# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_KK5
_database_code_depnum_ccdc_archive 'CCDC 2006270'
loop_
_audit_author_name
_audit_author_address
'saroj kumar kushvaha'
;Indian Institute of Technology Madras
India
;
_audit_update_record             
;
2020-05-28 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H53 Cl N4 Ni4 O12'
_chemical_formula_sum            'C60 H53 Cl N4 Ni4 O12'
_chemical_formula_weight         1292.35

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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 '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/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.831(2)
_cell_length_b                   23.697(5)
_cell_length_c                   14.715(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.577(8)
_cell_angle_gamma                90
_cell_volume                     5863.1(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1340
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      21.34

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_F_000             2664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.375
_shelx_estimated_absorpt_T_min   0.852
_shelx_estimated_absorpt_T_max   0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35932
_diffrn_reflns_av_unetI/netI     0.2051
_diffrn_reflns_av_R_equivalents  0.1545
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.630
_diffrn_reflns_theta_max         25.206
_diffrn_reflns_theta_full        25.206
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             10269
_reflns_number_gt                4743
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0505P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10269
_refine_ls_number_parameters     738
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1593
_refine_ls_R_factor_gt           0.0630
_refine_ls_wR_factor_ref         0.1622
_refine_ls_wR_factor_gt          0.1295
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_restrained_S_all      0.932
_refine_ls_shift/su_max          0.043
_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 0.20355(5) -0.04215(4) 0.80481(7) 0.0224(2) Uani 1 1 d . . . . .
Ni2 Ni 0.22210(5) 0.07309(4) 0.70351(7) 0.0279(3) Uani 1 1 d . . . . .
Ni3 Ni 0.37554(5) -0.00051(4) 0.76128(7) 0.0297(3) Uani 1 1 d . . . . .
Ni4 Ni 0.40164(5) 0.13108(4) 0.68383(6) 0.0240(3) Uani 1 1 d . . . . .
Cl1 Cl 0.41222(11) 0.14707(8) 0.53842(15) 0.0428(6) Uani 1 1 d . . . . .
O1 O 0.3173(2) 0.0363(2) 0.6550(3) 0.0319(13) Uani 1 1 d . . . . .
O2 O 0.4348(3) -0.0338(2) 0.6422(4) 0.0430(15) Uani 1 1 d . . . . .
O3 O 0.1642(3) 0.2063(2) 0.6084(4) 0.0461(15) Uani 1 1 d . . . . .
H3A H 0.205337 0.187777 0.621645 0.069 Uiso 1 1 d R U . . .
O4 O 0.1496(2) 0.00409(19) 0.7075(3) 0.0284(12) Uani 1 1 d . . . . .
O5 O 0.2799(2) 0.03535(19) 0.8240(3) 0.0282(12) Uani 1 1 d . . . . .
O6 O 0.3081(3) -0.0737(2) 0.7728(4) 0.0344(13) Uani 1 1 d . . . . .
O7 O 0.4461(3) 0.0701(2) 0.7631(3) 0.0345(13) Uani 1 1 d . . . . .
O8 O 0.2886(2) 0.1443(2) 0.7204(3) 0.0304(13) Uani 1 1 d . . . . .
O9 O 0.4039(3) 0.2149(2) 0.7512(4) 0.0428(15) Uani 1 1 d . . . . .
O10 O 0.5401(3) 0.1501(2) 0.7105(4) 0.0460(15) Uani 1 1 d . . . . .
O11 O 0.0178(4) -0.1712(3) 0.7446(5) 0.076(2) Uani 1 1 d . . . . .
O12 O 0.1318(3) -0.1070(2) 0.8060(4) 0.0410(15) Uani 1 1 d . . . . .
N1 N 0.1826(3) 0.0896(2) 0.5696(4) 0.0320(16) Uani 1 1 d . . . . .
N2 N 0.1322(3) 0.1097(3) 0.7640(4) 0.0280(15) Uani 1 1 d . . . . .
N3 N 0.4436(3) -0.0392(2) 0.8563(4) 0.0286(15) Uani 1 1 d . . . . .
N4 N 0.1772(3) -0.0171(2) 0.9323(4) 0.0322(16) Uani 1 1 d . . . . .
C1 C 0.3269(4) 0.0141(3) 0.5722(5) 0.0278(19) Uani 1 1 d . . . . .
C2 C 0.3916(4) -0.0233(3) 0.5618(6) 0.039(2) Uani 1 1 d . . . . .
C3 C 0.4092(5) -0.0439(4) 0.4780(6) 0.051(3) Uani 1 1 d . . . . .
H3 H 0.452952 -0.067279 0.471552 0.061 Uiso 1 1 calc R U . . .
C4 C 0.3612(5) -0.0294(4) 0.4039(7) 0.062(3) Uani 1 1 d . . . . .
H4 H 0.372162 -0.043545 0.346915 0.075 Uiso 1 1 calc R U . . .
C5 C 0.2979(5) 0.0053(4) 0.4126(6) 0.047(2) Uani 1 1 d . . . . .
H5 H 0.266138 0.014114 0.361270 0.056 Uiso 1 1 calc R U . . .
C6 C 0.2792(4) 0.0281(3) 0.4961(5) 0.0302(19) Uani 1 1 d . . . . .
C7 C 0.2109(4) 0.0645(3) 0.4996(6) 0.036(2) Uani 1 1 d . . . . .
H7 H 0.183373 0.070952 0.444394 0.044 Uiso 1 1 calc R U . . .
C8 C 0.1061(4) 0.1180(3) 0.5526(6) 0.040(2) Uani 1 1 d . . . . .
C9 C 0.0371(4) 0.0884(3) 0.5215(6) 0.040(2) Uani 1 1 d . . . . .
H9 H 0.041299 0.050427 0.506441 0.048 Uiso 1 1 calc R U . . .
C10 C -0.0355(5) 0.1142(4) 0.5130(6) 0.049(2) Uani 1 1 d . . . . .
C11 C -0.0387(5) 0.1703(4) 0.5352(7) 0.065(3) Uani 1 1 d . . . . .
H11 H -0.087603 0.188539 0.529634 0.078 Uiso 1 1 calc R U . . .
C12 C 0.0266(5) 0.2013(4) 0.5654(6) 0.055(3) Uani 1 1 d . . . . .
H12 H 0.021857 0.239502 0.578706 0.066 Uiso 1 1 calc R U . . .
C13 C 0.0989(4) 0.1745(3) 0.5755(6) 0.039(2) Uani 1 1 d . . . . .
C14 C -0.1105(4) 0.0798(4) 0.4842(6) 0.058(3) Uani 1 1 d . . . . .
H14A H -0.131943 0.093491 0.426720 0.087 Uiso 1 1 calc R U . . .
H14B H -0.149586 0.083930 0.529285 0.087 Uiso 1 1 calc R U . . .
H14C H -0.096640 0.040741 0.478600 0.087 Uiso 1 1 calc R U . . .
C15 C 0.4926(5) -0.0790(4) 0.6426(7) 0.064(3) Uani 1 1 d . . . . .
H15A H 0.516557 -0.083111 0.702621 0.096 Uiso 1 1 calc R U . . .
H15B H 0.532866 -0.070288 0.600620 0.096 Uiso 1 1 calc R U . . .
H15C H 0.466576 -0.113570 0.624670 0.096 Uiso 1 1 calc R U . . .
C16 C 0.2764(4) 0.1842(3) 0.7835(5) 0.0300(19) Uani 1 1 d . . . . .
C17 C 0.3376(4) 0.2232(3) 0.8017(6) 0.036(2) Uani 1 1 d . . . . .
C18 C 0.3304(4) 0.2642(3) 0.8677(6) 0.045(2) Uani 1 1 d . . . . .
H18 H 0.371945 0.289305 0.879709 0.054 Uiso 1 1 calc R U . . .
C19 C 0.2618(4) 0.2682(3) 0.9161(6) 0.043(2) Uani 1 1 d . . . . .
H19 H 0.257771 0.295213 0.961435 0.052 Uiso 1 1 calc R U . . .
C20 C 0.1997(4) 0.2316(3) 0.8964(6) 0.035(2) Uani 1 1 d . . . . .
H20 H 0.153177 0.235064 0.927623 0.042 Uiso 1 1 calc R U . . .
C21 C 0.2052(4) 0.1894(3) 0.8302(5) 0.0267(19) Uani 1 1 d . . . . .
C22 C 0.1361(4) 0.1544(3) 0.8167(5) 0.033(2) Uani 1 1 d . . . . .
H22 H 0.090940 0.163978 0.847438 0.039 Uiso 1 1 calc R U . . .
C23 C 0.0624(4) 0.0769(3) 0.7531(5) 0.0280(19) Uani 1 1 d . . . . .
C24 C -0.0163(4) 0.0962(3) 0.7628(5) 0.036(2) Uani 1 1 d . . . . .
H24 H -0.024331 0.133700 0.778723 0.044 Uiso 1 1 calc R U . . .
C25 C -0.0802(4) 0.0622(4) 0.7498(6) 0.042(2) Uani 1 1 d . . . . .
C26 C -0.0663(4) 0.0073(4) 0.7238(6) 0.048(2) Uani 1 1 d . . . . .
H26 H -0.109925 -0.016376 0.714311 0.057 Uiso 1 1 calc R U . . .
C27 C 0.0100(4) -0.0151(3) 0.7106(5) 0.039(2) Uani 1 1 d . . . . .
H27 H 0.016488 -0.052681 0.694161 0.047 Uiso 1 1 calc R U . . .
C28 C 0.0745(4) 0.0203(3) 0.7229(5) 0.032(2) Uani 1 1 d . . . . .
C29 C -0.1631(4) 0.0845(4) 0.7584(6) 0.058(3) Uani 1 1 d . . . . .
H29A H -0.198025 0.053946 0.772261 0.087 Uiso 1 1 calc R U . . .
H29B H -0.180943 0.101785 0.702190 0.087 Uiso 1 1 calc R U . . .
H29C H -0.163172 0.111923 0.806405 0.087 Uiso 1 1 calc R U . . .
C30 C 0.4472(5) 0.2645(4) 0.7254(7) 0.071(3) Uani 1 1 d . . . . .
H30A H 0.484232 0.254516 0.680273 0.107 Uiso 1 1 calc R U . . .
H30B H 0.475630 0.279689 0.777861 0.107 Uiso 1 1 calc R U . . .
H30C H 0.410644 0.292220 0.700839 0.107 Uiso 1 1 calc R U . . .
C31 C 0.3432(4) -0.1088(3) 0.8366(6) 0.034(2) Uani 1 1 d . . . . .
C32 C 0.3079(4) -0.1594(3) 0.8597(6) 0.040(2) Uani 1 1 d . . . . .
H32 H 0.259332 -0.170035 0.832366 0.048 Uiso 1 1 calc R U . . .
C33 C 0.3466(5) -0.1942(3) 0.9248(6) 0.046(2) Uani 1 1 d . . . . .
H33 H 0.322334 -0.227940 0.940257 0.055 Uiso 1 1 calc R U . . .
C34 C 0.4194(5) -0.1807(3) 0.9672(6) 0.043(2) Uani 1 1 d . . . . .
C35 C 0.4536(4) -0.1306(3) 0.9425(6) 0.038(2) Uani 1 1 d . . . . .
H35 H 0.503417 -0.121142 0.967927 0.045 Uiso 1 1 calc R U . . .
C36 C 0.4160(4) -0.0934(3) 0.8805(5) 0.0287(19) Uani 1 1 d . . . . .
C37 C 0.5092(4) -0.0189(3) 0.8919(5) 0.034(2) Uani 1 1 d . . . . .
H37 H 0.534604 -0.040540 0.937201 0.041 Uiso 1 1 calc R U . . .
C38 C 0.5475(4) 0.0335(3) 0.8693(5) 0.032(2) Uani 1 1 d . . . . .
C39 C 0.5182(4) 0.0735(3) 0.8051(5) 0.031(2) Uani 1 1 d . . . . .
C40 C 0.5703(4) 0.1171(3) 0.7817(6) 0.034(2) Uani 1 1 d . . . . .
C41 C 0.6432(4) 0.1255(3) 0.8244(6) 0.043(2) Uani 1 1 d . . . . .
H41 H 0.675420 0.155192 0.807114 0.051 Uiso 1 1 calc R U . . .
C42 C 0.6683(4) 0.0892(3) 0.8936(6) 0.041(2) Uani 1 1 d . . . . .
H42 H 0.716053 0.095657 0.926315 0.049 Uiso 1 1 calc R U . . .
C43 C 0.6218(4) 0.0435(3) 0.9135(5) 0.034(2) Uani 1 1 d . . . . .
H43 H 0.640256 0.018227 0.957889 0.040 Uiso 1 1 calc R U . . .
C44 C 0.5964(5) 0.1817(4) 0.6615(7) 0.064(3) Uani 1 1 d . . . . .
H44A H 0.572160 0.193889 0.604550 0.096 Uiso 1 1 calc R U . . .
H44B H 0.641562 0.158372 0.650426 0.096 Uiso 1 1 calc R U . . .
H44C H 0.613244 0.214020 0.696635 0.096 Uiso 1 1 calc R U . . .
C45 C 0.4602(5) -0.2192(3) 1.0350(6) 0.051(2) Uani 1 1 d . . . . .
H45A H 0.421378 -0.236147 1.072299 0.076 Uiso 1 1 calc R U . . .
H45B H 0.497393 -0.197903 1.072661 0.076 Uiso 1 1 calc R U . . .
H45C H 0.487930 -0.248103 1.003636 0.076 Uiso 1 1 calc R U . . .
C46 C 0.2777(4) 0.0535(3) 0.9122(5) 0.0269(19) Uani 1 1 d . . . . .
C47 C 0.3272(4) 0.0957(3) 0.9460(5) 0.032(2) Uani 1 1 d . . . . .
H47 H 0.364240 0.111758 0.908716 0.038 Uiso 1 1 calc R U . . .
C48 C 0.3226(4) 0.1144(3) 1.0343(6) 0.035(2) Uani 1 1 d . . . . .
H48 H 0.354971 0.144000 1.054762 0.042 Uiso 1 1 calc R U . . .
C49 C 0.2708(4) 0.0900(3) 1.0929(6) 0.042(2) Uani 1 1 d . . . . .
C50 C 0.2224(4) 0.0456(3) 1.0597(6) 0.037(2) Uani 1 1 d . . . . .
H50 H 0.187872 0.028133 1.098576 0.045 Uiso 1 1 calc R U . . .
C51 C 0.2246(4) 0.0269(3) 0.9702(5) 0.0255(18) Uani 1 1 d . . . . .
C52 C 0.1158(4) -0.0368(3) 0.9721(6) 0.038(2) Uani 1 1 d . . . . .
H52 H 0.105400 -0.021197 1.028363 0.046 Uiso 1 1 calc R U . . .
C53 C 0.0629(4) -0.0794(3) 0.9394(6) 0.035(2) Uani 1 1 d . . . . .
C54 C -0.0056(4) -0.0880(3) 0.9906(6) 0.044(2) Uani 1 1 d . . . . .
H54 H -0.010723 -0.068195 1.044646 0.053 Uiso 1 1 calc R U . . .
C55 C -0.0648(5) -0.1250(4) 0.9620(7) 0.054(3) Uani 1 1 d . . . . .
H55 H -0.108614 -0.131110 0.997091 0.065 Uiso 1 1 calc R U . . .
C56 C -0.0580(5) -0.1536(4) 0.8787(8) 0.057(3) Uani 1 1 d . . . . .
H56 H -0.098022 -0.178105 0.858192 0.068 Uiso 1 1 calc R U . . .
C57 C 0.0060(5) -0.1456(4) 0.8284(7) 0.052(3) Uani 1 1 d . . . . .
C58 C 0.0711(5) -0.1098(3) 0.8568(6) 0.040(2) Uani 1 1 d . . . . .
C59 C -0.0495(6) -0.2010(5) 0.7027(8) 0.108(5) Uani 1 1 d . . . . .
H59A H -0.038167 -0.210693 0.641299 0.162 Uiso 1 1 calc R U . . .
H59B H -0.095695 -0.177249 0.702593 0.162 Uiso 1 1 calc R U . . .
H59C H -0.059125 -0.234756 0.736526 0.162 Uiso 1 1 calc R U . . .
C60 C 0.2681(5) 0.1084(4) 1.1919(6) 0.062(3) Uani 1 1 d . . . . .
H60A H 0.218441 0.097060 1.215813 0.092 Uiso 1 1 calc R U . . .
H60B H 0.273177 0.148680 1.195656 0.092 Uiso 1 1 calc R U . . .
H60C H 0.311133 0.091019 1.226701 0.092 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 O12 1.955(5) . ?
Ni1 O6 1.987(4) . ?
Ni1 O4 1.989(5) . ?
Ni1 N4 2.035(6) . ?
Ni1 O5 2.252(5) . ?
Ni2 O1 1.986(4) . ?
Ni2 N2 1.990(6) . ?
Ni2 O8 2.034(5) . ?
Ni2 O4 2.042(4) . ?
Ni2 N1 2.088(6) . ?
Ni2 O5 2.176(5) . ?
Ni3 N3 1.991(6) . ?
Ni3 O1 2.007(5) . ?
Ni3 O7 2.051(5) . ?
Ni3 O5 2.073(4) . ?
Ni3 O6 2.084(5) . ?
Ni3 O2 2.200(5) . ?
Ni4 O7 1.982(5) . ?
Ni4 O8 2.025(4) . ?
Ni4 Cl1 2.188(2) . ?
Ni4 O9 2.220(5) . ?
Ni4 O10 2.388(5) . ?
O1 C1 1.344(8) . ?
O2 C2 1.383(9) . ?
O2 C15 1.447(8) . ?
O3 C13 1.401(8) . ?
O3 H3A 0.8356 . ?
O4 C28 1.350(8) . ?
O5 C46 1.369(8) . ?
O6 C31 1.370(9) . ?
O7 C39 1.340(8) . ?
O8 C16 1.348(8) . ?
O9 C17 1.383(8) . ?
O9 C30 1.443(8) . ?
O10 C40 1.385(9) . ?
O10 C44 1.428(8) . ?
O11 C57 1.396(11) . ?
O11 C59 1.448(9) . ?
O12 C58 1.294(9) . ?
N1 C7 1.297(9) . ?
N1 C8 1.466(9) . ?
N2 C22 1.311(9) . ?
N2 C23 1.411(8) . ?
N3 C37 1.292(9) . ?
N3 C36 1.419(9) . ?
N4 C52 1.297(9) . ?
N4 C51 1.414(9) . ?
C1 C6 1.388(10) . ?
C1 C2 1.417(10) . ?
C2 C3 1.371(11) . ?
C3 C4 1.372(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.355(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.441(10) . ?
C7 H7 0.9300 . ?
C8 C13 1.386(10) . ?
C8 C9 1.415(10) . ?
C9 C10 1.368(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.371(11) . ?
C10 C14 1.545(10) . ?
C11 C12 1.378(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.374(10) . ?
C12 H12 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.400(10) . ?
C16 C21 1.414(9) . ?
C17 C18 1.381(10) . ?
C18 C19 1.386(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.378(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.401(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.436(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.415(9) . ?
C23 C28 1.430(10) . ?
C24 C25 1.351(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.378(11) . ?
C25 C29 1.502(9) . ?
C26 C27 1.411(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.378(9) . ?
C27 H27 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.386(10) . ?
C31 C36 1.407(10) . ?
C32 C33 1.403(10) . ?
C32 H32 0.9300 . ?
C33 C34 1.387(11) . ?
C33 H33 0.9300 . ?
C34 C35 1.374(10) . ?
C34 C45 1.496(10) . ?
C35 C36 1.399(10) . ?
C35 H35 0.9300 . ?
C37 C38 1.445(10) . ?
C37 H37 0.9300 . ?
C38 C43 1.402(9) . ?
C38 C39 1.410(10) . ?
C39 C40 1.409(10) . ?
C40 C41 1.368(10) . ?
C41 C42 1.386(10) . ?
C41 H41 0.9300 . ?
C42 C43 1.376(10) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.381(10) . ?
C46 C51 1.411(10) . ?
C47 C48 1.378(10) . ?
C47 H47 0.9300 . ?
C48 C49 1.382(10) . ?
C48 H48 0.9300 . ?
C49 C50 1.405(10) . ?
C49 C60 1.523(11) . ?
C50 C51 1.391(10) . ?
C50 H50 0.9300 . ?
