# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_NiHf
_database_code_depnum_ccdc_archive 'CCDC 1503088'
_audit_update_record             
;
2016-11-15 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;

_vrf_PLAT331_NiHf                
;
PROBLEM: Small Average Phenyl   C-C Dist. C8S    -C13S          1.36 Ang.  
RESPONSE: The corresponding benzene molecule is slightly disordered; however,
the positions of the atoms of the two components are too close to properly
model this disorder.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C53 H37 Hf N14 Ni O3, Cl O4, 1.5(C6 H6), C H2 Cl2'
_chemical_formula_sum            'C63 H48 Cl3 Hf N14 Ni O7'
_chemical_formula_weight         1456.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   16.714(2)
_cell_length_b                   19.114(2)
_cell_length_c                   19.356(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.853(3)
_cell_angle_gamma                90
_cell_volume                     5852.1(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4052
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             2924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    2.301
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1019
_exptl_absorpt_correction_T_max  0.1561
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX2 DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16173
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_v_R_equivalents   ?
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.540
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16173
_reflns_number_gt                12473
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0376P)²+1.0686P] 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         16173
_refine_ls_number_parameters     901
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_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
Hf1 Hf 0.23075(2) 0.48275(2) 0.64356(2) 0.01599(5) Uani 1 1 d . . . . .
Ni1 Ni 0.44126(4) 0.58055(3) 0.69963(3) 0.01480(13) Uani 1 1 d . . . . .
O1 O 0.26215(19) 0.57470(17) 0.70287(17) 0.0158(7) Uani 1 1 d . . . . .
O2 O 0.3499(2) 0.44706(19) 0.71036(19) 0.0192(8) Uani 1 1 d . . . . .
O3 O 0.2997(2) 0.52134(18) 0.57703(18) 0.0184(8) Uani 1 1 d . . . . .
N1 N 0.3432(2) 0.5962(2) 0.7383(2) 0.0153(9) Uani 1 1 d . . . . .
N2 N 0.5022(3) 0.6129(2) 0.8066(2) 0.0199(10) Uani 1 1 d . . . . .
N3 N 0.4239(3) 0.4758(2) 0.7089(2) 0.0166(9) Uani 1 1 d . . . . .
N4 N 0.5522(3) 0.5382(2) 0.6876(2) 0.0179(9) Uani 1 1 d . . . . .
N5 N 0.3572(2) 0.5734(2) 0.5981(2) 0.0165(9) Uani 1 1 d . . . . .
N6 N 0.4584(3) 0.6766(2) 0.6524(2) 0.0177(9) Uani 1 1 d . . . . .
C1 C 0.2944(3) 0.6199(3) 0.8434(3) 0.0233(11) Uani 1 1 d . . . . .
H1A H 0.2410 0.5997 0.8123 0.035 Uiso 1 1 calc R U . . .
H1B H 0.2854 0.6688 0.8539 0.035 Uiso 1 1 calc R U . . .
H1C H 0.3146 0.5935 0.8892 0.035 Uiso 1 1 calc R U . . .
C2 C 0.3581(3) 0.6161(2) 0.8052(3) 0.0173(10) Uani 1 1 d . . . . .
C3 C 0.4480(3) 0.6312(3) 0.8434(3) 0.0181(11) Uani 1 1 d . . . . .
C4 C 0.4764(4) 0.6607(3) 0.9122(3) 0.0290(13) Uani 1 1 d . . . . .
H4A H 0.4374 0.6737 0.9364 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5626(4) 0.6711(3) 0.9457(3) 0.0336(15) Uani 1 1 d . . . . .
H5A H 0.5834 0.6912 0.9931 0.040 Uiso 1 1 calc R U . . .
C6 C 0.6170(4) 0.6520(3) 0.9093(3) 0.0310(14) Uani 1 1 d . . . . .
H6A H 0.6763 0.6578 0.9314 0.037 Uiso 1 1 calc R U . . .
C7 C 0.5845(3) 0.6242(3) 0.8396(3) 0.0252(12) Uani 1 1 d . . . . .
H7A H 0.6227 0.6125 0.8142 0.030 Uiso 1 1 calc R U . . .
C8 C 0.4768(4) 0.3549(3) 0.7080(4) 0.0390(17) Uani 1 1 d . . . . .
H8A H 0.4260 0.3413 0.7195 0.059 Uiso 1 1 calc R U . . .
H8B H 0.5269 0.3360 0.7451 0.059 Uiso 1 1 calc R U . . .
H8C H 0.4736 0.3363 0.6600 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4828(3) 0.4335(3) 0.7071(3) 0.0198(11) Uani 1 1 d . . . . .
C10 C 0.5581(3) 0.4675(3) 0.6995(3) 0.0212(12) Uani 1 1 d . . . . .
C11 C 0.6305(3) 0.4307(3) 0.7009(3) 0.0239(12) Uani 1 1 d . . . . .
H11B H 0.6335 0.3817 0.7096 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6972(3) 0.4647(3) 0.6897(3) 0.0263(13) Uani 1 1 d . . . . .
H12B H 0.7468 0.4399 0.6905 0.032 Uiso 1 1 calc R U . . .
C13 C 0.6907(4) 0.5365(3) 0.6773(3) 0.0323(14) Uani 1 1 d . . . . .
H13B H 0.7360 0.5617 0.6695 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6178(3) 0.5703(3) 0.6764(3) 0.0274(13) Uani 1 1 d . . . . .
H14C H 0.6139 0.6192 0.6673 0.033 Uiso 1 1 calc R U . . .
C15 C 0.3013(3) 0.6177(3) 0.4725(3) 0.0279(13) Uani 1 1 d . . . . .
H15A H 0.2834 0.5693 0.4588 0.042 Uiso 1 1 calc R U . . .
H15B H 0.3321 0.6354 0.4408 0.042 Uiso 1 1 calc R U . . .
H15C H 0.2514 0.6469 0.4668 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3577(3) 0.6197(3) 0.5503(3) 0.0179(10) Uani 1 1 d . . . . .
C17 C 0.4169(3) 0.6775(3) 0.5788(3) 0.0198(10) Uani 1 1 d . . . . .
C18 C 0.4305(3) 0.7319(3) 0.5356(3) 0.0270(13) Uani 1 1 d . . . . .
H18A H 0.4013 0.7325 0.4846 0.032 Uiso 1 1 calc R U . . .
C19 C 0.4858(4) 0.7842(3) 0.5671(3) 0.0343(15) Uani 1 1 d . . . . .
H19A H 0.4959 0.8210 0.5378 0.041 Uiso 1 1 calc R U . . .
C20 C 0.5274(4) 0.7837(3) 0.6418(3) 0.0283(13) Uani 1 1 d . . . . .
H20A H 0.5655 0.8202 0.6646 0.034 Uiso 1 1 calc R U . . .
C21 C 0.5118(3) 0.7284(3) 0.6821(3) 0.0220(12) Uani 1 1 d . . . . .
H21A H 0.5405 0.7274 0.7332 0.026 Uiso 1 1 calc R U . . .
N7 N 0.1168(3) 0.5170(2) 0.6731(2) 0.0167(9) Uani 1 1 d . . . . .
N8 N 0.1489(3) 0.4617(2) 0.7926(2) 0.0191(9) Uani 1 1 d . . . . .
N9 N 0.2086(3) 0.3965(2) 0.7134(2) 0.0182(9) Uani 1 1 d . . . . .
N10 N 0.2701(3) 0.2979(2) 0.6692(2) 0.0191(9) Uani 1 1 d . . . . .
N11 N 0.2250(3) 0.3867(2) 0.5755(2) 0.0181(9) Uani 1 1 d . . . . .
N12 N 0.1794(3) 0.4362(2) 0.4525(2) 0.0188(9) Uani 1 1 d . . . . .
N13 N 0.1307(3) 0.5074(2) 0.5357(2) 0.0185(9) Uani 1 1 d . . . . .
N14 N 0.0485(3) 0.5949(2) 0.5734(2) 0.0200(10) Uani 1 1 d . . . . .
C22 C 0.0648(3) 0.5713(3) 0.6413(3) 0.0203(11) Uani 1 1 d . . . . .
C23 C 0.0282(3) 0.6026(3) 0.6919(3) 0.0219(12) Uani 1 1 d . . . . .
C24 C -0.0300(3) 0.6563(3) 0.6850(3) 0.0254(12) Uani 1 1 d . . . . .
H24A H -0.0527 0.6811 0.6404 0.030 Uiso 1 1 calc R U . . .
C25 C -0.0539(4) 0.6725(3) 0.7448(4) 0.0331(15) Uani 1 1 d . . . . .
H25A H -0.0925 0.7097 0.7417 0.040 Uiso 1 1 calc R U . . .
C26 C -0.0223(4) 0.6350(3) 0.8099(4) 0.0328(13) Uani 1 1 d . . . . .
H26A H -0.0402 0.6471 0.8502 0.039 Uiso 1 1 calc R U . . .
C27 C 0.0348(4) 0.5806(3) 0.8170(3) 0.0295(13) Uani 1 1 d . . . . .
H27A H 0.0559 0.5548 0.8612 0.035 Uiso 1 1 calc R U . . .
C28 C 0.0597(3) 0.5655(3) 0.7568(3) 0.0200(10) Uani 1 1 d . . . . .
C29 C 0.1136(3) 0.5113(3) 0.7436(3) 0.0182(10) Uani 1 1 d . . . . .
C30 C 0.1892(3) 0.4077(3) 0.7760(3) 0.0172(10) Uani 1 1 d . . . . .
C31 C 0.2170(3) 0.3481(3) 0.8249(3) 0.0194(12) Uani 1 1 d . . . . .
C32 C 0.2130(3) 0.3343(3) 0.8946(3) 0.0211(10) Uani 1 1 d . . . . .
H32A H 0.1876 0.3663 0.9187 0.025 Uiso 1 1 calc R U . . .
C33 C 0.2477(3) 0.2721(3) 0.9268(3) 0.0226(12) Uani 1 1 d . . . . .
H33A H 0.2471 0.2615 0.9746 0.027 Uiso 1 1 calc R U . . .
C34 C 0.2837(3) 0.2242(3) 0.8907(3) 0.0235(12) Uani 1 1 d . . . . .
H34A H 0.3072 0.1819 0.9146 0.028 Uiso 1 1 calc R U . . .
C35 C 0.2857(3) 0.2370(3) 0.8210(3) 0.0220(12) Uani 1 1 d . . . . .
H35A H 0.3092 0.2041 0.7962 0.026 Uiso 1 1 calc R U . . .
C36 C 0.2520(3) 0.3001(3) 0.7887(3) 0.0201(11) Uani 1 1 d . . . . .
C37 C 0.2453(3) 0.3312(3) 0.7189(3) 0.0180(11) Uani 1 1 d . . . . .
C38 C 0.2596(3) 0.3230(3) 0.6029(3) 0.0180(11) Uani 1 1 d . . . . .
C39 C 0.2784(3) 0.2836(3) 0.5460(3) 0.0214(11) Uani 1 1 d . . . . .
C40 C 0.3159(4) 0.2177(3) 0.5471(3) 0.0282(13) Uani 1 1 d . . . . .
H40A H 0.3357 0.1910 0.5907 0.034 Uiso 1 1 calc R U . . .
C41 C 0.3230(4) 0.1936(3) 0.4829(4) 0.0366(16) Uani 1 1 d . . . . .
H41A H 0.3487 0.1494 0.4821 0.044 Uiso 1 1 calc R U . . .
C42 C 0.2928(4) 0.2329(3) 0.4174(4) 0.0337(14) Uani 1 1 d . . . . .
H42A H 0.2976 0.2144 0.3733 0.040 Uiso 1 1 calc R U . . .
C43 C 0.2563(3) 0.2980(3) 0.4172(3) 0.0270(13) Uani 1 1 d . . . . .
H43A H 0.2361 0.3247 0.3737 0.032 Uiso 1 1 calc R U . . .
C44 C 0.2502(3) 0.3230(3) 0.4827(3) 0.0203(11) Uani 1 1 d . . . . .
C45 C 0.2163(3) 0.3874(3) 0.5018(3) 0.0203(11) Uani 1 1 d . . . . .
C46 C 0.1391(3) 0.4905(3) 0.4694(3) 0.0193(11) Uani 1 1 d . . . . .
C47 C 0.0926(3) 0.5402(3) 0.4148(3) 0.0218(12) Uani 1 1 d . . . . .
C48 C 0.0832(3) 0.5477(3) 0.3406(3) 0.0258(12) Uani 1 1 d . . . . .
H48A H 0.1087 0.5158 0.3164 0.031 Uiso 1 1 calc R U . . .
C49 C 0.0356(3) 0.6029(3) 0.3040(3) 0.0281(13) Uani 1 1 d . . . . .
H49A H 0.0290 0.6099 0.2539 0.034 Uiso 1 1 calc R U . . .
C50 C -0.0037(3) 0.6493(3) 0.3393(3) 0.0304(14) Uani 1 1 d . . . . .
H50A H -0.0365 0.6870 0.3125 0.036 Uiso 1 1 calc R U . . .
C51 C 0.0044(3) 0.6413(3) 0.4126(3) 0.0250(12) Uani 1 1 d . . . . .
H51A H -0.0229 0.6721 0.4364 0.030 Uiso 1 1 calc R U . . .
C52 C 0.0538(3) 0.5868(3) 0.4491(3) 0.0200(11) Uani 1 1 d . . . . .
C53 C 0.0772(3) 0.5644(3) 0.5253(3) 0.0191(11) Uani 1 1 d . . . . .
Cl1 Cl 0.26203(11) 0.75924(11) 0.31362(11) 0.0530(5) Uani 1 1 d . . . . .
O1S O 0.2374(4) 0.8132(3) 0.2625(3) 0.0689(17) Uiso 1 1 d . . . . .
