# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_3
_audit_block_doi                 10.5517/ccdc.csd.cc1q1ls4
_database_code_depnum_ccdc_archive 'CCDC 1580466'
_audit_update_record             
;
2018-02-23 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H27 N3 Ni O6 Pb S'
_chemical_formula_weight         751.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   12.6526(7)
_cell_length_b                   14.8338(8)
_cell_length_c                   13.9646(8)
_cell_angle_alpha                90
_cell_angle_beta                 104.762(6)
_cell_angle_gamma                90
_cell_volume                     2534.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    15411
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      30.00

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    7.504
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a

_diffrn_reflns_number            15411
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.364
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             7177
_reflns_number_gt                5713
_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, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-97, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'

_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)+(0.0748P)²+4.8946P] 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         7177
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_ref         0.1494
_refine_ls_wR_factor_gt          0.1379
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Pb1 Pb 0.07029(2) 0.19039(2) 0.18438(2) 0.01146(9) Uani 1 1 d . . . . .
Ni1 Ni 0.33392(7) 0.13288(6) 0.20020(7) 0.00913(19) Uani 1 1 d . . . . .
O11 O 0.1867(4) 0.1172(4) 0.1001(4) 0.0113(10) Uani 1 1 d . . . . .
C12 C 0.1681(6) 0.1124(5) 0.0029(5) 0.0106(14) Uani 1 1 d . . . . .
C13 C 0.0566(6) 0.1114(5) -0.0562(6) 0.0128(14) Uani 1 1 d . . . . .
O131 O -0.0182(4) 0.1244(4) -0.0014(4) 0.0165(12) Uani 1 1 d . . . . .
C132 C -0.1328(6) 0.1184(6) -0.0537(6) 0.0163(16) Uani 1 1 d . . . . .
H13A H -0.148813 0.060174 -0.085706 0.020 Uiso 1 1 calc R U . . .
H13B H -0.151738 0.165153 -0.103735 0.020 Uiso 1 1 calc R U . . .
C133 C -0.1958(6) 0.1306(6) 0.0234(7) 0.0209(17) Uani 1 1 d . . . . .
H13C H -0.172028 0.086814 0.074976 0.031 Uiso 1 1 calc R U . . .
H13D H -0.272413 0.122779 -0.006572 0.031 Uiso 1 1 calc R U . . .
H13E H -0.183147 0.190147 0.050980 0.031 Uiso 1 1 calc R U . . .
C14 C 0.0314(7) 0.1001(6) -0.1560(6) 0.0187(17) Uani 1 1 d . . . . .
H14 H -0.041252 0.099334 -0.192253 0.022 Uiso 1 1 calc R U . . .
C15 C 0.1155(7) 0.0897(6) -0.2042(6) 0.0230(18) Uani 1 1 d . . . . .
H15 H 0.098299 0.080830 -0.272366 0.028 Uiso 1 1 calc R U . . .
C16 C 0.2225(7) 0.0926(6) -0.1514(6) 0.0219(18) Uani 1 1 d . . . . .
H16 H 0.277236 0.087040 -0.184592 0.026 Uiso 1 1 calc R U . . .
C17 C 0.2517(6) 0.1038(5) -0.0475(6) 0.0145(15) Uani 1 1 d . . . . .
C18 C 0.3673(6) 0.1053(6) 0.0004(6) 0.0183(17) Uani 1 1 d . . . . .
H18 H 0.413909 0.098192 -0.040891 0.022 Uiso 1 1 calc R U . . .
N19 N 0.4136(5) 0.1153(5) 0.0927(5) 0.0150(13) Uani 1 1 d . . . . .
C20 C 0.5339(6) 0.1121(7) 0.1226(7) 0.026(2) Uani 1 1 d . . . . .
H20A H 0.561814 0.119219 0.064485 0.031 Uiso 1 1 calc R U . . .
H20B H 0.557294 0.053675 0.151530 0.031 Uiso 1 1 calc R U . . .
C21 C 0.5806(6) 0.1846(6) 0.1961(7) 0.0218(19) Uani 1 1 d . . . . .
H21A H 0.539269 0.239636 0.176924 0.026 Uiso 1 1 calc R U . . .
H21B H 0.655443 0.196178 0.193957 0.026 Uiso 1 1 calc R U . . .
C22 C 0.5792(6) 0.1611(6) 0.3010(6) 0.0178(16) Uani 1 1 d . . . . .
H22A H 0.617810 0.104578 0.318985 0.021 Uiso 1 1 calc R U . . .
H22B H 0.618489 0.207293 0.345083 0.021 Uiso 1 1 calc R U . . .
N23 N 0.4683(5) 0.1524(4) 0.3160(5) 0.0112(12) Uani 1 1 d . . . . .
C24 C 0.4652(6) 0.1469(5) 0.4065(6) 0.0125(14) Uani 1 1 d . . . . .
H24 H 0.532276 0.150437 0.453167 0.015 Uiso 1 1 calc R U . . .
C25 C 0.3689(6) 0.1357(5) 0.4463(6) 0.0133(14) Uani 1 1 d . . . . .
C26 C 0.3916(7) 0.1197(6) 0.5493(6) 0.0191(17) Uani 1 1 d . . . . .
H25 H 0.463600 0.115518 0.586912 0.023 Uiso 1 1 calc R U . . .
C27 C 0.3075(7) 0.1104(6) 0.5936(6) 0.0224(18) Uani 1 1 d . . . . .
H27 H 0.323106 0.100156 0.661440 0.027 Uiso 1 1 calc R U . . .
C28 C 0.1990(7) 0.1161(6) 0.5393(6) 0.0208(17) Uani 1 1 d . . . . .
H28 H 0.142917 0.110535 0.570947 0.025 Uiso 1 1 calc R U . . .
C29 C 0.1752(6) 0.1299(5) 0.4387(6) 0.0129(14) Uani 1 1 d . . . . .
O291 O 0.0711(4) 0.1316(4) 0.3766(4) 0.0144(11) Uani 1 1 d . . . . .
C292 C -0.0180(6) 0.1350(6) 0.4239(7) 0.0209(18) Uani 1 1 d . . . . .
H31A H -0.008124 0.185318 0.469686 0.025 Uiso 1 1 calc R U . . .
H31B H -0.020087 0.079866 0.460735 0.025 Uiso 1 1 calc R U . . .
C293 C -0.1228(6) 0.1459(7) 0.3448(7) 0.0235(19) Uani 1 1 d . . . . .
H32A H -0.121051 0.201680 0.310344 0.035 Uiso 1 1 calc R U . . .
H32B H -0.183237 0.146449 0.374676 0.035 Uiso 1 1 calc R U . . .
H32C H -0.130956 0.096663 0.298953 0.035 Uiso 1 1 calc R U . . .
C30 C 0.2591(6) 0.1403(5) 0.3891(5) 0.0114(14) Uani 1 1 d . . . . .
O31 O 0.2337(4) 0.1529(4) 0.2921(4) 0.0125(11) Uani 1 1 d . . . . .
O3 O 0.1525(4) 0.3087(4) 0.1260(4) 0.0169(12) Uani 1 1 d . . . . .
C2 C 0.2553(6) 0.3230(5) 0.1334(6) 0.0156(16) Uani 1 1 d . . . . .
O1 O 0.3316(4) 0.2706(4) 0.1702(4) 0.0160(11) Uani 1 1 d . . . . .
C4 C 0.2816(7) 0.4133(6) 0.0995(7) 0.0232(19) Uani 1 1 d . . . . .
H4A H 0.278843 0.457500 0.149028 0.035 Uiso 1 1 calc R U . . .
H4B H 0.229463 0.428473 0.038734 0.035 Uiso 1 1 calc R U . . .
H4C H 0.353670 0.412218 0.088902 0.035 Uiso 1 1 calc R U . . .
N1 N 0.3479(6) -0.0063(5) 0.2258(5) 0.0191(14) Uani 1 1 d . . . . .
C1 C 0.3952(6) -0.0689(5) 0.2078(6) 0.0154(15) Uani 1 1 d . . . . .
S1 S 0.45970(16) -0.15671(14) 0.17741(15) 0.0170(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O3 2.293(6) . ?
Pb1 O31 2.294(5) . ?
Pb1 O11 2.370(5) . ?
Pb1 O131 2.731(6) . ?
Pb1 S1 3.064(2) 2 ?
Ni1 N19 2.026(6) . ?
Ni1 O11 2.037(5) . ?
Ni1 O31 2.043(5) . ?
Ni1 N23 2.047(6) . ?
Ni1 O1 2.084(6) . ?
Ni1 N1 2.095(7) . ?
O11 C12 1.318(8) . ?
C12 C17 1.418(9) . ?
C12 C13 1.443(10) . ?
C13 C14 1.358(10) . ?
C13 O131 1.374(8) . ?
O131 C132 1.451(8) . ?
C132 C133 1.505(11) . ?
C132 H13A 0.9700 . ?
C132 H13B 0.9700 . ?
C133 H13C 0.9600 . ?
C133 H13D 0.9600 . ?
C133 H13E 0.9600 . ?
C14 C15 1.406(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.367(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.413(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.445(11) . ?
C18 N19 1.281(11) . ?
C18 H18 0.9300 . ?
N19 C20 1.473(9) . ?
C20 C21 1.500(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.510(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N23 1.477(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N23 C24 1.277(9) . ?
C24 C25 1.472(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.413(11) . ?
C25 C30 1.417(10) . ?
C26 C27 1.367(11) . ?
C26 H25 0.9300 . ?
C27 C28 1.391(12) . ?
C27 H27 0.9300 . ?
C28 C29 1.376(11) . ?
C28 H28 0.9300 . ?
C29 O291 1.379(9) . ?
C29 C30 1.416(10) . ?
O291 C292 1.446(8) . ?
C292 C293 1.502(12) . ?
C292 H31A 0.9700 . ?
C292 H31B 0.9700 . ?
C293 H32A 0.9600 . ?
C293 H32B 0.9600 . ?
C293 H32C 0.9600 . ?
C30 O31 1.323(9) . ?
O3 C2 1.295(9) . ?
C2 O1 1.245(9) . ?
C2 C4 1.487(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
N1 C1 1.166(10) . ?
C1 S1 1.650(8) . ?