C52 C53 1.416(10) . ?
C52 H52 0.9300 . ?
C53 C54 1.421(10) . ?
C53 C58 1.426(11) . ?
C54 C55 1.380(11) . ?
C54 H54 0.9300 . ?
C55 C56 1.409(12) . ?
C55 H55 0.9300 . ?
C56 C57 1.347(12) . ?
C56 H56 0.9300 . ?
C57 C58 1.433(11) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 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
O12 Ni1 O6 105.1(2) . . ?
O12 Ni1 O4 100.2(2) . . ?
O6 Ni1 O4 114.6(2) . . ?
O12 Ni1 N4 93.5(2) . . ?
O6 Ni1 N4 124.1(2) . . ?
O4 Ni1 N4 113.0(2) . . ?
O12 Ni1 O5 171.6(2) . . ?
O6 Ni1 O5 80.22(17) . . ?
O4 Ni1 O5 83.12(18) . . ?
N4 Ni1 O5 78.1(2) . . ?
O1 Ni2 N2 174.4(2) . . ?
O1 Ni2 O8 87.70(19) . . ?
N2 Ni2 O8 90.5(2) . . ?
O1 Ni2 O4 98.71(19) . . ?
N2 Ni2 O4 82.5(2) . . ?
O8 Ni2 O4 170.7(2) . . ?
O1 Ni2 N1 88.3(2) . . ?
N2 Ni2 N1 97.1(2) . . ?
O8 Ni2 N1 96.3(2) . . ?
O4 Ni2 N1 90.7(2) . . ?
O1 Ni2 O5 76.93(18) . . ?
N2 Ni2 O5 97.8(2) . . ?
O8 Ni2 O5 91.05(18) . . ?
O4 Ni2 O5 83.86(18) . . ?
N1 Ni2 O5 163.3(2) . . ?
N3 Ni3 O1 173.0(2) . . ?
N3 Ni3 O7 93.0(2) . . ?
O1 Ni3 O7 85.3(2) . . ?
N3 Ni3 O5 108.1(2) . . ?
O1 Ni3 O5 78.89(19) . . ?
O7 Ni3 O5 96.92(18) . . ?
N3 Ni3 O6 81.9(2) . . ?
O1 Ni3 O6 100.1(2) . . ?
O7 Ni3 O6 174.3(2) . . ?
O5 Ni3 O6 82.40(18) . . ?
N3 Ni3 O2 97.3(2) . . ?
O1 Ni3 O2 75.99(19) . . ?
O7 Ni3 O2 91.2(2) . . ?
O5 Ni3 O2 152.86(19) . . ?
O6 Ni3 O2 92.0(2) . . ?
O7 Ni4 O8 106.90(19) . . ?
O7 Ni4 Cl1 131.03(15) . . ?
O8 Ni4 Cl1 110.59(15) . . ?
O7 Ni4 O9 113.0(2) . . ?
O8 Ni4 O9 74.95(18) . . ?
Cl1 Ni4 O9 106.34(16) . . ?
O7 Ni4 O10 72.65(18) . . ?
O8 Ni4 O10 148.1(2) . . ?
Cl1 Ni4 O10 90.36(15) . . ?
O9 Ni4 O10 76.15(18) . . ?
C1 O1 Ni2 129.0(4) . . ?
C1 O1 Ni3 117.5(4) . . ?
Ni2 O1 Ni3 106.5(2) . . ?
C2 O2 C15 117.6(6) . . ?
C2 O2 Ni3 112.2(4) . . ?
C15 O2 Ni3 126.3(5) . . ?
C13 O3 H3A 115.4 . . ?
C28 O4 Ni1 115.9(4) . . ?
C28 O4 Ni2 110.0(4) . . ?
Ni1 O4 Ni2 102.0(2) . . ?
C46 O5 Ni3 127.2(4) . . ?
C46 O5 Ni2 127.8(4) . . ?
Ni3 O5 Ni2 97.7(2) . . ?
C46 O5 Ni1 109.6(4) . . ?
Ni3 O5 Ni1 93.44(18) . . ?
Ni2 O5 Ni1 90.08(17) . . ?
C31 O6 Ni1 115.2(4) . . ?
C31 O6 Ni3 110.0(4) . . ?
Ni1 O6 Ni3 101.4(2) . . ?
C39 O7 Ni4 122.6(4) . . ?
C39 O7 Ni3 124.5(4) . . ?
Ni4 O7 Ni3 112.6(2) . . ?
C16 O8 Ni4 117.7(4) . . ?
C16 O8 Ni2 124.5(4) . . ?
Ni4 O8 Ni2 111.0(2) . . ?
C17 O9 C30 117.1(6) . . ?
C17 O9 Ni4 111.7(4) . . ?
C30 O9 Ni4 127.6(5) . . ?
C40 O10 C44 116.6(6) . . ?
C40 O10 Ni4 109.9(4) . . ?
C44 O10 Ni4 132.9(5) . . ?
C57 O11 C59 116.6(8) . . ?
C58 O12 Ni1 123.4(5) . . ?
C7 N1 C8 115.2(7) . . ?
C7 N1 Ni2 123.4(5) . . ?
C8 N1 Ni2 119.2(5) . . ?
C22 N2 C23 122.1(6) . . ?
C22 N2 Ni2 126.7(5) . . ?
C23 N2 Ni2 110.7(5) . . ?
C37 N3 C36 121.3(6) . . ?
C37 N3 Ni3 124.6(5) . . ?
C36 N3 Ni3 114.1(5) . . ?
C52 N4 C51 122.3(7) . . ?
C52 N4 Ni1 121.5(5) . . ?
C51 N4 Ni1 115.8(5) . . ?
O1 C1 C6 123.3(6) . . ?
O1 C1 C2 117.8(7) . . ?
C6 C1 C2 118.8(7) . . ?
C3 C2 O2 125.4(7) . . ?
C3 C2 C1 121.2(8) . . ?
O2 C2 C1 113.4(7) . . ?
C2 C3 C4 118.8(8) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 120.9(9) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.9(9) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 118.3(7) . . ?
C1 C6 C7 123.2(7) . . ?
C5 C6 C7 118.5(7) . . ?
N1 C7 C6 128.7(7) . . ?
N1 C7 H7 115.7 . . ?
C6 C7 H7 115.7 . . ?
C13 C8 C9 118.6(7) . . ?
C13 C8 N1 119.2(7) . . ?
C9 C8 N1 122.0(7) . . ?
C10 C9 C8 121.6(8) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 117.1(8) . . ?
C9 C10 C14 120.3(8) . . ?
C11 C10 C14 122.5(7) . . ?
C10 C11 C12 123.7(8) . . ?
C10 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C13 C12 C11 118.5(8) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C8 120.5(7) . . ?
C12 C13 O3 117.7(7) . . ?
C8 C13 O3 121.8(7) . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 C17 117.5(6) . . ?
O8 C16 C21 123.7(6) . . ?
C17 C16 C21 118.8(7) . . ?
C18 C17 O9 125.2(7) . . ?
C18 C17 C16 120.8(7) . . ?
O9 C17 C16 114.0(7) . . ?
C17 C18 C19 120.7(7) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 119.3(8) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 121.5(7) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 118.9(6) . . ?
C20 C21 C22 115.6(7) . . ?
C16 C21 C22 125.5(7) . . ?
N2 C22 C21 124.6(7) . . ?
N2 C22 H22 117.7 . . ?
C21 C22 H22 117.7 . . ?
N2 C23 C24 126.0(7) . . ?
N2 C23 C28 115.0(6) . . ?
C24 C23 C28 118.8(6) . . ?
C25 C24 C23 122.4(7) . . ?
C25 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C24 C25 C26 117.3(7) . . ?
C24 C25 C29 120.9(8) . . ?
C26 C25 C29 121.7(7) . . ?
C25 C26 C27 124.1(7) . . ?
C25 C26 H26 117.9 . . ?
C27 C26 H26 117.9 . . ?
C28 C27 C26 118.0(7) . . ?
C28 C27 H27 121.0 . . ?
C26 C27 H27 121.0 . . ?
O4 C28 C27 122.9(7) . . ?
O4 C28 C23 117.8(6) . . ?
C27 C28 C23 119.3(7) . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O9 C30 H30A 109.5 . . ?
O9 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O9 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O6 C31 C32 121.1(7) . . ?
O6 C31 C36 119.9(7) . . ?
C32 C31 C36 119.0(7) . . ?
C31 C32 C33 119.0(7) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C34 C33 C32 122.9(8) . . ?
C34 C33 H33 118.5 . . ?
C32 C33 H33 118.5 . . ?
C35 C34 C33 117.0(8) . . ?
C35 C34 C45 121.1(7) . . ?
C33 C34 C45 121.9(8) . . ?
C34 C35 C36 122.2(7) . . ?
C34 C35 H35 118.9 . . ?
C36 C35 H35 118.9 . . ?
C35 C36 C31 119.7(7) . . ?
C35 C36 N3 126.2(7) . . ?
C31 C36 N3 114.1(7) . . ?
N3 C37 C38 127.5(7) . . ?
N3 C37 H37 116.3 . . ?
C38 C37 H37 116.3 . . ?
C43 C38 C39 118.3(7) . . ?
C43 C38 C37 115.9(7) . . ?
C39 C38 C37 125.8(7) . . ?
O7 C39 C40 119.4(7) . . ?
O7 C39 C38 123.5(7) . . ?
C40 C39 C38 117.0(7) . . ?
C41 C40 O10 123.8(7) . . ?
C41 C40 C39 123.4(8) . . ?
O10 C40 C39 112.9(6) . . ?
C40 C41 C42 119.0(8) . . ?
C40 C41 H41 120.5 . . ?
C42 C41 H41 120.5 . . ?
C43 C42 C41 119.1(7) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C42 C43 C38 122.6(8) . . ?
C42 C43 H43 118.7 . . ?
C38 C43 H43 118.7 . . ?
O10 C44 H44A 109.5 . . ?
O10 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O10 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C34 C45 H45A 109.5 . . ?
C34 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C34 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O5 C46 C47 121.9(7) . . ?
O5 C46 C51 118.6(6) . . ?
C47 C46 C51 119.6(7) . . ?
C48 C47 C46 120.9(7) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C47 C48 C49 121.2(7) . . ?
C47 C48 H48 119.4 . . ?
C49 C48 H48 119.4 . . ?
C48 C49 C50 118.0(8) . . ?
C48 C49 C60 121.6(7) . . ?
C50 C49 C60 120.4(8) . . ?
C51 C50 C49 121.8(8) . . ?
C51 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C50 C51 C46 118.4(7) . . ?
C50 C51 N4 124.7(7) . . ?
C46 C51 N4 116.9(7) . . ?
N4 C52 C53 127.1(8) . . ?
N4 C52 H52 116.4 . . ?
C53 C52 H52 116.4 . . ?
C52 C53 C54 115.8(8) . . ?
C52 C53 C58 124.6(7) . . ?
C54 C53 C58 119.4(7) . . ?
C55 C54 C53 121.4(9) . . ?
C55 C54 H54 119.3 . . ?
C53 C54 H54 119.3 . . ?
C54 C55 C56 119.0(8) . . ?
C54 C55 H55 120.5 . . ?
C56 C55 H55 120.5 . . ?
C57 C56 C55 120.6(9) . . ?
C57 C56 H56 119.7 . . ?
C55 C56 H56 119.7 . . ?
C56 C57 O11 125.0(9) . . ?
C56 C57 C58 122.9(10) . . ?
O11 C57 C58 112.2(8) . . ?
O12 C58 C53 125.1(7) . . ?
O12 C58 C57 118.4(8) . . ?
C53 C58 C57 116.5(8) . . ?
O11 C59 H59A 109.5 . . ?
O11 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
O11 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C49 C60 H60A 109.5 . . ?
C49 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C49 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni2 O1 C1 C6 20.6(10) . . . . ?
Ni3 O1 C1 C6 167.3(5) . . . . ?
Ni2 O1 C1 C2 -162.7(5) . . . . ?
Ni3 O1 C1 C2 -16.1(8) . . . . ?
C15 O2 C2 C3 -14.0(12) . . . . ?
Ni3 O2 C2 C3 -173.0(7) . . . . ?
C15 O2 C2 C1 168.9(7) . . . . ?
Ni3 O2 C2 C1 10.0(8) . . . . ?
O1 C1 C2 C3 -174.4(7) . . . . ?
C6 C1 C2 C3 2.5(12) . . . . ?
O1 C1 C2 O2 2.8(10) . . . . ?
C6 C1 C2 O2 179.6(6) . . . . ?
O2 C2 C3 C4 -179.3(8) . . . . ?
C1 C2 C3 C4 -2.5(13) . . . . ?
C2 C3 C4 C5 0.9(14) . . . . ?
C3 C4 C5 C6 0.6(14) . . . . ?
O1 C1 C6 C5 175.7(7) . . . . ?
C2 C1 C6 C5 -0.9(11) . . . . ?
O1 C1 C6 C7 -5.0(12) . . . . ?
C2 C1 C6 C7 178.4(7) . . . . ?
C4 C5 C6 C1 -0.6(13) . . . . ?
C4 C5 C6 C7 -179.9(8) . . . . ?
C8 N1 C7 C6 -172.4(7) . . . . ?
Ni2 N1 C7 C6 -9.5(12) . . . . ?
C1 C6 C7 N1 0.0(13) . . . . ?
C5 C6 C7 N1 179.4(8) . . . . ?
C7 N1 C8 C13 -126.2(8) . . . . ?
Ni2 N1 C8 C13 70.1(9) . . . . ?
C7 N1 C8 C9 59.9(10) . . . . ?
Ni2 N1 C8 C9 -103.7(8) . . . . ?
C13 C8 C9 C10 0.6(13) . . . . ?
N1 C8 C9 C10 174.5(8) . . . . ?
C8 C9 C10 C11 0.5(14) . . . . ?
C8 C9 C10 C14 -176.4(8) . . . . ?
C9 C10 C11 C12 -0.2(15) . . . . ?
C14 C10 C11 C12 176.7(9) . . . . ?
C10 C11 C12 C13 -1.2(15) . . . . ?
C11 C12 C13 C8 2.3(14) . . . . ?
C11 C12 C13 O3 -178.5(8) . . . . ?
C9 C8 C13 C12 -2.0(13) . . . . ?
N1 C8 C13 C12 -176.1(8) . . . . ?
C9 C8 C13 O3 178.8(7) . . . . ?
N1 C8 C13 O3 4.8(12) . . . . ?
Ni4 O8 C16 C17 16.3(9) . . . . ?
Ni2 O8 C16 C17 164.7(5) . . . . ?
Ni4 O8 C16 C21 -165.2(5) . . . . ?
Ni2 O8 C16 C21 -16.8(9) . . . . ?
C30 O9 C17 C18 -36.1(11) . . . . ?
Ni4 O9 C17 C18 163.7(7) . . . . ?
C30 O9 C17 C16 146.5(7) . . . . ?
Ni4 O9 C17 C16 -13.7(8) . . . . ?
O8 C16 C17 C18 -177.9(7) . . . . ?
C21 C16 C17 C18 3.5(11) . . . . ?
O8 C16 C17 O9 -0.3(10) . . . . ?
C21 C16 C17 O9 -178.9(6) . . . . ?
O9 C17 C18 C19 -178.5(7) . . . . ?
C16 C17 C18 C19 -1.2(12) . . . . ?
C17 C18 C19 C20 -1.5(12) . . . . ?
C18 C19 C20 C21 1.9(12) . . . . ?
C19 C20 C21 C16 0.5(11) . . . . ?
C19 C20 C21 C22 180.0(7) . . . . ?
O8 C16 C21 C20 178.4(7) . . . . ?
C17 C16 C21 C20 -3.2(11) . . . . ?
O8 C16 C21 C22 -1.1(11) . . . . ?
C17 C16 C21 C22 177.4(7) . . . . ?
C23 N2 C22 C21 -179.9(7) . . . . ?
Ni2 N2 C22 C21 8.9(11) . . . . ?
C20 C21 C22 N2 -173.7(7) . . . . ?
C16 C21 C22 N2 5.7(12) . . . . ?
C22 N2 C23 C24 27.1(11) . . . . ?
Ni2 N2 C23 C24 -160.4(6) . . . . ?
C22 N2 C23 C28 -157.9(7) . . . . ?
Ni2 N2 C23 C28 14.6(8) . . . . ?
N2 C23 C24 C25 178.9(8) . . . . ?
C28 C23 C24 C25 4.1(12) . . . . ?
C23 C24 C25 C26 -1.8(13) . . . . ?
C23 C24 C25 C29 -178.5(8) . . . . ?
C24 C25 C26 C27 0.3(13) . . . . ?
C29 C25 C26 C27 177.1(8) . . . . ?
C25 C26 C27 C28 -1.3(13) . . . . ?
Ni1 O4 C28 C27 -78.8(8) . . . . ?
Ni2 O4 C28 C27 166.2(6) . . . . ?
Ni1 O4 C28 C23 101.3(6) . . . . ?
Ni2 O4 C28 C23 -13.7(8) . . . . ?
C26 C27 C28 O4 -176.5(7) . . . . ?
C26 C27 C28 C23 3.5(11) . . . . ?
N2 C23 C28 O4 -0.3(10) . . . . ?
C24 C23 C28 O4 175.1(7) . . . . ?
N2 C23 C28 C27 179.8(7) . . . . ?
C24 C23 C28 C27 -4.9(11) . . . . ?
Ni1 O6 C31 C32 63.4(8) . . . . ?
Ni3 O6 C31 C32 177.2(6) . . . . ?
Ni1 O6 C31 C36 -115.9(6) . . . . ?
Ni3 O6 C31 C36 -2.0(8) . . . . ?
O6 C31 C32 C33 179.4(7) . . . . ?
C36 C31 C32 C33 -1.3(11) . . . . ?
C31 C32 C33 C34 -0.5(13) . . . . ?
C32 C33 C34 C35 -0.2(13) . . . . ?
C32 C33 C34 C45 -178.7(8) . . . . ?
C33 C34 C35 C36 2.7(12) . . . . ?
C45 C34 C35 C36 -178.8(7) . . . . ?
C34 C35 C36 C31 -4.5(12) . . . . ?
C34 C35 C36 N3 174.9(7) . . . . ?
O6 C31 C36 C35 -177.0(6) . . . . ?
C32 C31 C36 C35 3.7(11) . . . . ?
O6 C31 C36 N3 3.5(10) . . . . ?
C32 C31 C36 N3 -175.7(7) . . . . ?
C37 N3 C36 C35 -0.2(11) . . . . ?
Ni3 N3 C36 C35 177.4(6) . . . . ?
C37 N3 C36 C31 179.2(7) . . . . ?
Ni3 N3 C36 C31 -3.2(8) . . . . ?
C36 N3 C37 C38 175.2(7) . . . . ?
Ni3 N3 C37 C38 -2.1(11) . . . . ?
N3 C37 C38 C43 -175.2(7) . . . . ?
N3 C37 C38 C39 2.2(13) . . . . ?
Ni4 O7 C39 C40 -10.5(9) . . . . ?
Ni3 O7 C39 C40 162.3(5) . . . . ?
Ni4 O7 C39 C38 172.9(5) . . . . ?
Ni3 O7 C39 C38 -14.2(10) . . . . ?
C43 C38 C39 O7 -175.7(7) . . . . ?
C37 C38 C39 O7 7.0(12) . . . . ?
C43 C38 C39 C40 7.7(11) . . . . ?
C37 C38 C39 C40 -169.6(7) . . . . ?
C44 O10 C40 C41 20.5(11) . . . . ?
Ni4 O10 C40 C41 -167.3(6) . . . . ?
C44 O10 C40 C39 -158.9(7) . . . . ?
Ni4 O10 C40 C39 13.3(8) . . . . ?
O7 C39 C40 C41 176.4(7) . . . . ?
C38 C39 C40 C41 -6.8(12) . . . . ?
O7 C39 C40 O10 -4.2(10) . . . . ?
C38 C39 C40 O10 172.6(6) . . . . ?
O10 C40 C41 C42 -178.6(7) . . . . ?
C39 C40 C41 C42 0.7(12) . . . . ?
C40 C41 C42 C43 4.4(12) . . . . ?
C41 C42 C43 C38 -3.3(12) . . . . ?
C39 C38 C43 C42 -3.0(11) . . . . ?
C37 C38 C43 C42 174.6(7) . . . . ?
Ni3 O5 C46 C47 60.8(8) . . . . ?
Ni2 O5 C46 C47 -82.5(7) . . . . ?
Ni1 O5 C46 C47 171.3(5) . . . . ?
Ni3 O5 C46 C51 -117.5(6) . . . . ?
Ni2 O5 C46 C51 99.2(7) . . . . ?
Ni1 O5 C46 C51 -7.0(7) . . . . ?
O5 C46 C47 C48 178.2(6) . . . . ?
C51 C46 C47 C48 -3.5(10) . . . . ?
C46 C47 C48 C49 2.8(11) . . . . ?
C47 C48 C49 C50 -0.4(11) . . . . ?
C47 C48 C49 C60 176.9(7) . . . . ?
C48 C49 C50 C51 -1.2(11) . . . . ?
C60 C49 C50 C51 -178.6(7) . . . . ?
C49 C50 C51 C46 0.5(11) . . . . ?
C49 C50 C51 N4 -179.4(6) . . . . ?
O5 C46 C51 C50 -179.8(6) . . . . ?
C47 C46 C51 C50 1.9(10) . . . . ?
O5 C46 C51 N4 0.1(9) . . . . ?
C47 C46 C51 N4 -178.2(6) . . . . ?
C52 N4 C51 C50 14.2(11) . . . . ?
Ni1 N4 C51 C50 -172.2(5) . . . . ?
C52 N4 C51 C46 -165.7(6) . . . . ?
Ni1 N4 C51 C46 7.9(8) . . . . ?
C51 N4 C52 C53 178.0(7) . . . . ?
Ni1 N4 C52 C53 4.7(10) . . . . ?
N4 C52 C53 C54 -172.0(7) . . . . ?
N4 C52 C53 C58 2.9(12) . . . . ?
C52 C53 C54 C55 174.8(7) . . . . ?
C58 C53 C54 C55 -0.4(11) . . . . ?
C53 C54 C55 C56 -1.9(12) . . . . ?
C54 C55 C56 C57 1.2(13) . . . . ?
C55 C56 C57 O11 -179.1(8) . . . . ?
C55 C56 C57 C58 2.0(14) . . . . ?
C59 O11 C57 C56 10.5(13) . . . . ?
C59 O11 C57 C58 -170.5(8) . . . . ?
Ni1 O12 C58 C53 -24.1(10) . . . . ?
Ni1 O12 C58 C57 154.9(6) . . . . ?
C52 C53 C58 O12 7.6(12) . . . . ?
C54 C53 C58 O12 -177.6(7) . . . . ?
C52 C53 C58 C57 -171.5(7) . . . . ?
C54 C53 C58 C57 3.3(11) . . . . ?
C56 C57 C58 O12 176.7(8) . . . . ?
O11 C57 C58 O12 -2.4(11) . . . . ?
C56 C57 C58 C53 -4.2(12) . . . . ?
O11 C57 C58 C53 176.8(7) . . . . ?