O2S O 0.1944(5) 0.7242(5) 0.3201(6) 0.078(3) Uani 0.742(5) 1 d . U P A 1
O3S O 0.2910(7) 0.8018(7) 0.3851(5) 0.124(4) Uani 0.742(5) 1 d . U P A 1
O4S O 0.3443(4) 0.7327(3) 0.3322(5) 0.057(2) Uani 0.742(5) 1 d . U P A 1
O2X O 0.2193(14) 0.6849(13) 0.2653(15) 0.078(3) Uani 0.258(5) 1 d . U P A 2
O3X O 0.222(2) 0.750(2) 0.3637(16) 0.124(4) Uani 0.258(5) 1 d . U P A 2
O4X O 0.2952(12) 0.7193(10) 0.2617(13) 0.057(2) Uani 0.258(5) 1 d . U P A 2
C1S C 0.1962(16) 0.4784(12) 1.1231(13) 0.072(8) Uani 0.5 1 d . U P B 1
H1SA H 0.1797 0.4315 1.1355 0.087 Uiso 0.5 1 calc R U P B 1
H1SB H 0.2556 0.4869 1.1533 0.087 Uiso 0.5 1 calc R U P B 1
Cl1S Cl 0.1332(6) 0.5398(4) 1.1421(4) 0.0544(17) Uani 0.5 1 d . U P B 1
Cl2S Cl 0.1875(6) 0.4807(4) 1.0260(5) 0.0645(19) Uani 0.5 1 d . U P B 1
C2S C 0.0539(12) 0.5069(10) 1.0195(12) 0.076(6) Uani 0.5 1 d G U P C -2
H2SA H -0.0014 0.5095 0.9850 0.091 Uiso 0.5 1 calc R U P C -2
C3S C 0.0725(11) 0.5353(8) 1.0939(9) 0.049(4) Uani 0.5 1 d G U P C -2
H3SA H 0.0298 0.5575 1.1087 0.059 Uiso 0.5 1 calc R U P C -2
C4S C 0.142(3) 0.530(2) 1.134(3) 0.104(19) Uani 0.5 1 d G U P C -2
H4SA H 0.1519 0.5423 1.1838 0.125 Uiso 0.5 1 calc R U P C -2
C5S C 0.2156(13) 0.5040(11) 1.1142(10) 0.050(5) Uani 0.5 1 d G U P C -2
H5SA H 0.2731 0.5121 1.1419 0.060 Uiso 0.5 1 calc R U P C -2
C6S C 0.184(2) 0.4616(16) 1.0404(19) 0.064(10) Uani 0.5 1 d G U P C -2
H6SA H 0.2175 0.4262 1.0282 0.076 Uiso 0.5 1 calc R U P C -2
C7S C 0.1171(11) 0.4775(9) 1.0021(9) 0.060(4) Uani 0.5 1 d G U P C -2
H7SA H 0.1060 0.4681 0.9517 0.072 Uiso 0.5 1 calc R U P C -2
C8S C 0.4254(5) 0.5424(4) 1.0618(6) 0.073(3) Uani 1 1 d G . . . .
H8SA H 0.3994 0.4986 1.0452 0.088 Uiso 1 1 calc R U . . .
C9S C 0.3779(4) 0.5999(4) 1.0588(4) 0.0463(19) Uani 1 1 d G . . . .
H9SA H 0.3180 0.5961 1.0424 0.056 Uiso 1 1 calc R U . . .
C10S C 0.4144(5) 0.6627(5) 1.0787(4) 0.058(2) Uani 1 1 d G . . . .
H10D H 0.3806 0.7035 1.0736 0.070 Uiso 1 1 calc R U . . .
C11S C 0.5012(5) 0.6674(6) 1.1067(5) 0.081(3) Uani 1 1 d G . . . .
H11A H 0.5269 0.7114 1.1228 0.097 Uiso 1 1 calc R U . . .
C12S C 0.5501(5) 0.6105(6) 1.1115(4) 0.060(2) Uani 1 1 d G . . . .
H12A H 0.6099 0.6143 1.1301 0.072 Uiso 1 1 calc R U . . .
C13S C 0.5130(6) 0.5479(5) 1.0895(6) 0.081(3) Uani 1 1 d G . . . .
H13A H 0.5470 0.5074 1.0930 0.097 Uiso 1 1 calc R U . . .
Cl4S Cl 0.4859(4) 0.4812(3) 0.5080(2) 0.0614(14) Uani 0.5 1 d . . P D -1
Cl3S Cl 0.5372(2) 0.6215(2) 0.4836(2) 0.0592(11) Uani 0.5 1 d . . P D -1
C14S C 0.5650(10) 0.5352(8) 0.4897(8) 0.044(4) Uani 0.5 1 d . . P D -1
H14A H 0.5730 0.5206 0.4449 0.052 Uiso 0.5 1 d R U P D -1
H14B H 0.6177 0.5297 0.5284 0.052 Uiso 0.5 1 d R U P D -1


_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
Hf1 O1 2.072(3) . ?
Hf1 O2 2.107(3) . ?
Hf1 O3 2.119(3) . ?
Hf1 N9 2.239(4) . ?
Hf1 N11 2.243(4) . ?
Hf1 N7 2.255(4) . ?
Hf1 N13 2.262(4) . ?
Ni1 N5 2.018(4) . ?
Ni1 N1 2.032(4) . ?
Ni1 N3 2.039(4) . ?
Ni1 N2 2.084(4) . ?
Ni1 N4 2.105(4) . ?
Ni1 N6 2.112(4) . ?
O1 N1 1.369(5) . ?
O2 N3 1.362(5) . ?
O3 N5 1.352(5) . ?
N1 C2 1.293(6) . ?
N2 C7 1.334(6) . ?
N2 C3 1.365(6) . ?
N3 C9 1.283(6) . ?
N4 C14 1.333(6) . ?
N4 C10 1.367(7) . ?
N5 C16 1.282(6) . ?
N6 C21 1.332(7) . ?
N6 C17 1.367(7) . ?
C1 C2 1.482(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.473(7) . ?
C3 C4 1.382(7) . ?
C4 C5 1.390(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.368(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.387(7) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.507(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.466(7) . ?
C10 C11 1.392(7) . ?
C11 C12 1.367(8) . ?
C11 H11B 0.9500 . ?
C12 C13 1.391(8) . ?
C12 H12B 0.9500 . ?
C13 C14 1.375(8) . ?
C13 H13B 0.9500 . ?
C14 H14C 0.9500 . ?
C15 C16 1.497(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.468(7) . ?
C17 C18 1.398(7) . ?
C18 C19 1.365(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.387(9) . ?
C19 H19A 0.9500 . ?
C20 C21 1.389(7) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
N7 C22 1.366(6) . ?
N7 C29 1.387(7) . ?
N8 C30 1.329(6) . ?
N8 C29 1.336(6) . ?
N9 C30 1.367(6) . ?
N9 C37 1.379(6) . ?
N10 C37 1.326(6) . ?
N10 C38 1.329(6) . ?
N11 C38 1.378(6) . ?
N11 C45 1.388(6) . ?
N12 C45 1.333(7) . ?
N12 C46 1.335(7) . ?
N13 C46 1.373(7) . ?
N13 C53 1.382(6) . ?
N14 C53 1.314(7) . ?
N14 C22 1.333(7) . ?
C22 C23 1.442(8) . ?
C23 C28 1.390(7) . ?
C23 C24 1.391(7) . ?
C24 C25 1.376(8) . ?
C24 H24A 0.9500 . ?
C25 C26 1.396(9) . ?
C25 H25A 0.9500 . ?
C26 C27 1.388(8) . ?
C26 H26A 0.9500 . ?
C27 C28 1.388(7) . ?
C27 H27A 0.9500 . ?
C28 C29 1.449(7) . ?
C30 C31 1.458(7) . ?
C31 C36 1.394(7) . ?
C31 C32 1.396(7) . ?
C32 C33 1.381(7) . ?
C32 H32A 0.9500 . ?
C33 C34 1.399(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.383(7) . ?
C34 H34A 0.9500 . ?
C35 C36 1.390(7) . ?
C35 H35A 0.9500 . ?
C36 C37 1.447(7) . ?
C38 C39 1.450(7) . ?
C39 C44 1.385(7) . ?
C39 C40 1.404(7) . ?
C40 C41 1.366(8) . ?
C40 H40A 0.9500 . ?
C41 C42 1.419(9) . ?
C41 H41A 0.9500 . ?
C42 C43 1.386(8) . ?
C42 H42A 0.9500 . ?
C43 C44 1.387(7) . ?
C43 H43A 0.9500 . ?
C44 C45 1.453(7) . ?
C46 C47 1.447(7) . ?
C47 C52 1.391(8) . ?
C47 C48 1.400(7) . ?
C48 C49 1.372(8) . ?
C48 H48A 0.9500 . ?
C49 C50 1.405(8) . ?
C49 H49A 0.9500 . ?
C50 C51 1.389(8) . ?
C50 H50A 0.9500 . ?
C51 C52 1.376(7) . ?
C51 H51A 0.9500 . ?
C52 C53 1.462(7) . ?
Cl1 O2S 1.353(8) . ?
Cl1 O3X 1.36(3) . ?
Cl1 O1S 1.397(6) . ?
Cl1 O4S 1.399(6) . ?
Cl1 O4X 1.50(2) . ?
Cl1 O3S 1.541(10) . ?
Cl1 O2X 1.72(3) . ?
O2X O4X 1.45(3) . ?
C1S Cl1S 1.69(3) . ?
C1S Cl2S 1.84(3) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.48(3) . ?
C2S C7S 1.33(2) . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.18(5) . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.49(5) . ?
C4S H4SA 0.9500 . ?
C5S C6S 1.58(4) . ?
C5S H5SA 0.9500 . ?
C6S C7S 1.17(4) . ?
C6S H6SA 0.9500 . ?
C7S H7SA 0.9500 . ?
C8S C9S 1.346(10) . ?
C8S C13S 1.391(12) . ?
C8S H8SA 0.9500 . ?
C9S C10S 1.345(10) . ?
C9S H9SA 0.9500 . ?
C10S C11S 1.378(10) . ?
C10S H10D 0.9500 . ?
C11S C12S 1.345(12) . ?
C11S H11A 0.9500 . ?
C12S C13S 1.352(12) . ?
C12S H12A 0.9500 . ?
C13S H13A 0.9500 . ?
Cl4S C14S 1.801(18) . ?
Cl3S C14S 1.707(15) . ?
C14S H14A 0.9598 . ?
C14S H14B 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 O2 85.10(13) . . ?
O1 Hf1 O3 87.21(13) . . ?
O2 Hf1 O3 83.90(13) . . ?
O1 Hf1 N9 110.61(14) . . ?
O2 Hf1 N9 72.47(14) . . ?
O3 Hf1 N9 148.48(14) . . ?
O1 Hf1 N11 167.07(14) . . ?
O2 Hf1 N11 87.03(14) . . ?
O3 Hf1 N11 81.76(14) . . ?
N9 Hf1 N11 76.57(15) . . ?
O1 Hf1 N7 72.34(14) . . ?
O2 Hf1 N7 130.27(14) . . ?
O3 Hf1 N7 136.30(14) . . ?
N9 Hf1 N7 75.06(15) . . ?
N11 Hf1 N7 120.46(15) . . ?
O1 Hf1 N13 108.29(13) . . ?
O2 Hf1 N13 154.65(15) . . ?
O3 Hf1 N13 75.62(15) . . ?
N9 Hf1 N13 119.59(15) . . ?
N11 Hf1 N13 75.52(15) . . ?
N7 Hf1 N13 74.99(16) . . ?
N5 Ni1 N1 88.74(16) . . ?
N5 Ni1 N3 86.86(17) . . ?
N1 Ni1 N3 87.57(16) . . ?
N5 Ni1 N2 161.91(17) . . ?
N1 Ni1 N2 77.48(16) . . ?
N3 Ni1 N2 103.98(17) . . ?
N5 Ni1 N4 103.18(16) . . ?
N1 Ni1 N4 160.37(16) . . ?
N3 Ni1 N4 77.72(16) . . ?
N2 Ni1 N4 93.37(17) . . ?
N5 Ni1 N6 77.64(16) . . ?
N1 Ni1 N6 105.66(16) . . ?
N3 Ni1 N6 159.20(16) . . ?
N2 Ni1 N6 94.67(17) . . ?
N4 Ni1 N6 92.25(16) . . ?
N1 O1 Hf1 124.4(3) . . ?
N3 O2 Hf1 122.7(3) . . ?
N5 O3 Hf1 123.1(3) . . ?
C2 N1 O1 115.4(4) . . ?
C2 N1 Ni1 119.6(3) . . ?
O1 N1 Ni1 123.8(3) . . ?
C7 N2 C3 117.6(5) . . ?
C7 N2 Ni1 128.4(4) . . ?
C3 N2 Ni1 113.6(3) . . ?
C9 N3 O2 117.2(4) . . ?
C9 N3 Ni1 118.9(3) . . ?
O2 N3 Ni1 123.7(3) . . ?
C14 N4 C10 117.6(4) . . ?
C14 N4 Ni1 129.8(4) . . ?
C10 N4 Ni1 112.3(3) . . ?
C16 N5 O3 117.4(4) . . ?
C16 N5 Ni1 119.5(3) . . ?
O3 N5 Ni1 123.1(3) . . ?
C21 N6 C17 118.9(5) . . ?
C21 N6 Ni1 128.6(4) . . ?
C17 N6 Ni1 111.6(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 113.3(4) . . ?
N1 C2 C1 125.2(5) . . ?
C3 C2 C1 121.5(5) . . ?
N2 C3 C4 121.9(5) . . ?
N2 C3 C2 115.4(4) . . ?
C4 C3 C2 122.7(5) . . ?
C3 C4 C5 119.3(6) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C6 C5 C4 118.9(5) . . ?
C6 C5 H5A 120.6 . . ?
C4 C5 H5A 120.6 . . ?
C5 C6 C7 119.1(5) . . ?
C5 C6 H6A 120.4 . . ?
C7 C6 H6A 120.4 . . ?
N2 C7 C6 123.2(5) . . ?
N2 C7 H7A 118.4 . . ?
C6 C7 H7A 118.4 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 114.5(5) . . ?
N3 C9 C8 125.0(5) . . ?
C10 C9 C8 120.4(5) . . ?
N4 C10 C11 121.2(5) . . ?
N4 C10 C9 115.9(4) . . ?
C11 C10 C9 122.9(5) . . ?
C12 C11 C10 120.3(6) . . ?
C12 C11 H11B 119.8 . . ?
C10 C11 H11B 119.8 . . ?