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
O3 Pb1 O31 90.24(19) . . ?
O3 Pb1 O11 77.20(17) . . ?
O31 Pb1 O11 69.18(18) . . ?
O3 Pb1 O131 92.89(19) . . ?
O31 Pb1 O131 128.23(18) . . ?
O11 Pb1 O131 61.34(16) . . ?
O3 Pb1 S1 78.30(14) . 2 ?
O31 Pb1 S1 90.11(14) . 2 ?
O11 Pb1 S1 147.60(13) . 2 ?
O131 Pb1 S1 140.99(13) . 2 ?
N19 Ni1 O11 91.0(2) . . ?
N19 Ni1 O31 171.7(2) . . ?
O11 Ni1 O31 80.9(2) . . ?
N19 Ni1 N23 97.7(2) . . ?
O11 Ni1 N23 171.3(2) . . ?
O31 Ni1 N23 90.4(2) . . ?
N19 Ni1 O1 87.8(2) . . ?
O11 Ni1 O1 90.6(2) . . ?
O31 Ni1 O1 90.3(2) . . ?
N23 Ni1 O1 89.2(2) . . ?
N19 Ni1 N1 87.9(3) . . ?
O11 Ni1 N1 91.6(2) . . ?
O31 Ni1 N1 94.3(2) . . ?
N23 Ni1 N1 89.3(3) . . ?
O1 Ni1 N1 175.2(2) . . ?
C12 O11 Ni1 127.2(4) . . ?
C12 O11 Pb1 124.4(4) . . ?
Ni1 O11 Pb1 100.5(2) . . ?
O11 C12 C17 123.8(7) . . ?
O11 C12 C13 118.8(6) . . ?
C17 C12 C13 117.4(7) . . ?
C14 C13 O131 125.1(7) . . ?
C14 C13 C12 121.9(7) . . ?
O131 C13 C12 113.1(6) . . ?
C13 O131 C132 116.9(6) . . ?
C13 O131 Pb1 113.9(4) . . ?
C132 O131 Pb1 128.0(4) . . ?
O131 C132 C133 106.0(6) . . ?
O131 C132 H13A 110.5 . . ?
C133 C132 H13A 110.5 . . ?
O131 C132 H13B 110.5 . . ?
C133 C132 H13B 110.5 . . ?
H13A C132 H13B 108.7 . . ?
C132 C133 H13C 109.5 . . ?
C132 C133 H13D 109.5 . . ?
H13C C133 H13D 109.5 . . ?
C132 C133 H13E 109.5 . . ?
H13C C133 H13E 109.5 . . ?
H13D C133 H13E 109.5 . . ?
C13 C14 C15 119.8(8) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.3(8) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 121.4(7) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 C12 119.2(7) . . ?
C16 C17 C18 116.5(7) . . ?
C12 C17 C18 124.3(7) . . ?
N19 C18 C17 128.1(7) . . ?
N19 C18 H18 116.0 . . ?
C17 C18 H18 116.0 . . ?
C18 N19 C20 117.1(7) . . ?
C18 N19 Ni1 125.0(5) . . ?
C20 N19 Ni1 117.9(5) . . ?
N19 C20 C21 111.7(7) . . ?
N19 C20 H20A 109.3 . . ?
C21 C20 H20A 109.3 . . ?
N19 C20 H20B 109.3 . . ?
C21 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
C20 C21 C22 113.4(7) . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
N23 C22 C21 113.9(7) . . ?
N23 C22 H22A 108.8 . . ?
C21 C22 H22A 108.8 . . ?
N23 C22 H22B 108.8 . . ?
C21 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C24 N23 C22 114.6(6) . . ?
C24 N23 Ni1 123.0(5) . . ?
C22 N23 Ni1 121.9(5) . . ?
N23 C24 C25 128.2(7) . . ?
N23 C24 H24 115.9 . . ?
C25 C24 H24 115.9 . . ?
C26 C25 C30 119.9(7) . . ?
C26 C25 C24 115.5(7) . . ?
C30 C25 C24 124.7(7) . . ?
C27 C26 C25 119.8(8) . . ?
C27 C26 H25 120.1 . . ?
C25 C26 H25 120.1 . . ?
C26 C27 C28 121.5(8) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C29 C28 C27 119.6(7) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 O291 124.8(7) . . ?
C28 C29 C30 121.2(7) . . ?
O291 C29 C30 113.9(7) . . ?
C29 O291 C292 116.4(6) . . ?
O291 C292 C293 108.2(7) . . ?
O291 C292 H31A 110.1 . . ?
C293 C292 H31A 110.1 . . ?
O291 C292 H31B 110.1 . . ?
C293 C292 H31B 110.1 . . ?
H31A C292 H31B 108.4 . . ?
C292 C293 H32A 109.5 . . ?
C292 C293 H32B 109.5 . . ?
H32A C293 H32B 109.5 . . ?
C292 C293 H32C 109.5 . . ?
H32A C293 H32C 109.5 . . ?
H32B C293 H32C 109.5 . . ?
O31 C30 C29 119.9(6) . . ?
O31 C30 C25 122.1(6) . . ?
C29 C30 C25 118.0(7) . . ?
C30 O31 Ni1 126.5(4) . . ?
C30 O31 Pb1 130.5(4) . . ?
Ni1 O31 Pb1 102.9(2) . . ?
C2 O3 Pb1 129.3(5) . . ?
O1 C2 O3 126.0(7) . . ?
O1 C2 C4 118.7(7) . . ?
O3 C2 C4 115.1(7) . . ?
C2 O1 Ni1 131.7(5) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 N1 Ni1 140.7(6) . . ?
N1 C1 S1 177.6(8) . . ?
C1 S1 Pb1 105.9(3) . 2_545 ?

