# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1487747'
_audit_update_record             
;
2016-06-24 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H68 Cl2 N8 O4 Pb'
_chemical_formula_sum            'C62 H68 Cl2 N8 O4 Pb'
_chemical_formula_weight         1267.33

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.8819(5)
_cell_length_b                   23.8685(11)
_cell_length_c                   13.7122(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.846(4)
_cell_angle_gamma                90
_cell_volume                     2905.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    3371
_cell_measurement_theta_min      3.2400
_cell_measurement_theta_max      27.2800

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.049
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.02533
_exptl_absorpt_correction_T_max  0.04753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       ω-scan
_diffrn_reflns_number            11316
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.774
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5120
_reflns_number_gt                3470
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2015)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0106P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5120
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0514
_refine_ls_wR_factor_gt          0.0459
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.0000 0.5000 0.0000 0.04058(7) Uani 1 2 d S . P . .
Cl1 Cl 0.25553(11) 0.55243(5) -0.07562(8) 0.0687(3) Uani 1 1 d . . . . .
O1 O 0.6059(3) 0.40353(12) 0.6654(2) 0.0631(8) Uani 1 1 d . . . . .
C2 C 0.6930(4) 0.39631(19) 0.7536(3) 0.0674(14) Uani 1 1 d . . . . .
H2A H 0.7492 0.4303 0.7685 0.081 Uiso 1 1 calc R U . . .
H2B H 0.7644 0.3660 0.7461 0.081 Uiso 1 1 calc R U . . .
C3 C 0.5909(4) 0.38327(19) 0.8347(3) 0.0666(13) Uani 1 1 d . . . . .
H3A H 0.6456 0.3859 0.8969 0.080 Uiso 1 1 calc R U . . .
H3B H 0.5081 0.4097 0.8346 0.080 Uiso 1 1 calc R U . . .
O4 O 0.5345(3) 0.32747(13) 0.82037(19) 0.0625(8) Uani 1 1 d . . . . .
C5 C 0.4594(4) 0.30245(19) 0.8945(3) 0.0523(11) Uani 1 1 d . . . . .
C6 C 0.4395(4) 0.32627(19) 0.9851(3) 0.0605(13) Uani 1 1 d . . . . .
H6 H 0.4754 0.3621 0.9985 0.073 Uiso 1 1 calc R U . . .
C7 C 0.3660(5) 0.2965(2) 1.0555(3) 0.0655(13) Uani 1 1 d . . . . .
H7 H 0.3511 0.3129 1.1159 0.079 Uiso 1 1 calc R U . . .
C8 C 0.3141(4) 0.2428(2) 1.0375(3) 0.0624(13) Uani 1 1 d . . . . .
H8 H 0.2685 0.2223 1.0862 0.075 Uiso 1 1 calc R U . . .
C9 C 0.3312(4) 0.22008(18) 0.9458(3) 0.0561(12) Uani 1 1 d . . . . .
H9 H 0.2959 0.1841 0.9331 0.067 Uiso 1 1 calc R U . . .
C10 C 0.3989(4) 0.24928(18) 0.8731(3) 0.0492(11) Uani 1 1 d . . . . .
C11 C 0.4074(4) 0.22536(16) 0.7712(3) 0.0520(11) Uani 1 1 d . . . . .
H11A H 0.5112 0.2261 0.7514 0.062 Uiso 1 1 calc R U . . .
H11B H 0.3748 0.1866 0.7719 0.062 Uiso 1 1 calc R U . . .
N12 N 0.3134(3) 0.25665(12) 0.6995(2) 0.0397(8) Uani 1 1 d . . . . .
C13 C 0.3234(4) 0.23261(16) 0.6020(3) 0.0504(11) Uani 1 1 d . . . . .
H13A H 0.2537 0.2015 0.5952 0.060 Uiso 1 1 calc R U . . .
H13B H 0.4244 0.2183 0.5935 0.060 Uiso 1 1 calc R U . . .
C14 C 0.2868(4) 0.27594(16) 0.5235(2) 0.0474(11) Uani 1 1 d . . . . .
H14A H 0.1884 0.2920 0.5344 0.057 Uiso 1 1 calc R U . . .
H14B H 0.2833 0.2580 0.4600 0.057 Uiso 1 1 calc R U . . .
C15 C 0.4051(4) 0.32239(16) 0.5249(2) 0.0459(10) Uani 1 1 d . . . . .
H15A H 0.4172 0.3368 0.5908 0.055 Uiso 1 1 calc R U . . .
H15B H 0.5009 0.3067 0.5067 0.055 Uiso 1 1 calc R U . . .
N16 N 0.3664(3) 0.36854(14) 0.4591(2) 0.0449(8) Uani 1 1 d . . . . .
C17 C 0.4273(4) 0.42308(16) 0.4938(3) 0.0521(11) Uani 1 1 d . . . . .
H17A H 0.3893 0.4302 0.5582 0.062 Uiso 1 1 calc R U . . .
H17B H 0.3878 0.4522 0.4508 0.062 Uiso 1 1 calc R U . . .
C18 C 0.5976(5) 0.42837(16) 0.4997(3) 0.0510(11) Uani 1 1 d . . . . .
C19 C 0.6735(5) 0.44536(18) 0.4177(3) 0.0675(13) Uani 1 1 d . . . . .
H19 H 0.6180 0.4546 0.3612 0.081 Uiso 1 1 calc R U . . .
C20 C 0.8286(6) 0.4490(2) 0.4172(4) 0.0786(15) Uani 1 1 d . . . . .
H20 H 0.8761 0.4602 0.3610 0.094 Uiso 1 1 calc R U . . .
C21 C 0.9117(5) 0.4362(2) 0.4992(4) 0.0852(17) Uani 1 1 d . . . . .
H21 H 1.0163 0.4378 0.4986 0.102 Uiso 1 1 calc R U . . .
C22 C 0.8413(5) 0.42070(19) 0.5832(3) 0.0711(14) Uani 1 1 d . . . . .
H22 H 0.8984 0.4128 0.6395 0.085 Uiso 1 1 calc R U . . .
C23 C 0.6851(5) 0.41689(17) 0.5839(3) 0.0566(12) Uani 1 1 d . . . . .
C24 C 0.1570(4) 0.26213(16) 0.7293(3) 0.0456(10) Uani 1 1 d . . . . .
H24A H 0.1316 0.2298 0.7683 0.055 Uiso 1 1 calc R U . . .
H24B H 0.0913 0.2619 0.6713 0.055 Uiso 1 1 calc R U . . .
C25 C 0.1267(4) 0.31426(17) 0.7868(3) 0.0393(10) Uani 1 1 d . . . . .
C26 C 0.0389(4) 0.31323(18) 0.8676(3) 0.0510(11) Uani 1 1 d . . . . .
H26 H -0.0006 0.2795 0.8891 0.061 Uiso 1 1 calc R U . . .
C27 C 0.0094(4) 0.3622(2) 0.9168(3) 0.0582(12) Uani 1 1 d . . . . .
H27 H -0.0498 0.3602 0.9714 0.070 Uiso 1 1 calc R U . . .
N28 N 0.0607(3) 0.41190(15) 0.8905(2) 0.0550(9) Uani 1 1 d . . . . .
C29 C 0.1476(4) 0.41273(18) 0.8129(3) 0.0566(12) Uani 1 1 d . . . . .
H29 H 0.1877 0.4469 0.7940 0.068 Uiso 1 1 calc R U . . .
C30 C 0.1811(4) 0.36570(18) 0.7594(3) 0.0506(11) Uani 1 1 d . . . . .
H30 H 0.2402 0.3687 0.7049 0.061 Uiso 1 1 calc R U . . .
C31 C 0.4054(4) 0.35550(16) 0.3594(3) 0.0470(10) Uani 1 1 d . . . . .
H31A H 0.3796 0.3168 0.3455 0.056 Uiso 1 1 calc R U . . .
H31B H 0.5134 0.3595 0.3533 0.056 Uiso 1 1 calc R U . . .
C32 C 0.3259(4) 0.39269(17) 0.2850(3) 0.0458(10) Uani 1 1 d . . . . .
C33 C 0.1711(4) 0.39776(18) 0.2857(3) 0.0602(13) Uani 1 1 d . . . . .
H33 H 0.1169 0.3810 0.3348 0.072 Uiso 1 1 calc R U . . .
C34 C 0.0981(5) 0.4279(2) 0.2130(3) 0.0749(16) Uani 1 1 d . . . . .
H34 H -0.0063 0.4304 0.2143 0.090 Uiso 1 1 calc R U . . .
N35 N 0.1667(4) 0.45392(16) 0.1407(2) 0.0653(11) Uani 1 1 d . . . . .
C36 C 0.3164(5) 0.44955(19) 0.1415(3) 0.0623(13) Uani 1 1 d . . . . .
H36 H 0.3684 0.4679 0.0931 0.075 Uiso 1 1 calc R U . . .
C37 C 0.3985(4) 0.41893(17) 0.2112(3) 0.0522(11) Uani 1 1 d . . . . .
H37 H 0.5026 0.4163 0.2077 0.063 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
Pb1 N35 2.634(3) 3_565 ?
Pb1 N35 2.634(3) . ?
Pb1 N28 2.649(3) 3_566 ?
Pb1 N28 2.649(3) 1_554 ?
Pb1 Cl1 2.8185(10) 3_565 ?
Pb1 Cl1 2.8185(10) . ?
O1 C23 1.377(4) . ?
O1 C2 1.425(4) . ?
C2 C3 1.490(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O4 1.434(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O4 C5 1.371(5) . ?
C5 C6 1.383(5) . ?
C5 C10 1.405(5) . ?
C6 C7 1.379(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.382(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.371(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.514(5) . ?
C11 N12 1.472(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N12 C13 1.460(4) . ?
N12 C24 1.467(4) . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.527(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N16 1.458(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
N16 C31 1.455(4) . ?
N16 C17 1.482(4) . ?
C17 C18 1.517(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.390(5) . ?
C18 C23 1.398(5) . ?
C19 C20 1.381(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.359(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.379(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.391(5) . ?
C22 H22 0.9300 . ?
C24 C25 1.502(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.376(5) . ?
C25 C30 1.376(5) . ?
C26 C27 1.378(5) . ?
C26 H26 0.9300 . ?
C27 N28 1.326(5) . ?
C27 H27 0.9300 . ?
N28 C29 1.334(4) . ?
N28 Pb1 2.649(3) 1_556 ?
C29 C30 1.379(5) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.510(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C37 1.369(5) . ?
C32 C33 1.380(4) . ?
C33 C34 1.376(5) . ?
C33 H33 0.9300 . ?
C34 N35 1.333(5) . ?
C34 H34 0.9300 . ?
N35 C36 1.333(4) . ?
C36 C37 1.391(5) . ?
C36 H36 0.9300 . ?
C37 H37 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
N35 Pb1 N35 180.0 3_565 . ?
N35 Pb1 N28 87.92(11) 3_565 3_566 ?
N35 Pb1 N28 92.08(11) . 3_566 ?
N35 Pb1 N28 92.08(10) 3_565 1_554 ?
N35 Pb1 N28 87.92(11) . 1_554 ?
N28 Pb1 N28 180.00(14) 3_566 1_554 ?
N35 Pb1 Cl1 90.84(8) 3_565 3_565 ?
N35 Pb1 Cl1 89.16(8) . 3_565 ?
N28 Pb1 Cl1 87.88(8) 3_566 3_565 ?
N28 Pb1 Cl1 92.12(8) 1_554 3_565 ?
N35 Pb1 Cl1 89.16(8) 3_565 . ?
N35 Pb1 Cl1 90.84(8) . . ?
N28 Pb1 Cl1 92.12(8) 3_566 . ?
N28 Pb1 Cl1 87.88(8) 1_554 . ?
Cl1 Pb1 Cl1 180.0 3_565 . ?
C23 O1 C2 116.0(3) . . ?
O1 C2 C3 109.3(3) . . ?
O1 C2 H2A 109.8 . . ?
C3 C2 H2A 109.8 . . ?
O1 C2 H2B 109.8 . . ?
C3 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
O4 C3 C2 108.1(4) . . ?
O4 C3 H3A 110.1 . . ?
C2 C3 H3A 110.1 . . ?
O4 C3 H3B 110.1 . . ?
C2 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
C5 O4 C3 118.6(3) . . ?
O4 C5 C6 124.5(4) . . ?
O4 C5 C10 115.5(4) . . ?
C6 C5 C10 120.0(4) . . ?
C7 C6 C5 119.6(4) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C8 121.1(4) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 118.7(4) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C10 C9 C8 121.7(4) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C5 118.8(4) . . ?
C9 C10 C11 121.0(4) . . ?
C5 C10 C11 120.2(4) . . ?
N12 C11 C10 112.4(3) . . ?
N12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
N12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C13 N12 C24 112.1(3) . . ?
C13 N12 C11 111.3(3) . . ?
C24 N12 C11 112.4(3) . . ?
N12 C13 C14 111.3(3) . . ?
N12 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
N12 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 C15 110.7(3) . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N16 C15 C14 113.1(3) . . ?
N16 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
N16 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C31 N16 C15 111.2(3) . . ?
C31 N16 C17 113.2(3) . . ?
C15 N16 C17 112.9(3) . . ?
N16 C17 C18 116.3(3) . . ?
N16 C17 H17A 108.2 . . ?
C18 C17 H17A 108.2 . . ?
N16 C17 H17B 108.2 . . ?
C18 C17 H17B 108.2 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C23 117.0(4) . . ?
C19 C18 C17 119.4(4) . . ?
C23 C18 C17 123.6(4) . . ?
C20 C19 C18 122.1(4) . . ?
C20 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
C21 C20 C19 119.8(5) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.1(5) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C23 120.2(4) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
O1 C23 C22 123.8(4) . . ?
O1 C23 C18 115.5(4) . . ?
C22 C23 C18 120.6(4) . . ?
N12 C24 C25 114.0(3) . . ?
N12 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
N12 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C26 C25 C30 116.7(4) . . ?
C26 C25 C24 121.6(4) . . ?
C30 C25 C24 121.7(4) . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
N28 C27 C26 123.6(4) . . ?
N28 C27 H27 118.2 . . ?
C26 C27 H27 118.2 . . ?
C27 N28 C29 116.3(4) . . ?
C27 N28 Pb1 118.6(3) . 1_556 ?
C29 N28 Pb1 125.0(3) . 1_556 ?
N28 C29 C30 123.6(4) . . ?
N28 C29 H29 118.2 . . ?
C30 C29 H29 118.2 . . ?
C25 C30 C29 119.8(4) . . ?
C25 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
N16 C31 C32 112.9(3) . . ?
N16 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
N16 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C37 C32 C33 117.3(4) . . ?
C37 C32 C31 123.2(4) . . ?
C33 C32 C31 119.4(4) . . ?
C34 C33 C32 119.1(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
N35 C34 C33 124.5(4) . . ?
N35 C34 H34 117.7 . . ?
C33 C34 H34 117.7 . . ?
C34 N35 C36 115.9(3) . . ?
C34 N35 Pb1 118.6(3) . . ?
C36 N35 Pb1 125.1(3) . . ?
N35 C36 C37 123.2(4) . . ?
N35 C36 H36 118.4 . . ?
C37 C36 H36 118.4 . . ?
C32 C37 C36 120.0(4) . . ?
C32 C37 H37 120.0 . . ?
C36 C37 H37 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
C23 O1 C2 C3 178.8(4) . . . . ?
O1 C2 C3 O4 71.5(4) . . . . ?
C2 C3 O4 C5 168.7(3) . . . . ?
C3 O4 C5 C6 -3.2(5) . . . . ?
C3 O4 C5 C10 176.1(3) . . . . ?
O4 C5 C6 C7 -177.9(4) . . . . ?
C10 C5 C6 C7 2.9(6) . . . . ?
C5 C6 C7 C8 1.2(6) . . . . ?
C6 C7 C8 C9 -2.8(6) . . . . ?
C7 C8 C9 C10 0.5(6) . . . . ?
C8 C9 C10 C5 3.5(6) . . . . ?
C8 C9 C10 C11 -175.8(3) . . . . ?
O4 C5 C10 C9 175.6(3) . . . . ?
C6 C5 C10 C9 -5.1(5) . . . . ?
O4 C5 C10 C11 -5.1(5) . . . . ?
C6 C5 C10 C11 174.2(3) . . . . ?
C9 C10 C11 N12 111.8(4) . . . . ?
C5 C10 C11 N12 -67.5(4) . . . . ?
C10 C11 N12 C13 -179.8(3) . . . . ?
C10 C11 N12 C24 -53.2(4) . . . . ?
C24 N12 C13 C14 77.8(4) . . . . ?
C11 N12 C13 C14 -155.5(3) . . . . ?
N12 C13 C14 C15 65.4(4) . . . . ?
C13 C14 C15 N16 -173.1(3) . . . . ?
C14 C15 N16 C31 -81.7(4) . . . . ?
C14 C15 N16 C17 149.8(3) . . . . ?
C31 N16 C17 C18 -63.0(4) . . . . ?
C15 N16 C17 C18 64.4(4) . . . . ?
N16 C17 C18 C19 87.1(5) . . . . ?
N16 C17 C18 C23 -92.7(4) . . . . ?
C23 C18 C19 C20 2.2(7) . . . . ?
C17 C18 C19 C20 -177.6(4) . . . . ?
C18 C19 C20 C21 -0.5(7) . . . . ?
C19 C20 C21 C22 -1.4(8) . . . . ?
C20 C21 C22 C23 1.5(8) . . . . ?
C2 O1 C23 C22 3.2(6) . . . . ?
C2 O1 C23 C18 -175.0(4) . . . . ?
C21 C22 C23 O1 -177.8(4) . . . . ?
C21 C22 C23 C18 0.3(7) . . . . ?
C19 C18 C23 O1 176.2(4) . . . . ?
C17 C18 C23 O1 -4.0(6) . . . . ?
C19 C18 C23 C22 -2.1(6) . . . . ?
C17 C18 C23 C22 177.7(4) . . . . ?
C13 N12 C24 C25 -142.4(3) . . . . ?
C11 N12 C24 C25 91.5(4) . . . . ?
N12 C24 C25 C26 -137.8(3) . . . . ?
N12 C24 C25 C30 44.5(5) . . . . ?
C30 C25 C26 C27 0.0(5) . . . . ?
C24 C25 C26 C27 -177.8(3) . . . . ?
C25 C26 C27 N28 0.4(6) . . . . ?
C26 C27 N28 C29 -1.3(6) . . . . ?
C26 C27 N28 Pb1 -177.4(3) . . . 1_556 ?
C27 N28 C29 C30 1.9(6) . . . . ?
Pb1 N28 C29 C30 177.7(3) 1_556 . . . ?
C26 C25 C30 C29 0.6(5) . . . . ?
C24 C25 C30 C29 178.4(3) . . . . ?
N28 C29 C30 C25 -1.6(6) . . . . ?
C15 N16 C31 C32 162.1(3) . . . . ?
C17 N16 C31 C32 -69.7(4) . . . . ?
N16 C31 C32 C37 132.0(4) . . . . ?
N16 C31 C32 C33 -52.9(5) . . . . ?
C37 C32 C33 C34 0.7(6) . . . . ?
C31 C32 C33 C34 -174.7(4) . . . . ?
C32 C33 C34 N35 -0.9(7) . . . . ?
C33 C34 N35 C36 -0.2(7) . . . . ?
C33 C34 N35 Pb1 173.6(4) . . . . ?
C34 N35 C36 C37 1.5(6) . . . . ?
Pb1 N35 C36 C37 -171.9(3) . . . . ?
C33 C32 C37 C36 0.6(6) . . . . ?
C31 C32 C37 C36 175.7(4) . . . . ?
N35 C36 C37 C32 -1.7(7) . . . . ?