_refine_diff_density_max         0.668
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.114



####################################################################### 
# 
# 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_mr101
_database_code_depnum_ccdc_archive 'CCDC 2092320'
loop_
_audit_author_name
_audit_author_address
'Maria Francis'
;IISER Tirupati
India
;
_audit_update_record             
;
2021-06-25 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
;
_audit_creation_date             2020-12-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H16 O2'
_chemical_formula_sum            'C16 H16 O2'
_chemical_formula_weight         240.29
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.421(3)
_cell_length_b                   15.783(4)
_cell_length_c                   7.4458(16)
_cell_angle_alpha                90
_cell_angle_beta                 93.411(6)
_cell_angle_gamma                90
_cell_volume                     1339.8(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    297.49
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      3.14
_shelx_estimated_absorpt_T_max   0.988
_shelx_estimated_absorpt_T_min   0.985
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6339
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1119 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.8503.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            18974
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.226
_diffrn_reflns_theta_min         3.434
_diffrn_ambient_temperature      297.49
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2031
_reflns_number_total             2773
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.34(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0807
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²+1.0589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2098
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C11(H11), C4(H4), C2(H2), C13(H13), C3(H3), C12(H12)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.45806(17) 0.41579(12) 0.1584(3) 0.0612(6) Uani 1 1 d . . . . .
O1 O 0.46126(19) 0.29254(12) 0.3066(3) 0.0687(7) Uani 1 1 d . . . . .
C6 C 0.2836(2) 0.48747(15) 0.3336(3) 0.0471(6) Uani 1 1 d . . . . .
C7 C 0.3197(2) 0.39787(15) 0.3753(3) 0.0475(7) Uani 1 1 d . . . . .
C15 C 0.4198(2) 0.36243(16) 0.2791(4) 0.0507(7) Uani 1 1 d . . . . .
C5 C 0.2027(3) 0.5057(2) 0.1935(4) 0.0596(8) Uani 1 1 d . . . . .
H5 H 0.165396 0.461989 0.128763 0.072 Uiso 1 1 calc R U . . .
C9 C 0.2294(3) 0.32925(17) 0.4169(4) 0.0590(8) Uani 1 1 d . . . . .
H9 H 0.245980 0.272232 0.372863 0.071 Uiso 1 1 calc R U . . .
C10 C 0.1043(3) 0.35122(19) 0.4237(5) 0.0643(8) Uani 1 1 d . . . . .
C1 C 0.3377(3) 0.55400(18) 0.4274(5) 0.0641(8) Uani 1 1 d . . . . .
H1 H 0.391820 0.542582 0.522639 0.077 Uiso 1 1 calc R U . . .
C8 C 0.3130(3) 0.36201(19) 0.5666(4) 0.0621(8) Uani 1 1 d . . . . .
H8 H 0.376441 0.323541 0.607559 0.075 Uiso 1 1 calc R U . . .
C11 C 0.0691(3) 0.4034(2) 0.5513(5) 0.0718(9) Uani 1 1 d . . . . .
H11 H -0.008983 0.420395 0.547406 0.086 Uiso 1 1 calc R U . . .
C4 C 0.1771(3) 0.5901(2) 0.1495(5) 0.0776(11) Uani 1 1 d . . . . .
H4 H 0.122011 0.602481 0.056113 0.093 Uiso 1 1 calc R U . . .
C2 C 0.3123(3) 0.6369(2) 0.3815(6) 0.0802(11) Uani 1 1 d . . . . .
H2 H 0.349738 0.680807 0.445289 0.096 Uiso 1 1 calc R U . . .
C16 C 0.5544(3) 0.3852(2) 0.0570(5) 0.0744(10) Uani 1 1 d . . . . .
H16A H 0.575391 0.427850 -0.027273 0.112 Uiso 1 1 calc R U . . .
H16B H 0.530725 0.334626 -0.006780 0.112 Uiso 1 1 calc R U . . .
H16C H 0.620760 0.373051 0.138146 0.112 Uiso 1 1 calc R U . . .
C13 C 0.2605(4) 0.4126(2) 0.7070(5) 0.0747(10) Uani 1 1 d . . . . .
H13 H 0.306988 0.430021 0.806977 0.090 Uiso 1 1 calc R U . . .
C14 C 0.0226(3) 0.3116(3) 0.2847(7) 0.0973(13) Uani 1 1 d . . . . .
H14A H 0.046078 0.326553 0.167125 0.146 Uiso 1 1 calc R U . . .
H14B H -0.055635 0.331688 0.299102 0.146 Uiso 1 1 calc R U . . .
H14C H 0.024688 0.251161 0.298281 0.146 Uiso 1 1 calc R U . . .
C3 C 0.2328(3) 0.6548(2) 0.2433(6) 0.0848(12) Uani 1 1 d . . . . .
H3 H 0.216325 0.710856 0.212510 0.102 Uiso 1 1 calc R U . . .
C12 C 0.1473(4) 0.4338(2) 0.6930(5) 0.0795(11) Uani 1 1 d . . . . .
H12 H 0.118350 0.469737 0.778883 0.095 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
O2 C15 1.324(3) . ?
O2 C16 1.453(3) . ?
O1 C15 1.213(3) . ?
C6 C7 1.500(3) . ?
C6 C5 1.382(4) . ?
C6 C1 1.386(4) . ?
C7 C15 1.493(4) . ?
C7 C9 1.539(4) . ?
C7 C8 1.539(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.399(4) . ?
C9 H9 0.9800 . ?
C9 C10 1.474(4) . ?
C9 C8 1.514(4) . ?
C10 C11 1.338(5) . ?
C10 C14 1.489(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.379(4) . ?
C8 H8 0.9800 . ?
C8 C13 1.471(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.424(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.372(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.361(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C13 H13 0.9300 . ?
C13 C12 1.334(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C3 H3 0.9300 . ?
C12 H12 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 O2 C16 115.6(2) . . ?
C5 C6 C7 121.0(2) . . ?
C5 C6 C1 118.7(3) . . ?
C1 C6 C7 120.1(2) . . ?
C6 C7 C9 121.7(2) . . ?
C6 C7 C8 120.7(2) . . ?
C15 C7 C6 117.6(2) . . ?
C15 C7 C9 112.0(2) . . ?
C15 C7 C8 112.8(2) . . ?
C8 C7 C9 58.94(19) . . ?
O2 C15 C7 112.3(2) . . ?
O1 C15 O2 123.5(3) . . ?
O1 C15 C7 124.2(2) . . ?
C6 C5 H5 120.1 . . ?
C6 C5 C4 119.7(3) . . ?
C4 C5 H5 120.1 . . ?
C7 C9 H9 115.7 . . ?
C10 C9 C7 120.2(2) . . ?
C10 C9 H9 115.7 . . ?
C10 C9 C8 117.7(3) . . ?
C8 C9 C7 60.51(18) . . ?
C8 C9 H9 115.7 . . ?
C9 C10 C14 116.5(3) . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 C14 123.3(3) . . ?
C6 C1 H1 119.6 . . ?
C2 C1 C6 120.9(3) . . ?
C2 C1 H1 119.6 . . ?
C7 C8 H8 116.1 . . ?
C9 C8 C7 60.55(18) . . ?
C9 C8 H8 116.1 . . ?
C13 C8 C7 120.2(2) . . ?
C13 C8 C9 116.3(3) . . ?
C13 C8 H8 116.1 . . ?
C10 C11 H11 118.9 . . ?
C10 C11 C12 122.1(3) . . ?
C12 C11 H11 118.9 . . ?
C5 C4 H4 119.8 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4 119.8 . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 H2 119.8 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C13 H13 119.5 . . ?
C12 C13 C8 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.0 . . ?
C11 C12 H12 118.8 . . ?
C13 C12 C11 122.4(3) . . ?
C13 C12 H12 118.8 . . ?

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
C6 C7 C15 O2 -4.2(3) . . . . ?
C6 C7 C15 O1 176.3(3) . . . . ?
C6 C7 C9 C10 -2.4(4) . . . . ?
C6 C7 C9 C8 -109.1(3) . . . . ?
C6 C7 C8 C9 110.9(3) . . . . ?
C6 C7 C8 C13 5.8(4) . . . . ?
C6 C5 C4 C3 0.7(4) . . . . ?
C6 C1 C2 C3 0.4(5) . . . . ?
C7 C6 C5 C4 -175.3(2) . . . . ?
C7 C6 C1 C2 174.8(3) . . . . ?
C7 C9 C10 C11 -65.5(4) . . . . ?
C7 C9 C10 C14 115.3(3) . . . . ?
C7 C9 C8 C13 111.4(3) . . . . ?
C7 C8 C13 C12 64.2(4) . . . . ?
C15 C7 C9 C10 -149.1(3) . . . . ?
C15 C7 C9 C8 104.2(3) . . . . ?
C15 C7 C8 C9 -102.7(2) . . . . ?
C15 C7 C8 C13 152.2(3) . . . . ?
C5 C6 C7 C15 88.0(3) . . . . ?
C5 C6 C7 C9 -56.9(4) . . . . ?
C5 C6 C7 C8 -127.1(3) . . . . ?
C5 C6 C1 C2 -0.5(4) . . . . ?
C5 C4 C3 C2 -0.9(5) . . . . ?
C9 C7 C15 O2 144.0(2) . . . . ?
C9 C7 C15 O1 -35.5(4) . . . . ?
C9 C7 C8 C13 -105.0(3) . . . . ?
C9 C10 C11 C12 -5.5(5) . . . . ?
C9 C8 C13 C12 -5.5(4) . . . . ?
C10 C9 C8 C7 -110.9(3) . . . . ?
C10 C9 C8 C13 0.5(4) . . . . ?
C10 C11 C12 C13 0.4(5) . . . . ?
C1 C6 C7 C15 -87.2(3) . . . . ?
C1 C6 C7 C9 127.9(3) . . . . ?
C1 C6 C7 C8 57.7(4) . . . . ?
C1 C6 C5 C4 0.0(4) . . . . ?
C1 C2 C3 C4 0.3(5) . . . . ?
C8 C7 C15 O2 -151.7(2) . . . . ?
C8 C7 C15 O1 28.8(4) . . . . ?
C8 C7 C9 C10 106.7(3) . . . . ?
C8 C9 C10 C11 4.8(4) . . . . ?
C8 C9 C10 C14 -174.5(3) . . . . ?
C8 C13 C12 C11 5.3(5) . . . . ?
C16 O2 C15 O1 0.4(4) . . . . ?
C16 O2 C15 C7 -179.1(3) . . . . ?
C14 C10 C11 C12 173.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2006271'
loop_
_audit_author_name
_audit_author_address
'saroj kumar kushvaha'
;Indian Institute of Technology Madras
India
;
_audit_update_record             
;
2020-10-14 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H61 Cl2 N5 Ni4 O13, C H4 O'

_chemical_formula_sum            'C64 H65 Cl2 N5 Ni4 O14'
_chemical_formula_weight         1429.91

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'
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                   14.070(7)
_cell_length_b                   14.216(8)
_cell_length_c                   19.039(11)
_cell_angle_alpha                76.64(3)
_cell_angle_beta                 68.85(2)
_cell_angle_gamma                63.449(18)
_cell_volume                     3166(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)

_cell_measurement_reflns_used    9673
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      26.40

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            yellow

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_F_000             1476
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.324
_shelx_estimated_absorpt_T_min   0.890
_shelx_estimated_absorpt_T_max   0.925

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_process_details   SADABS



_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'