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
C133 H13D S1 0.96 2.95 3.793(8) 147.9 3
C18 H18 S1 0.93 2.92 3.783(8) 155.8 3_655
C21 H21A O1 0.97 2.65 3.332(10) 128.1 .
C24 H24 O3 0.93 2.58 3.427(10) 152.2 4_666
C293 H32A S1 0.96 2.90 3.640(9) 134.3 2

_refine_diff_density_max         5.781
_refine_diff_density_min         -5.718
_refine_diff_density_rms         0.345

####################################################################### 
# 
# 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 1580464'
_audit_update_record             
;
2018-02-19 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H31 N3 Ni O8 Pb S2'
_chemical_formula_weight         819.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   10.5264(6)
_cell_length_b                   11.3184(6)
_cell_length_c                   12.5352(8)
_cell_angle_alpha                86.021(5)
_cell_angle_beta                 71.617(5)
_cell_angle_gamma                85.853(4)
_cell_volume                     1411.83(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9927
_cell_measurement_theta_min      3.40
_cell_measurement_theta_max      30.00

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_F_000             804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    6.821
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a

_diffrn_reflns_number            9927
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.400
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             7843
_reflns_number_gt                7120
_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, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-97, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'

_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)+(0.0363P)²+4.6814P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7843
_refine_ls_number_parameters     363
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0948
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.14015(2) 0.36893(2) 0.48708(2) 0.01391(6) Uani 1 1 d . . . . .
Ni1 Ni 1.18796(6) 0.48645(5) 0.20925(5) 0.00912(12) Uani 1 1 d . . . . .
O1 O 1.2208(5) 0.1344(4) 0.4620(5) 0.0420(13) Uani 1 1 d . . . . .
O2 O 1.3539(4) 0.2803(4) 0.3854(3) 0.0223(9) Uani 1 1 d . . . . .
O1W O 1.3644(4) 0.3667(3) 0.1730(3) 0.0132(7) Uani 1 1 d D . . . .
O11 O 1.2314(3) 0.5255(3) 0.3505(3) 0.0108(7) Uani 1 1 d . . . . .
C12 C 1.3271(5) 0.5941(4) 0.3552(4) 0.0123(9) Uani 1 1 d . . . . .
C13 C 1.3528(5) 0.6021(4) 0.4589(4) 0.0116(9) Uani 1 1 d . . . . .
C14 C 1.4513(5) 0.6719(5) 0.4692(5) 0.0160(10) Uani 1 1 d . . . . .
H14 H 1.465650 0.675193 0.538359 0.019 Uiso 1 1 calc R U . . .
C15 C 1.5287(6) 0.7370(5) 0.3753(5) 0.0202(11) Uani 1 1 d . . . . .
H15 H 1.595531 0.783103 0.381329 0.024 Uiso 1 1 calc R U . . .
C16 C 1.5048(5) 0.7322(4) 0.2741(5) 0.0150(10) Uani 1 1 d . . . . .
H16 H 1.555979 0.776143 0.211923 0.018 Uiso 1 1 calc R U . . .
C17 C 1.4046(5) 0.6624(4) 0.2619(4) 0.0139(10) Uani 1 1 d . . . . .
C18 C 1.3869(5) 0.6714(4) 0.1510(4) 0.0129(9) Uani 1 1 d . . . . .
H18 H 1.440372 0.723902 0.098336 0.016 Uiso 1 1 calc R U . . .
N19 N 1.3058(4) 0.6151(4) 0.1177(3) 0.0124(8) Uani 1 1 d . . . . .
C20 C 1.3052(5) 0.6421(4) 0.0017(4) 0.0143(10) Uani 1 1 d . . . . .
H20A H 1.375754 0.695236 -0.036202 0.017 Uiso 1 1 calc R U . . .
H20B H 1.220155 0.681766 0.002398 0.017 Uiso 1 1 calc R U . . .
C21 C 1.3268(5) 0.5287(5) -0.0622(4) 0.0153(10) Uani 1 1 d . . . . .
H21A H 1.361239 0.548872 -0.142250 0.018 Uiso 1 1 calc R U . . .
H21B H 1.394110 0.477284 -0.041833 0.018 Uiso 1 1 calc R U . . .
C22 C 1.2002(5) 0.4611(5) -0.0393(4) 0.0164(10) Uani 1 1 d . . . . .
H22A H 1.132260 0.512935 -0.058373 0.020 Uiso 1 1 calc R U . . .
H22B H 1.219869 0.394690 -0.087936 0.020 Uiso 1 1 calc R U . . .
N23 N 1.1455(4) 0.4159(4) 0.0787(3) 0.0111(8) Uani 1 1 d . . . . .
C24 C 1.0647(5) 0.3325(4) 0.0926(4) 0.0112(9) Uani 1 1 d . . . . .
H24 H 1.050804 0.309328 0.027603 0.013 Uiso 1 1 calc R U . . .
C25 C 0.9917(5) 0.2692(4) 0.1971(4) 0.0126(9) Uani 1 1 d . . . . .
C26 C 0.9063(6) 0.1829(5) 0.1850(5) 0.0188(11) Uani 1 1 d . . . . .
H26 H 0.898840 0.173060 0.114254 0.023 Uiso 1 1 calc R U . . .
C27 C 0.8349(6) 0.1141(5) 0.2747(5) 0.0169(10) Uani 1 1 d . . . . .
H27 H 0.780596 0.057399 0.264568 0.020 Uiso 1 1 calc R U . . .
C28 C 0.8438(5) 0.1290(5) 0.3818(5) 0.0166(10) Uani 1 1 d . . . . .
H28 H 0.795641 0.082327 0.443172 0.020 Uiso 1 1 calc R U . . .
C29 C 0.9247(5) 0.2137(4) 0.3960(4) 0.0127(9) Uani 1 1 d . . . . .
C30 C 1.0021(5) 0.2856(4) 0.3043(4) 0.0116(9) Uani 1 1 d . . . . .
C132 C 1.2888(6) 0.5423(5) 0.6560(4) 0.0166(10) Uani 1 1 d . . . . .
H13A H 1.273867 0.623345 0.677017 0.025 Uiso 1 1 calc R U . . .
H13B H 1.377959 0.514467 0.653392 0.025 Uiso 1 1 calc R U . . .
H13C H 1.225052 0.494381 0.710327 0.025 Uiso 1 1 calc R U . . .
C292 C 0.8858(6) 0.1553(5) 0.5908(4) 0.0195(11) Uani 1 1 d . . . . .
H29A H 0.790395 0.154033 0.607693 0.029 Uiso 1 1 calc R U . . .
H29B H 0.906220 0.179094 0.655384 0.029 Uiso 1 1 calc R U . . .
H29C H 0.925890 0.077501 0.571844 0.029 Uiso 1 1 calc R U . . .
O31 O 1.0821(4) 0.3626(3) 0.3217(3) 0.0141(7) Uani 1 1 d . . . . .
O131 O 1.2729(4) 0.5346(3) 0.5470(3) 0.0144(7) Uani 1 1 d . . . . .
O291 O 0.9382(4) 0.2380(3) 0.4973(3) 0.0159(8) Uani 1 1 d . . . . .
O41 O 1.6160(4) 0.8354(3) -0.0497(4) 0.0222(9) Uani 1 1 d . . . . .
C43 C 1.6795(7) 1.0116(5) 0.0475(5) 0.0257(13) Uani 1 1 d . . . . .
H43A H 1.656621 0.975549 0.122278 0.039 Uiso 1 1 calc R U . . .
H43B H 1.601709 1.053516 0.036432 0.039 Uiso 1 1 calc R U . . .
H43C H 1.748627 1.066000 0.037562 0.039 Uiso 1 1 calc R U . . .
C44 C 1.7782(7) 0.9927(6) -0.1778(5) 0.0325(15) Uani 1 1 d . . . . .
H44A H 1.702100 1.044890 -0.177491 0.049 Uiso 1 1 calc R U . . .
H44B H 1.801484 0.944679 -0.242049 0.049 Uiso 1 1 calc R U . . .
H44C H 1.852702 1.038654 -0.181245 0.049 Uiso 1 1 calc R U . . .
S42 S 1.73811(13) 0.89943(11) -0.05238(11) 0.0155(3) Uani 1 1 d . . . . .
N1 N 1.0227(4) 0.6073(4) 0.2354(4) 0.0166(9) Uani 1 1 d . . . . .
C1 C 0.9770(5) 0.6971(5) 0.2092(4) 0.0141(10) Uani 1 1 d . . . . .