_refine_diff_density_max         0.520
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.073

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1542746'
_audit_update_record             
;
2017-10-02 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H68 Cl2 Mn N8 O4'
_chemical_formula_sum            'C62 H68 Cl2 Mn N8 O4'
_chemical_formula_weight         1115.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.5005(2)
_cell_length_b                   23.2999(6)
_cell_length_c                   13.6047(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.102(2)
_cell_angle_gamma                90
_cell_volume                     2694.06(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(1)
_cell_measurement_reflns_used    4312
_cell_measurement_theta_min      3.4630
_cell_measurement_theta_max      28.1740

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_F_000             1174
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.402
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.99147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       '/w scan'
_diffrn_reflns_number            11378
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.801
_diffrn_reflns_theta_max         28.635
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5801
_reflns_number_gt                4324
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0268P)²+1.0931P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5801
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0812
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.5000 1.0000 0.01938(12) Uani 1 2 d S . P . .
Cl1 Cl -0.25449(6) 0.45746(2) 1.06078(4) 0.02435(13) Uani 1 1 d . . . . .
O1 O 0.50866(17) 0.33032(7) 0.81698(10) 0.0265(4) Uani 1 1 d . . . . .
C2 C 0.5677(3) 0.38733(10) 0.83221(15) 0.0271(5) Uani 1 1 d . . . . .
H2A H 0.6269 0.3896 0.8955 0.033 Uiso 1 1 calc R U . . .
H2B H 0.4797 0.4151 0.8337 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6736(3) 0.40054(11) 0.74862(14) 0.0272(5) Uani 1 1 d . . . . .
H3A H 0.7324 0.4364 0.7625 0.033 Uiso 1 1 calc R U . . .
H3B H 0.7506 0.3691 0.7408 0.033 Uiso 1 1 calc R U . . .
O4 O 0.58192(16) 0.40698(7) 0.65996(10) 0.0251(4) Uani 1 1 d . . . . .
C5 C 0.6633(2) 0.41942(10) 0.57646(15) 0.0236(5) Uani 1 1 d . . . . .
C6 C 0.5735(2) 0.43089(10) 0.49130(15) 0.0235(5) Uani 1 1 d . . . . .
C7 C 0.3956(2) 0.42579(10) 0.48587(15) 0.0232(5) Uani 1 1 d . . . . .
H7A H 0.3541 0.4333 0.5521 0.028 Uiso 1 1 calc R U . . .
H7B H 0.3544 0.4562 0.4416 0.028 Uiso 1 1 calc R U . . .
N8 N 0.3331(2) 0.37034(8) 0.45138(11) 0.0212(4) Uani 1 1 d . . . . .
C9 C 0.3702(2) 0.32351(9) 0.51931(14) 0.0218(5) Uani 1 1 d . . . . .
H9A H 0.3830 0.3393 0.5865 0.026 Uiso 1 1 calc R U . . .
H9B H 0.4717 0.3061 0.5009 0.026 Uiso 1 1 calc R U . . .
C10 C 0.2448(2) 0.27722(10) 0.51977(14) 0.0235(5) Uani 1 1 d . . . . .
H10A H 0.2400 0.2579 0.4550 0.028 Uiso 1 1 calc R U . . .
H10B H 0.1408 0.2948 0.5316 0.028 Uiso 1 1 calc R U . . .
C11 C 0.2826(3) 0.23361(10) 0.59970(14) 0.0235(5) Uani 1 1 d . . . . .
H11A H 0.2059 0.2017 0.5957 0.028 Uiso 1 1 calc R U . . .
H11B H 0.3888 0.2175 0.5893 0.028 Uiso 1 1 calc R U . . .
N12 N 0.27742(19) 0.25979(8) 0.69730(11) 0.0206(4) Uani 1 1 d . . . . .
C13 C 0.3744(2) 0.22666(10) 0.76762(14) 0.0242(5) Uani 1 1 d . . . . .
H13A H 0.4848 0.2267 0.7457 0.029 Uiso 1 1 calc R U . . .
H13B H 0.3374 0.1864 0.7680 0.029 Uiso 1 1 calc R U . . .
C14 C 0.3687(2) 0.25042(10) 0.87048(14) 0.0219(5) Uani 1 1 d . . . . .
C15 C 0.4307(2) 0.30482(10) 0.89210(14) 0.0230(5) Uani 1 1 d . . . . .
C16 C 0.4115(3) 0.32893(11) 0.98406(15) 0.0274(5) Uani 1 1 d . . . . .
H16 H 0.4509 0.3663 0.9980 0.033 Uiso 1 1 calc R U . . .
C17 C 0.3342(3) 0.29798(11) 1.05582(15) 0.0296(5) Uani 1 1 d . . . . .
H17 H 0.3181 0.3149 1.1184 0.035 Uiso 1 1 calc R U . . .
C18 C 0.2807(3) 0.24339(11) 1.03759(15) 0.0285(5) Uani 1 1 d . . . . .
H18 H 0.2326 0.2219 1.0881 0.034 Uiso 1 1 calc R U . . .
C19 C 0.2975(2) 0.21997(10) 0.94476(15) 0.0257(5) Uani 1 1 d . . . . .
H19 H 0.2595 0.1823 0.9319 0.031 Uiso 1 1 calc R U . . .
C20 C 0.8263(3) 0.42217(10) 0.57543(16) 0.0286(5) Uani 1 1 d . . . . .
H20 H 0.8861 0.4138 0.6333 0.034 Uiso 1 1 calc R U . . .
C21 C 0.9016(3) 0.43722(11) 0.48968(16) 0.0323(6) Uani 1 1 d . . . . .
H21 H 1.0133 0.4380 0.4885 0.039 Uiso 1 1 calc R U . . .
C22 C 0.8155(3) 0.45107(10) 0.40618(16) 0.0305(5) Uani 1 1 d . . . . .
H22 H 0.8669 0.4626 0.3481 0.037 Uiso 1 1 calc R U . . .
C23 C 0.6537(3) 0.44793(10) 0.40809(16) 0.0274(5) Uani 1 1 d . . . . .
H23 H 0.5948 0.4578 0.3505 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3796(2) 0.35637(10) 0.35161(14) 0.0228(5) Uani 1 1 d . . . . .
H24A H 0.3542 0.3156 0.3380 0.027 Uiso 1 1 calc R U . . .
H24B H 0.4950 0.3611 0.3466 0.027 Uiso 1 1 calc R U . . .
C25 C 0.2994(2) 0.39339(9) 0.27517(14) 0.0217(5) Uani 1 1 d . . . . .
C26 C 0.3800(2) 0.42097(10) 0.20090(14) 0.0238(5) Uani 1 1 d . . . . .
H26 H 0.4916 0.4193 0.1994 0.029 Uiso 1 1 calc R U . . .
C27 C 0.2970(3) 0.45077(10) 0.12930(14) 0.0249(5) Uani 1 1 d . . . . .
H27 H 0.3543 0.4698 0.0797 0.030 Uiso 1 1 calc R U . . .
N28 N 0.1391(2) 0.45426(8) 0.12600(11) 0.0228(4) Uani 1 1 d . . . . .
C29 C 0.0632(3) 0.42718(10) 0.19765(14) 0.0267(5) Uani 1 1 d . . . . .
H29 H -0.0486 0.4284 0.1966 0.032 Uiso 1 1 calc R U . . .
C30 C 0.1372(2) 0.39760(10) 0.27281(14) 0.0249(5) Uani 1 1 d . . . . .
H30 H 0.0772 0.3801 0.3228 0.030 Uiso 1 1 calc R U . . .
C31 C 0.1159(2) 0.26751(10) 0.73029(15) 0.0230(5) Uani 1 1 d . . . . .
H31A H 0.0853 0.2335 0.7692 0.028 Uiso 1 1 calc R U . . .
H31B H 0.0446 0.2696 0.6720 0.028 Uiso 1 1 calc R U . . .
C32 C 0.0940(2) 0.32073(9) 0.79177(14) 0.0202(5) Uani 1 1 d . . . . .
C33 C 0.1520(2) 0.37377(10) 0.76363(15) 0.0239(5) Uani 1 1 d . . . . .
H33 H 0.2108 0.3771 0.7052 0.029 Uiso 1 1 calc R U . . .
C34 C 0.1243(2) 0.42152(10) 0.82034(15) 0.0243(5) Uani 1 1 d . . . . .
H34 H 0.1669 0.4572 0.7999 0.029 Uiso 1 1 calc R U . . .
N35 N 0.0405(2) 0.42042(8) 0.90283(11) 0.0216(4) Uani 1 1 d . . . . .
C36 C -0.0149(2) 0.36947(10) 0.92947(15) 0.0250(5) Uani 1 1 d . . . . .
H36 H -0.0743 0.3674 0.9878 0.030 Uiso 1 1 calc R U . . .
C37 C 0.0088(2) 0.31949(10) 0.87752(14) 0.0233(5) Uani 1 1 d . . . . .
H37 H -0.0333 0.2843 0.9005 0.028 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
Mn1 N35 2.3069(17) 3_567 ?
Mn1 N35 2.3070(17) . ?
Mn1 N28 2.3224(17) 3_566 ?
Mn1 N28 2.3224(17) 1_556 ?
Mn1 Cl1 2.5327(5) . ?
Mn1 Cl1 2.5327(5) 3_567 ?
O1 C15 1.365(2) . ?
O1 C2 1.434(3) . ?
C2 C3 1.496(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O4 1.431(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C5 1.372(2) . ?
C5 C20 1.387(3) . ?
C5 C6 1.401(3) . ?
C6 C23 1.390(3) . ?
C6 C7 1.518(3) . ?
C7 N8 1.470(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C24 1.458(2) . ?
N8 C9 1.460(3) . ?
C9 C10 1.517(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.518(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N12 1.463(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N12 C31 1.464(3) . ?
N12 C13 1.470(3) . ?
C13 C14 1.506(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.384(3) . ?
C14 C15 1.402(3) . ?
C15 C16 1.384(3) . ?
C16 C17 1.389(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.372(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.387(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.378(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.504(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.382(3) . ?
C25 C26 1.389(3) . ?
C26 C27 1.379(3) . ?
C26 H26 0.9500 . ?
C27 N28 1.345(3) . ?
C27 H27 0.9500 . ?
N28 C29 1.337(3) . ?
N28 Mn1 2.3224(17) 1_554 ?
C29 C30 1.376(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.509(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C37 1.385(3) . ?
C32 C33 1.387(3) . ?
C33 C34 1.377(3) . ?
C33 H33 0.9500 . ?
C34 N35 1.341(2) . ?
C34 H34 0.9500 . ?
N35 C36 1.330(3) . ?
C36 C37 1.379(3) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?

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
N35 Mn1 N35 180.0 3_567 . ?
N35 Mn1 N28 88.54(6) 3_567 3_566 ?
N35 Mn1 N28 91.46(6) . 3_566 ?
N35 Mn1 N28 91.46(6) 3_567 1_556 ?
N35 Mn1 N28 88.54(6) . 1_556 ?
N28 Mn1 N28 180.0 3_566 1_556 ?
N35 Mn1 Cl1 89.41(4) 3_567 . ?
N35 Mn1 Cl1 90.60(4) . . ?
N28 Mn1 Cl1 89.70(4) 3_566 . ?
N28 Mn1 Cl1 90.30(4) 1_556 . ?
N35 Mn1 Cl1 90.59(4) 3_567 3_567 ?
N35 Mn1 Cl1 89.40(4) . 3_567 ?
N28 Mn1 Cl1 90.30(4) 3_566 3_567 ?
N28 Mn1 Cl1 89.70(4) 1_556 3_567 ?
Cl1 Mn1 Cl1 180.0 . 3_567 ?
C15 O1 C2 117.95(16) . . ?
O1 C2 C3 107.15(18) . . ?
O1 C2 H2A 110.3 . . ?
C3 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C3 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
O4 C3 C2 109.68(17) . . ?
O4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
O4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 O4 C3 116.43(15) . . ?
O4 C5 C20 122.50(19) . . ?
O4 C5 C6 116.75(18) . . ?
C20 C5 C6 120.7(2) . . ?
C23 C6 C5 117.4(2) . . ?
C23 C6 C7 119.11(19) . . ?
C5 C6 C7 123.49(19) . . ?
N8 C7 C6 115.95(18) . . ?
N8 C7 H7A 108.3 . . ?
C6 C7 H7A 108.3 . . ?
N8 C7 H7B 108.3 . . ?
C6 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C24 N8 C9 111.30(17) . . ?
C24 N8 C7 113.00(17) . . ?
C9 N8 C7 112.48(15) . . ?
N8 C9 C10 113.01(16) . . ?
N8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C11 109.85(17) . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N12 C11 C10 111.19(18) . . ?
N12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
N12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C11 N12 C31 112.00(16) . . ?
C11 N12 C13 110.21(16) . . ?
C31 N12 C13 112.50(16) . . ?
N12 C13 C14 112.56(17) . . ?
N12 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
N12 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C19 C14 C15 118.58(19) . . ?
C19 C14 C13 120.8(2) . . ?
C15 C14 C13 120.55(19) . . ?
O1 C15 C16 124.6(2) . . ?
O1 C15 C14 114.99(18) . . ?
C16 C15 C14 120.4(2) . . ?
C15 C16 C17 119.3(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 120.9(2) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C19 119.4(2) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C14 C19 C18 121.2(2) . . ?
C14 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C21 C20 C5 119.8(2) . . ?
C21 C20 H20 120.1 . . ?
C5 C20 H20 120.1 . . ?
C22 C21 C20 120.4(2) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 119.1(2) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C6 122.4(2) . . ?
C22 C23 H23 118.8 . . ?
C6 C23 H23 118.8 . . ?
N8 C24 C25 112.84(17) . . ?
N8 C24 H24A 109.0 . . ?
C25 C24 H24A 109.0 . . ?
N8 C24 H24B 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C30 C25 C26 117.13(19) . . ?
C30 C25 C24 119.71(19) . . ?
C26 C25 C24 123.00(19) . . ?
C27 C26 C25 119.59(19) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
N28 C27 C26 123.4(2) . . ?
N28 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
C29 N28 C27 116.25(17) . . ?
C29 N28 Mn1 120.58(13) . 1_554 ?
C27 N28 Mn1 123.09(14) . 1_554 ?
N28 C29 C30 123.9(2) . . ?
N28 C29 H29 118.0 . . ?
C30 C29 H29 118.0 . . ?
C29 C30 C25 119.7(2) . . ?
C29 C30 H30 120.2 . . ?
C25 C30 H30 120.2 . . ?
N12 C31 C32 113.41(18) . . ?
N12 C31 H31A 108.9 . . ?
C32 C31 H31A 108.9 . . ?
N12 C31 H31B 108.9 . . ?
C32 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C37 C32 C33 116.4(2) . . ?
C37 C32 C31 121.4(2) . . ?
C33 C32 C31 122.06(18) . . ?
C34 C33 C32 119.99(19) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
N35 C34 C33 123.6(2) . . ?
N35 C34 H34 118.2 . . ?
C33 C34 H34 118.2 . . ?
C36 N35 C34 116.22(19) . . ?
C36 N35 Mn1 120.24(13) . . ?
C34 N35 Mn1 123.49(15) . . ?
N35 C36 C37 123.93(19) . . ?
N35 C36 H36 118.0 . . ?
C37 C36 H36 118.0 . . ?
C36 C37 C32 119.9(2) . . ?
C36 C37 H37 120.1 . . ?
C32 C37 H37 120.1 . . ?