C11 C12 C13 118.3(5) . . ?
C11 C12 H12B 120.9 . . ?
C13 C12 H12B 120.9 . . ?
C14 C13 C12 119.0(5) . . ?
C14 C13 H13B 120.5 . . ?
C12 C13 H13B 120.5 . . ?
N4 C14 C13 123.6(6) . . ?
N4 C14 H14C 118.2 . . ?
C13 C14 H14C 118.2 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 C16 C17 114.1(4) . . ?
N5 C16 C15 124.0(5) . . ?
C17 C16 C15 121.8(5) . . ?
N6 C17 C18 120.4(5) . . ?
N6 C17 C16 115.9(4) . . ?
C18 C17 C16 123.7(5) . . ?
C19 C18 C17 119.7(5) . . ?
C19 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 . . ?
C18 C19 C20 119.9(5) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C19 C20 C21 118.0(5) . . ?
C19 C20 H20A 121.0 . . ?
C21 C20 H20A 121.0 . . ?
N6 C21 C20 123.0(5) . . ?
N6 C21 H21A 118.5 . . ?
C20 C21 H21A 118.5 . . ?
C22 N7 C29 106.3(4) . . ?
C22 N7 Hf1 124.9(3) . . ?
C29 N7 Hf1 122.1(3) . . ?
C30 N8 C29 121.4(5) . . ?
C30 N9 C37 107.5(4) . . ?
C30 N9 Hf1 123.5(3) . . ?
C37 N9 Hf1 123.8(3) . . ?
C37 N10 C38 123.6(4) . . ?
C38 N11 C45 107.2(4) . . ?
C38 N11 Hf1 124.4(3) . . ?
C45 N11 Hf1 124.5(3) . . ?
C45 N12 C46 121.5(5) . . ?
C46 N13 C53 107.8(4) . . ?
C46 N13 Hf1 123.0(3) . . ?
C53 N13 Hf1 123.3(3) . . ?
C53 N14 C22 122.9(5) . . ?
N14 C22 N7 126.8(5) . . ?
N14 C22 C23 122.2(5) . . ?
N7 C22 C23 110.9(5) . . ?
C28 C23 C24 120.8(5) . . ?
C28 C23 C22 106.4(4) . . ?
C24 C23 C22 132.7(5) . . ?
C25 C24 C23 118.0(5) . . ?
C25 C24 H24A 121.0 . . ?
C23 C24 H24A 121.0 . . ?
C24 C25 C26 121.1(5) . . ?
C24 C25 H25A 119.5 . . ?
C26 C25 H25A 119.5 . . ?
C27 C26 C25 121.5(6) . . ?
C27 C26 H26A 119.3 . . ?
C25 C26 H26A 119.3 . . ?
C26 C27 C28 117.1(6) . . ?
C26 C27 H27A 121.5 . . ?
C28 C27 H27A 121.5 . . ?
C27 C28 C23 121.6(5) . . ?
C27 C28 C29 132.0(5) . . ?
C23 C28 C29 106.3(5) . . ?
N8 C29 N7 127.3(5) . . ?
N8 C29 C28 122.6(5) . . ?
N7 C29 C28 110.0(4) . . ?
N8 C30 N9 128.4(5) . . ?
N8 C30 C31 122.0(5) . . ?
N9 C30 C31 109.6(4) . . ?
C36 C31 C32 121.4(5) . . ?
C36 C31 C30 106.5(4) . . ?
C32 C31 C30 132.1(5) . . ?
C33 C32 C31 117.1(5) . . ?
C33 C32 H32A 121.5 . . ?
C31 C32 H32A 121.5 . . ?
C32 C33 C34 121.5(5) . . ?
C32 C33 H33A 119.2 . . ?
C34 C33 H33A 119.2 . . ?
C35 C34 C33 121.4(5) . . ?
C35 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
C34 C35 C36 117.3(5) . . ?
C34 C35 H35A 121.3 . . ?
C36 C35 H35A 121.3 . . ?
C35 C36 C31 121.3(5) . . ?
C35 C36 C37 132.4(5) . . ?
C31 C36 C37 106.3(5) . . ?
N10 C37 N9 127.9(5) . . ?
N10 C37 C36 122.1(5) . . ?
N9 C37 C36 110.0(4) . . ?
N10 C38 N11 126.7(5) . . ?
N10 C38 C39 123.6(5) . . ?
N11 C38 C39 109.6(4) . . ?
C44 C39 C40 121.6(5) . . ?
C44 C39 C38 107.1(5) . . ?
C40 C39 C38 131.3(5) . . ?
C41 C40 C39 117.2(6) . . ?
C41 C40 H40A 121.4 . . ?
C39 C40 H40A 121.4 . . ?
C40 C41 C42 121.6(6) . . ?
C40 C41 H41A 119.2 . . ?
C42 C41 H41A 119.2 . . ?
C43 C42 C41 120.4(6) . . ?
C43 C42 H42A 119.8 . . ?
C41 C42 H42A 119.8 . . ?
C42 C43 C44 118.0(6) . . ?
C42 C43 H43A 121.0 . . ?
C44 C43 H43A 121.0 . . ?
C39 C44 C43 121.1(5) . . ?
C39 C44 C45 106.5(5) . . ?
C43 C44 C45 132.4(5) . . ?
N12 C45 N11 127.8(5) . . ?
N12 C45 C44 122.6(5) . . ?
N11 C45 C44 109.5(5) . . ?
N12 C46 N13 128.6(5) . . ?
N12 C46 C47 121.7(5) . . ?
N13 C46 C47 109.6(5) . . ?
C52 C47 C48 120.6(5) . . ?
C52 C47 C46 107.1(5) . . ?
C48 C47 C46 132.4(6) . . ?
C49 C48 C47 117.6(6) . . ?
C49 C48 H48A 121.2 . . ?
C47 C48 H48A 121.2 . . ?
C48 C49 C50 121.2(5) . . ?
C48 C49 H49A 119.4 . . ?
C50 C49 H49A 119.4 . . ?
C51 C50 C49 121.4(5) . . ?
C51 C50 H50A 119.3 . . ?
C49 C50 H50A 119.3 . . ?
C52 C51 C50 116.9(6) . . ?
C52 C51 H51A 121.6 . . ?
C50 C51 H51A 121.6 . . ?
C51 C52 C47 122.4(5) . . ?
C51 C52 C53 131.3(5) . . ?
C47 C52 C53 106.3(5) . . ?
N14 C53 N13 127.9(5) . . ?
N14 C53 C52 123.0(5) . . ?
N13 C53 C52 109.1(5) . . ?
O2S Cl1 O1S 111.6(4) . . ?
O3X Cl1 O1S 120.2(17) . . ?
O2S Cl1 O4S 125.3(4) . . ?
O1S Cl1 O4S 119.3(4) . . ?
O3X Cl1 O4X 142(2) . . ?
O1S Cl1 O4X 89.4(8) . . ?
O2S Cl1 O3S 102.0(6) . . ?
O1S Cl1 O3S 100.5(6) . . ?
O4S Cl1 O3S 87.9(5) . . ?
O3X Cl1 O2X 94(2) . . ?
O1S Cl1 O2X 104.4(8) . . ?
O4X Cl1 O2X 52.9(11) . . ?
O4X O2X Cl1 55.7(13) . . ?
O2X O4X Cl1 71.4(15) . . ?
Cl1S C1S Cl2S 110.9(13) . . ?
Cl1S C1S H1SA 109.5 . . ?
Cl2S C1S H1SA 109.5 . . ?
Cl1S C1S H1SB 109.5 . . ?
Cl2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 108.1 . . ?
C3S C2S C7S 117.9(17) . . ?
C3S C2S H2SA 121.1 . . ?
C7S C2S H2SA 121.1 . . ?
C2S C3S C4S 118(3) . . ?
C2S C3S H3SA 121.1 . . ?
C4S C3S H3SA 121.1 . . ?
C3S C4S C5S 125(4) . . ?
C3S C4S H4SA 117.3 . . ?
C5S C4S H4SA 117.3 . . ?
C6S C5S C4S 110(3) . . ?
C6S C5S H5SA 124.9 . . ?
C4S C5S H5SA 124.9 . . ?
C5S C6S C7S 114(3) . . ?
C5S C6S H6SA 122.9 . . ?
C7S C6S H6SA 122.9 . . ?
C6S C7S C2S 129(2) . . ?
C6S C7S H7SA 115.5 . . ?
C2S C7S H7SA 115.5 . . ?
C9S C8S C13S 119.3(8) . . ?
C9S C8S H8SA 120.4 . . ?
C13S C8S H8SA 120.4 . . ?
C10S C9S C8S 120.6(7) . . ?
C10S C9S H9SA 119.7 . . ?
C8S C9S H9SA 119.7 . . ?
C9S C10S C11S 119.6(8) . . ?
C9S C10S H10D 120.2 . . ?
C11S C10S H10D 120.2 . . ?
C12S C11S C10S 120.9(9) . . ?
C12S C11S H11A 119.5 . . ?
C10S C11S H11A 119.5 . . ?
C13S C12S C11S 119.2(8) . . ?
C13S C12S H12A 120.4 . . ?
C11S C12S H12A 120.4 . . ?
C12S C13S C8S 120.4(8) . . ?
C12S C13S H13A 119.8 . . ?
C8S C13S H13A 119.8 . . ?
Cl3S C14S Cl4S 111.5(8) . . ?
Cl3S C14S H14A 109.4 . . ?
Cl4S C14S H14A 109.6 . . ?
Cl3S C14S H14B 108.7 . . ?
Cl4S C14S H14B 109.3 . . ?
H14A C14S H14B 108.2 . . ?

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
Hf1 O1 N1 C2 -131.4(4) . . . . ?
Hf1 O1 N1 Ni1 36.2(4) . . . . ?
Hf1 O2 N3 C9 -134.2(4) . . . . ?
Hf1 O2 N3 Ni1 39.8(5) . . . . ?
Hf1 O3 N5 C16 -138.7(4) . . . . ?
Hf1 O3 N5 Ni1 41.8(4) . . . . ?
O1 N1 C2 C3 173.6(4) . . . . ?
Ni1 N1 C2 C3 5.4(6) . . . . ?
O1 N1 C2 C1 -2.8(7) . . . . ?
Ni1 N1 C2 C1 -171.0(4) . . . . ?
C7 N2 C3 C4 0.3(8) . . . . ?
Ni1 N2 C3 C4 -173.2(4) . . . . ?
C7 N2 C3 C2 -178.6(5) . . . . ?
Ni1 N2 C3 C2 7.9(5) . . . . ?
N1 C2 C3 N2 -8.8(6) . . . . ?
C1 C2 C3 N2 167.8(5) . . . . ?
N1 C2 C3 C4 172.4(5) . . . . ?
C1 C2 C3 C4 -11.0(8) . . . . ?
N2 C3 C4 C5 -1.0(9) . . . . ?
C2 C3 C4 C5 177.7(5) . . . . ?
C3 C4 C5 C6 0.2(9) . . . . ?
C4 C5 C6 C7 1.3(9) . . . . ?
C3 N2 C7 C6 1.3(8) . . . . ?
Ni1 N2 C7 C6 173.7(4) . . . . ?
C5 C6 C7 N2 -2.1(9) . . . . ?
O2 N3 C9 C10 175.2(4) . . . . ?
Ni1 N3 C9 C10 1.0(6) . . . . ?
O2 N3 C9 C8 -1.3(8) . . . . ?
Ni1 N3 C9 C8 -175.6(5) . . . . ?
C14 N4 C10 C11 0.9(7) . . . . ?
Ni1 N4 C10 C11 -174.0(4) . . . . ?
C14 N4 C10 C9 -176.3(5) . . . . ?
Ni1 N4 C10 C9 8.8(5) . . . . ?
N3 C9 C10 N4 -6.7(7) . . . . ?
C8 C9 C10 N4 170.0(5) . . . . ?
N3 C9 C10 C11 176.1(5) . . . . ?
C8 C9 C10 C11 -7.2(8) . . . . ?
N4 C10 C11 C12 -0.5(8) . . . . ?
C9 C10 C11 C12 176.6(5) . . . . ?
C10 C11 C12 C13 0.1(8) . . . . ?
C11 C12 C13 C14 -0.2(9) . . . . ?
C10 N4 C14 C13 -1.1(8) . . . . ?
Ni1 N4 C14 C13 172.8(4) . . . . ?
C12 C13 C14 N4 0.7(9) . . . . ?
O3 N5 C16 C17 175.2(4) . . . . ?
Ni1 N5 C16 C17 -5.3(6) . . . . ?
O3 N5 C16 C15 -2.7(7) . . . . ?
Ni1 N5 C16 C15 176.8(4) . . . . ?
C21 N6 C17 C18 0.0(7) . . . . ?
Ni1 N6 C17 C18 -170.3(4) . . . . ?
C21 N6 C17 C16 -178.6(4) . . . . ?
Ni1 N6 C17 C16 11.0(5) . . . . ?
N5 C16 C17 N6 -4.4(6) . . . . ?
C15 C16 C17 N6 173.6(4) . . . . ?
N5 C16 C17 C18 177.0(5) . . . . ?
C15 C16 C17 C18 -5.0(8) . . . . ?
N6 C17 C18 C19 0.3(8) . . . . ?
C16 C17 C18 C19 178.9(5) . . . . ?
C17 C18 C19 C20 -0.9(9) . . . . ?
C18 C19 C20 C21 1.0(9) . . . . ?
C17 N6 C21 C20 0.1(8) . . . . ?
Ni1 N6 C21 C20 168.6(4) . . . . ?
C19 C20 C21 N6 -0.7(8) . . . . ?
C53 N14 C22 N7 5.1(8) . . . . ?
C53 N14 C22 C23 -175.7(5) . . . . ?
C29 N7 C22 N14 -179.6(5) . . . . ?
Hf1 N7 C22 N14 28.8(7) . . . . ?
C29 N7 C22 C23 1.1(5) . . . . ?
Hf1 N7 C22 C23 -150.5(3) . . . . ?
N14 C22 C23 C28 -179.3(5) . . . . ?
N7 C22 C23 C28 0.1(6) . . . . ?
N14 C22 C23 C24 3.6(9) . . . . ?
