 2.364(7) 2_657 ?
Pb1 O4 2.521(8) 2_657 ?
Pb1 C33 2.836(7) 2_657 ?
Pb1 O2 2.453(7) . ?
Pb1 O4A 2.53(2) 2_657 ?
Pb1 O3A 2.38(2) 2_657 ?
Pb1 O2A 2.35(2) . ?
Pb1 O1A 2.53(2) . ?
N1 C14 1.287(8) . ?
N1 C15 1.381(8) . ?
N2 C4 1.421(7) . ?
N2 C14 1.350(8) . ?
N2 C16 1.396(8) . ?
N3 C11 1.430(7) . ?
N3 C21 1.357(7) . ?
N3 C22 1.376(8) . ?
N4 C21 1.274(8) . ?
N4 C27 1.379(8) . ?
O1 C30 1.275(11) . ?
O3 C33 1.287(10) . ?
O4 C33 1.189(10) . ?
O5 H5A 0.8493 . ?
O5 H5B 0.8510 . ?
C1 C2 1.513(7) . ?
C1 C9 1.524(7) . ?
C1 C28 1.526(8) . ?
C1 C31 1.529(8) . ?
C2 C3 1.378(8) . ?
C2 C7 1.413(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(8) . ?
C4 C5 1.394(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.362(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.366(8) . ?
C7 C8 1.462(8) . ?
C8 C9 1.382(8) . ?
C8 C13 1.383(7) . ?
C9 C10 1.373(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.380(8) . ?
C11 C12 1.371(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.369(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.387(9) . ?
C15 C20 1.393(9) . ?
C16 C17 1.401(9) . ?
C17 H17 0.9300 . ?
C17 C18 1.352(9) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(11) . ?
C19 H19 0.9300 . ?
C19 C20 1.367(10) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.389(9) . ?
C22 C27 1.400(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.365(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.402(10) . ?
C25 H25 0.9300 . ?
C25 C26 1.367(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.379(9) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.535(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.477(9) . ?
C30 O2 1.235(9) . ?
C30 O2A 1.29(2) . ?
C30 O1A 1.19(2) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.518(8) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.470(9) . ?
C33 O4A 1.14(3) . ?
C33 O3A 1.18(3) . ?

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
N4 Pb1 C33 89.36(19) 2_757 2_657 ?
O1 Pb1 N4 123.0(3) . 2_757 ?
O1 Pb1 O4 88.9(4) . 2_657 ?
O1 Pb1 C33 80.2(3) . 2_657 ?
O1 Pb1 O2 52.7(3) . . ?
O1 Pb1 O4A 101.1(7) . 2_657 ?
O3 Pb1 N4 70.6(2) 2_657 2_757 ?
O3 Pb1 O1 76.5(4) 2_657 . ?
O3 Pb1 O4 51.3(3) 2_657 2_657 ?
O3 Pb1 C33 26.7(2) 2_657 2_657 ?
O3 Pb1 O2 85.7(3) 2_657 . ?
O3 Pb1 O4A 29.3(6) 2_657 2_657 ?
O3 Pb1 O3A 41.4(7) 2_657 2_657 ?
O4 Pb1 N4 104.1(3) 2_657 2_757 ?
O4 Pb1 C33 24.8(2) 2_657 2_657 ?
O4 Pb1 O4A 36.2(6) 2_657 2_657 ?
O2 Pb1 N4 79.2(2) . 2_757 ?
O2 Pb1 O4 129.9(3) . 2_657 ?
O2 Pb1 C33 108.1(3) . 2_657 ?
O2 Pb1 O4A 113.4(7) . 2_657 ?
O4A Pb1 O1A 120.0(9) 2_657 . ?
O3A Pb1 O1A 79.1(9) 2_657 . ?
O2A Pb1 O3A 80.7(10) . 2_657 ?
O2A Pb1 O1A 52.2(8) . . ?
C14 N1 C15 105.5(6) . . ?
C14 N2 C4 125.3(5) . . ?
C14 N2 C16 105.8(5) . . ?
C16 N2 C4 128.4(5) . . ?
C21 N3 C11 125.2(6) . . ?
C21 N3 C22 106.3(5) . . ?
C22 N3 C11 128.5(5) . . ?
C21 N4 Pb1 126.0(5) . 2_757 ?
C21 N4 C27 106.0(5) . . ?
C27 N4 Pb1 126.1(4) . 2_757 ?
C30 O1 Pb1 92.8(5) . . ?
C33 O3 Pb1 97.5(5) . 2_657 ?
C33 O4 Pb1 92.6(6) . 2_657 ?