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
C15 O1 C2 C3 169.04(16) . . . . ?
O1 C2 C3 O4 70.0(2) . . . . ?
C2 C3 O4 C5 179.85(19) . . . . ?
C3 O4 C5 C20 4.0(3) . . . . ?
C3 O4 C5 C6 -174.41(19) . . . . ?
O4 C5 C6 C23 175.1(2) . . . . ?
C20 C5 C6 C23 -3.3(3) . . . . ?
O4 C5 C6 C7 -4.7(3) . . . . ?
C20 C5 C6 C7 176.9(2) . . . . ?
C23 C6 C7 N8 86.9(2) . . . . ?
C5 C6 C7 N8 -93.2(2) . . . . ?
C6 C7 N8 C24 -61.4(2) . . . . ?
C6 C7 N8 C9 65.7(2) . . . . ?
C24 N8 C9 C10 -83.7(2) . . . . ?
C7 N8 C9 C10 148.30(17) . . . . ?
N8 C9 C10 C11 -173.84(16) . . . . ?
C9 C10 C11 N12 64.2(2) . . . . ?
C10 C11 N12 C31 77.6(2) . . . . ?
C10 C11 N12 C13 -156.32(17) . . . . ?
C11 N12 C13 C14 -177.85(17) . . . . ?
C31 N12 C13 C14 -52.1(2) . . . . ?
N12 C13 C14 C19 112.3(2) . . . . ?
N12 C13 C14 C15 -65.5(3) . . . . ?
C2 O1 C15 C16 -3.6(3) . . . . ?
C2 O1 C15 C14 176.67(18) . . . . ?
C19 C14 C15 O1 175.54(18) . . . . ?
C13 C14 C15 O1 -6.6(3) . . . . ?
C19 C14 C15 C16 -4.2(3) . . . . ?
C13 C14 C15 C16 173.61(19) . . . . ?
O1 C15 C16 C17 -177.87(19) . . . . ?
C14 C15 C16 C17 1.9(3) . . . . ?
C15 C16 C17 C18 1.9(3) . . . . ?
C16 C17 C18 C19 -3.1(3) . . . . ?
C15 C14 C19 C18 3.0(3) . . . . ?
C13 C14 C19 C18 -174.9(2) . . . . ?
C17 C18 C19 C14 0.7(3) . . . . ?
O4 C5 C20 C21 -177.4(2) . . . . ?
C6 C5 C20 C21 0.9(4) . . . . ?
C5 C20 C21 C22 1.8(4) . . . . ?
C20 C21 C22 C23 -2.1(4) . . . . ?
C21 C22 C23 C6 -0.4(4) . . . . ?
C5 C6 C23 C22 3.1(3) . . . . ?
C7 C6 C23 C22 -177.1(2) . . . . ?
C9 N8 C24 C25 161.49(17) . . . . ?
C7 N8 C24 C25 -70.8(2) . . . . ?
N8 C24 C25 C30 -53.6(3) . . . . ?
N8 C24 C25 C26 131.2(2) . . . . ?
C30 C25 C26 C27 0.0(3) . . . . ?
C24 C25 C26 C27 175.3(2) . . . . ?
C25 C26 C27 N28 -1.0(3) . . . . ?
C26 C27 N28 C29 0.5(3) . . . . ?
C26 C27 N28 Mn1 -176.27(16) . . . 1_554 ?
C27 N28 C29 C30 0.9(3) . . . . ?
Mn1 N28 C29 C30 177.79(18) 1_554 . . . ?
N28 C29 C30 C25 -1.9(4) . . . . ?
C26 C25 C30 C29 1.4(3) . . . . ?
C24 C25 C30 C29 -174.1(2) . . . . ?
C11 N12 C31 C32 -145.72(17) . . . . ?
C13 N12 C31 C32 89.5(2) . . . . ?
N12 C31 C32 C37 -135.37(19) . . . . ?
N12 C31 C32 C33 47.4(3) . . . . ?
C37 C32 C33 C34 0.3(3) . . . . ?
C31 C32 C33 C34 177.71(19) . . . . ?
C32 C33 C34 N35 -1.0(3) . . . . ?
C33 C34 N35 C36 1.0(3) . . . . ?
C33 C34 N35 Mn1 178.28(15) . . . . ?
C34 N35 C36 C37 -0.3(3) . . . . ?
Mn1 N35 C36 C37 -177.65(16) . . . . ?
N35 C36 C37 C32 -0.4(3) . . . . ?
C33 C32 C37 C36 0.3(3) . . . . ?
C31 C32 C37 C36 -177.06(19) . . . . ?

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
C9 H9A O4 0.99 2.51 3.248(2) 131.6 .
C27 H27 Cl1 0.95 2.68 3.369(2) 129.9 3_566
C29 H29 Cl1 0.95 2.61 3.326(2) 132.5 1_554

_refine_diff_density_max         0.614
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.058

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1542748'
_audit_update_record             
;
2017-10-02 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H68 Cl2 Cu N8 O4'
_chemical_formula_weight         1123.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.7177(2)
_cell_length_b                   22.8785(7)
_cell_length_c                   13.3318(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.452(2)
_cell_angle_gamma                90
_cell_volume                     2658.15(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(1)
_cell_measurement_reflns_used    5191
_cell_measurement_theta_min      3.8110
_cell_measurement_theta_max      75.2000

_exptl_crystal_description       prism
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             1182
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.969
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.39957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.5357
_diffrn_measurement_method       '/w scan'
_diffrn_reflns_number            14133
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.838
_diffrn_reflns_theta_max         76.431
_diffrn_reflns_theta_full        70.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5491
_reflns_number_gt                4457
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0820P)²+1.2976P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5491
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1517
_refine_ls_wR_factor_gt          0.1420
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cu1 Cu -0.03630(8) 0.49389(4) 1.00650(7) 0.0363(2) Uani 0.5 1 d . . P A -1
Cl1 Cl -0.29836(7) 0.45069(3) 1.07487(5) 0.04357(17) Uani 1 1 d . . . . .
O1 O 0.4781(2) 0.32848(8) 0.82012(13) 0.0390(4) Uani 1 1 d . . . . .
C2 C 0.5443(3) 0.38495(12) 0.83700(19) 0.0400(5) Uani 1 1 d . . . . .
H2A H 0.6027 0.3856 0.9016 0.048 Uiso 1 1 calc R U . . .
H2B H 0.4628 0.4150 0.8392 0.048 Uiso 1 1 calc R U . . .
C3 C 0.6492(3) 0.39699(12) 0.75168(19) 0.0393(5) Uani 1 1 d . . . . .
H3A H 0.7111 0.4324 0.7665 0.047 Uiso 1 1 calc R U . . .
H3B H 0.7203 0.3637 0.7434 0.047 Uiso 1 1 calc R U . . .
O4 O 0.56060(18) 0.40547(8) 0.66124(13) 0.0373(4) Uani 1 1 d . . . . .
C5 C 0.6411(3) 0.41792(11) 0.57625(19) 0.0348(5) Uani 1 1 d . . . . .
C6 C 0.5548(3) 0.42971(11) 0.48865(19) 0.0355(5) Uani 1 1 d . . . . .
C7 C 0.3798(3) 0.42780(11) 0.48320(18) 0.0355(5) Uani 1 1 d . . . . .
H7A H 0.3414 0.4361 0.5510 0.043 Uiso 1 1 calc R U . . .
H7B H 0.3435 0.4597 0.4384 0.043 Uiso 1 1 calc R U . . .
N8 N 0.3101(2) 0.37295(10) 0.44767(15) 0.0344(4) Uani 1 1 d . . . . .
C9 C 0.3402(3) 0.32426(11) 0.51611(18) 0.0352(5) Uani 1 1 d . . . . .
H9A H 0.3552 0.3397 0.5850 0.042 Uiso 1 1 calc R U . . .
H9B H 0.4365 0.3047 0.4971 0.042 Uiso 1 1 calc R U . . .
C10 C 0.2109(3) 0.27943(12) 0.51545(18) 0.0362(5) Uani 1 1 d . . . . .
H10A H 0.1119 0.2993 0.5265 0.043 Uiso 1 1 calc R U . . .
H10B H 0.2044 0.2597 0.4494 0.043 Uiso 1 1 calc R U . . .
C11 C 0.2405(3) 0.23439(11) 0.59761(18) 0.0367(5) Uani 1 1 d . . . . .
H11A H 0.1602 0.2038 0.5935 0.044 Uiso 1 1 calc R U . . .
H11B H 0.3410 0.2154 0.5874 0.044 Uiso 1 1 calc R U . . .
N12 N 0.2403(2) 0.26161(9) 0.69725(15) 0.0328(4) Uani 1 1 d . . . . .
C13 C 0.3314(3) 0.22566(11) 0.76829(19) 0.0366(5) Uani 1 1 d . . . . .
H13A H 0.4386 0.2237 0.7458 0.044 Uiso 1 1 calc R U . . .
H13B H 0.2898 0.1854 0.7683 0.044 Uiso 1 1 calc R U . . .
C14 C 0.3301(3) 0.24966(11) 0.87338(18) 0.0345(5) Uani 1 1 d . . . . .
C15 C 0.3984(3) 0.30365(12) 0.89608(18) 0.0354(5) Uani 1 1 d . . . . .
C16 C 0.3834(3) 0.32866(12) 0.99042(19) 0.0392(5) Uani 1 1 d . . . . .
H16 H 0.4274 0.3658 1.0052 0.047 Uiso 1 1 calc R U . . .
C17 C 0.3027(3) 0.29826(13) 1.0631(2) 0.0420(6) Uani 1 1 d . . . . .
H17 H 0.2898 0.3155 1.1271 0.050 Uiso 1 1 calc R U . . .
C18 C 0.2414(3) 0.24384(13) 1.04370(19) 0.0422(6) Uani 1 1 d . . . . .
H18 H 0.1902 0.2230 1.0946 0.051 Uiso 1 1 calc R U . . .
C19 C 0.2555(3) 0.21978(12) 0.94866(19) 0.0384(5) Uani 1 1 d . . . . .
H19 H 0.2134 0.1822 0.9349 0.046 Uiso 1 1 calc R U . . .
C20 C 0.8020(3) 0.41991(12) 0.5766(2) 0.0403(5) Uani 1 1 d . . . . .
H20 H 0.8596 0.4112 0.6362 0.048 Uiso 1 1 calc R U . . .
C21 C 0.8765(3) 0.43468(13) 0.4893(2) 0.0446(6) Uani 1 1 d . . . . .
H21 H 0.9854 0.4353 0.4889 0.053 Uiso 1 1 calc R U . . .
C22 C 0.7939(3) 0.44846(13) 0.4033(2) 0.0448(6) Uani 1 1 d . . . . .
H22 H 0.8452 0.4597 0.3443 0.054 Uiso 1 1 calc R U . . .
C23 C 0.6344(3) 0.44577(12) 0.4036(2) 0.0410(5) Uani 1 1 d . . . . .
H23 H 0.5780 0.4552 0.3439 0.049 Uiso 1 1 calc R U . . .
C24 C 0.3489(3) 0.35840(12) 0.34484(18) 0.0360(5) Uani 1 1 d . . . . .
H24A H 0.3194 0.3173 0.3310 0.043 Uiso 1 1 calc R U . . .
H24B H 0.4614 0.3616 0.3378 0.043 Uiso 1 1 calc R U . . .
C25 C 0.2705(3) 0.39740(11) 0.26848(18) 0.0355(5) Uani 1 1 d . . . . .
C26 C 0.3499(3) 0.42672(13) 0.1945(2) 0.0435(6) Uani 1 1 d . . . . .
H26 H 0.4588 0.4259 0.1949 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2697(5) 0.45705(13) 0.1203(2) 0.0544(8) Uani 1 1 d . . . . .
H27 H 0.3256 0.4770 0.0705 0.065 Uiso 1 1 calc R U . . .
N28 N 0.1198(4) 0.45921(11) 0.11617(16) 0.0548(7) Uani 1 1 d . . . . .
C29 C 0.0403(4) 0.43105(16) 0.1871(2) 0.0542(8) Uani 1 1 d . . . . .
H29 H -0.0687 0.4320 0.1836 0.065 Uiso 1 1 calc R U . . .
C30 C 0.1124(3) 0.40089(13) 0.26457(19) 0.0421(6) Uani 1 1 d . . . . .
H30 H 0.0536 0.3827 0.3148 0.051 Uiso 1 1 calc R U . . .
C31 C 0.0842(3) 0.27221(11) 0.73111(18) 0.0342(5) Uani 1 1 d . . . . .
H31A H 0.0502 0.2379 0.7699 0.041 Uiso 1 1 calc R U . . .
H31B H 0.0147 0.2761 0.6716 0.041 Uiso 1 1 calc R U . . .
C32 C 0.0694(2) 0.32642(11) 0.79563(17) 0.0330(5) Uani 1 1 d . . . . .
C33 C 0.1378(3) 0.37905(11) 0.77093(19) 0.0372(5) Uani 1 1 d . . . . .
H33 H 0.1996 0.3816 0.7134 0.045 Uiso 1 1 calc R U . . .
C34 C 0.1158(3) 0.42793(12) 0.8302(2) 0.0425(6) Uani 1 1 d . . . . .
H34 H 0.1640 0.4635 0.8122 0.051 Uiso 1 1 calc R U . . .
N35 N 0.0294(3) 0.42718(11) 0.91189(16) 0.0452(5) Uani 1 1 d . . . . .
C36 C -0.0358(3) 0.37742(14) 0.9358(2) 0.0465(6) Uani 1 1 d . . . . .
H36 H -0.0970 0.3764 0.9937 0.056 Uiso 1 1 calc R U . . .
C37 C -0.0196(3) 0.32613(13) 0.88073(19) 0.0403(5) Uani 1 1 d . . . . .
H37 H -0.0690 0.2912 0.9011 0.048 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
Cu1 N35 2.070(2) . ?
Cu1 Cl1 2.6707(9) . ?
O1 C15 1.366(3) . ?
O1 C2 1.430(3) . ?
C2 C3 1.503(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O4 1.429(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C5 1.378(3) . ?
C5 C6 1.399(3) . ?
C5 C20 1.403(3) . ?
C6 C23 1.394(4) . ?
C6 C7 1.526(3) . ?
C7 N8 1.468(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C24 1.459(3) . ?
N8 C9 1.460(3) . ?
C9 C10 1.524(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.521(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N12 1.467(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N12 C31 1.465(3) . ?
N12 C13 1.472(3) . ?
C13 C14 1.505(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.389(4) . ?
C14 C15 1.401(4) . ?
C15 C16 1.391(4) . ?
C16 C17 1.397(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.377(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.390(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.390(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.374(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.392(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.505(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.381(3) . ?
C25 C26 1.391(4) . ?
C26 C27 1.383(4) . ?
C26 H26 0.9500 . ?
C27 N28 1.307(5) . ?
C27 H27 0.9500 . ?
N28 C29 1.350(5) . ?
C29 C30 1.380(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.517(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.387(4) . ?
C32 C37 1.391(3) . ?
C33 C34 1.386(4) . ?
C33 H33 0.9500 . ?
C34 N35 1.339(4) . ?
C34 H34 0.9500 . ?
N35 C36 1.315(4) . ?
C36 C37 1.394(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?