N7 C22 C23 C24 -177.0(5) . . . . ?
C28 C23 C24 C25 1.4(8) . . . . ?
C22 C23 C24 C25 178.2(6) . . . . ?
C23 C24 C25 C26 -1.6(9) . . . . ?
C24 C25 C26 C27 0.6(9) . . . . ?
C25 C26 C27 C28 0.6(9) . . . . ?
C26 C27 C28 C23 -0.8(8) . . . . ?
C26 C27 C28 C29 -176.3(6) . . . . ?
C24 C23 C28 C27 -0.2(8) . . . . ?
C22 C23 C28 C27 -177.8(5) . . . . ?
C24 C23 C28 C29 176.3(5) . . . . ?
C22 C23 C28 C29 -1.2(6) . . . . ?
C30 N8 C29 N7 -3.8(8) . . . . ?
C30 N8 C29 C28 171.5(5) . . . . ?
C22 N7 C29 N8 173.9(5) . . . . ?
Hf1 N7 C29 N8 -33.5(7) . . . . ?
C22 N7 C29 C28 -1.9(5) . . . . ?
Hf1 N7 C29 C28 150.8(3) . . . . ?
C27 C28 C29 N8 2.0(9) . . . . ?
C23 C28 C29 N8 -174.0(5) . . . . ?
C27 C28 C29 N7 178.0(5) . . . . ?
C23 C28 C29 N7 2.0(6) . . . . ?
C29 N8 C30 N9 6.8(8) . . . . ?
C29 N8 C30 C31 -170.8(4) . . . . ?
C37 N9 C30 N8 -175.8(5) . . . . ?
Hf1 N9 C30 N8 28.8(7) . . . . ?
C37 N9 C30 C31 1.9(5) . . . . ?
Hf1 N9 C30 C31 -153.4(3) . . . . ?
N8 C30 C31 C36 176.6(4) . . . . ?
N9 C30 C31 C36 -1.4(5) . . . . ?
N8 C30 C31 C32 -2.8(8) . . . . ?
N9 C30 C31 C32 179.2(5) . . . . ?
C36 C31 C32 C33 2.1(7) . . . . ?
C30 C31 C32 C33 -178.6(5) . . . . ?
C31 C32 C33 C34 -1.3(8) . . . . ?
C32 C33 C34 C35 -0.3(8) . . . . ?
C33 C34 C35 C36 1.1(8) . . . . ?
C34 C35 C36 C31 -0.4(7) . . . . ?
C34 C35 C36 C37 178.3(5) . . . . ?
C32 C31 C36 C35 -1.2(8) . . . . ?
C30 C31 C36 C35 179.3(4) . . . . ?
C32 C31 C36 C37 179.8(4) . . . . ?
C30 C31 C36 C37 0.3(5) . . . . ?
C38 N10 C37 N9 -2.8(8) . . . . ?
C38 N10 C37 C36 175.3(5) . . . . ?
C30 N9 C37 N10 176.5(5) . . . . ?
Hf1 N9 C37 N10 -28.2(7) . . . . ?
C30 N9 C37 C36 -1.7(5) . . . . ?
Hf1 N9 C37 C36 153.5(3) . . . . ?
C35 C36 C37 N10 3.6(9) . . . . ?
C31 C36 C37 N10 -177.5(5) . . . . ?
C35 C36 C37 N9 -178.0(5) . . . . ?
C31 C36 C37 N9 0.9(6) . . . . ?
C37 N10 C38 N11 2.2(8) . . . . ?
C37 N10 C38 C39 -173.1(5) . . . . ?
C45 N11 C38 N10 -172.3(5) . . . . ?
Hf1 N11 C38 N10 29.4(7) . . . . ?
C45 N11 C38 C39 3.5(5) . . . . ?
Hf1 N11 C38 C39 -154.8(3) . . . . ?
N10 C38 C39 C44 172.8(5) . . . . ?
N11 C38 C39 C44 -3.2(6) . . . . ?
N10 C38 C39 C40 -6.1(9) . . . . ?
N11 C38 C39 C40 177.9(5) . . . . ?
C44 C39 C40 C41 -0.6(8) . . . . ?
C38 C39 C40 C41 178.3(5) . . . . ?
C39 C40 C41 C42 -0.7(9) . . . . ?
C40 C41 C42 C43 1.1(9) . . . . ?
C41 C42 C43 C44 -0.2(8) . . . . ?
C40 C39 C44 C43 1.5(8) . . . . ?
C38 C39 C44 C43 -177.6(5) . . . . ?
C40 C39 C44 C45 -179.4(5) . . . . ?
C38 C39 C44 C45 1.5(6) . . . . ?
C42 C43 C44 C39 -1.1(8) . . . . ?
C42 C43 C44 C45 -179.8(5) . . . . ?
C46 N12 C45 N11 -5.2(8) . . . . ?
C46 N12 C45 C44 171.2(5) . . . . ?
C38 N11 C45 N12 174.1(5) . . . . ?
Hf1 N11 C45 N12 -27.6(7) . . . . ?
C38 N11 C45 C44 -2.6(5) . . . . ?
Hf1 N11 C45 C44 155.7(3) . . . . ?
C39 C44 C45 N12 -176.3(5) . . . . ?
C43 C44 C45 N12 2.6(9) . . . . ?
C39 C44 C45 N11 0.7(6) . . . . ?
C43 C44 C45 N11 179.5(5) . . . . ?
C45 N12 C46 N13 2.5(8) . . . . ?
C45 N12 C46 C47 -174.5(5) . . . . ?
C53 N13 C46 N12 -174.5(5) . . . . ?
Hf1 N13 C46 N12 31.8(7) . . . . ?
C53 N13 C46 C47 2.8(5) . . . . ?
Hf1 N13 C46 C47 -150.9(3) . . . . ?
N12 C46 C47 C52 175.9(5) . . . . ?
N13 C46 C47 C52 -1.6(6) . . . . ?
N12 C46 C47 C48 -5.0(9) . . . . ?
N13 C46 C47 C48 177.5(5) . . . . ?
C52 C47 C48 C49 0.9(8) . . . . ?
C46 C47 C48 C49 -178.1(5) . . . . ?
C47 C48 C49 C50 -1.3(8) . . . . ?
C48 C49 C50 C51 0.3(9) . . . . ?
C49 C50 C51 C52 1.2(8) . . . . ?
C50 C51 C52 C47 -1.6(8) . . . . ?
C50 C51 C52 C53 178.5(5) . . . . ?
C48 C47 C52 C51 0.6(8) . . . . ?
C46 C47 C52 C51 179.8(5) . . . . ?
C48 C47 C52 C53 -179.5(4) . . . . ?
C46 C47 C52 C53 -0.2(5) . . . . ?
C22 N14 C53 N13 -3.8(8) . . . . ?
C22 N14 C53 C52 174.9(5) . . . . ?
C46 N13 C53 N14 175.9(5) . . . . ?
Hf1 N13 C53 N14 -30.5(7) . . . . ?
C46 N13 C53 C52 -3.0(5) . . . . ?
Hf1 N13 C53 C52 150.7(3) . . . . ?
C51 C52 C53 N14 3.0(9) . . . . ?
C47 C52 C53 N14 -176.9(5) . . . . ?
C51 C52 C53 N13 -178.1(5) . . . . ?
C47 C52 C53 N13 2.0(5) . . . . ?
O3X Cl1 O2X O4X -159.6(19) . . . . ?
O1S Cl1 O2X O4X 78.0(12) . . . . ?
O3X Cl1 O4X O2X 34(3) . . . . ?
O1S Cl1 O4X O2X -108.7(11) . . . . ?
C7S C2S C3S C4S -1(4) . . . . ?
C2S C3S C4S C5S 8(6) . . . . ?
C3S C4S C5S C6S -20(5) . . . . ?
C4S C5S C6S C7S 26(4) . . . . ?
C5S C6S C7S C2S -25(4) . . . . ?
C3S C2S C7S C6S 12(4) . . . . ?
C13S C8S C9S C10S 3.4(14) . . . . ?
C8S C9S C10S C11S -4.0(13) . . . . ?
C9S C10S C11S C12S 2.8(14) . . . . ?
C10S C11S C12S C13S -1.0(14) . . . . ?
C11S C12S C13S C8S 0.4(14) . . . . ?
C9S C8S C13S C12S -1.6(15) . . . . ?

_refine_diff_density_max         1.340
_refine_diff_density_min         -1.522
_refine_diff_density_rms         0.144

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_FeZr
_database_code_depnum_ccdc_archive 'CCDC 1503089'
_audit_update_record             
;
2016-09-06 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;

_vrf_RINTA01_FeZr                
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Due to a low reflective power of the sample, only few
reflections at high angles were observed. Nevertheless,
the quality of the data is clearly sufficient to establish 
the connectivity of the structure.
;
_vrf_PLAT971_FeZr                
;
PROBLEM: Check Calcd Residual Density  1.08A From      N3       3.83 eA-3  
RESPONSE: High absoption effects have not been fully corrected for.
;
_vrf_PLAT020_FeZr                
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.189 Report
RESPONSE: Due to a low reflective power of the sample, only few
reflections at high angles were observed. Nevertheless,
the quality of the data is clearly sufficient to establish 
the connectivity of the structure.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H37 Fe N14 O3 Zr, Cl O4'
_chemical_formula_sum            'C53 H37 Cl Fe N14 O7 Zr'
_chemical_formula_weight         1164.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.7726(16)
_cell_length_b                   12.7063(16)
_cell_length_c                   29.868(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.255(2)
_cell_angle_gamma                90
_cell_volume                     4770.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4420
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_F_000             2368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.652
_shelx_estimated_absorpt_T_min   0.804
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3667
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX2 DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75600
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_av_R_equivalents  0.1888
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.746
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9372
_reflns_number_gt                6010
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0780P)²+2.0766P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9372
_refine_ls_number_parameters     697
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.1076
_refine_ls_wR_factor_ref         0.2488
_refine_ls_wR_factor_gt          0.2301
_refine_ls_goodness_of_fit_ref   1.558
_refine_ls_restrained_S_all      1.559
_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
Zr01 Zr 0.31765(6) 0.49505(6) 0.42229(3) 0.0253(2) Uani 1 1 d . . . . .
Fe1 Fe 0.15826(10) 0.54024(9) 0.30712(4) 0.0299(3) Uani 1 1 d . . . . .
O1 O 0.2995(5) 0.6363(5) 0.3807(2) 0.0357(15) Uani 1 1 d . . . . .
O2 O 0.1522(5) 0.4801(5) 0.3994(2) 0.0372(15) Uani 1 1 d . . . . .
O3 O 0.3304(5) 0.4260(4) 0.3592(2) 0.0352(15) Uani 1 1 d . . . . .
N1 N 0.2083(5) 0.6476(5) 0.3482(2) 0.0304(17) Uani 1 1 d . . . . .
N2 N 0.0372(5) 0.6351(5) 0.2948(2) 0.0293(17) Uani 1 1 d . . . . .
N3 N 0.1090(5) 0.4656(6) 0.3528(3) 0.039(2) Uani 1 1 d . U . . .
N4 N 0.0811(6) 0.4238(5) 0.2716(2) 0.0304(17) Uani 1 1 d . . . . .
N5 N 0.2904(6) 0.4765(5) 0.3190(3) 0.0351(19) Uani 1 1 d . . . . .
N6 N 0.2184(6) 0.5953(5) 0.2555(2) 0.0311(17) Uani 1 1 d . . . . .
C1 C 0.1899(7) 0.8255(7) 0.3786(3) 0.035(2) Uani 1 1 d . . . . .
H1A H 0.2659 0.8190 0.3912 0.053 Uiso 1 1 calc R U . . .
H1B H 0.1491 0.8268 0.4034 0.053 Uiso 1 1 calc R U . . .
H1C H 0.1775 0.8910 0.3611 0.053 Uiso 1 1 calc R U . . .
C2 C 0.1555(7) 0.7344(7) 0.3483(3) 0.030(2) Uani 1 1 d . . . . .
C3 C 0.0547(6) 0.7291(6) 0.3169(3) 0.0264(19) Uani 1 1 d . . . . .
C4 C -0.0197(7) 0.8110(7) 0.3104(3) 0.035(2) Uani 1 1 d . . . . .
H4A H -0.0064 0.8754 0.3266 0.042 Uiso 1 1 calc R U . . .
C5 C -0.1145(7) 0.7952(7) 0.2795(4) 0.045(3) Uani 1 1 d . . . . .
H5A H -0.1660 0.8498 0.2739 0.054 Uiso 1 1 calc R U . . .
C6 C -0.1322(7) 0.7022(7) 0.2578(3) 0.038(2) Uani 1 1 d . . . . .
H6A H -0.1969 0.6899 0.2373 0.045 Uiso 1 1 calc R U . . .
C7 C -0.0534(7) 0.6235(7) 0.2660(3) 0.040(2) Uani 1 1 d . . . . .
H7A H -0.0661 0.5588 0.2500 0.048 Uiso 1 1 calc R U . . .
C8 C 0.0012(7) 0.3288(7) 0.3798(3) 0.036(2) Uani 1 1 d . . . . .
H8A H -0.0046 0.3742 0.4058 0.055 Uiso 1 1 calc R U . . .
H8B H 0.0502 0.2707 0.3900 0.055 Uiso 1 1 calc R U . . .
H8C H -0.0690 0.3004 0.3670 0.055 Uiso 1 1 calc R U . . .
C9 C 0.0419(7) 0.3904(7) 0.3450(3) 0.031(2) Uani 1 1 d . . . . .
C10 C 0.0167(7) 0.3687(7) 0.2965(3) 0.034(2) Uani 1 1 d . . . . .
C11 C -0.0529(8) 0.2928(8) 0.2771(3) 0.044(3) Uani 1 1 d . . . . .
H11A H -0.0980 0.2571 0.2942 0.053 Uiso 1 1 calc R U . . .
C12 C -0.0553(9) 0.2699(8) 0.2316(3) 0.050(3) Uani 1 1 d . . . . .
H12A H -0.1025 0.2172 0.2174 0.060 Uiso 1 1 calc R U . . .
C13 C 0.0090(8) 0.3218(7) 0.2066(3) 0.043(3) Uani 1 1 d . . . . .