H5A O5 H5B 104.5 . . ?
C2 C1 C9 101.5(4) . . ?
C2 C1 C28 112.6(5) . . ?
C2 C1 C31 111.2(5) . . ?
C9 C1 C28 111.2(4) . . ?
C9 C1 C31 110.2(4) . . ?
C28 C1 C31 109.9(5) . . ?
C3 C2 C1 129.2(5) . . ?
C3 C2 C7 120.4(5) . . ?
C7 C2 C1 110.4(5) . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(6) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 N2 120.1(5) . . ?
C3 C4 C5 119.7(5) . . ?
C5 C4 N2 120.1(5) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.3(6) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.7(6) . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C8 108.2(5) . . ?
C6 C7 C2 119.8(5) . . ?
C6 C7 C8 132.0(5) . . ?
C9 C8 C7 108.9(5) . . ?
C9 C8 C13 120.1(5) . . ?
C13 C8 C7 130.9(5) . . ?
C8 C9 C1 111.0(5) . . ?
C10 C9 C1 127.9(5) . . ?
C10 C9 C8 121.1(5) . . ?
C9 C10 H10 120.9 . . ?
C9 C10 C11 118.2(6) . . ?
C11 C10 H10 120.9 . . ?
C10 C11 N3 118.9(6) . . ?
C12 C11 N3 120.4(5) . . ?
C12 C11 C10 120.7(6) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.2(6) . . ?
C13 C12 H12 119.4 . . ?
C8 C13 H13 120.7 . . ?
C12 C13 C8 118.5(6) . . ?
C12 C13 H13 120.7 . . ?
N1 C14 N2 114.1(6) . . ?
N1 C14 H14 123.0 . . ?
N2 C14 H14 123.0 . . ?
N1 C15 C16 109.6(6) . . ?
N1 C15 C20 129.7(7) . . ?
C16 C15 C20 120.7(7) . . ?
N2 C16 C17 133.8(6) . . ?
C15 C16 N2 105.0(6) . . ?
C15 C16 C17 121.1(6) . . ?
C16 C17 H17 121.4 . . ?
C18 C17 C16 117.2(7) . . ?
C18 C17 H17 121.4 . . ?
C17 C18 H18 119.1 . . ?
C17 C18 C19 121.8(8) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 H19 119.1 . . ?
C20 C19 C18 121.8(7) . . ?
C20 C19 H19 119.1 . . ?
C15 C20 H20 121.4 . . ?
C19 C20 C15 117.2(7) . . ?
C19 C20 H20 121.4 . . ?
N3 C21 H21 123.1 . . ?
N4 C21 N3 113.7(6) . . ?
N4 C21 H21 123.1 . . ?
N3 C22 C23 133.2(6) . . ?
N3 C22 C27 105.0(5) . . ?
C23 C22 C27 121.7(6) . . ?
C22 C23 H23 121.5 . . ?
C24 C23 C22 116.9(7) . . ?
C24 C23 H23 121.5 . . ?
C23 C24 H24 119.4 . . ?
C23 C24 C25 121.3(7) . . ?
C25 C24 H24 119.4 . . ?
C24 C25 H25 119.0 . . ?
C26 C25 C24 121.9(7) . . ?
C26 C25 H25 119.0 . . ?
C25 C26 H26 121.3 . . ?
C25 C26 C27 117.3(7) . . ?
C27 C26 H26 121.3 . . ?
N4 C27 C22 108.9(6) . . ?
N4 C27 C26 130.3(6) . . ?
C26 C27 C22 120.8(6) . . ?
C1 C28 H28A 108.7 . . ?
C1 C28 H28B 108.7 . . ?
C1 C28 C29 114.4(5) . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C28 C29 H29A 108.7 . . ?
C28 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 C28 114.1(5) . . ?
C30 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
O1 C30 C29 119.4(7) . . ?
O2 C30 O1 119.6(8) . . ?
O2 C30 C29 121.0(7) . . ?
O2A C30 C29 114.9(11) . . ?
O1A C30 C29 123.5(12) . . ?
O1A C30 O2A 121.1(15) . . ?
C1 C31 H31A 108.9 . . ?
C1 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 C1 113.6(5) . . ?
C32 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C31 C32 H32A 108.6 . . ?
C31 C32 H32B 108.6 . . ?
H32A C32 H32B 107.6 . . ?
C33 C32 C31 114.6(6) . . ?
C33 C32 H32A 108.6 . . ?
C33 C32 H32B 108.6 . . ?
O3 C33 Pb1 55.7(4) . 2_657 ?