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
N35 Cu1 Cl1 100.80(9) . . ?
C15 O1 C2 118.0(2) . . ?
O1 C2 C3 107.3(2) . . ?
O1 C2 H2A 110.3 . . ?
C3 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C3 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
O4 C3 C2 109.70(19) . . ?
O4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
O4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 O4 C3 116.50(18) . . ?
O4 C5 C6 116.8(2) . . ?
O4 C5 C20 122.3(2) . . ?
C6 C5 C20 120.9(2) . . ?
C23 C6 C5 117.5(2) . . ?
C23 C6 C7 119.1(2) . . ?
C5 C6 C7 123.4(2) . . ?
N8 C7 C6 116.5(2) . . ?
N8 C7 H7A 108.2 . . ?
C6 C7 H7A 108.2 . . ?
N8 C7 H7B 108.2 . . ?
C6 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C24 N8 C9 111.8(2) . . ?
C24 N8 C7 113.2(2) . . ?
C9 N8 C7 112.59(19) . . ?
N8 C9 C10 112.86(19) . . ?
N8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 109.85(19) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N12 C11 C10 111.1(2) . . ?
N12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
N12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C31 N12 C11 111.82(18) . . ?
C31 N12 C13 112.62(19) . . ?
C11 N12 C13 109.42(19) . . ?
N12 C13 C14 112.2(2) . . ?
N12 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
N12 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C19 C14 C15 118.8(2) . . ?
C19 C14 C13 120.5(2) . . ?
C15 C14 C13 120.6(2) . . ?
O1 C15 C16 124.1(2) . . ?
O1 C15 C14 115.3(2) . . ?
C16 C15 C14 120.6(2) . . ?
C15 C16 C17 118.9(2) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
C18 C17 C16 121.3(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 119.1(2) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C14 C19 C18 121.2(2) . . ?
C14 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C21 C20 C5 119.5(2) . . ?
C21 C20 H20 120.2 . . ?
C5 C20 H20 120.2 . . ?
C22 C21 C20 120.6(2) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 119.3(3) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C6 122.1(3) . . ?
C22 C23 H23 118.9 . . ?
C6 C23 H23 118.9 . . ?
N8 C24 C25 112.8(2) . . ?
N8 C24 H24A 109.0 . . ?
C25 C24 H24A 109.0 . . ?
N8 C24 H24B 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C30 C25 C26 117.3(2) . . ?
C30 C25 C24 119.7(2) . . ?
C26 C25 C24 122.7(2) . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
N28 C27 C26 122.3(3) . . ?
N28 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
C27 N28 C29 118.9(2) . . ?
N28 C29 C30 122.0(3) . . ?
N28 C29 H29 119.0 . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C25 119.5(3) . . ?
C29 C30 H30 120.2 . . ?
C25 C30 H30 120.2 . . ?
N12 C31 C32 113.76(19) . . ?
N12 C31 H31A 108.8 . . ?
C32 C31 H31A 108.8 . . ?
N12 C31 H31B 108.8 . . ?
C32 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C33 C32 C37 116.7(2) . . ?
C33 C32 C31 122.2(2) . . ?
C37 C32 C31 121.0(2) . . ?
C34 C33 C32 119.9(2) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
N35 C34 C33 122.8(3) . . ?
N35 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
C36 N35 C34 117.6(2) . . ?
C36 N35 Cu1 111.25(19) . . ?
C34 N35 Cu1 131.0(2) . . ?
N35 C36 C37 123.4(2) . . ?
N35 C36 H36 118.3 . . ?
C37 C36 H36 118.3 . . ?
C32 C37 C36 119.5(3) . . ?
C32 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 O1 C2 C3 169.3(2) . . . . ?
O1 C2 C3 O4 69.3(3) . . . . ?
C2 C3 O4 C5 179.0(2) . . . . ?
C3 O4 C5 C6 -176.3(2) . . . . ?
C3 O4 C5 C20 2.5(3) . . . . ?
O4 C5 C6 C23 176.3(2) . . . . ?
C20 C5 C6 C23 -2.6(4) . . . . ?
O4 C5 C6 C7 -1.6(4) . . . . ?
C20 C5 C6 C7 179.5(2) . . . . ?
C23 C6 C7 N8 86.8(3) . . . . ?
C5 C6 C7 N8 -95.3(3) . . . . ?
C6 C7 N8 C24 -62.5(3) . . . . ?
C6 C7 N8 C9 65.5(3) . . . . ?
C24 N8 C9 C10 -82.4(2) . . . . ?
C7 N8 C9 C10 148.9(2) . . . . ?
N8 C9 C10 C11 -172.8(2) . . . . ?
C9 C10 C11 N12 63.2(3) . . . . ?
C10 C11 N12 C31 78.9(2) . . . . ?
C10 C11 N12 C13 -155.6(2) . . . . ?
C31 N12 C13 C14 -52.4(3) . . . . ?
C11 N12 C13 C14 -177.38(19) . . . . ?
N12 C13 C14 C19 111.5(3) . . . . ?
N12 C13 C14 C15 -65.8(3) . . . . ?
C2 O1 C15 C16 -3.0(3) . . . . ?
C2 O1 C15 C14 177.0(2) . . . . ?
C19 C14 C15 O1 175.8(2) . . . . ?
C13 C14 C15 O1 -6.8(3) . . . . ?
C19 C14 C15 C16 -4.1(3) . . . . ?
C13 C14 C15 C16 173.3(2) . . . . ?
O1 C15 C16 C17 -178.2(2) . . . . ?
C14 C15 C16 C17 1.8(4) . . . . ?
C15 C16 C17 C18 1.5(4) . . . . ?
C16 C17 C18 C19 -2.4(4) . . . . ?
C15 C14 C19 C18 3.2(4) . . . . ?
C13 C14 C19 C18 -174.2(2) . . . . ?
C17 C18 C19 C14 0.0(4) . . . . ?
O4 C5 C20 C21 -177.8(2) . . . . ?
C6 C5 C20 C21 1.0(4) . . . . ?
C5 C20 C21 C22 1.3(4) . . . . ?
C20 C21 C22 C23 -2.0(4) . . . . ?
C21 C22 C23 C6 0.3(4) . . . . ?
C5 C6 C23 C22 2.0(4) . . . . ?
C7 C6 C23 C22 180.0(3) . . . . ?
C9 N8 C24 C25 159.8(2) . . . . ?
C7 N8 C24 C25 -71.8(2) . . . . ?
N8 C24 C25 C30 -57.9(3) . . . . ?
N8 C24 C25 C26 128.0(3) . . . . ?
C30 C25 C26 C27 -0.9(4) . . . . ?
C24 C25 C26 C27 173.3(3) . . . . ?
C25 C26 C27 N28 -0.4(5) . . . . ?
C26 C27 N28 C29 0.3(4) . . . . ?
C27 N28 C29 C30 1.0(4) . . . . ?
N28 C29 C30 C25 -2.3(5) . . . . ?
C26 C25 C30 C29 2.1(4) . . . . ?
C24 C25 C30 C29 -172.3(3) . . . . ?
C11 N12 C31 C32 -147.0(2) . . . . ?
C13 N12 C31 C32 89.3(2) . . . . ?
N12 C31 C32 C33 44.6(3) . . . . ?
N12 C31 C32 C37 -138.2(2) . . . . ?
C37 C32 C33 C34 0.1(3) . . . . ?
C31 C32 C33 C34 177.4(2) . . . . ?
C32 C33 C34 N35 -0.3(4) . . . . ?
C33 C34 N35 C36 0.3(4) . . . . ?
C33 C34 N35 Cu1 -174.62(19) . . . . ?
C34 N35 C36 C37 -0.2(4) . . . . ?
Cu1 N35 C36 C37 175.7(2) . . . . ?
C33 C32 C37 C36 0.0(3) . . . . ?
C31 C32 C37 C36 -177.3(2) . . . . ?
N35 C36 C37 C32 0.0(4) . . . . ?

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
C9 H9A O4 0.99 2.53 3.271(3) 131.3 .
C27 H27 Cl1 0.95 2.55 3.364(3) 143.3 3_566
C29 H29 Cl1 0.95 2.48 3.306(3) 145.6 1_554
C34 H34 Cl1 0.95 2.72 3.427(3) 131.7 3_567
C36 H36 Cl1 0.95 2.69 3.421(3) 134.2 .

_refine_diff_density_max         1.332
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.066

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1542744'
_audit_update_record             
;
2017-10-02 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H68 Cl2 N8 Ni O4'
_chemical_formula_sum            'C62 H68 Cl2 N8 Ni O4'
_chemical_formula_weight         1118.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.4606(3)
_cell_length_b                   23.1261(10)
_cell_length_c                   13.5197(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.899(5)
_cell_angle_gamma                90
_cell_volume                     2644.95(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    2112
_cell_measurement_theta_min      3.1230
_cell_measurement_theta_max      27.9680

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.527
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.99030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       '/w scan'
_diffrn_reflns_number            7403
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.820
_diffrn_reflns_theta_max         28.191
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.697
_diffrn_measured_fraction_theta_full 0.847
_diffrn_reflns_Laue_measured_fraction_max 0.697
_diffrn_reflns_Laue_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.697
_diffrn_reflns_point_group_measured_fraction_full 0.847
_reflns_number_total             4532
_reflns_number_gt                3242
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0219P)²+1.5232P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4532
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.0879
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ni1 Ni 0.0000 0.5000 1.0000 0.01459(14) Uani 1 2 d S . P . .
Cl1 Cl -0.25320(8) 0.45990(3) 1.05747(6) 0.01886(18) Uani 1 1 d . . . . .
O1 O 0.4954(2) 0.33055(8) 0.81890(15) 0.0214(5) Uani 1 1 d . . . . .
C2 C 0.5568(3) 0.38790(13) 0.8342(2) 0.0208(7) Uani 1 1 d . . . . .
H2A H 0.6169 0.3899 0.8975 0.025 Uiso 1 1 calc R U . . .
H2B H 0.4694 0.4163 0.8362 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6628(3) 0.40058(14) 0.7494(2) 0.0220(8) Uani 1 1 d . . . . .
H3A H 0.7231 0.4365 0.7629 0.026 Uiso 1 1 calc R U . . .
H3B H 0.7392 0.3685 0.7415 0.026 Uiso 1 1 calc R U . . .
O4 O 0.5710(2) 0.40725(9) 0.66064(15) 0.0192(5) Uani 1 1 d . . . . .
C5 C 0.6530(3) 0.41957(12) 0.5766(2) 0.0174(7) Uani 1 1 d . . . . .
C6 C 0.5628(3) 0.43137(12) 0.4900(2) 0.0174(7) Uani 1 1 d . . . . .
C7 C 0.3841(3) 0.42687(12) 0.4851(2) 0.0191(7) Uani 1 1 d . . . . .
H7A H 0.3429 0.4344 0.5520 0.023 Uiso 1 1 calc R U . . .
H7B H 0.3434 0.4578 0.4410 0.023 Uiso 1 1 calc R U . . .
N8 N 0.3191(3) 0.37127(10) 0.45006(18) 0.0179(6) Uani 1 1 d . . . . .
C9 C 0.3545(3) 0.32395(13) 0.5184(2) 0.0195(7) Uani 1 1 d . . . . .
H9A H 0.3683 0.3398 0.5859 0.023 Uiso 1 1 calc R U . . .
H9B H 0.4557 0.3058 0.4995 0.023 Uiso 1 1 calc R U . . .
C10 C 0.2256(3) 0.27778(13) 0.5193(2) 0.0208(7) Uani 1 1 d . . . . .
H10A H 0.1218 0.2960 0.5310 0.025 Uiso 1 1 calc R U . . .
H10B H 0.2205 0.2579 0.4545 0.025 Uiso 1 1 calc R U . . .
C11 C 0.2622(3) 0.23440(13) 0.6005(2) 0.0191(7) Uani 1 1 d . . . . .
H11A H 0.1832 0.2028 0.5978 0.023 Uiso 1 1 calc R U . . .
H11B H 0.3677 0.2172 0.5895 0.023 Uiso 1 1 calc R U . . .
N12 N 0.2602(3) 0.26142(10) 0.69856(18) 0.0166(6) Uani 1 1 d . . . . .
C13 C 0.3556(3) 0.22728(13) 0.7685(2) 0.0211(7) Uani 1 1 d . . . . .
H13A H 0.4665 0.2266 0.7461 0.025 Uiso 1 1 calc R U . . .
H13B H 0.3164 0.1870 0.7685 0.025 Uiso 1 1 calc R U . . .
C14 C 0.3517(3) 0.25049(13) 0.8720(2) 0.0174(7) Uani 1 1 d . . . . .
C15 C 0.4164(3) 0.30483(13) 0.8945(2) 0.0185(7) Uani 1 1 d . . . . .
C16 C 0.3981(3) 0.32867(13) 0.9871(2) 0.0212(7) Uani 1 1 d . . . . .
H16 H 0.4386 0.3661 1.0014 0.025 Uiso 1 1 calc R U . . .
C17 C 0.3205(3) 0.29762(14) 1.0592(2) 0.0243(7) Uani 1 1 d . . . . .
H17 H 0.3061 0.3145 1.1225 0.029 Uiso 1 1 calc R U . . .
C18 C 0.2639(3) 0.24307(13) 1.0413(2) 0.0222(7) Uani 1 1 d . . . . .
H18 H 0.2149 0.2215 1.0921 0.027 Uiso 1 1 calc R U . . .
C19 C 0.2797(3) 0.22002(13) 0.9473(2) 0.0206(7) Uani 1 1 d . . . . .
H19 H 0.2402 0.1823 0.9341 0.025 Uiso 1 1 calc R U . . .
C20 C 0.8177(3) 0.42204(13) 0.5744(2) 0.0216(7) Uani 1 1 d . . . . .
H20 H 0.8780 0.4133 0.6324 0.026 Uiso 1 1 calc R U . . .
C21 C 0.8933(3) 0.43710(13) 0.4884(2) 0.0248(8) Uani 1 1 d . . . . .
H21 H 1.0055 0.4379 0.4871 0.030 Uiso 1 1 calc R U . . .
C22 C 0.8074(3) 0.45083(13) 0.4049(2) 0.0229(8) Uani 1 1 d . . . . .
H22 H 0.8595 0.4622 0.3463 0.028 Uiso 1 1 calc R U . . .
C23 C 0.6444(3) 0.44802(12) 0.4065(2) 0.0218(7) Uani 1 1 d . . . . .
H23 H 0.5861 0.4579 0.3483 0.026 Uiso 1 1 calc R U . . .
C24 C 0.3652(3) 0.35718(13) 0.3496(2) 0.0195(7) Uani 1 1 d . . . . .
H24A H 0.3381 0.3163 0.3358 0.023 Uiso 1 1 calc R U . . .
H24B H 0.4812 0.3613 0.3444 0.023 Uiso 1 1 calc R U . . .
C25 C 0.2864(3) 0.39483(12) 0.2726(2) 0.0173(7) Uani 1 1 d . . . . .
C26 C 0.3677(3) 0.42289(13) 0.1977(2) 0.0200(7) Uani 1 1 d . . . . .
H26 H 0.4799 0.4216 0.1970 0.024 Uiso 1 1 calc R U . . .
C27 C 0.2858(3) 0.45251(13) 0.1247(2) 0.0192(7) Uani 1 1 d . . . . .
H27 H 0.3445 0.4713 0.0748 0.023 Uiso 1 1 calc R U . . .
N28 N 0.1276(3) 0.45623(10) 0.12041(18) 0.0169(6) Uani 1 1 d . . . . .
C29 C 0.0501(3) 0.42918(13) 0.1930(2) 0.0216(7) Uani 1 1 d . . . . .
H29 H -0.0621 0.4309 0.1921 0.026 Uiso 1 1 calc R U . . .
C30 C 0.1235(3) 0.39913(13) 0.2687(2) 0.0203(7) Uani 1 1 d . . . . .
H30 H 0.0620 0.3813 0.3184 0.024 Uiso 1 1 calc R U . . .
C31 C 0.0987(3) 0.27111(13) 0.7324(2) 0.0183(7) Uani 1 1 d . . . . .
H31A H 0.0647 0.2370 0.7709 0.022 Uiso 1 1 calc R U . . .
H31B H 0.0274 0.2745 0.6740 0.022 Uiso 1 1 calc R U . . .
C32 C 0.0809(3) 0.32473(12) 0.7959(2) 0.0167(7) Uani 1 1 d . . . . .
C33 C 0.1389(3) 0.37831(13) 0.7667(2) 0.0179(7) Uani 1 1 d . . . . .
H33 H 0.1952 0.3819 0.7068 0.022 Uiso 1 1 calc R U . . .
C34 C 0.1144(3) 0.42606(13) 0.8251(2) 0.0193(7) Uani 1 1 d . . . . .
H34 H 0.1562 0.4620 0.8040 0.023 Uiso 1 1 calc R U . . .
N35 N 0.0352(3) 0.42485(10) 0.91006(17) 0.0163(6) Uani 1 1 d . . . . .
C36 C -0.0207(3) 0.37340(13) 0.9379(2) 0.0193(7) Uani 1 1 d . . . . .
H36 H -0.0775 0.3711 0.9978 0.023 Uiso 1 1 calc R U . . .
C37 C 0.0002(3) 0.32340(13) 0.8838(2) 0.0178(7) Uani 1 1 d . . . . .
H37 H -0.0413 0.2879 0.9073 0.021 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
Ni1 N35 2.144(2) 3_567 ?
Ni1 N35 2.144(2) . ?
Ni1 N28 2.187(2) 3_566 ?
Ni1 N28 2.187(2) 1_556 ?
Ni1 Cl1 2.4708(7) . ?
Ni1 Cl1 2.4708(7) 3_567 ?
O1 C15 1.366(3) . ?
O1 C2 1.438(3) . ?
C2 C3 1.495(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O4 1.427(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C5 1.371(3) . ?
C5 C20 1.395(4) . ?
C5 C6 1.414(4) . ?
C6 C23 1.386(4) . ?
C6 C7 1.516(4) . ?
C7 N8 1.474(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C24 1.456(3) . ?
N8 C9 1.460(4) . ?
C9 C10 1.527(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.515(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N12 1.466(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N12 C13 1.465(4) . ?
N12 C31 1.465(3) . ?
C13 C14 1.499(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.386(4) . ?
C14 C15 1.402(4) . ?
C15 C16 1.380(4) . ?
C16 C17 1.385(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.370(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.381(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.370(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.505(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.382(4) . ?
C25 C26 1.393(4) . ?
C26 C27 1.379(4) . ?
C26 H26 0.9500 . ?
C27 N28 1.341(3) . ?
C27 H27 0.9500 . ?
N28 C29 1.343(4) . ?
N28 Ni1 2.187(2) 1_554 ?
C29 C30 1.377(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.517(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C37 1.380(4) . ?
C32 C33 1.392(4) . ?
C33 C34 1.375(4) . ?
C33 H33 0.9500 . ?
C34 N35 1.339(3) . ?
C34 H34 0.9500 . ?
N35 C36 1.336(4) . ?
C36 C37 1.381(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?