_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            118876
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.897
_diffrn_reflns_theta_max         26.451
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12961
_reflns_number_gt                9131
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0680P)²+6.5551P] 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         12961
_refine_ls_number_parameters     809
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.049
_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 0.83703(4) 0.48914(4) 0.71874(3) 0.02937(14) Uani 1 1 d . . . . .
Ni2 Ni 0.58318(4) 0.52435(4) 0.74448(3) 0.02941(15) Uani 1 1 d . . . . .
Ni3 Ni 0.52448(5) 0.77736(5) 0.65501(3) 0.03203(15) Uani 1 1 d . . . . .
Ni4 Ni 0.51954(4) 0.86049(5) 0.80101(3) 0.03235(15) Uani 1 1 d . . . . .
Cl1 Cl 0.70355(8) 0.59099(9) 0.64123(6) 0.0331(2) Uani 1 1 d . . . . .
Cl2 Cl 0.47004(9) 0.71621(9) 0.78605(6) 0.0346(2) Uani 1 1 d . . . . .
C1 C 0.9924(3) 0.5887(3) 0.6506(2) 0.0323(10) Uani 1 1 d . . . . .
C2 C 1.0810(4) 0.6165(4) 0.6061(3) 0.0375(11) Uani 1 1 d . . . . .
H2 H 1.139200 0.571568 0.568982 0.045 Uiso 1 1 calc R U . . .
C3 C 1.0858(4) 0.7074(4) 0.6150(3) 0.0416(12) Uani 1 1 d . . . . .
C4 C 0.9999(4) 0.7716(4) 0.6709(3) 0.0469(13) Uani 1 1 d . . . . .
H4 H 1.001494 0.835064 0.677449 0.056 Uiso 1 1 calc R U . . .
C5 C 0.9130(4) 0.7443(4) 0.7166(3) 0.0426(12) Uani 1 1 d . . . . .
H5 H 0.856376 0.788197 0.754964 0.051 Uiso 1 1 calc R U . . .
C6 C 0.9079(4) 0.6530(4) 0.7069(3) 0.0339(10) Uani 1 1 d . . . . .
C7 C 1.0363(3) 0.4431(3) 0.5870(2) 0.0320(10) Uani 1 1 d . . . . .
H7 H 1.092073 0.463819 0.550610 0.038 Uiso 1 1 calc R U . . .
C8 C 1.0283(3) 0.3522(3) 0.5729(2) 0.0317(10) Uani 1 1 d . . . . .
C9 C 0.9507(3) 0.3103(3) 0.6216(2) 0.0312(10) Uani 1 1 d . . . . .
C10 C 0.9606(4) 0.2144(4) 0.6023(3) 0.0380(11) Uani 1 1 d . . . . .
C11 C 1.0374(4) 0.1680(4) 0.5371(3) 0.0424(12) Uani 1 1 d . . . . .
H11 H 1.040710 0.104870 0.525611 0.051 Uiso 1 1 calc R U . . .
C12 C 1.1099(4) 0.2130(4) 0.4881(3) 0.0444(12) Uani 1 1 d . . . . .
H12 H 1.160948 0.181864 0.442736 0.053 Uiso 1 1 calc R U . . .
C13 C 1.1067(4) 0.3025(4) 0.5060(3) 0.0403(11) Uani 1 1 d . . . . .
H13 H 1.157624 0.332014 0.473312 0.048 Uiso 1 1 calc R U . . .
C14 C 1.1793(5) 0.7402(5) 0.5635(3) 0.0580(15) Uani 1 1 d . . . . .
H14A H 1.168876 0.806626 0.578217 0.087 Uiso 1 1 calc R U . . .
H14B H 1.250903 0.685217 0.567982 0.087 Uiso 1 1 calc R U . . .
H14C H 1.178452 0.749923 0.510997 0.087 Uiso 1 1 calc R U . . .
C15 C 0.9053(6) 0.0695(5) 0.6457(4) 0.0741(19) Uani 1 1 d . . . . .
H15A H 0.849584 0.048910 0.686175 0.111 Uiso 1 1 calc R U . . .
H15B H 0.897720 0.068934 0.596629 0.111 Uiso 1 1 calc R U . . .
H15C H 0.979947 0.019646 0.647994 0.111 Uiso 1 1 calc R U . . .
C16 C 0.6970(3) 0.4304(3) 0.8620(2) 0.0302(9) Uani 1 1 d . . . . .
C17 C 0.7968(3) 0.3898(4) 0.8822(3) 0.0339(10) Uani 1 1 d . . . . .
C18 C 0.8049(4) 0.3361(4) 0.9510(3) 0.0418(12) Uani 1 1 d . . . . .
H18 H 0.872681 0.310165 0.963121 0.050 Uiso 1 1 calc R U . . .
C19 C 0.7129(4) 0.3198(4) 1.0033(3) 0.0495(13) Uani 1 1 d . . . . .
H19 H 0.717574 0.283529 1.051334 0.059 Uiso 1 1 calc R U . . .
C20 C 0.6159(4) 0.3561(4) 0.9851(3) 0.0429(12) Uani 1 1 d . . . . .
H20 H 0.554253 0.343863 1.020999 0.051 Uiso 1 1 calc R U . . .
C21 C 0.6048(4) 0.4113(4) 0.9143(3) 0.0360(11) Uani 1 1 d . . . . .
C22 C 0.4998(4) 0.4429(4) 0.9001(3) 0.0350(10) Uani 1 1 d . . . . .
H22 H 0.442148 0.429895 0.940583 0.042 Uiso 1 1 calc R U . . .
C23 C 0.3727(3) 0.5204(3) 0.8259(2) 0.0314(10) Uani 1 1 d . . . . .
C24 C 0.3708(3) 0.5552(3) 0.7508(2) 0.0309(9) Uani 1 1 d . . . . .
C25 C 0.2705(4) 0.5910(4) 0.7346(3) 0.0376(11) Uani 1 1 d . . . . .
H25 H 0.268344 0.612610 0.683898 0.045 Uiso 1 1 calc R U . . .
C26 C 0.1748(4) 0.5954(4) 0.7913(3) 0.0434(12) Uani 1 1 d . . . . .
H26 H 0.107497 0.619809 0.778931 0.052 Uiso 1 1 calc R U . . .
C27 C 0.1741(4) 0.5650(4) 0.8661(3) 0.0444(12) Uani 1 1 d . . . . .
C28 C 0.2738(4) 0.5277(4) 0.8829(3) 0.0394(11) Uani 1 1 d . . . . .
H28 H 0.274839 0.506932 0.933806 0.047 Uiso 1 1 calc R U . . .
C29 C 0.0668(4) 0.5766(6) 0.9282(3) 0.071(2) Uani 1 1 d . . . . .
H29A H 0.082189 0.551293 0.976976 0.106 Uiso 1 1 calc R U . . .
H29B H 0.015120 0.651063 0.929062 0.106 Uiso 1 1 calc R U . . .
H29C H 0.033367 0.534970 0.918836 0.106 Uiso 1 1 calc R U . . .
C30 C 0.6064(4) 1.0091(4) 0.6887(3) 0.0391(11) Uani 1 1 d . . . . .
C31 C 0.6263(4) 1.0970(4) 0.6533(3) 0.0492(13) Uani 1 1 d . . . . .
H31 H 0.628094 1.142740 0.681696 0.059 Uiso 1 1 calc R U . . .
C32 C 0.6439(4) 1.1191(4) 0.5758(3) 0.0481(13) Uani 1 1 d . . . . .
H32 H 0.659373 1.179070 0.550912 0.058 Uiso 1 1 calc R U . . .
C33 C 0.6388(4) 1.0537(4) 0.5351(3) 0.0410(11) Uani 1 1 d . . . . .
H33 H 0.650217 1.069754 0.482190 0.049 Uiso 1 1 calc R U . . .
C34 C 0.6169(4) 0.9633(3) 0.5704(3) 0.0342(10) Uani 1 1 d . . . . .
C35 C 0.6012(3) 0.9396(3) 0.6493(3) 0.0330(10) Uani 1 1 d . . . . .
C36 C 0.6147(4) 0.8985(4) 0.5224(3) 0.0353(10) Uani 1 1 d . . . . .
H36 H 0.634503 0.916443 0.469444 0.042 Uiso 1 1 calc R U . . .
C37 C 0.6539(4) 0.7446(4) 0.4226(3) 0.0403(11) Uani 1 1 d . . . . .
H37 H 0.695532 0.786706 0.399031 0.048 Uiso 1 1 calc R U . . .
C38 C 0.6563(5) 0.6752(4) 0.3810(3) 0.0473(13) Uani 1 1 d . . . . .
C39 C 0.5950(4) 0.6140(4) 0.4172(3) 0.0454(12) Uani 1 1 d . . . . .
H39 H 0.595455 0.566148 0.389349 0.054 Uiso 1 1 calc R U . . .
C40 C 0.5332(4) 0.6211(4) 0.4928(3) 0.0410(11) Uani 1 1 d . . . . .
H40 H 0.492636 0.578075 0.516411 0.049 Uiso 1 1 calc R U . . .
C41 C 0.5309(4) 0.6905(4) 0.5334(2) 0.0330(10) Uani 1 1 d . . . . .
C42 C 0.5917(4) 0.7537(4) 0.4982(2) 0.0329(10) Uani 1 1 d . . . . .
C43 C 0.7252(6) 0.6658(6) 0.2985(3) 0.0703(19) Uani 1 1 d . . . . .
H43A H 0.717209 0.613413 0.278010 0.105 Uiso 1 1 calc R U . . .
H43B H 0.699175 0.734394 0.269845 0.105 Uiso 1 1 calc R U . . .
H43C H 0.803573 0.643699 0.294349 0.105 Uiso 1 1 calc R U . . .
C44 C 0.6408(5) 1.0049(5) 0.8052(3) 0.0591(15) Uani 1 1 d . . . . .
H44A H 0.618412 0.981934 0.859047 0.089 Uiso 1 1 calc R U . . .
H44B H 0.721364 0.967694 0.783930 0.089 Uiso 1 1 calc R U . . .
H44C H 0.621167 1.081128 0.799251 0.089 Uiso 1 1 calc R U . . .
C45 C 0.5547(4) 0.8120(4) 0.9469(3) 0.0391(11) Uani 1 1 d . . . . .
C46 C 0.6571(4) 0.7536(4) 0.8970(3) 0.0369(11) Uani 1 1 d . . . . .
C47 C 0.7495(4) 0.6987(4) 0.9233(3) 0.0490(13) Uani 1 1 d . . . . .
H47 H 0.819299 0.658514 0.890435 0.059 Uiso 1 1 calc R U . . .
C48 C 0.7394(5) 0.7031(5) 0.9975(3) 0.0587(16) Uani 1 1 d . . . . .
H48 H 0.803451 0.665732 1.014503 0.070 Uiso 1 1 calc R U . . .
C49 C 0.6397(5) 0.7596(5) 1.0482(3) 0.0636(17) Uani 1 1 d . . . . .
C50 C 0.5462(5) 0.8141(5) 1.0222(3) 0.0548(15) Uani 1 1 d . . . . .
H50 H 0.476481 0.852909 1.055818 0.066 Uiso 1 1 calc R U . . .
C51 C 0.3659(4) 0.9211(5) 0.9517(3) 0.0571(16) Uani 1 1 d . . . . .
H51 H 0.350782 0.915576 1.004997 0.069 Uiso 1 1 calc R U . . .
C52 C 0.2734(4) 0.9857(5) 0.9218(3) 0.0598(16) Uani 1 1 d . . . . .
C53 C 0.1680(5) 1.0289(7) 0.9748(4) 0.106(3) Uani 1 1 d . . . . .
H53 H 0.161455 1.013161 1.027204 0.127 Uiso 1 1 calc R U . . .
C54 C 0.0744(5) 1.0930(7) 0.9528(5) 0.116(4) Uani 1 1 d . . . . .
H54 H 0.004193 1.120884 0.989675 0.139 Uiso 1 1 calc R U . . .
C55 C 0.0832(5) 1.1168(6) 0.8758(4) 0.078(2) Uani 1 1 d . . . . .
H55 H 0.018690 1.160153 0.860185 0.093 Uiso 1 1 calc R U . . .
C56 C 0.1851(4) 1.0777(4) 0.8228(3) 0.0499(13) Uani 1 1 d . . . . .
C57 C 0.2844(4) 1.0079(4) 0.8434(3) 0.0424(12) Uani 1 1 d . . . . .
C58 C 0.1089(5) 1.1582(5) 0.7201(4) 0.0724(19) Uani 1 1 d . . . . .
H58A H 0.132957 1.165993 0.664709 0.109 Uiso 1 1 calc R U . . .
H58B H 0.057358 1.122902 0.737729 0.109 Uiso 1 1 calc R U . . .
H58C H 0.071298 1.227991 0.739482 0.109 Uiso 1 1 calc R U . . .
C59 C 0.6315(6) 0.7644(7) 1.1296(4) 0.095(3) Uani 1 1 d . . . . .
H59A H 0.554711 0.807862 1.156483 0.143 Uiso 1 1 calc R U . . .
H59B H 0.653212 0.692875 1.154931 0.143 Uiso 1 1 calc R U . . .
H59C H 0.681141 0.795389 1.129738 0.143 Uiso 1 1 calc R U . . .
C61 C 0.9673(4) 0.4151(5) 0.8462(3) 0.0526(14) Uani 1 1 d . . . . .
H61A H 1.023830 0.426721 0.800888 0.079 Uiso 1 1 calc R U . . .
H61B H 0.932639 0.474557 0.877435 0.079 Uiso 1 1 calc R U . . .
H61C H 1.002413 0.349749 0.875191 0.079 Uiso 1 1 calc R U . . .
C62 C 0.6585(5) 0.3560(5) 0.6383(4) 0.0635(17) Uani 1 1 d . . . . .
H62A H 0.702984 0.282034 0.627369 0.095 Uiso 1 1 calc R U . . .
H62B H 0.580170 0.373342 0.645145 0.095 Uiso 1 1 calc R U . . .
H62C H 0.684747 0.401584 0.596119 0.095 Uiso 1 1 calc R U . . .
N1 N 0.4672(3) 0.8701(3) 0.9129(2) 0.0371(9) Uani 1 1 d . . . . .
N2 N 0.4775(3) 0.4869(3) 0.8376(2) 0.0320(8) Uani 1 1 d . . . . .
N3 N 0.9763(3) 0.4992(3) 0.6436(2) 0.0303(8) Uani 1 1 d . . . . .
N5 N 0.5880(3) 0.8185(3) 0.5465(2) 0.0313(8) Uani 1 1 d . . . . .
O1 O 0.8890(3) 0.1727(3) 0.6547(2) 0.0503(9) Uani 1 1 d . . . . .
O2 O 0.8742(2) 0.3515(2) 0.68361(17) 0.0339(7) Uani 1 1 d . . . . .
O3 O 0.8248(2) 0.6218(2) 0.75006(18) 0.0354(7) Uani 1 1 d . . . . .
H3 H 0.774607 0.669914 0.777399 0.053 Uiso 1 1 calc R U . . .
O4 O 0.6615(2) 0.7558(3) 0.82489(17) 0.0409(8) Uani 1 1 d . . . . .
O5 O 0.3757(2) 0.9695(3) 0.78922(18) 0.0396(8) Uani 1 1 d . . . . .
O6 O 0.5851(3) 0.9819(3) 0.76683(19) 0.0477(9) Uani 1 1 d . . . . .
O7 O 0.5843(2) 0.8549(2) 0.68808(16) 0.0336(7) Uani 1 1 d . . . . .
O8 O 0.4689(3) 0.7043(2) 0.60807(16) 0.0342(7) Uani 1 1 d . . . . .
H8 H 0.463464 0.647489 0.629668 0.051 Uiso 1 1 calc R U . . .
O9 O 0.4661(2) 0.5520(2) 0.69645(16) 0.0319(7) Uani 1 1 d . . . . .
O10 O 0.6963(2) 0.4850(2) 0.79544(16) 0.0310(7) Uani 1 1 d . . . . .
O11 O 0.8847(2) 0.4067(3) 0.82461(17) 0.0376(7) Uani 1 1 d . . . . .
O12 O 0.2032(3) 1.0966(3) 0.7467(2) 0.0538(10) Uani 1 1 d . . . . .
O14 O 0.6695(3) 0.3724(3) 0.70624(19) 0.0384(8) Uani 1 1 d . . . . .
C64 C 0.1783(7) 0.8639(8) 0.7206(6) 0.107(3) Uani 1 1 d D U . . .
H64A H 0.159598 0.857944 0.775841 0.160 Uiso 1 1 calc R U . . .
H64B H 0.190694 0.797904 0.704065 0.160 Uiso 1 1 calc R U . . .
H64C H 0.116900 0.922208 0.704580 0.160 Uiso 1 1 calc R U . . .
C63 C 0.2850(9) 0.8853(10) 0.6850(7) 0.175(6) Uani 1 1 d D U . . .
N4 N 0.3753(3) 0.9089(3) 0.6654(2) 0.0315(8) Uani 1 1 d D U . . .
O15 O 0.2086(8) 0.8418(6) 1.1671(5) 0.154(3) Uani 1 1 d D . . . .
C65 C 0.3139(8) 0.8066(7) 1.1819(5) 0.096(3) Uani 1 1 d D . . . .
H14 H 0.734(5) 0.366(5) 0.696(4) 0.07(2) 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
Ni1 O2 1.997(3) . ?
Ni1 O10 2.008(3) . ?
Ni1 N3 2.010(4) . ?
Ni1 O3 2.024(3) . ?
Ni1 O11 2.251(3) . ?
Ni1 Cl1 2.5264(16) . ?
Ni2 O10 1.964(3) . ?
Ni2 N2 2.001(4) . ?
Ni2 O9 2.012(3) . ?