O3 C33 C32 120.3(7) . . ?
O4 C33 Pb1 62.6(5) . 2_657 ?
O4 C33 O3 117.8(8) . . ?
O4 C33 C32 121.9(8) . . ?
C32 C33 Pb1 170.7(5) . 2_657 ?
O4A C33 C32 124.1(14) . . ?
O4A C33 O3A 118.4(19) . . ?
O3A C33 C32 117.4(13) . . ?
C30 O2 Pb1 93.0(5) . . ?
C33 O4A Pb1 93.5(16) . 2_657 ?
C33 O3A Pb1 100.3(16) . 2_657 ?
C30 O2A Pb1 96.4(12) . . ?
C30 O1A Pb1 90.4(12) . . ?

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
C12 H12 O4 0.93 2.59 3.461(10) 156.2 2_667 yes
C20 H20 O4 0.93 2.48 3.129(12) 127.1 1_554 yes

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
Pb1 N4 C21 N3 -165.0(4) 2_757 . . . ?
Pb1 N4 C27 C22 164.5(4) 2_757 . . . ?
Pb1 N4 C27 C26 -14.6(10) 2_757 . . . ?
Pb1 O1 C30 C29 -166.6(6) . . . . ?
Pb1 O1 C30 O2 14.2(10) . . . . ?
Pb1 O3 C33 O4 -8.7(10) 2_657 . . . ?
Pb1 O3 C33 C32 170.0(6) 2_657 . . . ?
Pb1 O4 C33 O3 8.1(9) 2_657 . . . ?
Pb1 O4 C33 C32 -170.6(6) 2_657 . . . ?
N1 C15 C16 N2 -0.3(7) . . . . ?
N1 C15 C16 C17 -177.9(6) . . . . ?
N1 C15 C20 C19 -179.0(7) . . . . ?
N2 C4 C5 C6 -178.2(6) . . . . ?
N2 C16 C17 C18 179.3(7) . . . . ?
N3 C11 C12 C13 -177.5(6) . . . . ?
N3 C22 C23 C24 -178.5(7) . . . . ?
N3 C22 C27 N4 0.8(7) . . . . ?
N3 C22 C27 C26 179.9(6) . . . . ?
O1 C30 O2 Pb1 -14.1(10) . . . . ?
C1 C2 C3 C4 179.0(5) . . . . ?
C1 C2 C7 C6 -178.3(5) . . . . ?
C1 C2 C7 C8 1.2(6) . . . . ?
C1 C9 C10 C11 -177.5(5) . . . . ?
C1 C28 C29 C30 165.6(5) . . . . ?
C1 C31 C32 C33 -157.6(5) . . . . ?
C2 C1 C9 C8 0.0(6) . . . . ?
C2 C1 C9 C10 179.0(6) . . . . ?
C2 C1 C28 C29 53.8(6) . . . . ?
C2 C1 C31 C32 -52.1(6) . . . . ?
C2 C3 C4 N2 176.7(5) . . . . ?
C2 C3 C4 C5 -1.6(9) . . . . ?
C2 C7 C8 C9 -1.2(6) . . . . ?
C2 C7 C8 C13 178.4(6) . . . . ?
C3 C2 C7 C6 -0.7(8) . . . . ?
C3 C2 C7 C8 178.8(5) . . . . ?
C3 C4 C5 C6 0.1(9) . . . . ?
C4 N2 C14 N1 -174.0(6) . . . . ?
C4 N2 C16 C15 173.4(6) . . . . ?
C4 N2 C16 C17 -9.4(11) . . . . ?
C4 C5 C6 C7 1.1(9) . . . . ?
C5 C6 C7 C2 -0.8(9) . . . . ?
C5 C6 C7 C8 179.9(6) . . . . ?
C6 C7 C8 C9 178.2(6) . . . . ?
C6 C7 C8 C13 -2.2(11) . . . . ?
C7 C2 C3 C4 1.9(8) . . . . ?
C7 C8 C9 C1 0.7(6) . . . . ?
C7 C8 C9 C10 -178.3(5) . . . . ?
C7 C8 C13 C12 177.4(6) . . . . ?
C8 C9 C10 C11 1.4(8) . . . . ?
C9 C1 C2 C3 -178.1(6) . . . . ?
C9 C1 C2 C7 -0.8(6) . . . . ?
C9 C1 C28 C29 -59.3(6) . . . . ?
C9 C1 C31 C32 59.6(6) . . . . ?
C9 C8 C13 C12 -3.1(8) . . . . ?
C9 C10 C11 N3 176.5(5) . . . . ?