S1 S 0.9123(2) 0.82420(14) 0.17487(17) 0.0361(4) Uani 1 1 d . . . . .
C2 C 1.3292(6) 0.1741(6) 0.4069(5) 0.0228(13) Uani 1 1 d . . . . .
C3 C 1.4494(7) 0.0840(6) 0.3552(7) 0.0388(17) Uani 1 1 d . . . . .
H3A H 1.521378 0.095755 0.384394 0.058 Uiso 1 1 calc R U . . .
H3B H 1.479783 0.096536 0.274764 0.058 Uiso 1 1 calc R U . . .
H3C H 1.420855 0.004561 0.374600 0.058 Uiso 1 1 calc R U . . .
H1 H 1.358(8) 0.345(6) 0.240(3) 0.047 Uiso 1 1 d D U . . .
H2 H 1.365(8) 0.308(4) 0.134(5) 0.047 Uiso 1 1 d D 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 O31 2.346(3) . ?
Pb1 O2 2.394(4) . ?
Pb1 O11 2.405(3) . ?
Pb1 O291 2.643(4) . ?
Pb1 O131 2.696(4) . ?
Pb1 O1 2.737(5) . ?
Ni1 N19 2.027(4) . ?
Ni1 O31 2.038(3) . ?
Ni1 O11 2.047(3) . ?
Ni1 N23 2.051(4) . ?
Ni1 N1 2.089(5) . ?
Ni1 O1W 2.164(4) . ?
O1 C2 1.231(7) . ?
O2 C2 1.241(7) . ?
O1W H1 0.846(19) . ?
O1W H2 0.850(19) . ?
O11 C12 1.334(6) . ?
C12 C17 1.412(7) . ?
C12 C13 1.419(7) . ?
C13 O131 1.379(6) . ?
C13 C14 1.390(7) . ?
C14 C15 1.397(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.374(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.414(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.455(7) . ?
C18 N19 1.285(7) . ?
C18 H18 0.9300 . ?
N19 C20 1.467(6) . ?
C20 C21 1.525(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.523(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N23 1.477(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N23 C24 1.282(6) . ?
C24 C25 1.461(7) . ?
C24 H24 0.9300 . ?
C25 C30 1.408(7) . ?
C25 C26 1.420(7) . ?
C26 C27 1.367(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.397(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.383(7) . ?
C28 H28 0.9300 . ?
C29 O291 1.370(6) . ?
C29 C30 1.422(7) . ?
C30 O31 1.328(6) . ?
C132 O131 1.437(6) . ?
C132 H13A 0.9600 . ?
C132 H13B 0.9600 . ?
C132 H13C 0.9600 . ?
C292 O291 1.439(6) . ?
C292 H29A 0.9600 . ?
C292 H29B 0.9600 . ?
C292 H29C 0.9600 . ?
O41 S42 1.511(4) . ?
C43 S42 1.783(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 S42 1.783(6) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
N1 C1 1.164(7) . ?
C1 S1 1.636(5) . ?
C2 C3 1.565(9) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O31 Pb1 O2 86.95(13) . . ?
O31 Pb1 O11 66.97(12) . . ?
O2 Pb1 O11 78.53(13) . . ?
O31 Pb1 O291 63.22(11) . . ?
O2 Pb1 O291 113.06(13) . . ?
O11 Pb1 O291 127.66(11) . . ?
O31 Pb1 O131 128.86(11) . . ?
O2 Pb1 O131 87.66(13) . . ?
O11 Pb1 O131 62.12(11) . . ?
O291 Pb1 O131 157.78(12) . . ?
O31 Pb1 O1 87.08(15) . . ?
O2 Pb1 O1 50.45(14) . . ?
O11 Pb1 O1 124.26(14) . . ?
O291 Pb1 O1 68.44(14) . . ?
O131 Pb1 O1 125.62(14) . . ?
N19 Ni1 O31 170.58(16) . . ?
N19 Ni1 O11 90.85(16) . . ?
O31 Ni1 O11 79.83(14) . . ?
N19 Ni1 N23 97.46(17) . . ?
O31 Ni1 N23 91.66(16) . . ?
O11 Ni1 N23 169.57(15) . . ?
N19 Ni1 N1 88.93(17) . . ?
O31 Ni1 N1 93.21(17) . . ?
O11 Ni1 N1 94.90(16) . . ?
N23 Ni1 N1 91.57(17) . . ?
N19 Ni1 O1W 88.19(15) . . ?
O31 Ni1 O1W 89.89(15) . . ?
O11 Ni1 O1W 86.78(14) . . ?
N23 Ni1 O1W 87.18(15) . . ?
N1 Ni1 O1W 176.69(16) . . ?
C2 O1 Pb1 83.5(4) . . ?
C2 O2 Pb1 99.4(4) . . ?
Ni1 O1W H1 97(5) . . ?
Ni1 O1W H2 116(6) . . ?
H1 O1W H2 112(3) . . ?
C12 O11 Ni1 126.7(3) . . ?
C12 O11 Pb1 124.5(3) . . ?
Ni1 O11 Pb1 104.88(14) . . ?
O11 C12 C17 123.5(4) . . ?
O11 C12 C13 119.4(4) . . ?
C17 C12 C13 117.1(5) . . ?
O131 C13 C14 123.5(4) . . ?
O131 C13 C12 114.3(4) . . ?
C14 C13 C12 122.2(5) . . ?
C13 C14 C15 119.9(5) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 119.2(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 121.8(5) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C12 C17 C16 119.8(5) . . ?
C12 C17 C18 124.9(5) . . ?
C16 C17 C18 115.3(4) . . ?
N19 C18 C17 127.3(5) . . ?
N19 C18 H18 116.3 . . ?
C17 C18 H18 116.3 . . ?
C18 N19 C20 116.7(4) . . ?
C18 N19 Ni1 125.2(3) . . ?
C20 N19 Ni1 118.0(3) . . ?
N19 C20 C21 110.6(4) . . ?
N19 C20 H20A 109.5 . . ?
C21 C20 H20A 109.5 . . ?
N19 C20 H20B 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C22 C21 C20 113.8(4) . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N23 C22 C21 113.6(4) . . ?
N23 C22 H22A 108.8 . . ?
C21 C22 H22A 108.8 . . ?
N23 C22 H22B 108.8 . . ?
C21 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C24 N23 C22 113.9(4) . . ?
C24 N23 Ni1 123.2(3) . . ?
C22 N23 Ni1 122.8(3) . . ?
N23 C24 C25 128.5(5) . . ?
N23 C24 H24 115.7 . . ?
C25 C24 H24 115.7 . . ?
C30 C25 C26 119.4(5) . . ?
C30 C25 C24 125.5(5) . . ?
C26 C25 C24 115.0(5) . . ?
C27 C26 C25 121.7(5) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 119.8(5) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C29 C28 C27 119.6(5) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
O291 C29 C28 124.5(4) . . ?
O291 C29 C30 113.3(4) . . ?
C28 C29 C30 122.2(5) . . ?
O31 C30 C25 122.8(4) . . ?
O31 C30 C29 119.8(4) . . ?
C25 C30 C29 117.3(4) . . ?
O131 C132 H13A 109.5 . . ?
O131 C132 H13B 109.5 . . ?
H13A C132 H13B 109.5 . . ?
O131 C132 H13C 109.5 . . ?
H13A C132 H13C 109.5 . . ?
H13B C132 H13C 109.5 . . ?
O291 C292 H29A 109.5 . . ?
O291 C292 H29B 109.5 . . ?
H29A C292 H29B 109.5 . . ?
O291 C292 H29C 109.5 . . ?
H29A C292 H29C 109.5 . . ?
H29B C292 H29C 109.5 . . ?
C30 O31 Ni1 127.5(3) . . ?
C30 O31 Pb1 125.1(3) . . ?
Ni1 O31 Pb1 107.29(15) . . ?
C13 O131 C132 117.6(4) . . ?
C13 O131 Pb1 115.1(3) . . ?
C132 O131 Pb1 126.1(3) . . ?
C29 O291 C292 117.3(4) . . ?
C29 O291 Pb1 115.8(3) . . ?
C292 O291 Pb1 121.3(3) . . ?
S42 C43 H43A 109.5 . . ?
S42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
S42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
S42 C44 H44A 109.5 . . ?
S42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
S42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O41 S42 C44 106.3(3) . . ?
O41 S42 C43 106.0(3) . . ?
C44 S42 C43 98.5(3) . . ?
C1 N1 Ni1 148.2(4) . . ?
N1 C1 S1 178.9(5) . . ?
O1 C2 O2 126.6(7) . . ?
O1 C2 C3 118.2(6) . . ?
O2 C2 C3 115.2(5) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1 O2 0.846(19) 1.90(2) 2.744(5) 174(7) .
O1W H2 O41 0.850(19) 1.96(2) 2.808(5) 173(8) 2_865
O1W H1 O2 0.846(19) 1.90(2) 2.744(5) 174(7) .
O1W H2 O41 0.850(19) 1.96(2) 2.808(5) 173(8) 2_865
O1W H2 S42 0.850(19) 3.02(4) 3.828(4) 159(7) 2_865