Ni2 O14 2.101(4) . ?
Ni2 Cl1 2.4085(15) . ?
Ni2 Cl2 2.6088(19) . ?
Ni3 O7 1.962(3) . ?
Ni3 N5 1.997(4) . ?
Ni3 O8 2.037(3) . ?
Ni3 N4 2.075(4) . ?
Ni3 Cl2 2.4042(17) . ?
Ni3 Cl1 2.7042(17) . ?
Ni4 O5 1.977(3) . ?
Ni4 N1 2.004(4) . ?
Ni4 O7 2.015(3) . ?
Ni4 O4 2.024(3) . ?
Ni4 O6 2.173(4) . ?
Ni4 Cl2 2.5423(17) . ?
C1 C2 1.396(6) . ?
C1 C6 1.399(6) . ?
C1 N3 1.430(6) . ?
C2 C3 1.375(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.400(8) . ?
C3 C14 1.522(7) . ?
C4 C5 1.380(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(7) . ?
C5 H5 0.9500 . ?
C6 O3 1.357(5) . ?
C7 N3 1.283(6) . ?
C7 C8 1.438(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.415(6) . ?
C8 C13 1.431(6) . ?
C9 O2 1.317(5) . ?
C9 C10 1.428(7) . ?
C10 O1 1.377(6) . ?
C10 C11 1.385(7) . ?
C11 C12 1.392(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O1 1.422(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 O10 1.325(5) . ?
C16 C21 1.416(6) . ?
C16 C17 1.419(6) . ?
C17 C18 1.372(6) . ?
C17 O11 1.398(5) . ?
C18 C19 1.397(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.418(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.448(6) . ?
C22 N2 1.287(6) . ?
C22 H22 0.9500 . ?
C23 C28 1.399(6) . ?
C23 C24 1.406(6) . ?
C23 N2 1.418(5) . ?
C24 O9 1.355(5) . ?
C24 C25 1.395(6) . ?
C25 C26 1.375(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(6) . ?
C27 C29 1.512(7) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.372(7) . ?
C30 O6 1.402(6) . ?
C30 C35 1.412(7) . ?
C31 C32 1.388(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.379(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.415(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.419(6) . ?
C34 C36 1.456(7) . ?
C35 O7 1.331(5) . ?
C36 N5 1.289(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.383(7) . ?
C37 C42 1.390(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.393(7) . ?
C38 C43 1.519(7) . ?
C39 C40 1.388(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.370(7) . ?
C40 H40 0.9500 . ?
C41 O8 1.378(5) . ?
C41 C42 1.409(6) . ?
C42 N5 1.417(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 O6 1.418(6) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C50 1.402(7) . ?
C45 C46 1.405(6) . ?
C45 N1 1.426(6) . ?
C46 O4 1.345(5) . ?
C46 C47 1.391(6) . ?
C47 C48 1.381(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.385(8) . ?
C48 H48 0.9500 . ?
C49 C50 1.399(8) . ?
C49 C59 1.528(8) . ?
C50 H50 0.9500 . ?
C51 N1 1.291(6) . ?
C51 C52 1.445(7) . ?
C51 H51 0.9500 . ?
C52 C53 1.409(8) . ?
C52 C57 1.418(8) . ?
C53 C54 1.374(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.399(10) . ?
C54 H54 0.9500 . ?
C55 C56 1.373(8) . ?
C55 H55 0.9500 . ?
C56 O12 1.360(7) . ?
C56 C57 1.439(7) . ?
C57 O5 1.300(6) . ?
C58 O12 1.423(6) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C61 O11 1.424(6) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 O14 1.438(7) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
O3 H3 0.8400 . ?
O8 H8 0.8400 . ?
O14 H14 0.83(6) . ?
C64 C63 1.544(12) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C63 N4 1.358(12) . ?
O15 C65 1.449(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O10 91.09(13) . . ?
O2 Ni1 N3 91.38(14) . . ?
O10 Ni1 N3 177.52(14) . . ?
O2 Ni1 O3 171.25(12) . . ?
O10 Ni1 O3 96.37(13) . . ?
N3 Ni1 O3 81.15(14) . . ?
O2 Ni1 O11 90.97(13) . . ?
O10 Ni1 O11 74.68(12) . . ?
N3 Ni1 O11 105.22(13) . . ?
O3 Ni1 O11 86.63(13) . . ?
O2 Ni1 Cl1 92.59(10) . . ?
O10 Ni1 Cl1 80.71(9) . . ?
N3 Ni1 Cl1 99.23(11) . . ?
O3 Ni1 Cl1 93.11(10) . . ?
O11 Ni1 Cl1 155.19(8) . . ?
O10 Ni2 N2 93.03(14) . . ?
O10 Ni2 O9 174.74(12) . . ?
N2 Ni2 O9 83.43(14) . . ?
O10 Ni2 O14 87.07(13) . . ?
N2 Ni2 O14 95.84(15) . . ?
O9 Ni2 O14 89.42(13) . . ?
O10 Ni2 Cl1 84.66(9) . . ?
N2 Ni2 Cl1 171.86(12) . . ?
O9 Ni2 Cl1 99.38(9) . . ?
O14 Ni2 Cl1 91.85(11) . . ?
O10 Ni2 Cl2 96.11(10) . . ?
N2 Ni2 Cl2 84.95(12) . . ?
O9 Ni2 Cl2 87.47(10) . . ?
O14 Ni2 Cl2 176.69(10) . . ?
Cl1 Ni2 Cl2 87.54(6) . . ?
O7 Ni3 N5 91.61(14) . . ?
O7 Ni3 O8 173.21(12) . . ?
N5 Ni3 O8 81.64(14) . . ?
O7 Ni3 N4 90.11(15) . . ?
N5 Ni3 N4 93.17(15) . . ?
O8 Ni3 N4 89.56(14) . . ?
O7 Ni3 Cl2 85.67(10) . . ?
N5 Ni3 Cl2 173.32(11) . . ?
O8 Ni3 Cl2 101.12(9) . . ?
N4 Ni3 Cl2 92.94(11) . . ?
O7 Ni3 Cl1 97.37(10) . . ?
N5 Ni3 Cl1 88.83(11) . . ?
O8 Ni3 Cl1 83.28(10) . . ?
N4 Ni3 Cl1 172.21(11) . . ?
Cl2 Ni3 Cl1 85.47(5) . . ?
O5 Ni4 N1 92.18(14) . . ?
O5 Ni4 O7 90.72(13) . . ?
N1 Ni4 O7 174.28(14) . . ?
O5 Ni4 O4 173.23(13) . . ?
N1 Ni4 O4 81.45(14) . . ?
O7 Ni4 O4 95.44(13) . . ?
O5 Ni4 O6 88.54(15) . . ?
N1 Ni4 O6 98.30(15) . . ?
O7 Ni4 O6 76.84(13) . . ?
O4 Ni4 O6 90.12(15) . . ?
O5 Ni4 Cl2 90.71(11) . . ?
N1 Ni4 Cl2 103.89(12) . . ?
O7 Ni4 Cl2 80.99(10) . . ?
O4 Ni4 Cl2 93.02(11) . . ?
O6 Ni4 Cl2 157.81(10) . . ?
Ni2 Cl1 Ni1 82.04(6) . . ?
Ni2 Cl1 Ni3 85.31(5) . . ?
Ni1 Cl1 Ni3 133.17(6) . . ?
Ni3 Cl2 Ni4 81.48(5) . . ?
Ni3 Cl2 Ni2 87.54(6) . . ?
Ni4 Cl2 Ni2 135.01(6) . . ?
C2 C1 C6 119.6(4) . . ?
C2 C1 N3 126.0(4) . . ?
C6 C1 N3 114.4(4) . . ?
C3 C2 C1 121.5(5) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 118.2(4) . . ?
C2 C3 C14 121.2(5) . . ?
C4 C3 C14 120.6(5) . . ?
C5 C4 C3 121.2(5) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 120.3(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
O3 C6 C5 123.1(4) . . ?
O3 C6 C1 117.7(4) . . ?
C5 C6 C1 119.2(4) . . ?
N3 C7 C8 127.0(4) . . ?
N3 C7 H7 116.5 . . ?
C8 C7 H7 116.5 . . ?
C9 C8 C13 120.2(4) . . ?
C9 C8 C7 123.8(4) . . ?
C13 C8 C7 115.9(4) . . ?
O2 C9 C8 124.7(4) . . ?
O2 C9 C10 118.9(4) . . ?
C8 C9 C10 116.4(4) . . ?
O1 C10 C11 124.1(5) . . ?
O1 C10 C9 113.9(4) . . ?
C11 C10 C9 122.0(4) . . ?
C10 C11 C12 120.8(5) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 119.3(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C8 121.2(5) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 C15 H15A 109.5 . . ?
O1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O10 C16 C21 124.4(4) . . ?
O10 C16 C17 117.4(4) . . ?
C21 C16 C17 118.2(4) . . ?
C18 C17 O11 124.4(4) . . ?
C18 C17 C16 122.1(4) . . ?
O11 C17 C16 113.5(4) . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 119.9(4) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 122.0(4) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C16 C21 C20 118.2(4) . . ?
C16 C21 C22 124.5(4) . . ?
C20 C21 C22 117.3(4) . . ?
N2 C22 C21 125.9(4) . . ?
N2 C22 H22 117.1 . . ?
C21 C22 H22 117.1 . . ?
C28 C23 C24 119.7(4) . . ?
C28 C23 N2 125.2(4) . . ?
C24 C23 N2 115.0(4) . . ?
O9 C24 C25 122.0(4) . . ?
O9 C24 C23 119.3(4) . . ?
C25 C24 C23 118.7(4) . . ?
C26 C25 C24 120.6(4) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 121.7(4) . . ?
C25 C26 H26 119.2 . . ?
C27 C26 H26 119.2 . . ?
C26 C27 C28 118.3(4) . . ?
C26 C27 C29 120.9(4) . . ?
C28 C27 C29 120.8(5) . . ?
C27 C28 C23 121.0(4) . . ?
C27 C28 H28 119.5 . . ?
C23 C28 H28 119.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 O6 124.0(5) . . ?
C31 C30 C35 122.3(5) . . ?
O6 C30 C35 113.7(4) . . ?
C30 C31 C32 119.9(5) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 119.7(5) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 121.5(5) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C33 C34 C35 118.7(4) . . ?
C33 C34 C36 117.4(4) . . ?
C35 C34 C36 123.9(4) . . ?
O7 C35 C30 118.1(4) . . ?
O7 C35 C34 124.1(4) . . ?
C30 C35 C34 117.8(4) . . ?
N5 C36 C34 124.9(4) . . ?
N5 C36 H36 117.5 . . ?
C34 C36 H36 117.5 . . ?
C38 C37 C42 121.1(5) . . ?
C38 C37 H37 119.4 . . ?
C42 C37 H37 119.4 . . ?
C37 C38 C39 118.2(5) . . ?
C37 C38 C43 120.4(5) . . ?
C39 C38 C43 121.4(5) . . ?
C40 C39 C38 121.6(5) . . ?
C40 C39 H39 119.2 . . ?
C38 C39 H39 119.2 . . ?
C41 C40 C39 119.8(5) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 O8 123.1(4) . . ?
C40 C41 C42 119.8(4) . . ?
O8 C41 C42 117.1(4) . . ?
C37 C42 C41 119.5(4) . . ?
C37 C42 N5 125.5(4) . . ?
C41 C42 N5 115.0(4) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O6 C44 H44A 109.5 . . ?
O6 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O6 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C50 C45 C46 120.2(4) . . ?
C50 C45 N1 125.3(4) . . ?
C46 C45 N1 114.4(4) . . ?
O4 C46 C47 122.9(4) . . ?
O4 C46 C45 118.0(4) . . ?
C47 C46 C45 119.1(4) . . ?
C48 C47 C46 119.6(5) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
C47 C48 C49 122.8(5) . . ?
C47 C48 H48 118.6 . . ?
C49 C48 H48 118.6 . . ?
C48 C49 C50 117.9(5) . . ?
C48 C49 C59 121.6(5) . . ?
C50 C49 C59 120.6(6) . . ?
C49 C50 C45 120.5(5) . . ?
C49 C50 H50 119.8 . . ?
C45 C50 H50 119.8 . . ?
N1 C51 C52 126.2(5) . . ?
N1 C51 H51 116.9 . . ?
C52 C51 H51 116.9 . . ?
C53 C52 C57 119.8(5) . . ?
C53 C52 C51 116.8(5) . . ?
C57 C52 C51 123.4(5) . . ?
C54 C53 C52 121.9(7) . . ?
C54 C53 H53 119.1 . . ?
C52 C53 H53 119.1 . . ?
C53 C54 C55 119.5(6) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
C56 C55 C54 120.1(6) . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
O12 C56 C55 124.9(5) . . ?
O12 C56 C57 113.0(4) . . ?
C55 C56 C57 122.1(5) . . ?
O5 C57 C52 125.7(4) . . ?
O5 C57 C56 117.7(5) . . ?
C52 C57 C56 116.6(5) . . ?
O12 C58 H58A 109.5 . . ?
O12 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O12 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C49 C59 H59A 109.5 . . ?
C49 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C49 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
O11 C61 H61A 109.5 . . ?
O11 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
O11 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O14 C62 H62A 109.5 . . ?
O14 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
O14 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C51 N1 C45 122.5(4) . . ?
C51 N1 Ni4 125.0(3) . . ?
C45 N1 Ni4 112.5(3) . . ?
C22 N2 C23 124.8(4) . . ?
C22 N2 Ni2 125.0(3) . . ?
C23 N2 Ni2 110.1(3) . . ?
C7 N3 C1 121.4(4) . . ?
C7 N3 Ni1 124.7(3) . . ?
C1 N3 Ni1 113.0(3) . . ?
C36 N5 C42 123.7(4) . . ?
C36 N5 Ni3 124.7(3) . . ?
C42 N5 Ni3 111.4(3) . . ?
C10 O1 C15 117.2(4) . . ?
C9 O2 Ni1 126.4(3) . . ?
C6 O3 Ni1 113.6(3) . . ?
C6 O3 H3 109.5 . . ?
Ni1 O3 H3 135.5 . . ?
C46 O4 Ni4 113.0(3) . . ?
C57 O5 Ni4 126.3(3) . . ?
C30 O6 C44 118.0(4) . . ?
C30 O6 Ni4 110.9(3) . . ?
C44 O6 Ni4 127.0(3) . . ?
C35 O7 Ni3 123.7(3) . . ?
C35 O7 Ni4 116.1(3) . . ?
Ni3 O7 Ni4 108.60(14) . . ?
C41 O8 Ni3 109.9(3) . . ?
C41 O8 H8 109.5 . . ?
Ni3 O8 H8 118.8 . . ?
C24 O9 Ni2 109.8(3) . . ?
C16 O10 Ni2 125.7(3) . . ?
C16 O10 Ni1 121.3(3) . . ?
Ni2 O10 Ni1 109.32(14) . . ?
C17 O11 C61 117.6(4) . . ?
C17 O11 Ni1 112.3(2) . . ?
C61 O11 Ni1 123.8(3) . . ?
C56 O12 C58 117.5(5) . . ?
C62 O14 Ni2 118.4(3) . . ?
C62 O14 H14 107(4) . . ?
Ni2 O14 H14 100(4) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N4 C63 C64 170.4(11) . . ?
C63 N4 Ni3 113.8(6) . . ?