H13A H 0.0088 0.3049 0.1757 0.052 Uiso 1 1 calc R U . . .
C14 C 0.0741(8) 0.3999(7) 0.2286(3) 0.039(2) Uani 1 1 d . . . . .
H14A H 0.1165 0.4387 0.2113 0.047 Uiso 1 1 calc R U . . .
C15 C 0.4654(8) 0.4375(8) 0.2958(4) 0.050(3) Uani 1 1 d . . . . .
H15A H 0.4717 0.3802 0.3180 0.074 Uiso 1 1 calc R U . . .
H15B H 0.5180 0.4922 0.3066 0.074 Uiso 1 1 calc R U . . .
H15C H 0.4782 0.4102 0.2665 0.074 Uiso 1 1 calc R U . . .
C16 C 0.3573(7) 0.4830(7) 0.2899(3) 0.036(2) Uani 1 1 d . . . . .
C17 C 0.3137(7) 0.5518(7) 0.2522(3) 0.035(2) Uani 1 1 d . . . . .
C18 C 0.3670(9) 0.5753(8) 0.2158(3) 0.046(3) Uani 1 1 d . . . . .
H18A H 0.4342 0.5438 0.2151 0.056 Uiso 1 1 calc R U . . .
C19 C 0.3246(7) 0.6416(7) 0.1818(3) 0.040(3) Uani 1 1 d . . . . .
H19A H 0.3568 0.6533 0.1559 0.048 Uiso 1 1 calc R U . . .
C20 C 0.2276(8) 0.6931(6) 0.1875(3) 0.035(2) Uani 1 1 d . . . . .
H20A H 0.1975 0.7456 0.1665 0.042 Uiso 1 1 calc R U . . .
C21 C 0.1775(7) 0.6665(7) 0.2238(3) 0.036(2) Uani 1 1 d . . . . .
H21A H 0.1121 0.6998 0.2262 0.043 Uiso 1 1 calc R U . . .
N7 N 0.3337(6) 0.6211(5) 0.4751(2) 0.0315(18) Uani 1 1 d . . . . .
N8 N 0.4701(6) 0.7293(6) 0.4513(3) 0.037(2) Uani 1 1 d . . . . .
N9 N 0.4855(6) 0.5484(5) 0.4296(3) 0.0338(18) Uani 1 1 d . . . . .
N10 N 0.5646(6) 0.3927(6) 0.4025(3) 0.043(2) Uani 1 1 d . . . . .
N11 N 0.4115(5) 0.3455(5) 0.4354(2) 0.0284(17) Uani 1 1 d . . . . .
N12 N 0.2774(6) 0.2374(5) 0.4607(2) 0.0303(17) Uani 1 1 d . . . . .
N13 N 0.2575(5) 0.4194(5) 0.4803(2) 0.0278(17) Uani 1 1 d . . . . .
N14 N 0.1927(6) 0.5720(5) 0.5165(2) 0.0338(18) Uani 1 1 d . . . . .
C22 C 0.2585(8) 0.6393(7) 0.5031(3) 0.037(2) Uani 1 1 d . . . . .
C23 C 0.2640(8) 0.7508(7) 0.5153(3) 0.041(2) Uani 1 1 d . . . . .
C24 C 0.2020(9) 0.8117(7) 0.5398(3) 0.049(3) Uani 1 1 d . . . . .
H24A H 0.1479 0.7807 0.5535 0.059 Uiso 1 1 calc R U . . .
C25 C 0.2226(9) 0.9186(8) 0.5432(3) 0.048(3) Uani 1 1 d . . . . .
H25A H 0.1808 0.9628 0.5587 0.057 Uiso 1 1 calc R U . . .
C26 C 0.3046(9) 0.9612(8) 0.5239(4) 0.052(3) Uani 1 1 d . . . . .
H26A H 0.3180 1.0346 0.5271 0.062 Uiso 1 1 calc R U . . .
C27 C 0.3665(9) 0.9031(7) 0.5007(3) 0.045(3) Uani 1 1 d . . . . .
H27A H 0.4226 0.9338 0.4881 0.054 Uiso 1 1 calc R U . . .
C28 C 0.3431(8) 0.7950(7) 0.4965(3) 0.036(2) Uani 1 1 d . . . . .
C29 C 0.3886(8) 0.7141(6) 0.4719(3) 0.034(2) Uani 1 1 d . . . . .
C30 C 0.5161(7) 0.6516(7) 0.4317(3) 0.034(2) Uani 1 1 d . . . . .
C31 C 0.6052(7) 0.6663(8) 0.4101(3) 0.038(2) Uani 1 1 d . . . . .
C32 C 0.6642(8) 0.7570(8) 0.4011(3) 0.046(3) Uani 1 1 d . . . . .
H32A H 0.6473 0.8249 0.4110 0.055 Uiso 1 1 calc R U . . .
C33 C 0.7453(7) 0.7426(9) 0.3778(4) 0.046(3) Uani 1 1 d . . . . .
H33A H 0.7838 0.8026 0.3708 0.056 Uiso 1 1 calc R U . . .
C34 C 0.7748(8) 0.6438(9) 0.3637(4) 0.055(3) Uani 1 1 d . . . . .
H34A H 0.8328 0.6379 0.3479 0.066 Uiso 1 1 calc R U . . .
C35 C 0.7192(8) 0.5526(9) 0.3728(4) 0.052(3) Uani 1 1 d . . . . .
H35A H 0.7376 0.4848 0.3633 0.063 Uiso 1 1 calc R U . . .
C36 C 0.6355(7) 0.5678(7) 0.3964(3) 0.038(2) Uani 1 1 d . . . . .
C37 C 0.5608(7) 0.4944(8) 0.4100(3) 0.040(2) Uani 1 1 d . . . . .
C38 C 0.4941(7) 0.3249(7) 0.4141(3) 0.032(2) Uani 1 1 d . . . . .
C39 C 0.4974(6) 0.2132(7) 0.4028(3) 0.031(2) Uani 1 1 d . . . . .
C40 C 0.5599(7) 0.1544(7) 0.3802(3) 0.035(2) Uani 1 1 d . . . . .
H40A H 0.6179 0.1853 0.3690 0.042 Uiso 1 1 calc R U . . .
C41 C 0.5373(7) 0.0501(8) 0.3738(3) 0.042(2) Uani 1 1 d . . . . .
H41A H 0.5811 0.0077 0.3586 0.050 Uiso 1 1 calc R U . . .
C42 C 0.4507(7) 0.0041(7) 0.3894(3) 0.036(2) Uani 1 1 d . . . . .
H42A H 0.4363 -0.0686 0.3839 0.043 Uiso 1 1 calc R U . . .
C43 C 0.3865(7) 0.0618(7) 0.4123(3) 0.032(2) Uani 1 1 d . . . . .
H43A H 0.3282 0.0307 0.4231 0.039 Uiso 1 1 calc R U . . .
C44 C 0.4106(7) 0.1682(6) 0.4189(3) 0.029(2) Uani 1 1 d . . . . .
C45 C 0.3602(7) 0.2531(6) 0.4398(3) 0.0263(19) Uani 1 1 d . . . . .
C46 C 0.2343(7) 0.3153(6) 0.4806(3) 0.028(2) Uani 1 1 d . . . . .
C47 C 0.1490(7) 0.2966(7) 0.5061(3) 0.031(2) Uani 1 1 d . . . . .
C48 C 0.0954(7) 0.2063(7) 0.5166(3) 0.040(2) Uani 1 1 d . . . . .
H48A H 0.1115 0.1393 0.5055 0.048 Uiso 1 1 calc R U . . .
C49 C 0.0198(8) 0.2164(8) 0.5432(4) 0.045(3) Uani 1 1 d . . . . .
H49A H -0.0152 0.1554 0.5515 0.054 Uiso 1 1 calc R U . . .
C50 C -0.0070(8) 0.3147(8) 0.5582(4) 0.045(3) Uani 1 1 d . . . . .
H50A H -0.0624 0.3198 0.5755 0.054 Uiso 1 1 calc R U . . .
C51 C 0.0446(7) 0.4049(8) 0.5488(3) 0.038(2) Uani 1 1 d . . . . .
H51A H 0.0263 0.4715 0.5596 0.046 Uiso 1 1 calc R U . . .
C52 C 0.1240(7) 0.3954(6) 0.5230(3) 0.033(2) Uani 1 1 d . . . . .
C53 C 0.1923(7) 0.4700(6) 0.5061(3) 0.033(2) Uani 1 1 d . . . . .
Cl1S Cl -0.3354(2) 0.55228(19) 0.16851(9) 0.0457(6) Uani 1 1 d . . . . .
O1S O -0.2527(10) 0.4812(7) 0.1718(5) 0.141(6) Uani 1 1 d . . . . .
O2S O -0.2995(5) 0.6549(5) 0.1577(2) 0.0469(18) Uani 1 1 d . . . . .
O3S O -0.4179(13) 0.5215(11) 0.1349(4) 0.196(9) Uani 1 1 d . . . . .
O4S O -0.3725(7) 0.5536(5) 0.2095(3) 0.064(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr01 O2 2.111(6) . ?
Zr01 O3 2.112(6) . ?
Zr01 O1 2.170(6) . ?
Zr01 N9 2.222(7) . ?
Zr01 N7 2.232(7) . ?
Zr01 N13 2.233(7) . ?
Zr01 N11 2.244(7) . ?
Fe1 N5 1.848(8) . ?
Fe1 N3 1.860(9) . ?
Fe1 N1 1.869(7) . ?
Fe1 N2 1.944(7) . ?
Fe1 N6 1.968(7) . ?
Fe1 N4 1.978(7) . ?
O1 N1 1.386(8) . ?
O2 N3 1.415(10) . ?
O3 N5 1.375(9) . ?
N1 C2 1.293(10) . ?
N2 C7 1.321(10) . ?
N2 C3 1.364(11) . ?
N3 C9 1.276(10) . ?
N4 C14 1.306(11) . ?
N4 C10 1.394(11) . ?
N5 C16 1.327(12) . ?
N6 C21 1.347(11) . ?
N6 C17 1.357(11) . ?
C1 C2 1.487(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.453(11) . ?
C3 C4 1.399(11) . ?
C4 C5 1.400(13) . ?
C4 H4A 0.9500 . ?
C5 C6 1.347(13) . ?
C5 H5A 0.9500 . ?
C6 C7 1.409(12) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.468(12) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.454(12) . ?
C10 C11 1.369(12) . ?
C11 C12 1.383(14) . ?
C11 H11A 0.9500 . ?
C12 C13 1.373(14) . ?
C12 H12A 0.9500 . ?
C13 C14 1.382(12) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.477(13) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.456(12) . ?
C17 C18 1.414(13) . ?
C18 C19 1.356(13) . ?
C18 H18A 0.9500 . ?
C19 C20 1.438(14) . ?
C19 H19A 0.9500 . ?
C20 C21 1.394(13) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
N7 C29 1.385(11) . ?
N7 C22 1.401(12) . ?
N8 C29 1.315(12) . ?
N8 C30 1.335(12) . ?
N9 C30 1.367(11) . ?
N9 C37 1.392(13) . ?
N10 C37 1.315(12) . ?
N10 C38 1.334(11) . ?
N11 C38 1.351(11) . ?
N11 C45 1.362(10) . ?
N12 C46 1.325(11) . ?
N12 C45 1.334(11) . ?
N13 C46 1.357(10) . ?
N13 C53 1.388(12) . ?
N14 C22 1.310(12) . ?
N14 C53 1.333(11) . ?
C22 C23 1.461(12) . ?
C23 C28 1.362(13) . ?
C23 C24 1.403(14) . ?
C24 C25 1.384(13) . ?
C24 H24A 0.9500 . ?
C25 C26 1.393(15) . ?
C25 H25A 0.9500 . ?
C26 C27 1.357(15) . ?
C26 H26A 0.9500 . ?
C27 C28 1.408(12) . ?
C27 H27A 0.9500 . ?
C28 C29 1.443(13) . ?
C30 C31 1.416(13) . ?
C31 C36 1.393(14) . ?
C31 C32 1.429(12) . ?
C32 C33 1.360(14) . ?
C32 H32A 0.9500 . ?
C33 C34 1.398(15) . ?
C33 H33A 0.9500 . ?
C34 C35 1.409(14) . ?
C34 H34A 0.9500 . ?
C35 C36 1.397(14) . ?
C35 H35A 0.9500 . ?
C36 C37 1.442(12) . ?
C38 C39 1.462(12) . ?
C39 C40 1.358(12) . ?
C39 C44 1.406(12) . ?
C40 C41 1.362(13) . ?
C40 H40A 0.9500 . ?
C41 C42 1.401(13) . ?
C41 H41A 0.9500 . ?
C42 C43 1.370(12) . ?
C42 H42A 0.9500 . ?
C43 C44 1.393(12) . ?
C43 H43A 0.9500 . ?
C44 C45 1.453(12) . ?
C46 C47 1.455(12) . ?
C47 C48 1.401(12) . ?
C47 C52 1.411(12) . ?
C48 C49 1.360(13) . ?
C48 H48A 0.9500 . ?
C49 C50 1.392(14) . ?
C49 H49A 0.9500 . ?
C50 C51 1.376(13) . ?
C50 H50A 0.9500 . ?
C51 C52 1.384(13) . ?
C51 H51A 0.9500 . ?
C52 C53 1.439(12) . ?
Cl1S O3S 1.376(10) . ?
Cl1S O1S 1.381(9) . ?
Cl1S O4S 1.389(7) . ?
Cl1S O2S 1.438(7) . ?

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 Zr01 O3 84.5(2) . . ?
O2 Zr01 O1 83.7(2) . . ?
O3 Zr01 O1 81.4(2) . . ?
O2 Zr01 N9 162.2(2) . . ?
O3 Zr01 N9 89.3(3) . . ?
O1 Zr01 N9 78.9(2) . . ?
O2 Zr01 N7 104.8(3) . . ?
O3 Zr01 N7 156.5(2) . . ?
O1 Zr01 N7 78.3(2) . . ?
N9 Zr01 N7 75.3(3) . . ?
O2 Zr01 N13 75.5(2) . . ?
O3 Zr01 N13 127.3(2) . . ?
O1 Zr01 N13 141.5(3) . . ?