_refine_diff_density_max         3.208
_refine_diff_density_min         -3.310
_refine_diff_density_rms         0.225

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1580467'
_audit_update_record             
;
2018-02-19 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H30 Cl N3 Ni O5 Pb S'
_chemical_formula_weight         773.92

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   9.8038(8)
_cell_length_b                   11.9201(11)
_cell_length_c                   12.8868(8)
_cell_angle_alpha                95.767(6)
_cell_angle_beta                 104.841(6)
_cell_angle_gamma                111.721(8)
_cell_volume                     1320.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5897
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_F_000             756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    7.302
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a

_diffrn_reflns_number            5897
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.298
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.937
_reflns_number_total             4369
_reflns_number_gt                3750
_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, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4369
_refine_ls_number_parameters     335
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.2275
_refine_ls_wR_factor_gt          0.2061
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_restrained_S_all      0.918
_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
Pb1 Pb 0.21533(5) 0.40489(4) 0.20017(3) 0.0185(3) Uani 1 1 d . . . . .
Ni1 Ni 0.48821(18) 0.69423(16) 0.23082(12) 0.0151(4) Uani 1 1 d D . . . .
S1 S 0.1960(5) 0.8461(4) 0.4127(3) 0.0325(9) Uani 1 1 d . . . . .
C1 C 0.3027(14) 0.8015(11) 0.3552(10) 0.014(3) Uani 1 1 d . U . . .
N1 N 0.3801(13) 0.7690(12) 0.3151(10) 0.023(3) Uani 1 1 d . . . . .
O11 O 0.4587(10) 0.5503(9) 0.3043(7) 0.018(2) Uani 1 1 d . . . . .
Cl1 Cl 0.3476(4) 0.3113(4) 0.0828(3) 0.0254(8) Uani 1 1 d . . . . .
C12 C 0.5697(14) 0.5243(13) 0.3709(9) 0.016(3) Uani 1 1 d . . . . .
C13 C 0.5353(15) 0.4090(14) 0.3974(11) 0.021(3) Uani 1 1 d . . . . .
O131 O 0.3821(11) 0.3258(10) 0.3505(8) 0.026(2) Uani 1 1 d . . . . .
C132 C 0.3403(17) 0.1990(14) 0.3649(13) 0.028(3) Uani 1 1 d . U . . .
H13A H 0.228750 0.157324 0.346818 0.034 Uiso 1 1 calc R U . . .
H13B H 0.386675 0.199637 0.441189 0.034 Uiso 1 1 calc R U . . .
C133 C 0.394(2) 0.1297(16) 0.2928(14) 0.037(4) Uani 1 1 d . U . . .
H13C H 0.340451 0.121745 0.217008 0.055 Uiso 1 1 calc R U . . .
H13D H 0.373651 0.049012 0.308242 0.055 Uiso 1 1 calc R U . . .
H13E H 0.503625 0.174128 0.306939 0.055 Uiso 1 1 calc R U . . .
C14 C 0.6470(16) 0.3818(15) 0.4640(11) 0.024(3) Uani 1 1 d . U . . .
H14 H 0.621557 0.303227 0.478871 0.028 Uiso 1 1 calc R U . . .
C15 C 0.8010(15) 0.4728(14) 0.5104(12) 0.025(3) Uani 1 1 d . . . . .
H15 H 0.876781 0.455589 0.557084 0.030 Uiso 1 1 calc R U . . .
C16 C 0.8351(16) 0.5852(15) 0.4850(12) 0.027(3) Uani 1 1 d . . . . .
H16 H 0.936739 0.644321 0.513727 0.032 Uiso 1 1 calc R U . . .
C17 C 0.7239(14) 0.6170(13) 0.4170(10) 0.017(3) Uani 1 1 d . U . . .
C18 C 0.7750(14) 0.7443(13) 0.4044(10) 0.015(3) Uani 1 1 d . U . . .
H18 H 0.875968 0.797001 0.446355 0.018 Uiso 1 1 calc R U . . .
N19 N 0.6978(12) 0.7938(11) 0.3420(8) 0.020(3) Uani 1 1 d . . . . .
C20 C 0.7674(17) 0.9263(14) 0.3612(12) 0.028(3) Uani 1 1 d . . . . .
H20A H 0.872185 0.956706 0.411358 0.033 Uiso 1 1 calc R U . . .
H20B H 0.709664 0.959193 0.396431 0.033 Uiso 1 1 calc R U . . .
C21 C 0.7725(15) 0.9745(12) 0.2556(11) 0.019(3) Uani 1 1 d . . . . .
C22 C 0.6108(16) 0.9491(13) 0.1797(11) 0.025(3) Uani 1 1 d . . . . .
H22A H 0.561196 0.985066 0.220774 0.030 Uiso 1 1 calc R U . . .
H22B H 0.622453 0.991219 0.119778 0.030 Uiso 1 1 calc R U . . .
N23 N 0.5072(11) 0.8172(10) 0.1323(8) 0.012(2) Uani 1 1 d . U . . .
C24 C 0.4348(14) 0.7852(13) 0.0297(11) 0.018(3) Uani 1 1 d . . . . .
H24 H 0.462109 0.846228 -0.010030 0.022 Uiso 1 1 calc R U . . .
C25 C 0.3155(15) 0.6662(12) -0.0334(11) 0.020(3) Uani 1 1 d . . . . .
C26 C 0.2679(14) 0.6552(14) -0.1502(11) 0.021(3) Uani 1 1 d . . . . .
H26 H 0.317553 0.720080 -0.180382 0.025 Uiso 1 1 calc R U . . .
C27 C 0.1495(16) 0.5491(14) -0.2173(11) 0.023(3) Uani 1 1 d . U . . .
H27 H 0.121128 0.542185 -0.293027 0.028 Uiso 1 1 calc R U . . .
C28 C 0.0738(14) 0.4552(12) -0.1765(10) 0.016(3) Uani 1 1 d . U . . .
H28 H -0.008762 0.385566 -0.223892 0.020 Uiso 1 1 calc R U . . .
C29 C 0.1175(15) 0.4606(13) -0.0624(11) 0.019(3) Uani 1 1 d . . . . .
C30 C 0.2419(14) 0.5693(12) 0.0090(10) 0.014(3) Uani 1 1 d . . . . .
C211 C 0.8581(17) 0.9222(15) 0.1933(11) 0.026(3) Uani 1 1 d . . . . .
H21A H 0.962204 0.945465 0.239811 0.038 Uiso 1 1 calc R U . . .
H21B H 0.860089 0.954909 0.128342 0.038 Uiso 1 1 calc R U . . .
H21C H 0.805361 0.833635 0.172886 0.038 Uiso 1 1 calc R U . . .
C212 C 0.8595(15) 1.1164(13) 0.2906(12) 0.023(3) Uani 1 1 d . . . . .
H21D H 0.965444 1.138015 0.332363 0.034 Uiso 1 1 calc R U . . .
H21E H 0.811554 1.148537 0.334908 0.034 Uiso 1 1 calc R U . . .
H21F H 0.855873 1.150940 0.226333 0.034 Uiso 1 1 calc R U . . .
O291 O 0.0495(10) 0.3705(9) -0.0118(7) 0.023(2) Uani 1 1 d . . . . .
C292 C -0.0579(16) 0.2502(14) -0.0839(11) 0.023(3) Uani 1 1 d . . . . .
H29A H -0.011917 0.226168 -0.135574 0.028 Uiso 1 1 calc R U . . .
H29B H -0.152772 0.254818 -0.125165 0.028 Uiso 1 1 calc R U . . .
C293 C -0.0924(17) 0.1566(14) -0.0130(12) 0.029(3) Uani 1 1 d . U . . .
H29C H 0.000373 0.147212 0.022399 0.043 Uiso 1 1 calc R U . . .
H29D H -0.169687 0.078506 -0.057986 0.043 Uiso 1 1 calc R U . . .
H29E H -0.129980 0.184606 0.041823 0.043 Uiso 1 1 calc R U . . .
O31 O 0.2795(10) 0.5722(9) 0.1193(7) 0.017(2) Uani 1 1 d . . . . .
O1 O 0.5957(11) 0.6045(10) 0.1407(8) 0.024(2) Uani 1 1 d D . . . .
H2 H 0.617(16) 0.542(9) 0.155(8) 0.029 Uiso 1 1 d D U . . .
H1 H 0.613(16) 0.618(10) 0.080(7) 0.029 Uiso 1 1 d D 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 O31 2.299(9) . ?
Pb1 O11 2.309(9) . ?
Pb1 Cl1 2.637(3) . ?
Pb1 O131 2.684(9) . ?
Pb1 O291 2.698(9) . ?
Ni1 O11 2.005(10) . ?
Ni1 N19 2.007(10) . ?
Ni1 N23 2.022(10) . ?
Ni1 N1 2.048(12) . ?
Ni1 O31 2.059(9) . ?
Ni1 O1 2.194(9) . ?
S1 C1 1.630(13) . ?
C1 N1 1.170(17) . ?
O11 C12 1.358(15) . ?
C12 C13 1.39(2) . ?
C12 C17 1.425(19) . ?
C13 C14 1.369(19) . ?
C13 O131 1.385(17) . ?
O131 C132 1.457(19) . ?
C132 C133 1.50(2) . ?
C132 H13A 0.9700 . ?
C132 H13B 0.9700 . ?
C133 H13C 0.9600 . ?
C133 H13D 0.9600 . ?
C133 H13E 0.9600 . ?
C14 C15 1.42(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.35(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.408(18) . ?
C16 H16 0.9300 . ?
C17 C18 1.45(2) . ?
C18 N19 1.297(17) . ?
C18 H18 0.9300 . ?
N19 C20 1.43(2) . ?
C20 C21 1.53(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.535(18) . ?
C21 C211 1.539(19) . ?
C21 C212 1.541(18) . ?
C22 N23 1.478(17) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N23 C24 1.271(16) . ?
C24 C25 1.447(19) . ?
C24 H24 0.9300 . ?
C25 C30 1.37(2) . ?
C25 C26 1.434(19) . ?
C26 C27 1.37(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.33(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.410(18) . ?
C28 H28 0.9300 . ?
C29 O291 1.363(18) . ?
C29 C30 1.424(18) . ?
C30 O31 1.367(15) . ?
C211 H21A 0.9600 . ?
C211 H21B 0.9600 . ?
C211 H21C 0.9600 . ?
C212 H21D 0.9600 . ?
C212 H21E 0.9600 . ?
C212 H21F 0.9600 . ?
O291 C292 1.463(16) . ?
C292 C293 1.51(2) . ?
C292 H29A 0.9700 . ?
C292 H29B 0.9700 . ?
C293 H29C 0.9600 . ?
C293 H29D 0.9600 . ?
C293 H29E 0.9600 . ?
O1 H2 0.865(18) . ?
O1 H1 0.864(18) . ?