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
C6 C1 C2 C3 -1.7(7) . . . . ?
N3 C1 C2 C3 176.6(4) . . . . ?
C1 C2 C3 C4 1.0(7) . . . . ?
C1 C2 C3 C14 -176.6(4) . . . . ?
C2 C3 C4 C5 0.6(7) . . . . ?
C14 C3 C4 C5 178.2(5) . . . . ?
C3 C4 C5 C6 -1.4(7) . . . . ?
C4 C5 C6 O3 179.9(4) . . . . ?
C4 C5 C6 C1 0.6(7) . . . . ?
C2 C1 C6 O3 -178.4(4) . . . . ?
N3 C1 C6 O3 3.1(6) . . . . ?
C2 C1 C6 C5 1.0(6) . . . . ?
N3 C1 C6 C5 -177.6(4) . . . . ?
N3 C7 C8 C9 -0.6(7) . . . . ?
N3 C7 C8 C13 -179.0(4) . . . . ?
C13 C8 C9 O2 -178.7(4) . . . . ?
C7 C8 C9 O2 2.9(6) . . . . ?
C13 C8 C9 C10 3.7(6) . . . . ?
C7 C8 C9 C10 -174.7(4) . . . . ?
O2 C9 C10 O1 -2.6(6) . . . . ?
C8 C9 C10 O1 175.1(4) . . . . ?
O2 C9 C10 C11 178.4(4) . . . . ?
C8 C9 C10 C11 -3.8(6) . . . . ?
O1 C10 C11 C12 -177.6(4) . . . . ?
C9 C10 C11 C12 1.2(7) . . . . ?
C10 C11 C12 C13 1.7(7) . . . . ?
C11 C12 C13 C8 -1.8(7) . . . . ?
C9 C8 C13 C12 -1.0(6) . . . . ?
C7 C8 C13 C12 177.5(4) . . . . ?
O10 C16 C17 C18 177.1(4) . . . . ?
C21 C16 C17 C18 -2.0(7) . . . . ?
O10 C16 C17 O11 -5.1(6) . . . . ?
C21 C16 C17 O11 175.8(4) . . . . ?
O11 C17 C18 C19 -177.1(5) . . . . ?
C16 C17 C18 C19 0.4(8) . . . . ?
C17 C18 C19 C20 0.9(9) . . . . ?
C18 C19 C20 C21 -0.5(9) . . . . ?
O10 C16 C21 C20 -176.8(4) . . . . ?
C17 C16 C21 C20 2.3(7) . . . . ?
O10 C16 C21 C22 4.3(8) . . . . ?
C17 C16 C21 C22 -176.7(5) . . . . ?
C19 C20 C21 C16 -1.1(8) . . . . ?
C19 C20 C21 C22 177.9(5) . . . . ?
C16 C21 C22 N2 4.0(8) . . . . ?
C20 C21 C22 N2 -175.0(5) . . . . ?
C28 C23 C24 O9 177.3(4) . . . . ?
N2 C23 C24 O9 1.7(6) . . . . ?
C28 C23 C24 C25 -3.5(7) . . . . ?
N2 C23 C24 C25 -179.1(4) . . . . ?
O9 C24 C25 C26 -178.7(4) . . . . ?
C23 C24 C25 C26 2.1(7) . . . . ?
C24 C25 C26 C27 0.2(8) . . . . ?
C25 C26 C27 C28 -1.1(8) . . . . ?
C25 C26 C27 C29 176.2(6) . . . . ?
C26 C27 C28 C23 -0.3(8) . . . . ?
C29 C27 C28 C23 -177.7(5) . . . . ?
C24 C23 C28 C27 2.6(7) . . . . ?
N2 C23 C28 C27 177.8(5) . . . . ?
O6 C30 C31 C32 -178.4(5) . . . . ?
C35 C30 C31 C32 -1.0(8) . . . . ?
C30 C31 C32 C33 1.4(8) . . . . ?
C31 C32 C33 C34 -0.6(8) . . . . ?
C32 C33 C34 C35 -0.7(7) . . . . ?
C32 C33 C34 C36 -179.2(4) . . . . ?
C31 C30 C35 O7 178.3(4) . . . . ?
O6 C30 C35 O7 -4.1(6) . . . . ?
C31 C30 C35 C34 -0.2(7) . . . . ?
O6 C30 C35 C34 177.4(4) . . . . ?
C33 C34 C35 O7 -177.4(4) . . . . ?
C36 C34 C35 O7 1.0(7) . . . . ?
C33 C34 C35 C30 1.1(6) . . . . ?
C36 C34 C35 C30 179.5(4) . . . . ?
C33 C34 C36 N5 -174.6(4) . . . . ?
C35 C34 C36 N5 7.0(7) . . . . ?
C42 C37 C38 C39 -0.4(8) . . . . ?
C42 C37 C38 C43 -179.7(5) . . . . ?
C37 C38 C39 C40 -0.3(8) . . . . ?
C43 C38 C39 C40 179.1(5) . . . . ?
C38 C39 C40 C41 0.6(8) . . . . ?
C39 C40 C41 O8 178.0(4) . . . . ?
C39 C40 C41 C42 -0.3(7) . . . . ?
C38 C37 C42 C41 0.7(7) . . . . ?
C38 C37 C42 N5 176.9(5) . . . . ?
C40 C41 C42 C37 -0.3(7) . . . . ?
O8 C41 C42 C37 -178.7(4) . . . . ?
C40 C41 C42 N5 -176.9(4) . . . . ?
O8 C41 C42 N5 4.7(6) . . . . ?
C50 C45 C46 O4 -178.7(5) . . . . ?
N1 C45 C46 O4 -2.0(7) . . . . ?
C50 C45 C46 C47 -0.3(8) . . . . ?
N1 C45 C46 C47 176.4(5) . . . . ?
O4 C46 C47 C48 177.9(5) . . . . ?
C45 C46 C47 C48 -0.4(8) . . . . ?
C46 C47 C48 C49 0.6(10) . . . . ?
C47 C48 C49 C50 0.0(10) . . . . ?
C47 C48 C49 C59 -179.0(7) . . . . ?
C48 C49 C50 C45 -0.8(10) . . . . ?
C59 C49 C50 C45 178.3(7) . . . . ?
C46 C45 C50 C49 0.9(9) . . . . ?
N1 C45 C50 C49 -175.4(6) . . . . ?
N1 C51 C52 C53 175.9(7) . . . . ?
N1 C51 C52 C57 -4.9(11) . . . . ?
C57 C52 C53 C54 -0.4(14) . . . . ?
C51 C52 C53 C54 178.9(9) . . . . ?
C52 C53 C54 C55 -0.2(16) . . . . ?
C53 C54 C55 C56 -1.0(15) . . . . ?
C54 C55 C56 O12 -179.4(7) . . . . ?
C54 C55 C56 C57 2.9(11) . . . . ?
C53 C52 C57 O5 -176.9(7) . . . . ?
C51 C52 C57 O5 3.9(10) . . . . ?
C53 C52 C57 C56 2.1(10) . . . . ?
C51 C52 C57 C56 -177.1(6) . . . . ?
O12 C56 C57 O5 -2.3(7) . . . . ?
C55 C56 C57 O5 175.7(6) . . . . ?
O12 C56 C57 C52 178.7(5) . . . . ?
C55 C56 C57 C52 -3.4(9) . . . . ?
C52 C51 N1 C45 177.0(6) . . . . ?
C52 C51 N1 Ni4 -4.3(9) . . . . ?
C50 C45 N1 C51 -9.2(8) . . . . ?
C46 C45 N1 C51 174.3(5) . . . . ?
C50 C45 N1 Ni4 172.0(5) . . . . ?
C46 C45 N1 Ni4 -4.5(5) . . . . ?
C21 C22 N2 C23 -177.7(4) . . . . ?
C21 C22 N2 Ni2 -0.9(7) . . . . ?
C28 C23 N2 C22 11.7(8) . . . . ?
C24 C23 N2 C22 -172.9(4) . . . . ?
C28 C23 N2 Ni2 -165.5(4) . . . . ?
C24 C23 N2 Ni2 9.8(5) . . . . ?
C8 C7 N3 C1 -179.5(4) . . . . ?
C8 C7 N3 Ni1 -11.1(6) . . . . ?
C2 C1 N3 C7 -10.0(6) . . . . ?
C6 C1 N3 C7 168.4(4) . . . . ?
C2 C1 N3 Ni1 -179.7(4) . . . . ?
C6 C1 N3 Ni1 -1.2(5) . . . . ?
C34 C36 N5 C42 -176.8(4) . . . . ?
C34 C36 N5 Ni3 8.5(6) . . . . ?
C37 C42 N5 C36 20.9(7) . . . . ?
C41 C42 N5 C36 -162.8(4) . . . . ?
C37 C42 N5 Ni3 -163.8(4) . . . . ?
C41 C42 N5 Ni3 12.5(5) . . . . ?
C11 C10 O1 C15 8.4(7) . . . . ?
C9 C10 O1 C15 -170.5(5) . . . . ?
C8 C9 O2 Ni1 7.0(6) . . . . ?
C10 C9 O2 Ni1 -175.5(3) . . . . ?
C5 C6 O3 Ni1 177.3(4) . . . . ?
C1 C6 O3 Ni1 -3.4(5) . . . . ?
C47 C46 O4 Ni4 -170.9(4) . . . . ?
C45 C46 O4 Ni4 7.4(6) . . . . ?
C52 C57 O5 Ni4 6.1(8) . . . . ?
C56 C57 O5 Ni4 -172.8(4) . . . . ?
C31 C30 O6 C44 -34.9(7) . . . . ?
C35 C30 O6 C44 147.5(5) . . . . ?
C31 C30 O6 Ni4 166.2(4) . . . . ?
C35 C30 O6 Ni4 -11.4(5) . . . . ?
C30 C35 O7 Ni3 158.2(3) . . . . ?
C34 C35 O7 Ni3 -23.3(6) . . . . ?
C30 C35 O7 Ni4 19.3(5) . . . . ?
C34 C35 O7 Ni4 -162.3(3) . . . . ?
C40 C41 O8 Ni3 162.7(4) . . . . ?
C42 C41 O8 Ni3 -19.0(4) . . . . ?
C25 C24 O9 Ni2 168.6(4) . . . . ?
C23 C24 O9 Ni2 -12.2(5) . . . . ?
C21 C16 O10 Ni2 -14.4(6) . . . . ?
C17 C16 O10 Ni2 166.5(3) . . . . ?
C21 C16 O10 Ni1 -170.5(4) . . . . ?
C17 C16 O10 Ni1 10.5(5) . . . . ?
C18 C17 O11 C61 -30.4(7) . . . . ?
C16 C17 O11 C61 151.9(4) . . . . ?
C18 C17 O11 Ni1 176.2(4) . . . . ?
C16 C17 O11 Ni1 -1.5(5) . . . . ?
C55 C56 O12 C58 -2.6(9) . . . . ?
C57 C56 O12 C58 175.2(5) . . . . ?