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
N35 Ni1 N35 180.0 3_567 . ?
N35 Ni1 N28 88.61(9) 3_567 3_566 ?
N35 Ni1 N28 91.39(9) . 3_566 ?
N35 Ni1 N28 91.39(9) 3_567 1_556 ?
N35 Ni1 N28 88.61(9) . 1_556 ?
N28 Ni1 N28 180.0 3_566 1_556 ?
N35 Ni1 Cl1 89.84(6) 3_567 . ?
N35 Ni1 Cl1 90.16(6) . . ?
N28 Ni1 Cl1 89.29(6) 3_566 . ?
N28 Ni1 Cl1 90.71(6) 1_556 . ?
N35 Ni1 Cl1 90.16(6) 3_567 3_567 ?
N35 Ni1 Cl1 89.84(6) . 3_567 ?
N28 Ni1 Cl1 90.71(6) 3_566 3_567 ?
N28 Ni1 Cl1 89.29(6) 1_556 3_567 ?
Cl1 Ni1 Cl1 180.0 . 3_567 ?
C15 O1 C2 118.3(2) . . ?
O1 C2 C3 106.9(2) . . ?
O1 C2 H2A 110.3 . . ?
C3 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C3 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
O4 C3 C2 109.9(2) . . ?
O4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
O4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 O4 C3 116.4(2) . . ?
O4 C5 C20 123.0(3) . . ?
O4 C5 C6 116.9(2) . . ?
C20 C5 C6 120.1(3) . . ?
C23 C6 C5 117.3(3) . . ?
C23 C6 C7 119.5(3) . . ?
C5 C6 C7 123.2(3) . . ?
N8 C7 C6 116.1(2) . . ?
N8 C7 H7A 108.3 . . ?
C6 C7 H7A 108.3 . . ?
N8 C7 H7B 108.3 . . ?
C6 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C24 N8 C9 111.5(2) . . ?
C24 N8 C7 113.0(2) . . ?
C9 N8 C7 112.3(2) . . ?
N8 C9 C10 113.0(2) . . ?
N8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 109.3(2) . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
N12 C11 C10 111.6(2) . . ?
N12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C13 N12 C31 112.8(2) . . ?
C13 N12 C11 109.9(2) . . ?
C31 N12 C11 111.8(2) . . ?
N12 C13 C14 112.9(2) . . ?
N12 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N12 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C19 C14 C15 118.1(3) . . ?
C19 C14 C13 121.3(3) . . ?
C15 C14 C13 120.6(3) . . ?
O1 C15 C16 124.6(3) . . ?
O1 C15 C14 115.0(3) . . ?
C16 C15 C14 120.4(3) . . ?
C15 C16 C17 119.6(3) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 118.5(3) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C14 121.8(3) . . ?
C18 C19 H19 119.1 . . ?
C14 C19 H19 119.1 . . ?
C21 C20 C5 120.2(3) . . ?
C21 C20 H20 119.9 . . ?
C5 C20 H20 119.9 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 119.5(3) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C6 122.4(3) . . ?
C22 C23 H23 118.8 . . ?
C6 C23 H23 118.8 . . ?
N8 C24 C25 113.2(2) . . ?
N8 C24 H24A 108.9 . . ?
C25 C24 H24A 108.9 . . ?
N8 C24 H24B 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.8 . . ?
C30 C25 C26 116.3(3) . . ?
C30 C25 C24 119.9(3) . . ?
C26 C25 C24 123.6(2) . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
N28 C27 C26 123.6(3) . . ?
N28 C27 H27 118.2 . . ?
C26 C27 H27 118.2 . . ?
C27 N28 C29 115.9(3) . . ?
C27 N28 Ni1 122.84(19) . 1_554 ?
C29 N28 Ni1 121.24(18) . 1_554 ?
N28 C29 C30 124.0(3) . . ?
N28 C29 H29 118.0 . . ?
C30 C29 H29 118.0 . . ?
C29 C30 C25 120.1(3) . . ?
C29 C30 H30 119.9 . . ?
C25 C30 H30 119.9 . . ?
N12 C31 C32 113.8(2) . . ?
N12 C31 H31A 108.8 . . ?
C32 C31 H31A 108.8 . . ?
N12 C31 H31B 108.8 . . ?
C32 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C37 C32 C33 116.4(3) . . ?
C37 C32 C31 121.6(3) . . ?
C33 C32 C31 121.9(3) . . ?
C34 C33 C32 119.7(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
N35 C34 C33 123.9(3) . . ?
N35 C34 H34 118.0 . . ?
C33 C34 H34 118.0 . . ?
C36 N35 C34 116.4(2) . . ?
C36 N35 Ni1 120.60(19) . . ?
C34 N35 Ni1 123.04(19) . . ?
N35 C36 C37 123.2(3) . . ?
N35 C36 H36 118.4 . . ?
C37 C36 H36 118.4 . . ?
C32 C37 C36 120.4(3) . . ?
C32 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?

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
C15 O1 C2 C3 169.1(2) . . . . ?
O1 C2 C3 O4 69.8(3) . . . . ?
C2 C3 O4 C5 179.5(2) . . . . ?
C3 O4 C5 C20 4.0(4) . . . . ?
C3 O4 C5 C6 -174.5(2) . . . . ?
O4 C5 C6 C23 175.4(2) . . . . ?
C20 C5 C6 C23 -3.2(4) . . . . ?
O4 C5 C6 C7 -4.4(4) . . . . ?
C20 C5 C6 C7 177.1(3) . . . . ?
C23 C6 C7 N8 86.5(3) . . . . ?
C5 C6 C7 N8 -93.8(3) . . . . ?
C6 C7 N8 C24 -61.2(3) . . . . ?
C6 C7 N8 C9 66.0(3) . . . . ?
C24 N8 C9 C10 -84.0(3) . . . . ?
C7 N8 C9 C10 148.0(2) . . . . ?
N8 C9 C10 C11 -173.2(2) . . . . ?
C9 C10 C11 N12 63.3(3) . . . . ?
C10 C11 N12 C13 -156.8(2) . . . . ?
C10 C11 N12 C31 77.1(3) . . . . ?
C31 N12 C13 C14 -51.2(3) . . . . ?
C11 N12 C13 C14 -176.7(2) . . . . ?
N12 C13 C14 C19 112.6(3) . . . . ?
N12 C13 C14 C15 -65.3(3) . . . . ?
C2 O1 C15 C16 -3.7(4) . . . . ?
C2 O1 C15 C14 176.2(2) . . . . ?
C19 C14 C15 O1 175.4(2) . . . . ?
C13 C14 C15 O1 -6.7(4) . . . . ?
C19 C14 C15 C16 -4.7(4) . . . . ?
C13 C14 C15 C16 173.2(3) . . . . ?
O1 C15 C16 C17 -177.7(3) . . . . ?
C14 C15 C16 C17 2.5(4) . . . . ?
C15 C16 C17 C18 1.3(5) . . . . ?
C16 C17 C18 C19 -2.8(4) . . . . ?
C17 C18 C19 C14 0.4(4) . . . . ?
C15 C14 C19 C18 3.2(4) . . . . ?
C13 C14 C19 C18 -174.6(3) . . . . ?
O4 C5 C20 C21 -177.2(3) . . . . ?
C6 C5 C20 C21 1.2(4) . . . . ?
C5 C20 C21 C22 1.3(4) . . . . ?
C20 C21 C22 C23 -1.7(4) . . . . ?
C21 C22 C23 C6 -0.4(5) . . . . ?
C5 C6 C23 C22 2.8(4) . . . . ?
C7 C6 C23 C22 -177.5(3) . . . . ?
C9 N8 C24 C25 161.5(2) . . . . ?
C7 N8 C24 C25 -70.8(3) . . . . ?
N8 C24 C25 C30 -54.9(4) . . . . ?
N8 C24 C25 C26 130.6(3) . . . . ?
C30 C25 C26 C27 -0.5(4) . . . . ?
C24 C25 C26 C27 174.3(3) . . . . ?
C25 C26 C27 N28 -0.2(5) . . . . ?
C26 C27 N28 C29 0.4(4) . . . . ?
C26 C27 N28 Ni1 -177.0(2) . . . 1_554 ?
C27 N28 C29 C30 0.1(4) . . . . ?
Ni1 N28 C29 C30 177.5(2) 1_554 . . . ?
N28 C29 C30 C25 -0.8(5) . . . . ?
C26 C25 C30 C29 0.9(4) . . . . ?
C24 C25 C30 C29 -174.0(3) . . . . ?
C13 N12 C31 C32 88.5(3) . . . . ?
C11 N12 C31 C32 -147.1(3) . . . . ?
N12 C31 C32 C37 -132.9(3) . . . . ?
N12 C31 C32 C33 49.9(4) . . . . ?
C37 C32 C33 C34 0.2(4) . . . . ?
C31 C32 C33 C34 177.5(3) . . . . ?
C32 C33 C34 N35 -0.7(4) . . . . ?
C33 C34 N35 C36 0.6(4) . . . . ?
C33 C34 N35 Ni1 179.6(2) . . . . ?
C34 N35 C36 C37 0.0(4) . . . . ?
Ni1 N35 C36 C37 -179.1(2) . . . . ?
C33 C32 C37 C36 0.4(4) . . . . ?
C31 C32 C37 C36 -176.9(3) . . . . ?
N35 C36 C37 C32 -0.5(4) . . . . ?

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
C9 H9A O4 0.99 2.52 3.264(3) 132.0 .
C27 H27 Cl1 0.95 2.51 3.198(3) 129.7 3_566
C29 H29 Cl1 0.95 2.51 3.210(3) 130.8 1_554
C34 H34 Cl1 0.95 2.72 3.286(3) 118.9 3_567
C36 H36 Cl1 0.95 2.67 3.254(3) 120.5 .

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.062

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_cd
_database_code_depnum_ccdc_archive 'CCDC 1580496'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H68 Cd Cl2 N8 O4'
_chemical_formula_sum            'C62 H68 Cd Cl2 N8 O4'
_chemical_formula_weight         1172.54

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'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.57170(10)
_cell_length_b                   23.4186(3)
_cell_length_c                   13.6664(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.2460(10)
_cell_angle_gamma                90
_cell_volume                     2742.71(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6840
_cell_measurement_theta_min      3.7720
_cell_measurement_theta_max      72.9320

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_F_000             1220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    4.536
_shelx_estimated_absorpt_T_min   0.612
_shelx_estimated_absorpt_T_max   0.713
_exptl_absorpt_correction_T_min  0.70709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_method       'ω scan'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            11566
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.745
_diffrn_reflns_theta_max         73.352
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5415
_reflns_number_gt                4971
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43'
_computing_data_reduction        'CrysAlisPro 1.171.38.43'
_computing_structure_solution    OLEX2
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0266P)²+0.8649P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5415
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0649
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.000000 0.500000 1.000000 0.02211(6) Uani 1 2 d S . P . .
Cl2 Cl -0.25853(5) 0.54477(2) 1.06357(3) 0.02939(10) Uani 1 1 d . . . . .
O14 O 0.51299(17) 0.66956(6) 0.81622(10) 0.0304(3) Uani 1 1 d . . . . .
O11 O 0.58546(15) 0.59328(6) 0.65988(10) 0.0291(3) Uani 1 1 d . . . . .
C21 C 0.3808(2) 0.77343(9) 0.76708(14) 0.0278(4) Uani 1 1 d . . . . .
H21A H 0.345151 0.813636 0.767640 0.033 Uiso 1 1 calc R U . . .
H21B H 0.490335 0.773021 0.745559 0.033 Uiso 1 1 calc R U . . .
C33 C 0.1233(2) 0.73386(8) 0.72871(13) 0.0252(4) Uani 1 1 d . . . . .
H33A H 0.052990 0.732311 0.670348 0.030 Uiso 1 1 calc R U . . .
H33B H 0.093959 0.767716 0.767572 0.030 Uiso 1 1 calc R U . . .
N27 N 0.14410(19) 0.54673(7) 1.12844(11) 0.0262(3) Uani 1 1 d . . . . .
N3 N 0.33933(18) 0.63007(7) 0.45205(11) 0.0236(3) Uani 1 1 d . . . . .
N22 N 0.28367(18) 0.74088(7) 0.69662(11) 0.0230(3) Uani 1 1 d . . . . .
C5 C 0.5772(2) 0.56936(8) 0.49168(14) 0.0261(4) Uani 1 1 d . . . . .
N34 N 0.04273(18) 0.58149(7) 0.89894(11) 0.0245(3) Uani 1 1 d . . . . .
C12 C 0.6766(2) 0.59959(10) 0.74834(14) 0.0314(4) Uani 1 1 d . . . . .
H12A H 0.753129 0.630864 0.740766 0.038 Uiso 1 1 calc R U . . .
H12B H 0.734811 0.563883 0.762265 0.038 Uiso 1 1 calc R U . . .
C10 C 0.6666(2) 0.58073(8) 0.57669(14) 0.0268(4) Uani 1 1 d . . . . .
C38 C 0.1577(2) 0.62798(9) 0.76127(13) 0.0258(4) Uani 1 1 d . . . . .
H38 H 0.217474 0.624803 0.703815 0.031 Uiso 1 1 calc R U . . .
C30 C 0.3037(2) 0.60704(8) 0.27647(13) 0.0247(4) Uani 1 1 d . . . . .
C35 C -0.0138(2) 0.63223(9) 0.92563(14) 0.0277(4) Uani 1 1 d . . . . .
H35 H -0.074316 0.634241 0.982946 0.033 Uiso 1 1 calc R U . . .
C31 C 0.3838(2) 0.57943(9) 0.20275(14) 0.0267(4) Uani 1 1 d . . . . .
H31 H 0.494477 0.580971 0.201384 0.032 Uiso 1 1 calc R U . . .
C24 C 0.2523(2) 0.72323(9) 0.51956(13) 0.0262(4) Uani 1 1 d . . . . .
H24A H 0.148998 0.705913 0.531379 0.031 Uiso 1 1 calc R U . . .
H24B H 0.247673 0.742296 0.454913 0.031 Uiso 1 1 calc R U . . .
C23 C 0.2903(2) 0.76708(8) 0.59927(13) 0.0260(4) Uani 1 1 d . . . . .
H23A H 0.395996 0.782804 0.589310 0.031 Uiso 1 1 calc R U . . .
H23B H 0.214734 0.798992 0.594760 0.031 Uiso 1 1 calc R U . . .
C4 C 0.4003(2) 0.57464(8) 0.48625(13) 0.0254(4) Uani 1 1 d . . . . .
H4A H 0.358995 0.544499 0.442005 0.030 Uiso 1 1 calc R U . . .
H4B H 0.359273 0.567125 0.552171 0.030 Uiso 1 1 calc R U . . .
C37 C 0.0987(2) 0.68075(8) 0.78960(13) 0.0225(4) Uani 1 1 d . . . . .
C32 C 0.3001(2) 0.54952(9) 0.13100(13) 0.0265(4) Uani 1 1 d . . . . .
H32 H 0.356052 0.530237 0.081688 0.032 Uiso 1 1 calc R U . . .
C25 C 0.3769(2) 0.67682(9) 0.51968(13) 0.0250(4) Uani 1 1 d . . . . .
H25A H 0.477693 0.693990 0.501450 0.030 Uiso 1 1 calc R U . . .
H25B H 0.389325 0.661212 0.586718 0.030 Uiso 1 1 calc R U . . .
C29 C 0.1426(2) 0.60326(9) 0.27472(14) 0.0291(4) Uani 1 1 d . . . . .
H29 H 0.083748 0.620835 0.324563 0.035 Uiso 1 1 calc R U . . .
C19 C 0.3041(2) 0.77975(9) 0.94350(14) 0.0290(4) Uani 1 1 d . . . . .
H19 H 0.267366 0.817348 0.930734 0.035 Uiso 1 1 calc R U . . .
C39 C 0.1281(2) 0.58005(9) 0.81787(14) 0.0272(4) Uani 1 1 d . . . . .
H39 H 0.170532 0.544488 0.798172 0.033 Uiso 1 1 calc R U . . .
C36 C 0.0118(2) 0.68213(9) 0.87344(14) 0.0276(4) Uani 1 1 d . . . . .
H36 H -0.030501 0.717234 0.895467 0.033 Uiso 1 1 calc R U . . .
C15 C 0.4354(2) 0.69505(9) 0.89111(14) 0.0261(4) Uani 1 1 d . . . . .
C26 C 0.3844(2) 0.64409(9) 0.35251(13) 0.0257(4) Uani 1 1 d . . . . .
H26A H 0.498738 0.639507 0.347201 0.031 Uiso 1 1 calc R U . . .
H26B H 0.358824 0.684598 0.339061 0.031 Uiso 1 1 calc R U . . .
C13 C 0.5713(2) 0.61278(9) 0.83131(14) 0.0309(4) Uani 1 1 d . . . . .
H13A H 0.483875 0.585174 0.832449 0.037 Uiso 1 1 calc R U . . .
H13B H 0.629727 0.610371 0.894453 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3741(2) 0.74955(9) 0.86956(14) 0.0260(4) Uani 1 1 d . . . . .
C28 C 0.0679(2) 0.57360(10) 0.19956(14) 0.0309(4) Uani 1 1 d . . . . .
H28 H -0.042927 0.572248 0.198381 0.037 Uiso 1 1 calc R U . . .
C18 C 0.2861(2) 0.75644(10) 1.03622(15) 0.0329(4) Uani 1 1 d . . . . .
H18 H 0.237847 0.777786 1.086353 0.040 Uiso 1 1 calc R U . . .
C6 C 0.6566(3) 0.55238(9) 0.40852(15) 0.0320(4) Uani 1 1 d . . . . .
H6 H 0.598096 0.542738 0.351042 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8289(2) 0.57782(9) 0.57534(16) 0.0327(4) Uani 1 1 d . . . . .
H9 H 0.888487 0.586084 0.633042 0.039 Uiso 1 1 calc R U . . .
C17 C 0.3396(3) 0.70173(10) 1.05405(15) 0.0347(5) Uani 1 1 d . . . . .
H17 H 0.324055 0.684850 1.116298 0.042 Uiso 1 1 calc R U . . .
C16 C 0.4158(2) 0.67089(10) 0.98233(15) 0.0317(4) Uani 1 1 d . . . . .
H16 H 0.453988 0.633585 0.995936 0.038 Uiso 1 1 calc R U . . .
C7 C 0.8179(3) 0.54912(10) 0.40696(16) 0.0370(5) Uani 1 1 d . . . . .
H7 H 0.868820 0.537510 0.349205 0.044 Uiso 1 1 calc R U . . .
C8 C 0.9038(2) 0.56292(10) 0.49027(17) 0.0362(5) Uani 1 1 d . . . . .
H8 H 1.014605 0.562201 0.489226 0.043 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
Cd1 N34 2.3886(16) 3_567 ?
Cd1 N34 2.3886(16) . ?
Cd1 N27 2.3896(16) . ?
Cd1 N27 2.3897(15) 3_567 ?
Cd1 Cl2 2.6170(5) . ?
Cd1 Cl2 2.6170(5) 3_567 ?
O14 C15 1.369(2) . ?
O14 C13 1.434(2) . ?
O11 C10 1.377(2) . ?
O11 C12 1.433(2) . ?
C21 N22 1.472(2) . ?
C21 C20 1.510(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C33 N22 1.461(2) . ?
C33 C37 1.514(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
N27 C32 1.338(3) 1_556 ?
N27 C28 1.340(3) 1_556 ?
N3 C26 1.460(2) . ?
N3 C25 1.464(2) . ?
N3 C4 1.472(2) . ?
N22 C23 1.467(2) . ?
C5 C6 1.395(3) . ?
C5 C10 1.403(3) . ?
C5 C4 1.521(3) . ?
N34 C35 1.337(3) . ?
N34 C39 1.342(2) . ?
C12 C13 1.497(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10 C9 1.394(3) . ?
C38 C39 1.390(3) . ?
C38 C37 1.393(3) . ?
C38 H38 0.9500 . ?
C30 C29 1.384(3) . ?
C30 C31 1.391(3) . ?
C30 C26 1.510(2) . ?
C35 C36 1.389(3) . ?
C35 H35 0.9500 . ?
C31 C32 1.392(3) . ?
C31 H31 0.9500 . ?
C24 C25 1.524(3) . ?
C24 C23 1.527(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C37 C36 1.380(3) . ?
C32 H32 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C29 C28 1.385(3) . ?
C29 H29 0.9500 . ?
C19 C20 1.381(3) . ?
C19 C18 1.391(3) . ?
C19 H19 0.9500 . ?
C39 H39 0.9500 . ?
C36 H36 0.9500 . ?
C15 C16 1.383(3) . ?
C15 C20 1.409(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C28 H28 0.9500 . ?
C18 C17 1.381(3) . ?
C18 H18 0.9500 . ?
C6 C7 1.385(3) . ?
C6 H6 0.9500 . ?
C9 C8 1.385(3) . ?
C9 H9 0.9500 . ?
C17 C16 1.392(3) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C7 C8 1.381(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?