N9 Zr01 N13 120.9(3) . . ?
N7 Zr01 N13 76.2(2) . . ?
O2 Zr01 N11 116.9(2) . . ?
O3 Zr01 N11 71.3(2) . . ?
O1 Zr01 N11 143.0(3) . . ?
N9 Zr01 N11 76.4(3) . . ?
N7 Zr01 N11 120.4(3) . . ?
N13 Zr01 N11 75.4(3) . . ?
N5 Fe1 N3 93.0(3) . . ?
N5 Fe1 N1 90.0(3) . . ?
N3 Fe1 N1 90.7(3) . . ?
N5 Fe1 N2 167.6(3) . . ?
N3 Fe1 N2 95.4(3) . . ?
N1 Fe1 N2 80.8(3) . . ?
N5 Fe1 N6 80.6(3) . . ?
N3 Fe1 N6 170.0(3) . . ?
N1 Fe1 N6 96.8(3) . . ?
N2 Fe1 N6 92.2(3) . . ?
N5 Fe1 N4 97.2(3) . . ?
N3 Fe1 N4 79.1(3) . . ?
N1 Fe1 N4 167.8(3) . . ?
N2 Fe1 N4 93.4(3) . . ?
N6 Fe1 N4 94.1(3) . . ?
N1 O1 Zr01 118.6(4) . . ?
N3 O2 Zr01 121.6(5) . . ?
N5 O3 Zr01 120.6(5) . . ?
C2 N1 O1 117.4(7) . . ?
C2 N1 Fe1 120.5(6) . . ?
O1 N1 Fe1 122.1(5) . . ?
C7 N2 C3 117.5(7) . . ?
C7 N2 Fe1 129.0(6) . . ?
C3 N2 Fe1 113.3(5) . . ?
C9 N3 O2 114.0(8) . . ?
C9 N3 Fe1 123.6(7) . . ?
O2 N3 Fe1 122.1(5) . . ?
C14 N4 C10 117.6(8) . . ?
C14 N4 Fe1 130.0(6) . . ?
C10 N4 Fe1 112.0(6) . . ?
C16 N5 O3 114.7(7) . . ?
C16 N5 Fe1 121.3(6) . . ?
O3 N5 Fe1 123.8(6) . . ?
C21 N6 C17 117.5(8) . . ?
C21 N6 Fe1 129.3(7) . . ?
C17 N6 Fe1 113.1(6) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 111.2(8) . . ?
N1 C2 C1 124.6(8) . . ?
C3 C2 C1 124.1(8) . . ?
N2 C3 C4 122.3(8) . . ?
N2 C3 C2 113.8(7) . . ?
C4 C3 C2 123.9(8) . . ?
C3 C4 C5 118.1(9) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
C6 C5 C4 119.6(8) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C7 119.1(8) . . ?
C5 C6 H6A 120.5 . . ?
C7 C6 H6A 120.5 . . ?
N2 C7 C6 123.3(9) . . ?
N2 C7 H7A 118.4 . . ?
C6 C7 H7A 118.4 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 110.2(8) . . ?
N3 C9 C8 125.6(9) . . ?
C10 C9 C8 124.1(8) . . ?
C11 C10 N4 121.9(9) . . ?
C11 C10 C9 124.6(9) . . ?
N4 C10 C9 113.0(7) . . ?
C10 C11 C12 117.6(10) . . ?
C10 C11 H11A 121.2 . . ?
C12 C11 H11A 121.2 . . ?
C13 C12 C11 121.5(9) . . ?
C13 C12 H12A 119.3 . . ?
C11 C12 H12A 119.3 . . ?
C12 C13 C14 117.0(9) . . ?
C12 C13 H13A 121.5 . . ?
C14 C13 H13A 121.5 . . ?
N4 C14 C13 124.4(9) . . ?
N4 C14 H14A 117.8 . . ?
C13 C14 H14A 117.8 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 C16 C17 110.0(8) . . ?
N5 C16 C15 126.5(8) . . ?
C17 C16 C15 123.2(9) . . ?
N6 C17 C18 122.1(9) . . ?
N6 C17 C16 114.4(8) . . ?
C18 C17 C16 123.4(9) . . ?
C19 C18 C17 121.6(10) . . ?
C19 C18 H18A 119.2 . . ?
C17 C18 H18A 119.2 . . ?
C18 C19 C20 115.6(9) . . ?
C18 C19 H19A 122.2 . . ?
C20 C19 H19A 122.2 . . ?
C21 C20 C19 120.4(8) . . ?
C21 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 . . ?
N6 C21 C20 122.4(9) . . ?
N6 C21 H21A 118.8 . . ?
C20 C21 H21A 118.8 . . ?
C29 N7 C22 108.0(7) . . ?
C29 N7 Zr01 123.2(6) . . ?
C22 N7 Zr01 123.7(5) . . ?
C29 N8 C30 122.9(8) . . ?
C30 N9 C37 106.2(8) . . ?
C30 N9 Zr01 124.0(6) . . ?
C37 N9 Zr01 122.4(6) . . ?
C37 N10 C38 122.9(9) . . ?
C38 N11 C45 108.0(7) . . ?
C38 N11 Zr01 121.3(5) . . ?
C45 N11 Zr01 119.7(5) . . ?
C46 N12 C45 121.7(7) . . ?
C46 N13 C53 107.1(7) . . ?
C46 N13 Zr01 122.1(6) . . ?
C53 N13 Zr01 123.7(5) . . ?
C22 N14 C53 122.7(9) . . ?
N14 C22 N7 128.2(8) . . ?
N14 C22 C23 124.2(10) . . ?
N7 C22 C23 107.5(8) . . ?
C28 C23 C24 121.2(9) . . ?
C28 C23 C22 107.6(9) . . ?
C24 C23 C22 131.1(10) . . ?
C25 C24 C23 117.5(10) . . ?
C25 C24 H24A 121.2 . . ?
C23 C24 H24A 121.2 . . ?
C24 C25 C26 119.8(11) . . ?
C24 C25 H25A 120.1 . . ?
C26 C25 H25A 120.1 . . ?
C27 C26 C25 123.3(10) . . ?
C27 C26 H26A 118.3 . . ?
C25 C26 H26A 118.3 . . ?
C26 C27 C28 116.3(10) . . ?
C26 C27 H27A 121.8 . . ?
C28 C27 H27A 121.8 . . ?
C23 C28 C27 121.7(10) . . ?
C23 C28 C29 108.2(8) . . ?
C27 C28 C29 130.0(10) . . ?
N8 C29 N7 127.6(9) . . ?
N8 C29 C28 123.9(8) . . ?
N7 C29 C28 108.5(9) . . ?
N8 C30 N9 125.8(9) . . ?
N8 C30 C31 123.6(8) . . ?
N9 C30 C31 110.6(9) . . ?
C36 C31 C30 107.7(8) . . ?
C36 C31 C32 119.1(9) . . ?
C30 C31 C32 133.3(10) . . ?
C33 C32 C31 117.7(11) . . ?
C33 C32 H32A 121.2 . . ?
C31 C32 H32A 121.2 . . ?
C32 C33 C34 123.0(10) . . ?
C32 C33 H33A 118.5 . . ?
C34 C33 H33A 118.5 . . ?
C33 C34 C35 120.6(11) . . ?
C33 C34 H34A 119.7 . . ?
C35 C34 H34A 119.7 . . ?
C36 C35 C34 116.2(11) . . ?
C36 C35 H35A 121.9 . . ?
C34 C35 H35A 121.9 . . ?
C31 C36 C35 123.4(9) . . ?
C31 C36 C37 105.4(9) . . ?
C35 C36 C37 131.1(10) . . ?
N10 C37 N9 127.2(8) . . ?
N10 C37 C36 122.8(10) . . ?
N9 C37 C36 109.9(8) . . ?
N10 C38 N11 128.1(8) . . ?
N10 C38 C39 121.3(9) . . ?
N11 C38 C39 110.7(8) . . ?
C40 C39 C44 121.0(8) . . ?
C40 C39 C38 133.8(8) . . ?
C44 C39 C38 105.0(8) . . ?
C39 C40 C41 118.4(9) . . ?
C39 C40 H40A 120.8 . . ?
C41 C40 H40A 120.8 . . ?
C40 C41 C42 121.3(9) . . ?
C40 C41 H41A 119.3 . . ?
C42 C41 H41A 119.3 . . ?
C43 C42 C41 121.3(9) . . ?
C43 C42 H42A 119.3 . . ?
C41 C42 H42A 119.3 . . ?
C42 C43 C44 117.0(9) . . ?
C42 C43 H43A 121.5 . . ?
C44 C43 H43A 121.5 . . ?
C43 C44 C39 120.9(8) . . ?
C43 C44 C45 132.7(9) . . ?
C39 C44 C45 106.4(7) . . ?
N12 C45 N11 127.6(8) . . ?
N12 C45 C44 122.6(7) . . ?
N11 C45 C44 109.9(8) . . ?
N12 C46 N13 128.1(8) . . ?
N12 C46 C47 121.6(7) . . ?
N13 C46 C47 110.3(8) . . ?
C48 C47 C52 119.8(9) . . ?
C48 C47 C46 133.8(9) . . ?
C52 C47 C46 106.3(7) . . ?
C49 C48 C47 118.7(9) . . ?
C49 C48 H48A 120.6 . . ?
C47 C48 H48A 120.6 . . ?
C48 C49 C50 120.9(9) . . ?
C48 C49 H49A 119.5 . . ?
C50 C49 H49A 119.5 . . ?
C51 C50 C49 121.8(10) . . ?
C51 C50 H50A 119.1 . . ?
C49 C50 H50A 119.1 . . ?
C50 C51 C52 117.8(9) . . ?
C50 C51 H51A 121.1 . . ?
C52 C51 H51A 121.1 . . ?
C51 C52 C47 120.8(8) . . ?
C51 C52 C53 133.5(8) . . ?
C47 C52 C53 105.7(8) . . ?
N14 C53 N13 127.0(8) . . ?
N14 C53 C52 122.4(9) . . ?
N13 C53 C52 110.6(7) . . ?
O3S Cl1S O1S 110.1(10) . . ?
O3S Cl1S O4S 108.0(8) . . ?
O1S Cl1S O4S 108.8(7) . . ?
O3S Cl1S O2S 109.1(6) . . ?
O1S Cl1S O2S 109.8(5) . . ?
O4S Cl1S O2S 111.0(4) . . ?

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
Zr01 O1 N1 C2 128.5(7) . . . . ?
Zr01 O1 N1 Fe1 -48.5(8) . . . . ?
N5 Fe1 N1 C2 164.8(7) . . . . ?
N3 Fe1 N1 C2 -102.2(7) . . . . ?
N2 Fe1 N1 C2 -6.8(7) . . . . ?
N6 Fe1 N1 C2 84.3(7) . . . . ?
N4 Fe1 N1 C2 -68.8(16) . . . . ?
N5 Fe1 N1 O1 -18.2(6) . . . . ?
N3 Fe1 N1 O1 74.8(6) . . . . ?
N2 Fe1 N1 O1 170.2(7) . . . . ?
N6 Fe1 N1 O1 -98.7(6) . . . . ?
N4 Fe1 N1 O1 108.2(14) . . . . ?
Zr01 O2 N3 C9 131.4(6) . . . . ?
Zr01 O2 N3 Fe1 -42.1(8) . . . . ?
N5 Fe1 N3 C9 -106.7(7) . . . . ?
N1 Fe1 N3 C9 163.3(7) . . . . ?
N2 Fe1 N3 C9 82.5(7) . . . . ?
N4 Fe1 N3 C9 -9.9(7) . . . . ?
N5 Fe1 N3 O2 66.2(6) . . . . ?
N1 Fe1 N3 O2 -23.9(6) . . . . ?
N2 Fe1 N3 O2 -104.7(6) . . . . ?
N4 Fe1 N3 O2 162.9(6) . . . . ?
Zr01 O3 N5 C16 130.5(6) . . . . ?
Zr01 O3 N5 Fe1 -44.9(8) . . . . ?
N3 Fe1 N5 C16 165.8(7) . . . . ?
N1 Fe1 N5 C16 -103.5(7) . . . . ?
N2 Fe1 N5 C16 -61.8(18) . . . . ?
N6 Fe1 N5 C16 -6.6(7) . . . . ?
N4 Fe1 N5 C16 86.4(7) . . . . ?
N3 Fe1 N5 O3 -19.1(6) . . . . ?
N1 Fe1 N5 O3 71.6(6) . . . . ?
N2 Fe1 N5 O3 113.3(15) . . . . ?
N6 Fe1 N5 O3 168.5(6) . . . . ?
N4 Fe1 N5 O3 -98.5(6) . . . . ?
O1 N1 C2 C3 -171.8(7) . . . . ?
Fe1 N1 C2 C3 5.3(10) . . . . ?
O1 N1 C2 C1 4.7(13) . . . . ?
Fe1 N1 C2 C1 -178.2(7) . . . . ?
C7 N2 C3 C4 0.7(13) . . . . ?
Fe1 N2 C3 C4 175.9(7) . . . . ?
C7 N2 C3 C2 179.2(8) . . . . ?
Fe1 N2 C3 C2 -5.7(9) . . . . ?
N1 C2 C3 N2 0.6(11) . . . . ?
C1 C2 C3 N2 -175.9(8) . . . . ?
N1 C2 C3 C4 179.0(8) . . . . ?
C1 C2 C3 C4 2.5(14) . . . . ?
N2 C3 C4 C5 -0.9(14) . . . . ?
C2 C3 C4 C5 -179.2(9) . . . . ?
C3 C4 C5 C6 1.3(15) . . . . ?
C4 C5 C6 C7 -1.5(15) . . . . ?
C3 N2 C7 C6 -0.9(14) . . . . ?
Fe1 N2 C7 C6 -175.2(7) . . . . ?
C5 C6 C7 N2 1.3(16) . . . . ?
O2 N3 C9 C10 -169.6(7) . . . . ?
Fe1 N3 C9 C10 3.8(11) . . . . ?
O2 N3 C9 C8 6.2(13) . . . . ?
Fe1 N3 C9 C8 179.6(7) . . . . ?
C14 N4 C10 C11 -0.8(13) . . . . ?