_refine_diff_density_max         1.640
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.098

# start Validation Reply Form
_vrf_PLAT241_shelx               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C63 Check 
RESPONSE: Due to disorder in the position of atoms.
;
_vrf_PLAT242_shelx               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         N4 Check 
RESPONSE: Due to disorder in the position of atoms.
;
_vrf_PLAT315_shelx               
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).        C65 Check 
RESPONSE: Hydrogen on methanol could not be located and refined. 
Hence ignored, however added in the formula unit
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These are affected by the beam-stop, hence omitted from refinement.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_MF127
_database_code_depnum_ccdc_archive 'CCDC 2072516'
loop_
_audit_author_name
_audit_author_address
'saroj kumar kushvaha'
;Indian Institute of Technology Madras
India
;
_audit_update_record             
;
2021-03-23 deposited with the CCDC.	2021-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H27 N O5'
_chemical_formula_sum            'C24 H27 N O5'
_chemical_formula_weight         409.46

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   9.2258(11)
_cell_length_b                   15.495(2)
_cell_length_c                   15.6334(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2234.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9949
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      26.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_F_000             872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.085
_shelx_estimated_absorpt_T_min   0.990
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61760
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.673
_diffrn_reflns_theta_max         26.516
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             4588
_reflns_number_gt                4000
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.993