C9 C10 C11 C12 -3.8(9) . . . . ?
C10 C11 C12 C13 2.8(9) . . . . ?
C11 N3 C21 N4 178.8(6) . . . . ?
C11 N3 C22 C23 -1.0(11) . . . . ?
C11 N3 C22 C27 -179.0(6) . . . . ?
C11 C12 C13 C8 0.7(9) . . . . ?
C13 C8 C9 C1 -178.9(5) . . . . ?
C13 C8 C9 C10 2.0(8) . . . . ?
C14 N1 C15 C16 -0.4(8) . . . . ?
C14 N1 C15 C20 177.5(7) . . . . ?
C14 N2 C4 C3 -32.6(9) . . . . ?
C14 N2 C4 C5 145.7(6) . . . . ?
C14 N2 C16 C15 0.8(7) . . . . ?
C14 N2 C16 C17 178.0(7) . . . . ?
C15 N1 C14 N2 0.9(8) . . . . ?
C15 C16 C17 C18 -3.8(10) . . . . ?
C16 N2 C4 C3 156.2(6) . . . . ?
C16 N2 C4 C5 -25.5(9) . . . . ?
C16 N2 C14 N1 -1.1(8) . . . . ?
C16 C15 C20 C19 -1.4(11) . . . . ?
C16 C17 C18 C19 1.2(12) . . . . ?
C17 C18 C19 C20 1.3(13) . . . . ?
C18 C19 C20 C15 -1.3(12) . . . . ?
C20 C15 C16 N2 -178.4(6) . . . . ?
C20 C15 C16 C17 4.0(10) . . . . ?
C21 N3 C11 C10 143.9(6) . . . . ?
C21 N3 C11 C12 -35.8(9) . . . . ?
C21 N3 C22 C23 177.1(7) . . . . ?
C21 N3 C22 C27 -0.8(7) . . . . ?
C21 N4 C27 C22 -0.4(7) . . . . ?
C21 N4 C27 C26 -179.5(7) . . . . ?
C22 N3 C11 C10 -38.3(9) . . . . ?
C22 N3 C11 C12 142.1(6) . . . . ?
C22 N3 C21 N4 0.6(8) . . . . ?
C22 C23 C24 C25 -1.4(11) . . . . ?
C23 C22 C27 N4 -177.5(6) . . . . ?
C23 C22 C27 C26 1.7(10) . . . . ?
C23 C24 C25 C26 3.0(12) . . . . ?
C24 C25 C26 C27 -2.1(11) . . . . ?
C25 C26 C27 N4 178.8(7) . . . . ?
C25 C26 C27 C22 -0.2(10) . . . . ?
C27 N4 C21 N3 -0.1(8) . . . . ?
C27 C22 C23 C24 -0.9(10) . . . . ?
C28 C1 C2 C3 62.9(8) . . . . ?
C28 C1 C2 C7 -119.8(5) . . . . ?
C28 C1 C9 C8 120.0(5) . . . . ?
C28 C1 C9 C10 -61.0(7) . . . . ?
C28 C1 C31 C32 -177.5(5) . . . . ?
C28 C29 C30 O1 35.4(11) . . . . ?
C28 C29 C30 O2 -145.4(8) . . . . ?
C28 C29 C30 O2A -89.6(16) . . . . ?
C28 C29 C30 O1A 82.2(18) . . . . ?
C29 C30 O2 Pb1 166.7(6) . . . . ?
C29 C30 O2A Pb1 171.0(6) . . . . ?
C29 C30 O1A Pb1 -170.3(7) . . . . ?
C31 C1 C2 C3 -60.9(8) . . . . ?
C31 C1 C2 C7 116.4(5) . . . . ?
C31 C1 C9 C8 -117.8(5) . . . . ?
C31 C1 C9 C10 61.1(8) . . . . ?
C31 C1 C28 C29 178.4(5) . . . . ?
C31 C32 C33 O3 -34.4(10) . . . . ?
C31 C32 C33 O4 144.2(9) . . . . ?
C31 C32 C33 O4A -109(2) . . . . ?
C31 C32 C33 O3A 67.5(18) . . . . ?
C32 C33 O4A Pb1 172.8(8) . . . 2_657 ?
C32 C33 O3A Pb1 -172.8(6) . . . 2_657 ?
O4A C33 O3A Pb1 4(2) . . . 2_657 ?
O3A C33 O4A Pb1 -3(2) . . . 2_657 ?
O2A C30 O1A Pb1 0.9(19) . . . . ?
O1A C30 O2A Pb1 -1(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'