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
O31 Pb1 O11 71.0(3) . . ?
O31 Pb1 Cl1 87.7(2) . . ?
O11 Pb1 Cl1 88.3(2) . . ?
O31 Pb1 O131 133.2(3) . . ?
O11 Pb1 O131 64.2(3) . . ?
Cl1 Pb1 O131 78.3(2) . . ?
O31 Pb1 O291 63.0(3) . . ?
O11 Pb1 O291 131.1(3) . . ?
Cl1 Pb1 O291 74.4(2) . . ?
O131 Pb1 O291 147.6(3) . . ?
O11 Ni1 N19 91.4(4) . . ?
O11 Ni1 N23 170.0(4) . . ?
N19 Ni1 N23 95.0(5) . . ?
O11 Ni1 N1 94.6(4) . . ?
N19 Ni1 N1 93.0(4) . . ?
N23 Ni1 N1 92.7(4) . . ?
O11 Ni1 O31 82.3(4) . . ?
N19 Ni1 O31 172.5(4) . . ?
N23 Ni1 O31 90.7(4) . . ?
N1 Ni1 O31 91.6(4) . . ?
O11 Ni1 O1 82.9(4) . . ?
N19 Ni1 O1 88.7(4) . . ?
N23 Ni1 O1 89.5(4) . . ?
N1 Ni1 O1 177.0(5) . . ?
O31 Ni1 O1 86.4(4) . . ?
N1 C1 S1 179.1(12) . . ?
C1 N1 Ni1 172.3(11) . . ?
C12 O11 Ni1 127.7(9) . . ?
C12 O11 Pb1 124.6(8) . . ?
Ni1 O11 Pb1 103.8(3) . . ?
O11 C12 C13 121.2(12) . . ?
O11 C12 C17 119.9(12) . . ?
C13 C12 C17 118.9(11) . . ?
C14 C13 O131 123.8(14) . . ?
C14 C13 C12 121.5(13) . . ?
O131 C13 C12 114.7(11) . . ?
C13 O131 C132 118.0(10) . . ?
C13 O131 Pb1 113.5(8) . . ?
C132 O131 Pb1 126.4(8) . . ?
O131 C132 C133 110.9(13) . . ?
O131 C132 H13A 109.5 . . ?
C133 C132 H13A 109.5 . . ?
O131 C132 H13B 109.5 . . ?
C133 C132 H13B 109.5 . . ?
H13A C132 H13B 108.0 . . ?
C132 C133 H13C 109.5 . . ?
C132 C133 H13D 109.5 . . ?
H13C C133 H13D 109.5 . . ?
C132 C133 H13E 109.5 . . ?
H13C C133 H13E 109.5 . . ?
H13D C133 H13E 109.5 . . ?
C13 C14 C15 120.4(14) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 118.4(13) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
C15 C16 C17 123.0(13) . . ?
C15 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C16 C17 C12 117.8(13) . . ?
C16 C17 C18 116.7(12) . . ?
C12 C17 C18 125.4(11) . . ?
N19 C18 C17 128.3(12) . . ?
N19 C18 H18 115.8 . . ?
C17 C18 H18 115.8 . . ?
C18 N19 C20 115.9(11) . . ?
C18 N19 Ni1 122.8(10) . . ?
C20 N19 Ni1 121.2(9) . . ?
N19 C20 C21 113.2(11) . . ?
N19 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
N19 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 C22 112.4(12) . . ?
C20 C21 C211 111.7(11) . . ?
C22 C21 C211 110.5(10) . . ?
C20 C21 C212 106.8(11) . . ?
C22 C21 C212 105.7(11) . . ?
C211 C21 C212 109.3(12) . . ?
N23 C22 C21 115.3(12) . . ?
N23 C22 H22A 108.4 . . ?
C21 C22 H22A 108.4 . . ?
N23 C22 H22B 108.4 . . ?
C21 C22 H22B 108.4 . . ?
H22A C22 H22B 107.5 . . ?
C24 N23 C22 118.1(12) . . ?
C24 N23 Ni1 122.4(10) . . ?
C22 N23 Ni1 119.5(8) . . ?
N23 C24 C25 128.6(13) . . ?
N23 C24 H24 115.7 . . ?
C25 C24 H24 115.7 . . ?
C30 C25 C26 119.0(12) . . ?
C30 C25 C24 125.8(13) . . ?
C26 C25 C24 115.1(13) . . ?
C27 C26 C25 120.0(14) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 121.5(13) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 120.7(12) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
O291 C29 C28 125.8(12) . . ?
O291 C29 C30 115.4(11) . . ?
C28 C29 C30 118.8(13) . . ?
O31 C30 C25 122.8(12) . . ?
O31 C30 C29 117.2(12) . . ?
C25 C30 C29 119.9(12) . . ?
C21 C211 H21A 109.5 . . ?
C21 C211 H21B 109.5 . . ?
H21A C211 H21B 109.5 . . ?
C21 C211 H21C 109.5 . . ?
H21A C211 H21C 109.5 . . ?
H21B C211 H21C 109.5 . . ?
C21 C212 H21D 109.5 . . ?
C21 C212 H21E 109.5 . . ?
H21D C212 H21E 109.5 . . ?
C21 C212 H21F 109.5 . . ?
H21D C212 H21F 109.5 . . ?
H21E C212 H21F 109.5 . . ?
C29 O291 C292 116.0(10) . . ?
C29 O291 Pb1 113.5(7) . . ?
C292 O291 Pb1 124.9(8) . . ?
O291 C292 C293 108.1(11) . . ?
O291 C292 H29A 110.1 . . ?
C293 C292 H29A 110.1 . . ?
O291 C292 H29B 110.1 . . ?
C293 C292 H29B 110.1 . . ?
H29A C292 H29B 108.4 . . ?
C292 C293 H29C 109.5 . . ?
C292 C293 H29D 109.5 . . ?
H29C C293 H29D 109.5 . . ?
C292 C293 H29E 109.5 . . ?
H29C C293 H29E 109.5 . . ?
H29D C293 H29E 109.5 . . ?
C30 O31 Ni1 122.9(8) . . ?
C30 O31 Pb1 126.6(8) . . ?
Ni1 O31 Pb1 102.5(3) . . ?
Ni1 O1 H2 126(2) . . ?
Ni1 O1 H1 126(2) . . ?
H2 O1 H1 108(2) . . ?