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
N34 Cd1 N34 180.0 3_567 . ?
N34 Cd1 N27 91.40(5) 3_567 . ?
N34 Cd1 N27 88.60(5) . . ?
N34 Cd1 N27 88.60(5) 3_567 3_567 ?
N34 Cd1 N27 91.40(5) . 3_567 ?
N27 Cd1 N27 180.0 . 3_567 ?
N34 Cd1 Cl2 89.23(4) 3_567 . ?
N34 Cd1 Cl2 90.77(4) . . ?
N27 Cd1 Cl2 90.03(4) . . ?
N27 Cd1 Cl2 89.97(4) 3_567 . ?
N34 Cd1 Cl2 90.77(4) 3_567 3_567 ?
N34 Cd1 Cl2 89.23(4) . 3_567 ?
N27 Cd1 Cl2 89.97(4) . 3_567 ?
N27 Cd1 Cl2 90.03(4) 3_567 3_567 ?
Cl2 Cd1 Cl2 180.0 . 3_567 ?
C15 O14 C13 118.03(16) . . ?
C10 O11 C12 116.27(16) . . ?
N22 C21 C20 112.50(16) . . ?
N22 C21 H21A 109.1 . . ?
C20 C21 H21A 109.1 . . ?
N22 C21 H21B 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
N22 C33 C37 113.65(15) . . ?
N22 C33 H33A 108.8 . . ?
C37 C33 H33A 108.8 . . ?
N22 C33 H33B 108.8 . . ?
C37 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C32 N27 C28 117.44(17) 1_556 1_556 ?
C32 N27 Cd1 122.80(13) 1_556 . ?
C28 N27 Cd1 119.70(13) 1_556 . ?
C26 N3 C25 111.17(15) . . ?
C26 N3 C4 113.26(15) . . ?
C25 N3 C4 112.79(14) . . ?
C33 N22 C23 112.00(14) . . ?
C33 N22 C21 112.60(15) . . ?
C23 N22 C21 110.13(15) . . ?
C6 C5 C10 117.48(19) . . ?
C6 C5 C4 119.13(18) . . ?
C10 C5 C4 123.39(18) . . ?
C35 N34 C39 117.07(17) . . ?
C35 N34 Cd1 119.43(12) . . ?
C39 N34 Cd1 123.42(13) . . ?
O11 C12 C13 109.48(16) . . ?
O11 C12 H12A 109.8 . . ?
C13 C12 H12A 109.8 . . ?
O11 C12 H12B 109.8 . . ?
C13 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
O11 C10 C9 122.93(18) . . ?
O11 C10 C5 116.60(17) . . ?
C9 C10 C5 120.46(19) . . ?
C39 C38 C37 119.35(17) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C29 C30 C31 117.76(18) . . ?
C29 C30 C26 119.39(17) . . ?
C31 C30 C26 122.68(18) . . ?
N34 C35 C36 123.06(17) . . ?
N34 C35 H35 118.5 . . ?
C36 C35 H35 118.5 . . ?
C30 C31 C32 119.30(18) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 H31 120.3 . . ?
C25 C24 C23 109.88(15) . . ?
C25 C24 H24A 109.7 . . ?
C23 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 . . ?
C23 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
N22 C23 C24 110.71(16) . . ?
N22 C23 H23A 109.5 . . ?
C24 C23 H23A 109.5 . . ?
N22 C23 H23B 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
N3 C4 C5 115.71(15) . . ?
N3 C4 H4A 108.4 . . ?
C5 C4 H4A 108.4 . . ?
N3 C4 H4B 108.4 . . ?
C5 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C36 C37 C38 117.20(18) . . ?
C36 C37 C33 121.43(18) . . ?
C38 C37 C33 121.33(16) . . ?
N27 C32 C31 122.86(18) 1_554 . ?
N27 C32 H32 118.6 1_554 . ?
C31 C32 H32 118.6 . . ?
N3 C25 C24 112.85(15) . . ?
N3 C25 H25A 109.0 . . ?
C24 C25 H25A 109.0 . . ?
N3 C25 H25B 109.0 . . ?
C24 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C30 C29 C28 119.34(18) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C20 C19 C18 121.6(2) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
N34 C39 C38 123.28(18) . . ?
N34 C39 H39 118.4 . . ?
C38 C39 H39 118.4 . . ?
C37 C36 C35 120.04(19) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
O14 C15 C16 124.49(19) . . ?
O14 C15 C20 115.05(17) . . ?
C16 C15 C20 120.46(19) . . ?
N3 C26 C30 112.68(16) . . ?
N3 C26 H26A 109.1 . . ?
C30 C26 H26A 109.1 . . ?
N3 C26 H26B 109.1 . . ?
C30 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
O14 C13 C12 107.25(17) . . ?
O14 C13 H13A 110.3 . . ?
C12 C13 H13A 110.3 . . ?
O14 C13 H13B 110.3 . . ?
C12 C13 H13B 110.3 . . ?
H13A C13 H13B 108.5 . . ?
C19 C20 C15 118.48(19) . . ?
C19 C20 C21 120.97(19) . . ?
C15 C20 C21 120.52(18) . . ?
N27 C28 C29 123.27(18) 1_554 . ?
N27 C28 H28 118.4 1_554 . ?
C29 C28 H28 118.4 . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C7 C6 C5 122.2(2) . . ?
C7 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
C8 C9 C10 120.3(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C18 C17 C16 121.1(2) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C15 C16 C17 119.4(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C8 C7 C6 119.3(2) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C7 C8 C9 120.1(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?

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
C37 C33 N22 C23 145.55(16) . . . . ?
C37 C33 N22 C21 -89.69(19) . . . . ?
C20 C21 N22 C33 52.3(2) . . . . ?
C20 C21 N22 C23 178.05(16) . . . . ?
C10 O11 C12 C13 -179.72(17) . . . . ?
C12 O11 C10 C9 -4.1(3) . . . . ?
C12 O11 C10 C5 174.37(18) . . . . ?
C6 C5 C10 O11 -175.32(18) . . . . ?
C4 C5 C10 O11 4.7(3) . . . . ?
C6 C5 C10 C9 3.2(3) . . . . ?
C4 C5 C10 C9 -176.78(18) . . . . ?
C39 N34 C35 C36 0.2(3) . . . . ?
Cd1 N34 C35 C36 177.01(15) . . . . ?
C29 C30 C31 C32 0.1(3) . . . . ?
C26 C30 C31 C32 -175.19(18) . . . . ?
C33 N22 C23 C24 -77.90(19) . . . . ?
C21 N22 C23 C24 155.97(16) . . . . ?
C25 C24 C23 N22 -64.5(2) . . . . ?
C26 N3 C4 C5 61.8(2) . . . . ?
C25 N3 C4 C5 -65.6(2) . . . . ?
C6 C5 C4 N3 -86.9(2) . . . . ?
C10 C5 C4 N3 93.1(2) . . . . ?
C39 C38 C37 C36 -0.5(3) . . . . ?
C39 C38 C37 C33 -178.06(17) . . . . ?
N22 C33 C37 C36 136.32(18) . . . . ?
N22 C33 C37 C38 -46.2(2) . . . . ?
C30 C31 C32 N27 1.1(3) . . . 1_554 ?
C26 N3 C25 C24 83.19(19) . . . . ?
C4 N3 C25 C24 -148.34(16) . . . . ?
C23 C24 C25 N3 173.91(15) . . . . ?
C31 C30 C29 C28 -1.4(3) . . . . ?
C26 C30 C29 C28 174.05(19) . . . . ?
C35 N34 C39 C38 -0.8(3) . . . . ?
Cd1 N34 C39 C38 -177.49(14) . . . . ?
C37 C38 C39 N34 1.0(3) . . . . ?
C38 C37 C36 C35 -0.1(3) . . . . ?
C33 C37 C36 C35 177.48(17) . . . . ?
N34 C35 C36 C37 0.2(3) . . . . ?
C13 O14 C15 C16 3.3(3) . . . . ?
C13 O14 C15 C20 -176.77(16) . . . . ?
C25 N3 C26 C30 -161.52(16) . . . . ?
C4 N3 C26 C30 70.3(2) . . . . ?
C29 C30 C26 N3 54.1(2) . . . . ?
C31 C30 C26 N3 -130.77(19) . . . . ?
C15 O14 C13 C12 -168.93(16) . . . . ?
O11 C12 C13 O14 -70.1(2) . . . . ?
C18 C19 C20 C15 -3.3(3) . . . . ?
C18 C19 C20 C21 174.83(18) . . . . ?
O14 C15 C20 C19 -175.42(17) . . . . ?
C16 C15 C20 C19 4.5(3) . . . . ?
O14 C15 C20 C21 6.4(3) . . . . ?
C16 C15 C20 C21 -173.65(18) . . . . ?
N22 C21 C20 C19 -112.1(2) . . . . ?
N22 C21 C20 C15 66.0(2) . . . . ?
C30 C29 C28 N27 1.7(3) . . . 1_554 ?
C20 C19 C18 C17 -0.1(3) . . . . ?
C10 C5 C6 C7 -2.9(3) . . . . ?
C4 C5 C6 C7 177.1(2) . . . . ?
O11 C10 C9 C8 177.6(2) . . . . ?
C5 C10 C9 C8 -0.8(3) . . . . ?
C19 C18 C17 C16 2.5(3) . . . . ?
O14 C15 C16 C17 177.69(19) . . . . ?
C20 C15 C16 C17 -2.3(3) . . . . ?
C18 C17 C16 C15 -1.3(3) . . . . ?
C5 C6 C7 C8 0.2(3) . . . . ?
C6 C7 C8 C9 2.4(4) . . . . ?
C10 C9 C8 C7 -2.0(4) . . . . ?

_refine_diff_density_max         0.609
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_L2
_database_code_depnum_ccdc_archive 'CCDC 1542747'
_audit_update_record             
;
2017-10-02 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H34 N4 O2'
_chemical_formula_sum            'C31 H34 N4 O2'
_chemical_formula_weight         494.62

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.0288(3)
_cell_length_b                   16.1383(5)
_cell_length_c                   16.1962(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.845(3)
_cell_angle_gamma                90
_cell_volume                     2621.03(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(1)
_cell_measurement_reflns_used    3188
_cell_measurement_theta_min      3.4330
_cell_measurement_theta_max      26.3440

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.080
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.91793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       '/w scan'
_diffrn_reflns_number            9899
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.241
_diffrn_reflns_theta_max         26.574
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5042
_reflns_number_gt                3842
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0398P)²+0.0454P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5042
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
O1 O 0.86985(9) 0.56647(6) 0.42595(5) 0.0236(2) Uani 1 1 d . . . . .
C2 C 0.80180(15) 0.54523(9) 0.50008(8) 0.0220(3) Uani 1 1 d . . . . .
H2B H 0.7463(14) 0.5912(8) 0.5171(8) 0.016(3) Uiso 1 1 d . . . . .
H2A H 0.8680(14) 0.5325(8) 0.5449(8) 0.023(4) Uiso 1 1 d . . . . .
C3 C 0.72095(15) 0.46916(9) 0.48515(9) 0.0217(3) Uani 1 1 d . . . . .
H3B H 0.6819(13) 0.4527(8) 0.5376(8) 0.017(3) Uiso 1 1 d . . . . .
H3A H 0.7771(14) 0.4247(9) 0.4655(8) 0.021(4) Uiso 1 1 d . . . . .
O4 O 0.61754(9) 0.48754(5) 0.42646(5) 0.0214(2) Uani 1 1 d . . . . .
C5 C 0.53357(13) 0.42398(8) 0.40418(8) 0.0195(3) Uani 1 1 d . . . . .
C6 C 0.44632(13) 0.43941(8) 0.33748(8) 0.0201(3) Uani 1 1 d . . . . .
C7 C 0.45467(15) 0.51923(9) 0.28796(9) 0.0216(3) Uani 1 1 d . . . . .
H7B H 0.3623(15) 0.5352(8) 0.2679(8) 0.022(4) Uiso 1 1 d . . . . .
H7A H 0.4883(13) 0.5647(8) 0.3237(8) 0.017(3) Uiso 1 1 d . . . . .
N8 N 0.54006(11) 0.51631(7) 0.21437(7) 0.0213(3) Uani 1 1 d . . . . .
C9 C 0.67649(15) 0.48918(9) 0.23506(9) 0.0239(3) Uani 1 1 d . . . . .
H9B H 0.7007(14) 0.5134(8) 0.2892(9) 0.023(4) Uiso 1 1 d . . . . .
H9A H 0.6798(14) 0.4255(9) 0.2404(8) 0.025(4) Uiso 1 1 d . . . . .
C10 C 0.77852(16) 0.51747(9) 0.17230(9) 0.0266(3) Uani 1 1 d . . . . .
H10B H 0.7509(15) 0.5010(8) 0.1137(10) 0.029(4) Uiso 1 1 d . . . . .
H10A H 0.8703(17) 0.4866(9) 0.1851(9) 0.037(4) Uiso 1 1 d . . . . .
C11 C 0.80030(16) 0.61056(9) 0.17246(9) 0.0261(3) Uani 1 1 d . . . . .
H11B H 0.8636(15) 0.6274(8) 0.1268(9) 0.028(4) Uiso 1 1 d . . . . .
H11A H 0.7129(16) 0.6375(9) 0.1573(8) 0.027(4) Uiso 1 1 d . . . . .
N12 N 0.84415(11) 0.64462(7) 0.25225(7) 0.0225(3) Uani 1 1 d . . . . .
C13 C 0.97910(15) 0.61692(10) 0.27588(9) 0.0247(3) Uani 1 1 d . . . . .
H13B H 0.9808(14) 0.5568(9) 0.2782(8) 0.023(4) Uiso 1 1 d . . . . .
H13A H 1.0469(15) 0.6340(9) 0.2333(9) 0.028(4) Uiso 1 1 d . . . . .
C14 C 1.02323(14) 0.65268(9) 0.35799(9) 0.0230(3) Uani 1 1 d . . . . .
C15 C 0.95916(13) 0.63079(8) 0.43135(8) 0.0212(3) Uani 1 1 d . . . . .
C16 C 0.98808(15) 0.67287(9) 0.50422(9) 0.0250(3) Uani 1 1 d . . . . .
H16 H 0.9431(14) 0.6589(8) 0.5534(9) 0.023(4) Uiso 1 1 d . . . . .
C17 C 1.08644(15) 0.73355(9) 0.50564(10) 0.0285(4) Uani 1 1 d . . . . .
H17 H 1.1058(15) 0.7615(9) 0.5576(9) 0.030(4) Uiso 1 1 d . . . . .
C18 C 1.15566(16) 0.75210(9) 0.43559(10) 0.0300(4) Uani 1 1 d . . . . .
H18 H 1.2279(16) 0.7945(9) 0.4375(9) 0.034(4) Uiso 1 1 d . . . . .
C19 C 1.12249(15) 0.71216(9) 0.36236(10) 0.0284(3) Uani 1 1 d . . . . .
H19 H 1.1692(15) 0.7250(9) 0.3127(9) 0.030(4) Uiso 1 1 d . . . . .
C20 C 0.53133(15) 0.34841(9) 0.44570(9) 0.0222(3) Uani 1 1 d . . . . .
H20 H 0.5943(14) 0.3376(8) 0.4910(8) 0.021(4) Uiso 1 1 d . . . . .
C21 C 0.43946(15) 0.28812(9) 0.42277(9) 0.0248(3) Uani 1 1 d . . . . .
H21 H 0.4396(15) 0.2361(9) 0.4523(9) 0.028(4) Uiso 1 1 d . . . . .
C22 C 0.34973(15) 0.30295(9) 0.35918(9) 0.0253(3) Uani 1 1 d . . . . .
H22 H 0.2838(16) 0.2622(9) 0.3438(9) 0.032(4) Uiso 1 1 d . . . . .
C23 C 0.35450(14) 0.37799(9) 0.31729(9) 0.0233(3) Uani 1 1 d . . . . .
H23 H 0.2919(14) 0.3888(8) 0.2726(8) 0.019(3) Uiso 1 1 d . . . . .
C24 C 0.48162(15) 0.46493(9) 0.14833(9) 0.0236(3) Uani 1 1 d . . . . .
H24B H 0.5526(14) 0.4567(8) 0.1063(8) 0.023(4) Uiso 1 1 d . . . . .
H24A H 0.4541(14) 0.4066(9) 0.1683(8) 0.023(4) Uiso 1 1 d . . . . .
C25 C 0.36422(14) 0.50728(8) 0.10758(8) 0.0226(3) Uani 1 1 d . . . . .
C26 C 0.23682(15) 0.47448(9) 0.10798(9) 0.0252(3) Uani 1 1 d . . . . .
H26 H 0.2187(15) 0.4221(9) 0.1339(9) 0.033(4) Uiso 1 1 d . . . . .
C27 C 0.13390(17) 0.51627(10) 0.06900(9) 0.0294(4) Uani 1 1 d . . . . .
H27 H 0.0434(18) 0.4920(9) 0.0677(10) 0.041(5) Uiso 1 1 d . . . . .
N28 N 0.14817(13) 0.58818(8) 0.02906(7) 0.0317(3) Uani 1 1 d . . . . .
C29 C 0.27213(16) 0.61931(10) 0.02876(9) 0.0313(4) Uani 1 1 d . . . . .
H29 H 0.2835(15) 0.6727(10) -0.0009(10) 0.036(4) Uiso 1 1 d . . . . .
C30 C 0.38032(16) 0.58213(9) 0.06645(9) 0.0276(3) Uani 1 1 d . . . . .
H30 H 0.4674(17) 0.6073(9) 0.0653(9) 0.037(4) Uiso 1 1 d . . . . .
C31 C 0.82993(15) 0.73501(9) 0.25089(10) 0.0254(3) Uani 1 1 d . . . . .
H31B H 0.8658(15) 0.7593(8) 0.1978(9) 0.028(4) Uiso 1 1 d . . . . .
H31A H 0.8844(15) 0.7593(9) 0.2980(9) 0.031(4) Uiso 1 1 d . . . . .
C32 C 0.68730(14) 0.75984(8) 0.26435(8) 0.0222(3) Uani 1 1 d . . . . .
C33 C 0.62409(15) 0.81987(9) 0.21667(9) 0.0247(3) Uani 1 1 d . . . . .
H33 H 0.6714(16) 0.8474(9) 0.1704(10) 0.038(4) Uiso 1 1 d . . . . .
C34 C 0.49493(16) 0.84258(9) 0.23424(9) 0.0284(4) Uani 1 1 d . . . . .
H34 H 0.4502(16) 0.8853(9) 0.2004(9) 0.036(4) Uiso 1 1 d . . . . .
N35 N 0.42338(13) 0.80984(8) 0.29455(8) 0.0314(3) Uani 1 1 d . . . . .
C36 C 0.48524(17) 0.75154(10) 0.33948(10) 0.0356(4) Uani 1 1 d . . . . .
H36 H 0.4307(16) 0.7269(10) 0.3842(10) 0.040(5) Uiso 1 1 d . . . . .
C37 C 0.61396(16) 0.72550(10) 0.32717(10) 0.0311(4) Uani 1 1 d . . . . .
H37 H 0.6526(15) 0.6824(9) 0.3617(9) 0.037(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.3730(16) . ?
O1 C2 1.4314(16) . ?
C2 C3 1.489(2) . ?
C2 H2B 0.970(14) . ?
C2 H2A 0.998(14) . ?
C3 O4 1.4275(16) . ?
C3 H3B 0.977(14) . ?
C3 H3A 0.969(14) . ?
O4 C5 1.3721(15) . ?
C5 C20 1.3930(19) . ?
C5 C6 1.4024(18) . ?
C6 C23 1.3887(19) . ?
C6 C7 1.5205(19) . ?
C7 N8 1.4786(17) . ?
C7 H7B 1.011(14) . ?
C7 H7A 0.991(14) . ?
N8 C24 1.4686(17) . ?
N8 C9 1.4706(18) . ?
C9 C10 1.523(2) . ?
C9 H9B 0.988(14) . ?
C9 H9A 1.032(14) . ?
C10 C11 1.518(2) . ?
C10 H10B 1.020(15) . ?
C10 H10A 1.064(16) . ?
C11 N12 1.4659(18) . ?
C11 H11B 1.019(15) . ?
C11 H11A 1.005(15) . ?
N12 C31 1.4658(18) . ?
N12 C13 1.4706(18) . ?
C13 C14 1.510(2) . ?
C13 H13B 0.970(14) . ?
C13 H13A 1.014(15) . ?
C14 C19 1.384(2) . ?
C14 C15 1.4043(19) . ?
C15 C16 1.3885(19) . ?
C16 C17 1.390(2) . ?
C16 H16 0.949(14) . ?
C17 C18 1.372(2) . ?
C17 H17 0.972(15) . ?
C18 C19 1.386(2) . ?
C18 H18 0.996(16) . ?
C19 H19 0.959(16) . ?
C20 C21 1.387(2) . ?
C20 H20 0.977(14) . ?
C21 C22 1.379(2) . ?
C21 H21 0.967(14) . ?
C22 C23 1.389(2) . ?
C22 H22 0.963(15) . ?
C23 H23 0.968(13) . ?
C24 C25 1.505(2) . ?
C24 H24B 1.001(14) . ?
C24 H24A 1.034(14) . ?
C25 C26 1.383(2) . ?
C25 C30 1.390(2) . ?
C26 C27 1.378(2) . ?
C26 H26 0.962(15) . ?
C27 N28 1.3374(19) . ?
C27 H27 0.988(17) . ?
N28 C29 1.341(2) . ?
C29 C30 1.375(2) . ?
C29 H29 0.995(16) . ?
C30 H30 0.964(16) . ?
C31 C32 1.504(2) . ?
C31 H31B 1.016(15) . ?
C31 H31A 1.012(15) . ?
C32 C37 1.380(2) . ?
C32 C33 1.386(2) . ?
C33 C34 1.380(2) . ?
C33 H33 0.997(16) . ?
C34 N35 1.3299(19) . ?
C34 H34 0.984(15) . ?
N35 C36 1.3365(19) . ?
C36 C37 1.375(2) . ?
C36 H36 0.997(16) . ?
C37 H37 0.969(16) . ?