Fe1 N4 C10 C11 172.4(8) . . . . ?
C14 N4 C10 C9 171.5(8) . . . . ?
Fe1 N4 C10 C9 -15.2(9) . . . . ?
N3 C9 C10 C11 -179.8(9) . . . . ?
C8 C9 C10 C11 4.3(15) . . . . ?
N3 C9 C10 N4 8.1(11) . . . . ?
C8 C9 C10 N4 -167.8(8) . . . . ?
N4 C10 C11 C12 1.9(15) . . . . ?
C9 C10 C11 C12 -169.5(9) . . . . ?
C10 C11 C12 C13 -0.5(16) . . . . ?
C11 C12 C13 C14 -1.7(16) . . . . ?
C10 N4 C14 C13 -1.7(14) . . . . ?
Fe1 N4 C14 C13 -173.5(8) . . . . ?
C12 C13 C14 N4 2.9(16) . . . . ?
O3 N5 C16 C17 -170.8(7) . . . . ?
Fe1 N5 C16 C17 4.7(10) . . . . ?
O3 N5 C16 C15 3.2(13) . . . . ?
Fe1 N5 C16 C15 178.7(8) . . . . ?
C21 N6 C17 C18 -3.1(13) . . . . ?
Fe1 N6 C17 C18 175.7(7) . . . . ?
C21 N6 C17 C16 174.7(8) . . . . ?
Fe1 N6 C17 C16 -6.5(9) . . . . ?
N5 C16 C17 N6 1.6(11) . . . . ?
C15 C16 C17 N6 -172.7(9) . . . . ?
N5 C16 C17 C18 179.4(8) . . . . ?
C15 C16 C17 C18 5.1(15) . . . . ?
N6 C17 C18 C19 -1.0(15) . . . . ?
C16 C17 C18 C19 -178.6(9) . . . . ?
C17 C18 C19 C20 5.4(13) . . . . ?
C18 C19 C20 C21 -6.1(13) . . . . ?
C17 N6 C21 C20 2.4(12) . . . . ?
Fe1 N6 C21 C20 -176.2(6) . . . . ?
C19 C20 C21 N6 2.3(13) . . . . ?
C53 N14 C22 N7 3.3(14) . . . . ?
C53 N14 C22 C23 -177.6(8) . . . . ?
C29 N7 C22 N14 -177.3(8) . . . . ?
Zr01 N7 C22 N14 27.4(12) . . . . ?
C29 N7 C22 C23 3.5(9) . . . . ?
Zr01 N7 C22 C23 -151.7(6) . . . . ?
N14 C22 C23 C28 178.3(8) . . . . ?
N7 C22 C23 C28 -2.5(10) . . . . ?
N14 C22 C23 C24 -4.1(16) . . . . ?
N7 C22 C23 C24 175.1(10) . . . . ?
C28 C23 C24 C25 1.5(15) . . . . ?
C22 C23 C24 C25 -175.8(9) . . . . ?
C23 C24 C25 C26 -2.0(14) . . . . ?
C24 C25 C26 C27 0.9(15) . . . . ?
C25 C26 C27 C28 0.7(14) . . . . ?
C24 C23 C28 C27 0.2(14) . . . . ?
C22 C23 C28 C27 178.0(8) . . . . ?
C24 C23 C28 C29 -177.4(9) . . . . ?
C22 C23 C28 C29 0.5(10) . . . . ?
C26 C27 C28 C23 -1.2(14) . . . . ?
C26 C27 C28 C29 175.7(9) . . . . ?
C30 N8 C29 N7 -3.7(13) . . . . ?
C30 N8 C29 C28 174.8(8) . . . . ?
C22 N7 C29 N8 175.4(8) . . . . ?
Zr01 N7 C29 N8 -29.2(12) . . . . ?
C22 N7 C29 C28 -3.3(9) . . . . ?
Zr01 N7 C29 C28 152.1(6) . . . . ?
C23 C28 C29 N8 -177.0(8) . . . . ?
C27 C28 C29 N8 5.7(15) . . . . ?
C23 C28 C29 N7 1.8(10) . . . . ?
C27 C28 C29 N7 -175.5(9) . . . . ?
C29 N8 C30 N9 1.1(13) . . . . ?
C29 N8 C30 C31 -178.7(8) . . . . ?
C37 N9 C30 N8 -174.8(8) . . . . ?
Zr01 N9 C30 N8 34.9(12) . . . . ?
C37 N9 C30 C31 5.0(9) . . . . ?
Zr01 N9 C30 C31 -145.3(6) . . . . ?
N8 C30 C31 C36 176.2(8) . . . . ?
N9 C30 C31 C36 -3.6(10) . . . . ?
N8 C30 C31 C32 -3.5(15) . . . . ?
N9 C30 C31 C32 176.7(9) . . . . ?
C36 C31 C32 C33 2.4(13) . . . . ?
C30 C31 C32 C33 -178.0(9) . . . . ?
C31 C32 C33 C34 -1.8(14) . . . . ?
C32 C33 C34 C35 0.9(16) . . . . ?
C33 C34 C35 C36 -0.4(15) . . . . ?
C30 C31 C36 C35 178.1(9) . . . . ?
C32 C31 C36 C35 -2.2(14) . . . . ?
C30 C31 C36 C37 0.7(10) . . . . ?
C32 C31 C36 C37 -179.6(8) . . . . ?
C34 C35 C36 C31 1.1(15) . . . . ?
C34 C35 C36 C37 177.9(9) . . . . ?
C38 N10 C37 N9 -1.3(15) . . . . ?
C38 N10 C37 C36 -178.4(8) . . . . ?
C30 N9 C37 N10 178.1(9) . . . . ?
Zr01 N9 C37 N10 -30.9(12) . . . . ?
C30 N9 C37 C36 -4.5(9) . . . . ?
Zr01 N9 C37 C36 146.4(6) . . . . ?
C31 C36 C37 N10 179.8(8) . . . . ?
C35 C36 C37 N10 2.7(16) . . . . ?
C31 C36 C37 N9 2.4(10) . . . . ?
C35 C36 C37 N9 -174.8(10) . . . . ?
C37 N10 C38 N11 -1.5(14) . . . . ?
C37 N10 C38 C39 176.5(8) . . . . ?
C45 N11 C38 N10 179.3(8) . . . . ?
Zr01 N11 C38 N10 35.5(12) . . . . ?
C45 N11 C38 C39 1.2(9) . . . . ?
Zr01 N11 C38 C39 -142.7(6) . . . . ?
N10 C38 C39 C40 -1.8(15) . . . . ?
N11 C38 C39 C40 176.5(9) . . . . ?
N10 C38 C39 C44 -178.3(8) . . . . ?
N11 C38 C39 C44 0.0(9) . . . . ?
C44 C39 C40 C41 -0.8(13) . . . . ?
C38 C39 C40 C41 -176.9(9) . . . . ?
C39 C40 C41 C42 1.3(14) . . . . ?
C40 C41 C42 C43 -1.2(14) . . . . ?
C41 C42 C43 C44 0.7(13) . . . . ?
C42 C43 C44 C39 -0.2(12) . . . . ?
C42 C43 C44 C45 177.8(9) . . . . ?
C40 C39 C44 C43 0.3(13) . . . . ?
C38 C39 C44 C43 177.4(8) . . . . ?
C40 C39 C44 C45 -178.2(8) . . . . ?
C38 C39 C44 C45 -1.1(9) . . . . ?
C46 N12 C45 N11 -0.4(13) . . . . ?
C46 N12 C45 C44 178.2(8) . . . . ?
C38 N11 C45 N12 176.8(8) . . . . ?
Zr01 N11 C45 N12 -38.7(11) . . . . ?
C38 N11 C45 C44 -1.9(9) . . . . ?
Zr01 N11 C45 C44 142.7(6) . . . . ?
C43 C44 C45 N12 4.9(14) . . . . ?
C39 C44 C45 N12 -176.8(7) . . . . ?
C43 C44 C45 N11 -176.4(8) . . . . ?
C39 C44 C45 N11 1.9(9) . . . . ?
C45 N12 C46 N13 6.1(13) . . . . ?
C45 N12 C46 C47 -175.5(8) . . . . ?
C53 N13 C46 N12 -179.6(8) . . . . ?
Zr01 N13 C46 N12 29.1(11) . . . . ?
C53 N13 C46 C47 1.9(9) . . . . ?
Zr01 N13 C46 C47 -149.4(6) . . . . ?
N12 C46 C47 C48 1.1(15) . . . . ?
N13 C46 C47 C48 179.7(9) . . . . ?
N12 C46 C47 C52 179.1(8) . . . . ?
N13 C46 C47 C52 -2.3(10) . . . . ?
C52 C47 C48 C49 0.0(14) . . . . ?
C46 C47 C48 C49 177.8(10) . . . . ?
C47 C48 C49 C50 2.4(15) . . . . ?
C48 C49 C50 C51 -2.9(16) . . . . ?
C49 C50 C51 C52 0.9(15) . . . . ?
C50 C51 C52 C47 1.6(14) . . . . ?
C50 C51 C52 C53 178.8(10) . . . . ?
C48 C47 C52 C51 -2.1(14) . . . . ?
C46 C47 C52 C51 179.6(8) . . . . ?
C48 C47 C52 C53 -180.0(8) . . . . ?
C46 C47 C52 C53 1.7(10) . . . . ?
C22 N14 C53 N13 -0.5(14) . . . . ?
C22 N14 C53 C52 176.3(8) . . . . ?
C46 N13 C53 N14 176.4(8) . . . . ?
Zr01 N13 C53 N14 -32.9(11) . . . . ?
C46 N13 C53 C52 -0.7(9) . . . . ?
Zr01 N13 C53 C52 150.0(6) . . . . ?
C51 C52 C53 N14 4.5(16) . . . . ?
C47 C52 C53 N14 -177.9(8) . . . . ?
C51 C52 C53 N13 -178.2(10) . . . . ?
C47 C52 C53 N13 -0.7(10) . . . . ?

_refine_diff_density_max         3.937
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.147

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_FeHf
_database_code_depnum_ccdc_archive 'CCDC 1503090'
_audit_update_record             
;
2016-09-06 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;

_vrf_PLAT094_FeHf                
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       5.43 Report
RESPONSE: High absoption effects have not been fully corrected for.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H37 Fe Hf N14 O3, Cl O4'
_chemical_formula_sum            'C53 H37 Cl Fe Hf N14 O7'
_chemical_formula_weight         1251.75

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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                   12.1688(19)
_cell_length_b                   13.742(2)
_cell_length_c                   15.640(2)
_cell_angle_alpha                79.198(3)
_cell_angle_beta                 81.175(3)
_cell_angle_gamma                89.104(4)
_cell_volume                     2538.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3666
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_F_000             1248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.451
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0013
_exptl_absorpt_correction_T_max  0.0132
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX2 DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33117
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.993
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9953
_reflns_number_gt                7030
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.1033P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9953
_refine_ls_number_parameters     698
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.1807
_refine_ls_wR_factor_gt          0.1653
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.004
_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
Hf1 Hf 0.41095(3) 0.64454(3) 0.83579(3) 0.05129(15) Uani 1 1 d . . . . .
Fe1 Fe 0.29043(11) 0.66858(10) 0.63009(8) 0.0530(3) Uani 1 1 d . . . . .
O1 O 0.3700(5) 0.5337(5) 0.7671(4) 0.0555(14) Uani 1 1 d . . . . .
O2 O 0.2560(5) 0.7030(5) 0.8063(4) 0.0527(14) Uani 1 1 d . . . . .
O3 O 0.4741(6) 0.7195(5) 0.7086(4) 0.0611(16) Uani 1 1 d . . . . .
N1 N 0.2931(6) 0.5505(6) 0.7127(5) 0.0538(18) Uani 1 1 d . . . . .
N2 N 0.1465(6) 0.6110(6) 0.6224(5) 0.0550(18) Uani 1 1 d . . . . .
N3 N 0.2445(6) 0.7393(6) 0.7223(5) 0.0531(17) Uani 1 1 d . . . . .
N4 N 0.2596(6) 0.7976(6) 0.5594(5) 0.0535(17) Uani 1 1 d . . . . .
N5 N 0.4396(6) 0.6982(6) 0.6366(5) 0.0563(18) Uani 1 1 d . . . . .
N6 N 0.3649(7) 0.6205(6) 0.5249(5) 0.0573(19) Uani 1 1 d . . . . .
C1 C 0.2162(9) 0.3820(7) 0.7786(7) 0.064(2) Uani 1 1 d . . . . .
H1A H 0.2905 0.3678 0.7943 0.096 Uiso 1 1 calc R U . . .
H1B H 0.1943 0.3309 0.7482 0.096 Uiso 1 1 calc R U . . .
H1C H 0.1627 0.3823 0.8322 0.096 Uiso 1 1 calc R U . . .
C2 C 0.2177(8) 0.4817(7) 0.7190(6) 0.056(2) Uani 1 1 d . . . . .
C3 C 0.1325(8) 0.5161(7) 0.6657(6) 0.058(2) Uani 1 1 d . . . . .
C4 C 0.0400(9) 0.4596(8) 0.6640(6) 0.062(2) Uani 1 1 d . . . . .
H4A H 0.0313 0.3934 0.6958 0.075 Uiso 1 1 calc R U . . .
C5 C -0.0391(9) 0.5017(8) 0.6150(6) 0.063(2) Uani 1 1 d . . . . .
H5A H -0.1031 0.4645 0.6120 0.075 Uiso 1 1 calc R U . . .
C6 C -0.0250(8) 0.5971(8) 0.5707(6) 0.059(2) Uani 1 1 d . . . . .
H6A H -0.0792 0.6270 0.5368 0.071 Uiso 1 1 calc R U . . .
C7 C 0.0678(7) 0.6492(7) 0.5757(6) 0.055(2) Uani 1 1 d . . . . .
H7A H 0.0767 0.7156 0.5445 0.066 Uiso 1 1 calc R U . . .
C8 C 0.1861(9) 0.8930(7) 0.7687(7) 0.063(2) Uani 1 1 d . . . . .
H8A H 0.1537 0.8526 0.8252 0.094 Uiso 1 1 calc R U . . .
H8B H 0.1324 0.9427 0.7487 0.094 Uiso 1 1 calc R U . . .