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+0.2750P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.7(14)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         4588
_refine_ls_number_parameters     278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.0981
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
O3 O 0.4553(2) 0.31908(12) 0.18985(14) 0.0796(6) Uani 1 1 d . . . . .
O5 O -0.11339(19) 0.53801(11) 0.02484(10) 0.0609(4) Uani 1 1 d . . . . .
O1 O 0.0213(3) 0.68032(16) 0.38577(12) 0.0880(7) Uani 1 1 d . . . . .
O4 O -0.2100(2) 0.55044(14) 0.15819(12) 0.0725(5) Uani 1 1 d . . . . .
N1 N 0.0017(2) 0.61493(12) 0.12365(11) 0.0490(4) Uani 1 1 d . . . . .
O2 O 0.2312(3) 0.60997(15) 0.40013(11) 0.0846(6) Uani 1 1 d . . . . .
C15 C 0.4458(3) 0.46765(16) 0.21120(15) 0.0562(5) Uani 1 1 d . . . . .
H15 H 0.545919 0.468601 0.204219 0.067 Uiso 1 1 calc R U . . .
C24 C 0.3869(5) 0.23746(18) 0.1871(3) 0.1040(12) Uani 1 1 d . . . . .
H24A H 0.309638 0.238729 0.145987 0.156 Uiso 1 1 calc R U . . .
H24B H 0.348207 0.223970 0.242546 0.156 Uiso 1 1 calc R U . . .
H24C H 0.456277 0.194266 0.170982 0.156 Uiso 1 1 calc R U . . .
C14 C 0.3709(3) 0.39027(15) 0.20619(14) 0.0545(5) Uani 1 1 d . . . . .
C13 C 0.2227(3) 0.38903(15) 0.21537(15) 0.0564(6) Uani 1 1 d . . . . .
H13 H 0.172037 0.337340 0.210769 0.068 Uiso 1 1 calc R U . . .
C12 C 0.1488(3) 0.46583(15) 0.23164(14) 0.0523(5) Uani 1 1 d . . . . .
H12 H 0.048593 0.464965 0.238031 0.063 Uiso 1 1 calc R U . . .
C11 C 0.2227(3) 0.54345(14) 0.23840(12) 0.0450(5) Uani 1 1 d . . . . .
C9 C 0.1411(3) 0.62404(14) 0.26149(13) 0.0495(5) Uani 1 1 d . . . . .
C8 C 0.0148(2) 0.65427(15) 0.20689(14) 0.0501(5) Uani 1 1 d . . . . .
H8 H -0.072128 0.677103 0.234934 0.060 Uiso 1 1 calc R U . . .
C19 C -0.1176(3) 0.56466(15) 0.10559(15) 0.0526(5) Uani 1 1 d . . . . .
C20 C -0.2331(3) 0.48778(16) -0.01315(16) 0.0602(6) Uani 1 1 d . . . . .
C23 C -0.2432(4) 0.40045(18) 0.0302(2) 0.0796(8) Uani 1 1 d . . . . .
H23A H -0.150597 0.372341 0.027943 0.119 Uiso 1 1 calc R U . . .
H23B H -0.314035 0.365627 0.001324 0.119 Uiso 1 1 calc R U . . .
H23C H -0.271540 0.408097 0.088815 0.119 Uiso 1 1 calc R U . . .
C22 C -0.1822(4) 0.4787(2) -0.10527(18) 0.0806(9) Uani 1 1 d . . . . .
H22A H -0.169724 0.534941 -0.129943 0.121 Uiso 1 1 calc R U . . .
H22B H -0.253154 0.447131 -0.137488 0.121 Uiso 1 1 calc R U . . .
H22C H -0.091559 0.448277 -0.106500 0.121 Uiso 1 1 calc R U . . .
C17 C 0.1213(3) 0.64134(17) 0.35469(15) 0.0606(6) Uani 1 1 d . . . . .
C18 C 0.2278(5) 0.6239(3) 0.49187(18) 0.1077(13) Uani 1 1 d . . . . .
H18A H 0.263397 0.680671 0.504577 0.162 Uiso 1 1 calc R U . . .
H18B H 0.287677 0.581698 0.519648 0.162 Uiso 1 1 calc R U . . .
H18C H 0.129925 0.618518 0.512093 0.162 Uiso 1 1 calc R U . . .
C16 C 0.3710(3) 0.54348(15) 0.22662(14) 0.0526(5) Uani 1 1 d . . . . .
H16 H 0.421565 0.595361 0.229091 0.063 Uiso 1 1 calc R U . . .
C7 C 0.1508(3) 0.70775(14) 0.20604(15) 0.0512(5) Uani 1 1 d . . . . .
C10 C 0.1683(3) 0.79623(16) 0.24551(19) 0.0684(7) Uani 1 1 d . . . . .
H10A H 0.115410 0.798717 0.298340 0.103 Uiso 1 1 calc R U . . .
H10B H 0.131459 0.839122 0.206896 0.103 Uiso 1 1 calc R U . . .
H10C H 0.269090 0.807014 0.256353 0.103 Uiso 1 1 calc R U . . .
C1 C 0.2119(3) 0.69262(13) 0.11915(14) 0.0489(5) Uani 1 1 d . . . . .
C2 C 0.1234(2) 0.63709(14) 0.07268(13) 0.0474(5) Uani 1 1 d . . . . .
C3 C 0.1581(3) 0.61411(17) -0.01041(15) 0.0586(6) Uani 1 1 d . . . . .
H3 H 0.099751 0.576781 -0.041764 0.070 Uiso 1 1 calc R U . . .
C4 C 0.2833(3) 0.64892(19) -0.04494(17) 0.0716(8) Uani 1 1 d . . . . .
H4 H 0.309750 0.633628 -0.100309 0.086 Uiso 1 1 calc R U . . .
C5 C 0.3696(3) 0.70509(17) -0.00042(18) 0.0712(7) Uani 1 1 d . . . . .
H5 H 0.451759 0.728170 -0.026213 0.085 Uiso 1 1 calc R U . . .
C6 C 0.3353(3) 0.72755(15) 0.08236(18) 0.0609(6) Uani 1 1 d . . . . .
H6 H 0.393820 0.765427 0.112972 0.073 Uiso 1 1 calc R U . . .
C21 C -0.3718(3) 0.5393(2) -0.0087(2) 0.0780(8) Uani 1 1 d . . . . .
H21A H -0.404871 0.541654 0.049477 0.117 Uiso 1 1 calc R U . . .
H21B H -0.444368 0.512097 -0.043550 0.117 Uiso 1 1 calc R U . . .
H21C H -0.354489 0.596730 -0.029210 0.117 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
O3 C14 1.374(3) . ?
O3 C24 1.414(4) . ?
O5 C19 1.329(3) . ?
O5 C20 1.476(3) . ?
O1 C17 1.204(3) . ?
O4 C19 1.205(3) . ?
N1 C19 1.377(3) . ?
N1 C2 1.419(3) . ?
N1 C8 1.442(3) . ?
O2 C17 1.330(3) . ?
O2 C18 1.451(3) . ?
C15 C16 1.384(3) . ?
C15 C14 1.386(3) . ?
C15 H15 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C14 C13 1.375(4) . ?
C13 C12 1.395(3) . ?
C13 H13 0.9300 . ?
C12 C11 1.387(3) . ?
C12 H12 0.9300 . ?
C11 C16 1.381(3) . ?
C11 C9 1.502(3) . ?
C9 C17 1.493(3) . ?
C9 C8 1.518(3) . ?
C9 C7 1.563(3) . ?
C8 C7 1.504(3) . ?
C8 H8 0.9800 . ?
C20 C21 1.510(4) . ?
C20 C23 1.516(4) . ?
C20 C22 1.521(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C16 H16 0.9300 . ?
C7 C1 1.489(3) . ?
C7 C10 1.512(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C1 C6 1.385(3) . ?
C1 C2 1.391(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 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
C14 O3 C24 118.0(3) . . ?
C19 O5 C20 121.64(19) . . ?
C19 N1 C2 130.83(18) . . ?
C19 N1 C8 119.40(18) . . ?
C2 N1 C8 109.76(18) . . ?
C17 O2 C18 117.2(3) . . ?
C16 C15 C14 119.7(2) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C14 C13 124.9(2) . . ?
O3 C14 C15 115.0(2) . . ?
C13 C14 C15 120.1(2) . . ?
C14 C13 C12 119.5(2) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C11 C12 C13 120.9(2) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C16 C11 C12 118.5(2) . . ?
C16 C11 C9 121.9(2) . . ?
C12 C11 C9 119.5(2) . . ?
C17 C9 C11 116.43(19) . . ?
C17 C9 C8 113.5(2) . . ?
C11 C9 C8 120.41(18) . . ?
C17 C9 C7 113.55(19) . . ?
C11 C9 C7 121.86(18) . . ?
C8 C9 C7 58.41(15) . . ?
N1 C8 C7 107.15(18) . . ?
N1 C8 C9 116.18(19) . . ?
C7 C8 C9 62.28(15) . . ?
N1 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
O4 C19 O5 127.7(2) . . ?
O4 C19 N1 121.9(2) . . ?
O5 C19 N1 110.33(19) . . ?
O5 C20 C21 109.7(2) . . ?
O5 C20 C23 109.7(2) . . ?
C21 C20 C23 113.5(3) . . ?
O5 C20 C22 101.5(2) . . ?
C21 C20 C22 110.7(2) . . ?
C23 C20 C22 111.1(2) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 C17 O2 123.5(2) . . ?
O1 C17 C9 125.3(3) . . ?
O2 C17 C9 111.2(2) . . ?
O2 C18 H18A 109.5 . . ?
O2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C16 C15 121.1(2) . . ?
C11 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C1 C7 C8 103.73(18) . . ?
C1 C7 C10 118.3(2) . . ?
C8 C7 C10 125.8(2) . . ?
C1 C7 C9 113.39(17) . . ?
C8 C7 C9 59.31(15) . . ?
C10 C7 C9 122.2(2) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C1 C2 120.5(2) . . ?
C6 C1 C7 128.9(2) . . ?
C2 C1 C7 110.55(19) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 N1 130.4(2) . . ?
C1 C2 N1 108.73(18) . . ?
C4 C3 C2 117.3(3) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C5 C4 C3 122.3(3) . . ?
C5 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 118.7(3) . . ?
C5 C6 H6 120.6 . . ?
C1 C6 H6 120.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C24 O3 C14 C13 -3.9(4) . . . . ?
C24 O3 C14 C15 177.6(3) . . . . ?
C16 C15 C14 O3 179.4(2) . . . . ?
C16 C15 C14 C13 0.9(4) . . . . ?
O3 C14 C13 C12 -179.8(2) . . . . ?
C15 C14 C13 C12 -1.4(4) . . . . ?
C14 C13 C12 C11 0.2(3) . . . . ?
C13 C12 C11 C16 1.5(3) . . . . ?
C13 C12 C11 C9 -176.13(19) . . . . ?
C16 C11 C9 C17 -91.2(3) . . . . ?
C12 C11 C9 C17 86.4(3) . . . . ?
C16 C11 C9 C8 124.8(2) . . . . ?
C12 C11 C9 C8 -57.6(3) . . . . ?
C16 C11 C9 C7 55.3(3) . . . . ?
C12 C11 C9 C7 -127.1(2) . . . . ?
C19 N1 C8 C7 -177.46(19) . . . . ?
C2 N1 C8 C7 2.7(2) . . . . ?
C19 N1 C8 C9 115.5(2) . . . . ?
C2 N1 C8 C9 -64.3(2) . . . . ?
C17 C9 C8 N1 -159.4(2) . . . . ?
C11 C9 C8 N1 -14.5(3) . . . . ?
C7 C9 C8 N1 96.5(2) . . . . ?
C17 C9 C8 C7 104.1(2) . . . . ?
C11 C9 C8 C7 -111.0(2) . . . . ?
C20 O5 C19 O4 3.0(4) . . . . ?
C20 O5 C19 N1 -175.86(19) . . . . ?
C2 N1 C19 O4 177.8(2) . . . . ?
C8 N1 C19 O4 -2.1(4) . . . . ?
C2 N1 C19 O5 -3.3(3) . . . . ?
C8 N1 C19 O5 176.86(19) . . . . ?
C19 O5 C20 C21 59.3(3) . . . . ?
C19 O5 C20 C23 -66.0(3) . . . . ?
C19 O5 C20 C22 176.4(2) . . . . ?
C18 O2 C17 O1 0.3(5) . . . . ?
C18 O2 C17 C9 178.7(3) . . . . ?
C11 C9 C17 O1 -151.2(3) . . . . ?
C8 C9 C17 O1 -4.8(4) . . . . ?
C7 C9 C17 O1 59.6(3) . . . . ?
C11 C9 C17 O2 30.5(3) . . . . ?
C8 C9 C17 O2 176.9(2) . . . . ?
C7 C9 C17 O2 -118.7(2) . . . . ?
C12 C11 C16 C15 -2.1(3) . . . . ?
C9 C11 C16 C15 175.49(19) . . . . ?
C14 C15 C16 C11 0.9(4) . . . . ?
N1 C8 C7 C1 -1.8(2) . . . . ?
C9 C8 C7 C1 109.28(19) . . . . ?
N1 C8 C7 C10 139.4(2) . . . . ?
C9 C8 C7 C10 -109.6(3) . . . . ?
N1 C8 C7 C9 -111.1(2) . . . . ?
C17 C9 C7 C1 163.4(2) . . . . ?
C11 C9 C7 C1 16.0(3) . . . . ?
C8 C9 C7 C1 -92.5(2) . . . . ?
C17 C9 C7 C8 -104.1(2) . . . . ?
C11 C9 C7 C8 108.5(2) . . . . ?
C17 C9 C7 C10 11.4(3) . . . . ?
C11 C9 C7 C10 -136.0(2) . . . . ?
C8 C9 C7 C10 115.5(3) . . . . ?
C8 C7 C1 C6 178.3(2) . . . . ?
C10 C7 C1 C6 33.6(4) . . . . ?
C9 C7 C1 C6 -119.6(2) . . . . ?
C8 C7 C1 C2 0.3(2) . . . . ?
C10 C7 C1 C2 -144.4(2) . . . . ?
C9 C7 C1 C2 62.5(2) . . . . ?
C6 C1 C2 C3 1.4(3) . . . . ?
C7 C1 C2 C3 179.6(2) . . . . ?
C6 C1 C2 N1 -176.83(19) . . . . ?
C7 C1 C2 N1 1.3(2) . . . . ?
C19 N1 C2 C3 -0.4(4) . . . . ?
C8 N1 C2 C3 179.5(2) . . . . ?
C19 N1 C2 C1 177.6(2) . . . . ?
C8 N1 C2 C1 -2.5(2) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
N1 C2 C3 C4 177.5(2) . . . . ?
C2 C3 C4 C5 -1.1(4) . . . . ?
C3 C4 C5 C6 1.5(4) . . . . ?
C4 C5 C6 C1 -0.3(4) . . . . ?
C2 C1 C6 C5 -1.1(3) . . . . ?
C7 C1 C6 C5 -178.8(2) . . . . ?

_refine_diff_density_max         0.118
_refine_diff_density_min         -0.106
_refine_diff_density_rms         0.025