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
O1 H1 Cl1 0.864(18) 2.40(2) 3.256(11) 170(4) 2_665

_refine_diff_density_max         4.635
_refine_diff_density_min         -5.982
_refine_diff_density_rms         0.438

####################################################################### 
# 
# 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 1580465'
_audit_update_record             
;
2018-02-19 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H28 Cl2 N2 Ni O6 Pb'
_chemical_formula_weight         741.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   14.760(3)
_cell_length_b                   12.3947(15)
_cell_length_c                   14.300(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.72(2)
_cell_angle_gamma                90
_cell_volume                     2447.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5706
_cell_measurement_theta_min      3.410
_cell_measurement_theta_max      30.00

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    7.898
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a

_diffrn_reflns_number            5706
_diffrn_reflns_av_unetI/netI     0.1329
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.410
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             3387
_reflns_number_gt                2420
_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, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-97, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0540P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3387
_refine_ls_number_parameters     162
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0758
_refine_ls_wR_factor_ref         0.1766
_refine_ls_wR_factor_gt          0.1570
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.060
_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 0.000000 0.77938(4) 0.250000 0.0348(2) Uani 1 2 d S T P . .
Ni1 Ni 0.000000 1.05883(13) 0.250000 0.0244(4) Uani 1 2 d S T P A .
Cl1 Cl 0.0611(2) 0.8099(2) 0.0772(2) 0.0454(7) Uani 1 1 d . . . . .
O1 O 0.0463(7) 1.0567(6) 0.1255(6) 0.0346(18) Uani 1 1 d D . . . .
O11 O -0.0915(5) 0.9330(5) 0.1954(5) 0.0259(14) Uani 1 1 d . . . . .
C12 C -0.1849(7) 0.9337(8) 0.1381(7) 0.0220(19) Uani 1 1 d . . . . .
C13 C -0.2374(7) 0.8387(8) 0.1169(6) 0.0197(18) Uani 1 1 d . . . . .
O131 O -0.1854(5) 0.7467(5) 0.1549(5) 0.0261(15) Uani 1 1 d . . . . .
C14 C -0.3343(8) 0.8378(9) 0.0602(7) 0.028(2) Uani 1 1 d . . . . .
H14 H -0.367510 0.772451 0.047497 0.034 Uiso 1 1 calc R U . . .
C15 C -0.3840(8) 0.9324(11) 0.0213(9) 0.043(3) Uani 1 1 d . . . . .
H15 H -0.449171 0.930974 -0.018776 0.052 Uiso 1 1 calc R U . . .
C16 C -0.3342(8) 1.0272(10) 0.0436(7) 0.034(2) Uani 1 1 d . . . . .
H16 H -0.366614 1.091184 0.018621 0.041 Uiso 1 1 calc R U . . .
C17 C -0.2354(7) 1.0313(9) 0.1032(7) 0.027(2) Uani 1 1 d . . . . .
C18 C -0.1922(8) 1.1393(8) 0.1247(7) 0.031(2) Uani 1 1 d . . . . .
H18 H -0.232967 1.196208 0.093943 0.037 Uiso 1 1 calc R U . . .
C20A C -0.0869(12) 1.2829(10) 0.1891(10) 0.057(4) Uani 0.5 1 d . . P A 1
H20A H -0.145704 1.320688 0.185286 0.068 Uiso 0.5 1 calc R U P A 1
H20B H -0.069241 1.306570 0.133175 0.068 Uiso 0.5 1 calc R U P A 1
C21A C -0.0030(17) 1.3152(17) 0.2901(18) 0.036(5) Uani 0.25 1 d . . P A 1
H21A H -0.001647 1.393427 0.293125 0.044 Uiso 0.5 1 calc R U P A 1
H21B H -0.022889 1.290615 0.344364 0.044 Uiso 0.5 1 calc R U P A 1
C20B C -0.0869(12) 1.2829(10) 0.1891(10) 0.057(4) Uani 0.5 1 d . . P A 2
H20C H -0.126353 1.316776 0.126806 0.068 Uiso 0.5 1 calc R U P A 2
H20D H -0.109006 1.310437 0.240853 0.068 Uiso 0.5 1 calc R U P A 2
C21B C -0.0030(17) 1.3152(17) 0.2901(18) 0.036(5) Uani 0.25 1 d . . P B 2
C132 C -0.2390(8) 0.6479(8) 0.1494(8) 0.031(2) Uani 1 1 d . . . . .
H13A H -0.270077 0.625922 0.080292 0.037 Uiso 1 1 calc R U . . .
H13B H -0.288551 0.658212 0.178548 0.037 Uiso 1 1 calc R U . . .
C133 C -0.1680(9) 0.5638(10) 0.2064(9) 0.039(3) Uani 1 1 d . . . . .
H13C H -0.123671 0.548480 0.172587 0.059 Uiso 1 1 calc R U . . .
H13D H -0.202146 0.499120 0.210625 0.059 Uiso 1 1 calc R U . . .
H13E H -0.132658 0.589833 0.272541 0.059 Uiso 1 1 calc R U . . .
N19 N -0.1069(7) 1.1657(7) 0.1796(7) 0.033(2) Uani 1 1 d . . . . .
H1 H 0.055(8) 0.989(2) 0.128(7) 0.040 Uiso 1 1 d D U . . .