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
C15 O1 C2 116.51(10) . . ?
O1 C2 C3 109.06(11) . . ?
O1 C2 H2B 109.8(8) . . ?
C3 C2 H2B 111.3(8) . . ?
O1 C2 H2A 109.8(8) . . ?
C3 C2 H2A 107.6(8) . . ?
H2B C2 H2A 109.2(11) . . ?
O4 C3 C2 108.98(12) . . ?
O4 C3 H3B 109.8(8) . . ?
C2 C3 H3B 107.9(8) . . ?
O4 C3 H3A 110.8(8) . . ?
C2 C3 H3A 110.3(8) . . ?
H3B C3 H3A 109.0(11) . . ?
C5 O4 C3 117.18(10) . . ?
O4 C5 C20 122.80(12) . . ?
O4 C5 C6 116.32(11) . . ?
C20 C5 C6 120.86(13) . . ?
C23 C6 C5 117.30(12) . . ?
C23 C6 C7 121.47(12) . . ?
C5 C6 C7 121.21(12) . . ?
N8 C7 C6 115.80(11) . . ?
N8 C7 H7B 106.8(8) . . ?
C6 C7 H7B 109.1(8) . . ?
N8 C7 H7A 107.4(8) . . ?
C6 C7 H7A 109.9(7) . . ?
H7B C7 H7A 107.6(11) . . ?
C24 N8 C9 110.96(11) . . ?
C24 N8 C7 112.05(11) . . ?
C9 N8 C7 111.95(11) . . ?
N8 C9 C10 113.00(12) . . ?
N8 C9 H9B 107.5(8) . . ?
C10 C9 H9B 108.4(8) . . ?
N8 C9 H9A 110.2(8) . . ?
C10 C9 H9A 109.4(8) . . ?
H9B C9 H9A 108.3(11) . . ?
C11 C10 C9 113.18(13) . . ?
C11 C10 H10B 107.3(8) . . ?
C9 C10 H10B 111.5(8) . . ?
C11 C10 H10A 109.8(8) . . ?
C9 C10 H10A 108.5(8) . . ?
H10B C10 H10A 106.4(12) . . ?
N12 C11 C10 114.45(12) . . ?
N12 C11 H11B 111.0(8) . . ?
C10 C11 H11B 110.7(8) . . ?
N12 C11 H11A 107.6(8) . . ?
C10 C11 H11A 107.6(8) . . ?
H11B C11 H11A 105.0(11) . . ?
C31 N12 C11 109.39(11) . . ?
C31 N12 C13 113.29(12) . . ?
C11 N12 C13 112.24(11) . . ?
N12 C13 C14 111.70(12) . . ?
N12 C13 H13B 109.2(8) . . ?
C14 C13 H13B 110.1(8) . . ?
N12 C13 H13A 111.3(8) . . ?
C14 C13 H13A 107.7(8) . . ?
H13B C13 H13A 106.7(12) . . ?
C19 C14 C15 117.96(13) . . ?
C19 C14 C13 120.76(13) . . ?
C15 C14 C13 121.15(13) . . ?
O1 C15 C16 123.49(12) . . ?
O1 C15 C14 116.25(12) . . ?
C16 C15 C14 120.25(13) . . ?
C15 C16 C17 119.86(14) . . ?
C15 C16 H16 120.1(9) . . ?
C17 C16 H16 120.0(9) . . ?
C18 C17 C16 120.51(15) . . ?
C18 C17 H17 121.2(9) . . ?
C16 C17 H17 118.3(9) . . ?
C17 C18 C19 119.22(15) . . ?
C17 C18 H18 120.0(9) . . ?
C19 C18 H18 120.8(9) . . ?
C14 C19 C18 121.99(15) . . ?
C14 C19 H19 117.8(9) . . ?
C18 C19 H19 120.2(9) . . ?
C21 C20 C5 120.02(14) . . ?
C21 C20 H20 119.7(8) . . ?
C5 C20 H20 120.3(8) . . ?
C22 C21 C20 120.13(14) . . ?
C22 C21 H21 121.1(9) . . ?
C20 C21 H21 118.8(9) . . ?
C21 C22 C23 119.30(14) . . ?
C21 C22 H22 120.9(9) . . ?
C23 C22 H22 119.8(9) . . ?
C6 C23 C22 122.32(14) . . ?
C6 C23 H23 117.9(8) . . ?
C22 C23 H23 119.7(8) . . ?
N8 C24 C25 111.35(11) . . ?
N8 C24 H24B 106.8(8) . . ?
C25 C24 H24B 108.8(8) . . ?
N8 C24 H24A 113.0(7) . . ?
C25 C24 H24A 109.9(8) . . ?
H24B C24 H24A 106.7(11) . . ?
C26 C25 C30 116.66(14) . . ?
C26 C25 C24 122.74(13) . . ?
C30 C25 C24 120.60(13) . . ?
C27 C26 C25 119.75(14) . . ?
C27 C26 H26 119.0(9) . . ?
C25 C26 H26 121.2(9) . . ?
N28 C27 C26 124.16(15) . . ?
N28 C27 H27 116.0(9) . . ?
C26 C27 H27 119.8(9) . . ?
C27 N28 C29 115.64(13) . . ?
N28 C29 C30 124.09(15) . . ?
N28 C29 H29 116.1(9) . . ?
C30 C29 H29 119.9(9) . . ?
C29 C30 C25 119.71(15) . . ?
C29 C30 H30 121.1(9) . . ?
C25 C30 H30 119.2(9) . . ?
N12 C31 C32 110.81(12) . . ?
N12 C31 H31B 111.2(8) . . ?
C32 C31 H31B 111.6(8) . . ?
N12 C31 H31A 108.9(8) . . ?
C32 C31 H31A 106.9(8) . . ?
H31B C31 H31A 107.2(11) . . ?
C37 C32 C33 116.54(14) . . ?
C37 C32 C31 121.20(13) . . ?
C33 C32 C31 122.23(13) . . ?
C34 C33 C32 119.58(14) . . ?
C34 C33 H33 119.7(9) . . ?
C32 C33 H33 120.7(9) . . ?
N35 C34 C33 124.34(14) . . ?
N35 C34 H34 116.1(9) . . ?
C33 C34 H34 119.6(9) . . ?
C34 N35 C36 115.37(14) . . ?
N35 C36 C37 124.44(15) . . ?
N35 C36 H36 114.9(9) . . ?
C37 C36 H36 120.6(9) . . ?
C36 C37 C32 119.72(14) . . ?
C36 C37 H37 120.3(9) . . ?
C32 C37 H37 120.0(9) . . ?

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
C15 O1 C2 C3 -173.93(11) . . . . ?
O1 C2 C3 O4 -65.98(15) . . . . ?
C2 C3 O4 C5 179.15(11) . . . . ?
C3 O4 C5 C20 10.96(18) . . . . ?
C3 O4 C5 C6 -170.38(12) . . . . ?
O4 C5 C6 C23 -175.90(11) . . . . ?
C20 C5 C6 C23 2.79(19) . . . . ?
O4 C5 C6 C7 5.71(18) . . . . ?
C20 C5 C6 C7 -175.60(13) . . . . ?
C23 C6 C7 N8 -86.27(16) . . . . ?
C5 C6 C7 N8 92.05(15) . . . . ?
C6 C7 N8 C24 70.24(15) . . . . ?
C6 C7 N8 C9 -55.17(16) . . . . ?
C24 N8 C9 C10 77.11(15) . . . . ?
C7 N8 C9 C10 -156.88(12) . . . . ?
N8 C9 C10 C11 68.16(17) . . . . ?
C9 C10 C11 N12 58.03(18) . . . . ?
C10 C11 N12 C31 -166.06(13) . . . . ?
C10 C11 N12 C13 67.30(16) . . . . ?
C31 N12 C13 C14 55.28(16) . . . . ?
C11 N12 C13 C14 179.79(12) . . . . ?
N12 C13 C14 C19 -109.91(15) . . . . ?
N12 C13 C14 C15 65.85(17) . . . . ?
C2 O1 C15 C16 2.06(18) . . . . ?
C2 O1 C15 C14 -178.50(12) . . . . ?
C19 C14 C15 O1 -174.36(12) . . . . ?
C13 C14 C15 O1 9.77(19) . . . . ?
C19 C14 C15 C16 5.1(2) . . . . ?
C13 C14 C15 C16 -170.77(13) . . . . ?
O1 C15 C16 C17 175.62(13) . . . . ?
C14 C15 C16 C17 -3.8(2) . . . . ?
C15 C16 C17 C18 -0.2(2) . . . . ?
C16 C17 C18 C19 2.8(2) . . . . ?
C15 C14 C19 C18 -2.5(2) . . . . ?
C13 C14 C19 C18 173.35(13) . . . . ?
C17 C18 C19 C14 -1.4(2) . . . . ?
O4 C5 C20 C21 176.76(12) . . . . ?
C6 C5 C20 C21 -1.8(2) . . . . ?
C5 C20 C21 C22 -0.4(2) . . . . ?
C20 C21 C22 C23 1.5(2) . . . . ?
C5 C6 C23 C22 -1.7(2) . . . . ?
C7 C6 C23 C22 176.72(13) . . . . ?
C21 C22 C23 C6 -0.5(2) . . . . ?
C9 N8 C24 C25 -161.32(12) . . . . ?
C7 N8 C24 C25 72.73(15) . . . . ?
N8 C24 C25 C26 -118.57(15) . . . . ?
N8 C24 C25 C30 62.13(17) . . . . ?
C30 C25 C26 C27 -0.3(2) . . . . ?
C24 C25 C26 C27 -179.59(13) . . . . ?
C25 C26 C27 N28 0.4(2) . . . . ?
C26 C27 N28 C29 -0.2(2) . . . . ?
C27 N28 C29 C30 -0.2(2) . . . . ?
N28 C29 C30 C25 0.4(2) . . . . ?
C26 C25 C30 C29 -0.1(2) . . . . ?
C24 C25 C30 C29 179.20(13) . . . . ?
C11 N12 C31 C32 79.29(15) . . . . ?
C13 N12 C31 C32 -154.68(12) . . . . ?
N12 C31 C32 C37 47.34(19) . . . . ?
N12 C31 C32 C33 -134.87(14) . . . . ?
C37 C32 C33 C34 0.7(2) . . . . ?
C31 C32 C33 C34 -177.21(13) . . . . ?
C32 C33 C34 N35 -0.8(2) . . . . ?
C33 C34 N35 C36 0.2(2) . . . . ?
C34 N35 C36 C37 0.5(2) . . . . ?
N35 C36 C37 C32 -0.6(3) . . . . ?
C33 C32 C37 C36 0.0(2) . . . . ?
C31 C32 C37 C36 177.87(15) . . . . ?

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
C9 H9B O4 0.988(14) 2.422(14) 3.1645(17) 131.6(10) .
C26 H26 N35 0.962(15) 2.589(16) 3.494(2) 156.7(12) 2_545

_refine_diff_density_max         0.152
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.040

####################################################################### 
# 
# 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_5_dmso
_database_code_depnum_ccdc_archive 'CCDC 1542749'
_audit_update_record             
;
2017-10-02 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H68 Cl2 N8 O4 Pb'
_chemical_formula_sum            'C62 H68 Cl2 N8 O4 Pb'
_chemical_formula_weight         1267.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.6900(2)
_cell_length_b                   23.6505(4)
_cell_length_c                   13.7975(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.038(2)
_cell_angle_gamma                90
_cell_volume                     2833.91(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    5102
_cell_measurement_theta_min      3.2990
_cell_measurement_theta_max      27.9320

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.126
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.76267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(1)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       '/w scan'
_diffrn_reflns_number            12499
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.816
_diffrn_reflns_theta_max         28.237
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5895
_reflns_number_gt                4374
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0150P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5895
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0522
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.0000 0.5000 1.0000 0.01610(5) Uani 1 2 d S . P . .
Cl1 Cl -0.26389(10) 0.44877(3) 1.07446(6) 0.02591(19) Uani 1 1 d . . . . .
O1 O 0.5335(3) 0.32771(8) 0.82174(16) 0.0243(5) Uani 1 1 d . . . . .
C2 C 0.5903(4) 0.38423(12) 0.8369(2) 0.0271(8) Uani 1 1 d . . . . .
H2A H 0.6484 0.3867 0.8998 0.033 Uiso 1 1 calc R U . . .
H2B H 0.5034 0.4113 0.8377 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6931(4) 0.39788(14) 0.7555(3) 0.0288(9) Uani 1 1 d . . . . .
H3A H 0.7499 0.4333 0.7701 0.035 Uiso 1 1 calc R U . . .
H3B H 0.7692 0.3672 0.7481 0.035 Uiso 1 1 calc R U . . .
O4 O 0.6022(3) 0.40426(8) 0.66701(17) 0.0257(6) Uani 1 1 d . . . . .
C5 C 0.6817(4) 0.41773(12) 0.5854(3) 0.0230(8) Uani 1 1 d . . . . .
C6 C 0.5913(4) 0.42864(11) 0.5011(3) 0.0201(8) Uani 1 1 d . . . . .
C7 C 0.4174(4) 0.42234(12) 0.4960(2) 0.0231(9) Uani 1 1 d . . . . .
H7A H 0.3785 0.4294 0.5615 0.028 Uiso 1 1 calc R U . . .
H7B H 0.3743 0.4522 0.4526 0.028 Uiso 1 1 calc R U . . .
N8 N 0.3566(3) 0.36703(9) 0.46168(19) 0.0189(6) Uani 1 1 d . . . . .
C9 C 0.4002(4) 0.32060(11) 0.5277(2) 0.0187(7) Uani 1 1 d . . . . .
H9A H 0.4127 0.3356 0.5945 0.022 Uiso 1 1 calc R U . . .
H9B H 0.5007 0.3050 0.5090 0.022 Uiso 1 1 calc R U . . .
C10 C 0.2803(4) 0.27284(12) 0.5262(2) 0.0196(7) Uani 1 1 d . . . . .
H10A H 0.1770 0.2886 0.5378 0.023 Uiso 1 1 calc R U . . .
H10B H 0.2767 0.2542 0.4619 0.023 Uiso 1 1 calc R U . . .
C11 C 0.3235(4) 0.22989(11) 0.6047(2) 0.0192(7) Uani 1 1 d . . . . .
H11A H 0.2540 0.1968 0.5985 0.023 Uiso 1 1 calc R U . . .
H11B H 0.4301 0.2166 0.5958 0.023 Uiso 1 1 calc R U . . .
N12 N 0.3122(3) 0.25454(9) 0.70203(19) 0.0167(6) Uani 1 1 d . . . . .
C13 C 0.4085(4) 0.22371(12) 0.7735(2) 0.0208(8) Uani 1 1 d . . . . .
H13A H 0.5168 0.2247 0.7536 0.025 Uiso 1 1 calc R U . . .
H13B H 0.3754 0.1837 0.7746 0.025 Uiso 1 1 calc R U . . .
C14 C 0.3997(4) 0.24811(12) 0.8744(2) 0.0197(7) Uani 1 1 d . . . . .
C15 C 0.4573(4) 0.30256(12) 0.8953(2) 0.0215(8) Uani 1 1 d . . . . .
C16 C 0.4368(4) 0.32702(13) 0.9856(2) 0.0248(8) Uani 1 1 d . . . . .
H16 H 0.4736 0.3641 0.9990 0.030 Uiso 1 1 calc R U . . .
C17 C 0.3618(4) 0.29662(13) 1.0560(2) 0.0261(8) Uani 1 1 d . . . . .
H17 H 0.3457 0.3136 1.1172 0.031 Uiso 1 1 calc R U . . .
C18 C 0.3104(4) 0.24228(13) 1.0385(2) 0.0245(8) Uani 1 1 d . . . . .
H18 H 0.2621 0.2214 1.0877 0.029 Uiso 1 1 calc R U . . .
C19 C 0.3305(4) 0.21857(12) 0.9477(2) 0.0229(8) Uani 1 1 d . . . . .
H19 H 0.2958 0.1811 0.9355 0.027 Uiso 1 1 calc R U . . .
C20 C 0.8403(4) 0.42149(12) 0.5844(3) 0.0284(9) Uani 1 1 d . . . . .
H20 H 0.9002 0.4139 0.6419 0.034 Uiso 1 1 calc R U . . .
C21 C 0.9122(4) 0.43621(13) 0.5002(3) 0.0319(9) Uani 1 1 d . . . . .
H21 H 1.0214 0.4372 0.4993 0.038 Uiso 1 1 calc R U . . .
C22 C 0.8259(4) 0.44949(13) 0.4177(3) 0.0294(9) Uani 1 1 d . . . . .
H22 H 0.8749 0.4611 0.3606 0.035 Uiso 1 1 calc R U . . .
C23 C 0.6673(4) 0.44581(12) 0.4189(3) 0.0258(8) Uani 1 1 d . . . . .
H23 H 0.6082 0.4553 0.3619 0.031 Uiso 1 1 calc R U . . .
C24 C 0.4005(4) 0.35410(12) 0.3628(2) 0.0190(7) Uani 1 1 d . . . . .
H24A H 0.3754 0.3141 0.3484 0.023 Uiso 1 1 calc R U . . .
H24B H 0.5133 0.3587 0.3585 0.023 Uiso 1 1 calc R U . . .
C25 C 0.3213(4) 0.39106(12) 0.2874(2) 0.0196(8) Uani 1 1 d . . . . .
C26 C 0.4013(4) 0.41731(12) 0.2139(2) 0.0218(8) Uani 1 1 d . . . . .
H26 H 0.5101 0.4143 0.2120 0.026 Uiso 1 1 calc R U . . .
C27 C 0.3192(4) 0.44792(12) 0.1438(2) 0.0248(8) Uani 1 1 d . . . . .
H27 H 0.3743 0.4657 0.0939 0.030 Uiso 1 1 calc R U . . .
N28 N 0.1669(3) 0.45361(10) 0.1429(2) 0.0273(7) Uani 1 1 d . . . . .
C29 C 0.0911(4) 0.42845(13) 0.2137(3) 0.0301(9) Uani 1 1 d . . . . .
H29 H -0.0179 0.4317 0.2133 0.036 Uiso 1 1 calc R U . . .
C30 C 0.1634(4) 0.39805(12) 0.2871(2) 0.0235(8) Uani 1 1 d . . . . .
H30 H 0.1052 0.3820 0.3371 0.028 Uiso 1 1 calc R U . . .
C31 C 0.1526(4) 0.25942(11) 0.7306(2) 0.0185(7) Uani 1 1 d . . . . .
H31A H 0.1259 0.2258 0.7694 0.022 Uiso 1 1 calc R U . . .
H31B H 0.0843 0.2597 0.6716 0.022 Uiso 1 1 calc R U . . .
C32 C 0.1230(4) 0.31205(11) 0.7890(2) 0.0169(7) Uani 1 1 d . . . . .
C33 C 0.1787(4) 0.36472(11) 0.7598(2) 0.0210(8) Uani 1 1 d . . . . .
H33 H 0.2389 0.3678 0.7039 0.025 Uiso 1 1 calc R U . . .
C34 C 0.1448(4) 0.41218(12) 0.8134(2) 0.0228(8) Uani 1 1 d . . . . .
H34 H 0.1852 0.4475 0.7935 0.027 Uiso 1 1 calc R U . . .
N35 N 0.0583(3) 0.41127(9) 0.8916(2) 0.0253(7) Uani 1 1 d . . . . .
C36 C 0.0046(4) 0.36081(12) 0.9191(2) 0.0247(8) Uani 1 1 d . . . . .
H36 H -0.0571 0.3590 0.9744 0.030 Uiso 1 1 calc R U . . .
C37 C 0.0353(4) 0.31113(12) 0.8702(2) 0.0207(8) Uani 1 1 d . . . . .
H37 H -0.0043 0.2763 0.8928 0.025 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
Pb1 N35 2.636(2) 3_567 ?
Pb1 N35 2.636(2) . ?
Pb1 N28 2.644(3) 3_566 ?
Pb1 N28 2.644(3) 1_556 ?
Pb1 Cl1 2.8196(8) . ?
Pb1 Cl1 2.8196(8) 3_567 ?
O1 C15 1.368(3) . ?
O1 C2 1.438(3) . ?
C2 C3 1.495(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O4 1.439(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C5 1.379(4) . ?
C5 C20 1.381(4) . ?
C5 C6 1.404(5) . ?
C6 C23 1.393(4) . ?
C6 C7 1.518(4) . ?
C7 N8 1.482(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C24 1.462(4) . ?
N8 C9 1.468(4) . ?
C9 C10 1.537(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.522(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N12 1.470(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N12 C31 1.461(4) . ?
N12 C13 1.465(4) . ?
C13 C14 1.512(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.383(4) . ?
C14 C15 1.408(4) . ?
C15 C16 1.391(4) . ?
C16 C17 1.388(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.383(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.377(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.506(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.383(4) . ?
C25 C26 1.395(4) . ?
C26 C27 1.386(5) . ?
C26 H26 0.9500 . ?
C27 N28 1.330(4) . ?
C27 H27 0.9500 . ?
N28 C29 1.337(4) . ?
N28 Pb1 2.644(3) 1_554 ?
C29 C30 1.375(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.509(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C37 1.378(4) . ?
C32 C33 1.400(4) . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 N35 1.338(4) . ?
C34 H34 0.9500 . ?
N35 C36 1.341(4) . ?
C36 C37 1.385(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?

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
N35 Pb1 N35 180.0 3_567 . ?
N35 Pb1 N28 88.93(8) 3_567 3_566 ?
N35 Pb1 N28 91.07(9) . 3_566 ?
N35 Pb1 N28 91.07(9) 3_567 1_556 ?
N35 Pb1 N28 88.93(8) . 1_556 ?
N28 Pb1 N28 180.0 3_566 1_556 ?
N35 Pb1 Cl1 87.73(6) 3_567 . ?
N35 Pb1 Cl1 92.28(6) . . ?
N28 Pb1 Cl1 91.06(6) 3_566 . ?
N28 Pb1 Cl1 88.94(6) 1_556 . ?
N35 Pb1 Cl1 92.27(6) 3_567 3_567 ?
N35 Pb1 Cl1 87.72(6) . 3_567 ?
N28 Pb1 Cl1 88.94(6) 3_566 3_567 ?
N28 Pb1 Cl1 91.06(6) 1_556 3_567 ?
Cl1 Pb1 Cl1 180.0 . 3_567 ?
C15 O1 C2 118.0(2) . . ?
O1 C2 C3 107.6(2) . . ?
O1 C2 H2A 110.2 . . ?
C3 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
C3 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O4 C3 C2 109.6(3) . . ?
O4 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
O4 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
C5 O4 C3 116.2(3) . . ?
O4 C5 C20 123.5(3) . . ?
O4 C5 C6 115.9(3) . . ?
C20 C5 C6 120.6(3) . . ?
C23 C6 C5 117.4(3) . . ?
C23 C6 C7 119.4(3) . . ?
C5 C6 C7 123.2(3) . . ?
N8 C7 C6 116.4(2) . . ?
N8 C7 H7A 108.2 . . ?
C6 C7 H7A 108.2 . . ?
N8 C7 H7B 108.2 . . ?
C6 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C24 N8 C9 110.6(2) . . ?
C24 N8 C7 112.4(2) . . ?
C9 N8 C7 112.4(3) . . ?
N8 C9 C10 112.4(3) . . ?
N8 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N8 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 109.3(3) . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
N12 C11 C10 111.3(2) . . ?
N12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
N12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C31 N12 C13 112.5(3) . . ?
C31 N12 C11 111.9(3) . . ?
C13 N12 C11 111.3(2) . . ?
N12 C13 C14 112.6(2) . . ?
N12 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
N12 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C19 C14 C15 118.2(3) . . ?
C19 C14 C13 121.2(3) . . ?
C15 C14 C13 120.6(3) . . ?
O1 C15 C16 124.4(3) . . ?
O1 C15 C14 115.1(3) . . ?
C16 C15 C14 120.5(3) . . ?
C17 C16 C15 119.3(3) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C18 C17 C16 121.1(3) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 118.9(3) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C14 C19 C18 121.8(3) . . ?
C14 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C5 C20 C21 120.3(4) . . ?
C5 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 120.2(4) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 119.4(3) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C6 122.0(4) . . ?
C22 C23 H23 119.0 . . ?
C6 C23 H23 119.0 . . ?
N8 C24 C25 113.2(2) . . ?
N8 C24 H24A 108.9 . . ?
C25 C24 H24A 108.9 . . ?
N8 C24 H24B 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C30 C25 C26 117.7(3) . . ?
C30 C25 C24 120.1(3) . . ?
C26 C25 C24 122.2(3) . . ?
C27 C26 C25 118.9(3) . . ?
C27 C26 H26 120.6 . . ?
C25 C26 H26 120.6 . . ?
N28 C27 C26 123.1(3) . . ?
N28 C27 H27 118.4 . . ?
C26 C27 H27 118.4 . . ?
C27 N28 C29 117.7(3) . . ?
C27 N28 Pb1 124.6(2) . 1_554 ?
C29 N28 Pb1 117.3(2) . 1_554 ?
N28 C29 C30 123.1(3) . . ?
N28 C29 H29 118.4 . . ?
C30 C29 H29 118.4 . . ?
C29 C30 C25 119.5(3) . . ?
C29 C30 H30 120.2 . . ?
C25 C30 H30 120.2 . . ?
N12 C31 C32 113.0(3) . . ?
N12 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
N12 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C37 C32 C33 117.0(3) . . ?
C37 C32 C31 122.0(3) . . ?
C33 C32 C31 120.9(3) . . ?
C34 C33 C32 119.1(3) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
N35 C34 C33 123.7(3) . . ?
N35 C34 H34 118.1 . . ?
C33 C34 H34 118.1 . . ?
C34 N35 C36 116.9(3) . . ?
C34 N35 Pb1 124.74(18) . . ?
C36 N35 Pb1 118.2(2) . . ?
N35 C36 C37 122.9(3) . . ?
N35 C36 H36 118.6 . . ?
C37 C36 H36 118.6 . . ?
C32 C37 C36 120.3(3) . . ?
C32 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?

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
C15 O1 C2 C3 169.5(3) . . . . ?
O1 C2 C3 O4 70.3(3) . . . . ?
C2 C3 O4 C5 179.2(2) . . . . ?
C3 O4 C5 C20 4.3(4) . . . . ?
C3 O4 C5 C6 -174.7(3) . . . . ?
O4 C5 C6 C23 176.1(2) . . . . ?
C20 C5 C6 C23 -2.9(4) . . . . ?
O4 C5 C6 C7 -4.2(4) . . . . ?
C20 C5 C6 C7 176.8(3) . . . . ?
C23 C6 C7 N8 86.5(4) . . . . ?
C5 C6 C7 N8 -93.2(3) . . . . ?
C6 C7 N8 C24 -61.3(3) . . . . ?
C6 C7 N8 C9 64.3(3) . . . . ?
C24 N8 C9 C10 -83.3(3) . . . . ?
C7 N8 C9 C10 150.2(3) . . . . ?
N8 C9 C10 C11 -173.2(2) . . . . ?
C9 C10 C11 N12 66.1(3) . . . . ?
C10 C11 N12 C31 76.1(3) . . . . ?
C10 C11 N12 C13 -157.1(2) . . . . ?
C31 N12 C13 C14 -53.7(3) . . . . ?
C11 N12 C13 C14 179.9(2) . . . . ?
N12 C13 C14 C19 111.7(3) . . . . ?
N12 C13 C14 C15 -66.1(4) . . . . ?
C2 O1 C15 C16 -3.0(5) . . . . ?
C2 O1 C15 C14 177.7(3) . . . . ?
C19 C14 C15 O1 175.7(3) . . . . ?
C13 C14 C15 O1 -6.5(4) . . . . ?
C19 C14 C15 C16 -3.7(5) . . . . ?
C13 C14 C15 C16 174.2(3) . . . . ?
O1 C15 C16 C17 -177.8(3) . . . . ?
C14 C15 C16 C17 1.5(5) . . . . ?
C15 C16 C17 C18 1.4(5) . . . . ?
C16 C17 C18 C19 -1.9(5) . . . . ?
C15 C14 C19 C18 3.1(5) . . . . ?
C13 C14 C19 C18 -174.7(3) . . . . ?
C17 C18 C19 C14 -0.4(5) . . . . ?
O4 C5 C20 C21 -178.8(3) . . . . ?
C6 C5 C20 C21 0.1(4) . . . . ?
C5 C20 C21 C22 2.7(5) . . . . ?
C20 C21 C22 C23 -2.5(5) . . . . ?
C21 C22 C23 C6 -0.4(5) . . . . ?
C5 C6 C23 C22 3.1(4) . . . . ?
C7 C6 C23 C22 -176.6(3) . . . . ?
C9 N8 C24 C25 163.7(3) . . . . ?
C7 N8 C24 C25 -69.8(3) . . . . ?
N8 C24 C25 C30 -49.9(4) . . . . ?
N8 C24 C25 C26 132.8(3) . . . . ?
C30 C25 C26 C27 -1.2(4) . . . . ?
C24 C25 C26 C27 176.2(3) . . . . ?
C25 C26 C27 N28 0.0(5) . . . . ?
C26 C27 N28 C29 0.1(5) . . . . ?
C26 C27 N28 Pb1 -171.8(2) . . . 1_554 ?
C27 N28 C29 C30 1.0(5) . . . . ?
Pb1 N28 C29 C30 173.5(2) 1_554 . . . ?
N28 C29 C30 C25 -2.2(5) . . . . ?
C26 C25 C30 C29 2.2(4) . . . . ?
C24 C25 C30 C29 -175.2(3) . . . . ?
C13 N12 C31 C32 90.4(3) . . . . ?
C11 N12 C31 C32 -143.5(3) . . . . ?
N12 C31 C32 C37 -136.9(3) . . . . ?
N12 C31 C32 C33 46.0(4) . . . . ?
C37 C32 C33 C34 0.6(5) . . . . ?
C31 C32 C33 C34 177.8(3) . . . . ?
C32 C33 C34 N35 -1.3(5) . . . . ?
C33 C34 N35 C36 1.0(5) . . . . ?
C33 C34 N35 Pb1 177.4(3) . . . . ?
C34 N35 C36 C37 0.0(5) . . . . ?
Pb1 N35 C36 C37 -176.6(3) . . . . ?
C33 C32 C37 C36 0.4(5) . . . . ?
C31 C32 C37 C36 -176.8(3) . . . . ?
N35 C36 C37 C32 -0.7(6) . . . . ?

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
C9 H9A O4 0.99 2.50 3.233(4) 130.9 .

_refine_diff_density_max         0.969
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.088