H2 H 0.011(7) 1.076(7) 0.066(3) 0.040 Uiso 1 1 d D 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 O11 2.306(6) 6_556 ?
Pb1 O11 2.306(6) . ?
Pb1 O131 2.621(7) . ?
Pb1 O131 2.621(7) 6_556 ?
Pb1 Cl1 2.939(3) . ?
Pb1 Cl1 2.939(3) 6_556 ?
Ni1 O11 2.030(7) 6_556 ?
Ni1 O11 2.030(7) . ?
Ni1 N19 2.032(9) 6_556 ?
Ni1 N19 2.032(9) . ?
Ni1 O1 2.121(8) . ?
Ni1 O1 2.121(8) 6_556 ?
O1 H1 0.85(2) . ?
O1 H2 0.85(2) . ?
O11 C12 1.331(12) . ?
C12 C13 1.383(13) . ?
C12 C17 1.415(14) . ?
C13 C14 1.373(14) . ?
C13 O131 1.374(12) . ?
O131 C132 1.445(11) . ?
C14 C15 1.390(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.363(18) . ?
C15 H15 0.9300 . ?
C16 C17 1.405(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.469(16) . ?
C18 N19 1.269(14) . ?
C18 H18 0.9300 . ?
C20A N19 1.480(15) . ?
C20A C21A 1.59(3) . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C21A H21A 0.9700 . ?
C21A H21B 0.9700 . ?
C20B C21B 1.32(3) 6_556 ?
C20B N19 1.480(15) . ?
C20B H20C 0.9700 . ?
C20B H20D 0.9700 . ?
C132 C133 1.499(16) . ?
C132 H13A 0.9700 . ?
C132 H13B 0.9700 . ?
C133 H13C 0.9600 . ?
C133 H13D 0.9600 . ?
C133 H13E 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Pb1 O11 68.6(3) 6_556 . ?
O11 Pb1 O131 133.0(2) 6_556 . ?
O11 Pb1 O131 64.7(2) . . ?
O11 Pb1 O131 64.7(2) 6_556 6_556 ?
O11 Pb1 O131 133.0(2) . 6_556 ?
O131 Pb1 O131 162.2(3) . 6_556 ?
O11 Pb1 Cl1 82.03(18) 6_556 . ?
O11 Pb1 Cl1 85.77(18) . . ?
O131 Pb1 Cl1 99.12(17) . . ?
O131 Pb1 Cl1 83.17(17) 6_556 . ?
O11 Pb1 Cl1 85.77(18) 6_556 6_556 ?
O11 Pb1 Cl1 82.02(18) . 6_556 ?
O131 Pb1 Cl1 83.17(17) . 6_556 ?
O131 Pb1 Cl1 99.13(17) 6_556 6_556 ?
Cl1 Pb1 Cl1 165.22(12) . 6_556 ?
O11 Ni1 O11 79.6(4) 6_556 . ?
O11 Ni1 N19 90.9(3) 6_556 6_556 ?
O11 Ni1 N19 170.2(3) . 6_556 ?
O11 Ni1 N19 170.2(3) 6_556 . ?
O11 Ni1 N19 90.9(3) . . ?
N19 Ni1 N19 98.7(6) 6_556 . ?
O11 Ni1 O1 86.9(3) 6_556 . ?
O11 Ni1 O1 92.0(3) . . ?
N19 Ni1 O1 90.0(3) 6_556 . ?
N19 Ni1 O1 90.9(3) . . ?
O11 Ni1 O1 92.0(3) 6_556 6_556 ?
O11 Ni1 O1 86.9(3) . 6_556 ?
N19 Ni1 O1 90.9(3) 6_556 6_556 ?
N19 Ni1 O1 90.0(3) . 6_556 ?
O1 Ni1 O1 178.6(4) . 6_556 ?
Ni1 O1 H1 94(7) . . ?
Ni1 O1 H2 124(8) . . ?
H1 O1 H2 111(4) . . ?
C12 O11 Ni1 129.4(6) . . ?
C12 O11 Pb1 124.7(5) . . ?
Ni1 O11 Pb1 105.9(3) . . ?
O11 C12 C13 120.4(8) . . ?
O11 C12 C17 121.6(9) . . ?
C13 C12 C17 117.8(9) . . ?
C14 C13 O131 123.1(9) . . ?
C14 C13 C12 121.5(9) . . ?
O131 C13 C12 115.4(8) . . ?
C13 O131 C132 117.6(8) . . ?
C13 O131 Pb1 114.3(5) . . ?
C132 O131 Pb1 127.6(6) . . ?
C13 C14 C15 121.4(10) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 118.0(10) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 122.0(11) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 H16 119.0 . . ?
C16 C17 C12 119.2(10) . . ?
C16 C17 C18 116.1(10) . . ?
C12 C17 C18 124.7(9) . . ?
N19 C18 C17 128.8(9) . . ?
N19 C18 H18 115.6 . . ?
C17 C18 H18 115.6 . . ?
N19 C20A C21A 113.4(12) . . ?
N19 C20A H20A 108.9 . . ?
C21A C20A H20A 108.9 . . ?
N19 C20A H20B 108.9 . . ?
C21A C20A H20B 108.9 . . ?
H20A C20A H20B 107.7 . . ?
C20A C21A C20A 121.9(18) 6_556 . ?
C20A C21A H21A 106.8 6_556 . ?
C20A C21A H21A 106.8 . . ?
C20A C21A H21B 106.8 6_556 . ?
C20A C21A H21B 106.8 . . ?
H21A C21A H21B 106.7 . . ?
C21B C20B N19 118.1(15) 6_556 . ?
C21B C20B H20C 107.8 6_556 . ?
N19 C20B H20C 107.8 . . ?
C21B C20B H20D 107.8 6_556 . ?
N19 C20B H20D 107.8 . . ?
H20C C20B H20D 107.1 . . ?
O131 C132 C133 107.2(9) . . ?
O131 C132 H13A 110.3 . . ?
C133 C132 H13A 110.3 . . ?
O131 C132 H13B 110.3 . . ?
C133 C132 H13B 110.3 . . ?
H13A C132 H13B 108.5 . . ?
C132 C133 H13C 109.5 . . ?
C132 C133 H13D 109.5 . . ?
H13C C133 H13D 109.5 . . ?
C132 C133 H13E 109.5 . . ?
H13C C133 H13E 109.5 . . ?
H13D C133 H13E 109.5 . . ?
C18 N19 C20B 115.5(10) . . ?
C18 N19 C20A 115.5(10) . . ?
C18 N19 Ni1 124.4(7) . . ?
C20B N19 Ni1 120.0(8) . . ?
C20A N19 Ni1 120.0(8) . . ?

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
O1 H1 Cl1 0.85(2) 2.34(4) 3.161(8) 160(8) .
O1 H2 Cl1 0.85(2) 2.41(4) 3.225(8) 160(9) 5_575
O1 H1 Cl1 0.85(2) 2.34(4) 3.161(8) 160(8) .
O1 H2 Cl1 0.85(2) 2.41(4) 3.225(8) 160(9) 5_575
C14 H14 Cl1 0.93 2.96 3.710(11) 138.2 7_465
C132 H13B O1 0.97 2.61 3.267(14) 125.5 3_445

_refine_diff_density_max         2.691
_refine_diff_density_min         -3.192
_refine_diff_density_rms         0.263