H8C H 0.2538 0.9263 0.7759 0.094 Uiso 1 1 calc R U . . .
C9 C 0.2136(7) 0.8296(7) 0.7036(6) 0.053(2) Uani 1 1 d . . . . .
C10 C 0.2174(8) 0.8630(7) 0.6088(6) 0.052(2) Uani 1 1 d . . . . .
C11 C 0.1838(9) 0.9558(7) 0.5708(6) 0.061(2) Uani 1 1 d . . . . .
H11A H 0.1544 1.0013 0.6069 0.073 Uiso 1 1 calc R U . . .
C12 C 0.1933(10) 0.9818(8) 0.4801(8) 0.074(3) Uani 1 1 d . . . . .
H12A H 0.1705 1.0449 0.4525 0.089 Uiso 1 1 calc R U . . .
C13 C 0.2362(10) 0.9139(9) 0.4322(8) 0.074(3) Uani 1 1 d . . . . .
H13A H 0.2432 0.9292 0.3698 0.089 Uiso 1 1 calc R U . . .
C14 C 0.2698(9) 0.8234(8) 0.4723(7) 0.067(3) Uani 1 1 d . . . . .
H14A H 0.3012 0.7779 0.4369 0.080 Uiso 1 1 calc R U . . .
C15 C 0.6341(9) 0.7182(9) 0.5665(8) 0.075(3) Uani 1 1 d . . . . .
H15A H 0.6643 0.6780 0.6159 0.112 Uiso 1 1 calc R U . . .
H15B H 0.6394 0.7885 0.5697 0.112 Uiso 1 1 calc R U . . .
H15C H 0.6766 0.7067 0.5109 0.112 Uiso 1 1 calc R U . . .
C16 C 0.5170(8) 0.6907(8) 0.5707(7) 0.064(2) Uani 1 1 d . . . . .
C17 C 0.4737(9) 0.6505(8) 0.5040(6) 0.064(3) Uani 1 1 d . . . . .
C18 C 0.5366(9) 0.6356(9) 0.4252(7) 0.070(3) Uani 1 1 d . . . . .
H18A H 0.6118 0.6579 0.4097 0.084 Uiso 1 1 calc R U . . .
C19 C 0.4882(10) 0.5885(9) 0.3708(7) 0.075(3) Uani 1 1 d . . . . .
H19A H 0.5291 0.5790 0.3162 0.089 Uiso 1 1 calc R U . . .
C20 C 0.3795(10) 0.5546(8) 0.3953(6) 0.068(3) Uani 1 1 d . . . . .
H20A H 0.3455 0.5184 0.3600 0.082 Uiso 1 1 calc R U . . .
C21 C 0.3224(10) 0.5749(8) 0.4722(7) 0.066(3) Uani 1 1 d . . . . .
H21A H 0.2467 0.5542 0.4880 0.079 Uiso 1 1 calc R U . . .
N7 N 0.5136(6) 0.5124(6) 0.8728(5) 0.0552(18) Uani 1 1 d . . . . .
N8 N 0.3676(7) 0.3924(6) 0.9432(5) 0.0559(18) Uani 1 1 d . . . . .
N9 N 0.3045(6) 0.5571(6) 0.9533(5) 0.0541(17) Uani 1 1 d . . . . .
N10 N 0.1971(7) 0.6883(6) 1.0076(5) 0.0586(19) Uani 1 1 d . . . . .
N11 N 0.3721(6) 0.7547(6) 0.9248(5) 0.0560(18) Uani 1 1 d . . . . .
N12 N 0.5253(7) 0.8688(6) 0.8725(5) 0.0589(19) Uani 1 1 d . . . . .
N13 N 0.5759(6) 0.7056(6) 0.8441(5) 0.0533(17) Uani 1 1 d . . . . .
N14 N 0.6904(6) 0.5774(6) 0.7954(5) 0.0563(18) Uani 1 1 d . . . . .
C22 C 0.6193(8) 0.5043(8) 0.8312(6) 0.058(2) Uani 1 1 d . . . . .
C23 C 0.6410(8) 0.4005(8) 0.8283(6) 0.058(2) Uani 1 1 d . . . . .
C24 C 0.7353(9) 0.3526(8) 0.7910(6) 0.062(2) Uani 1 1 d . . . . .
H24A H 0.8017 0.3882 0.7638 0.075 Uiso 1 1 calc R U . . .
C25 C 0.7263(9) 0.2545(8) 0.7960(7) 0.068(3) Uani 1 1 d . . . . .
H25A H 0.7876 0.2198 0.7712 0.082 Uiso 1 1 calc R U . . .
C26 C 0.6293(11) 0.2021(8) 0.8365(8) 0.076(3) Uani 1 1 d . . . . .
H26A H 0.6256 0.1330 0.8369 0.091 Uiso 1 1 calc R U . . .
C27 C 0.5399(9) 0.2463(7) 0.8752(7) 0.066(3) Uani 1 1 d . . . . .
H27A H 0.4752 0.2093 0.9044 0.079 Uiso 1 1 calc R U . . .
C28 C 0.5468(8) 0.3481(8) 0.8706(6) 0.060(2) Uani 1 1 d . . . . .
C29 C 0.4685(8) 0.4194(7) 0.8988(6) 0.055(2) Uani 1 1 d . . . . .
C30 C 0.2936(8) 0.4575(7) 0.9684(6) 0.055(2) Uani 1 1 d . . . . .
C31 C 0.1885(8) 0.4284(8) 1.0240(6) 0.058(2) Uani 1 1 d . . . . .
C32 C 0.1341(9) 0.3381(8) 1.0507(7) 0.066(3) Uani 1 1 d . . . . .
H32A H 0.1659 0.2793 1.0346 0.079 Uiso 1 1 calc R U . . .
C33 C 0.0307(8) 0.3376(8) 1.1022(6) 0.063(2) Uani 1 1 d . . . . .
H33A H -0.0102 0.2771 1.1215 0.075 Uiso 1 1 calc R U . . .
C34 C -0.0133(9) 0.4220(9) 1.1257(7) 0.071(3) Uani 1 1 d . . . . .
H34A H -0.0832 0.4180 1.1628 0.085 Uiso 1 1 calc R U . . .
C35 C 0.0389(8) 0.5131(8) 1.0983(6) 0.059(2) Uani 1 1 d . . . . .
H35A H 0.0064 0.5717 1.1142 0.071 Uiso 1 1 calc R U . . .
C36 C 0.1426(9) 0.5141(8) 1.0454(7) 0.063(2) Uani 1 1 d . . . . .
C37 C 0.2152(7) 0.5945(7) 1.0012(6) 0.054(2) Uani 1 1 d . . . . .
C38 C 0.2684(8) 0.7610(7) 0.9740(6) 0.055(2) Uani 1 1 d . . . . .
C39 C 0.2511(10) 0.8597(8) 0.9878(7) 0.066(3) Uani 1 1 d . . . . .
C40 C 0.1622(9) 0.9065(9) 1.0305(8) 0.071(3) Uani 1 1 d . . . . .
H40A H 0.0949 0.8716 1.0563 0.086 Uiso 1 1 calc R U . . .
C41 C 0.1751(11) 1.0036(10) 1.0338(9) 0.084(3) Uani 1 1 d . . . . .
H41A H 0.1155 1.0371 1.0622 0.101 Uiso 1 1 calc R U . . .
C42 C 0.2731(12) 1.0549(9) 0.9967(9) 0.082(3) Uani 1 1 d . . . . .
H42A H 0.2790 1.1228 1.0005 0.099 Uiso 1 1 calc R U . . .
C43 C 0.3625(10) 1.0104(8) 0.9545(8) 0.071(3) Uani 1 1 d . . . . .
H43A H 0.4297 1.0461 0.9298 0.086 Uiso 1 1 calc R U . . .
C44 C 0.3504(8) 0.9141(7) 0.9496(6) 0.058(2) Uani 1 1 d . . . . .
C45 C 0.4233(8) 0.8450(7) 0.9121(6) 0.057(2) Uani 1 1 d . . . . .
C46 C 0.5945(9) 0.8057(8) 0.8416(6) 0.062(2) Uani 1 1 d . . . . .
C47 C 0.7074(8) 0.8315(8) 0.7973(6) 0.057(2) Uani 1 1 d . . . . .
C48 C 0.7664(9) 0.9213(9) 0.7781(7) 0.067(3) Uani 1 1 d . . . . .
H48A H 0.7350 0.9797 0.7954 0.080 Uiso 1 1 calc R U . . .
C49 C 0.8711(9) 0.9206(9) 0.7331(7) 0.069(3) Uani 1 1 d . . . . .
H49A H 0.9155 0.9792 0.7213 0.083 Uiso 1 1 calc R U . . .
C50 C 0.9140(9) 0.8386(9) 0.7047(7) 0.070(3) Uani 1 1 d . . . . .
H50A H 0.9853 0.8436 0.6696 0.084 Uiso 1 1 calc R U . . .
C51 C 0.8590(9) 0.7482(8) 0.7244(7) 0.067(3) Uani 1 1 d . . . . .
H51A H 0.8917 0.6902 0.7073 0.081 Uiso 1 1 calc R U . . .
C52 C 0.7525(8) 0.7480(7) 0.7710(6) 0.056(2) Uani 1 1 d . . . . .
C53 C 0.6704(8) 0.6688(7) 0.8033(6) 0.057(2) Uani 1 1 d . . . . .
Cl1S Cl -0.0528(3) 0.7995(2) 0.3795(2) 0.0761(7) Uani 1 1 d . . . . .
O1S O 0.0465(8) 0.7469(7) 0.3601(6) 0.091(2) Uani 1 1 d . . . . .
O3S O -0.0526(9) 0.8334(7) 0.4584(6) 0.097(3) Uani 1 1 d . . . . .
O4S O -0.1461(7) 0.7359(7) 0.3883(6) 0.087(2) Uani 1 1 d . . . . .
O2S O -0.0588(11) 0.8801(7) 0.3093(7) 0.112(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O3 2.096(7) . ?
Hf1 O2 2.120(6) . ?
Hf1 O1 2.126(6) . ?
Hf1 N13 2.219(8) . ?
Hf1 N7 2.225(8) . ?
Hf1 N9 2.234(7) . ?
Hf1 N11 2.241(7) . ?
Fe1 N1 1.878(8) . ?
Fe1 N5 1.888(8) . ?
Fe1 N3 1.897(8) . ?
Fe1 N2 1.962(8) . ?
Fe1 N4 1.970(7) . ?
Fe1 N6 1.974(7) . ?
O1 N1 1.349(10) . ?
O2 N3 1.343(9) . ?
O3 N5 1.343(10) . ?
N1 C2 1.307(12) . ?
N2 C7 1.334(12) . ?
N2 C3 1.353(13) . ?
N3 C9 1.285(12) . ?
N4 C14 1.328(13) . ?
N4 C10 1.338(12) . ?
N5 C16 1.303(12) . ?
N6 C21 1.293(13) . ?
N6 C17 1.365(14) . ?
C1 C2 1.504(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.448(14) . ?
C3 C4 1.384(15) . ?
C4 C5 1.374(15) . ?
C4 H4A 0.9500 . ?
C5 C6 1.363(15) . ?
C5 H5A 0.9500 . ?
C6 C7 1.367(14) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.458(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.461(13) . ?
C10 C11 1.385(13) . ?
C11 C12 1.384(15) . ?
C11 H11A 0.9500 . ?
C12 C13 1.354(16) . ?
C12 H12A 0.9500 . ?
C13 C14 1.370(15) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.468(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.437(15) . ?
C17 C18 1.396(14) . ?
C18 C19 1.365(17) . ?
C18 H18A 0.9500 . ?
C19 C20 1.383(17) . ?
C19 H19A 0.9500 . ?
C20 C21 1.368(14) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
N7 C22 1.362(12) . ?
N7 C29 1.363(13) . ?
N8 C30 1.329(12) . ?
N8 C29 1.336(13) . ?
N9 C30 1.350(12) . ?
N9 C37 1.372(12) . ?
N10 C38 1.310(13) . ?
N10 C37 1.324(12) . ?
N11 C45 1.364(13) . ?
N11 C38 1.385(12) . ?
N12 C46 1.305(13) . ?
N12 C45 1.316(13) . ?
N13 C53 1.365(12) . ?
N13 C46 1.391(13) . ?
N14 C53 1.301(12) . ?
N14 C22 1.319(13) . ?
C22 C23 1.454(14) . ?
C23 C28 1.373(14) . ?
C23 C24 1.416(14) . ?
C24 C25 1.342(15) . ?
C24 H24A 0.9500 . ?
C25 C26 1.392(17) . ?
C25 H25A 0.9500 . ?
C26 C27 1.354(16) . ?
C26 H26A 0.9500 . ?
C27 C28 1.390(15) . ?
C27 H27A 0.9500 . ?
C28 C29 1.437(13) . ?
C30 C31 1.448(13) . ?
C31 C36 1.372(15) . ?
C31 C32 1.377(15) . ?
C32 C33 1.386(15) . ?
C32 H32A 0.9500 . ?
C33 C34 1.360(16) . ?
C33 H33A 0.9500 . ?
C34 C35 1.376(16) . ?
C34 H34A 0.9500 . ?
C35 C36 1.397(14) . ?
C35 H35A 0.9500 . ?
C36 C37 1.427(14) . ?
C38 C39 1.420(14) . ?
C39 C40 1.395(15) . ?
C39 C44 1.420(15) . ?
C40 C41 1.358(17) . ?
C40 H40A 0.9500 . ?
C41 C42 1.384(19) . ?
C41 H41A 0.9500 . ?
C42 C43 1.380(17) . ?
C42 H42A 0.9500 . ?
C43 C44 1.352(15) . ?
C43 H43A 0.9500 . ?
C44 C45 1.433(14) . ?
C46 C47 1.457(14) . ?
C47 C52 1.369(14) . ?
C47 C48 1.396(15) . ?
C48 C49 1.358(15) . ?
C48 H48A 0.9500 . ?
C49 C50 1.356(16) . ?
C49 H49A 0.9500 . ?
C50 C51 1.381(16) . ?
C50 H50A 0.9500 . ?
C51 C52 1.386(14) . ?
C51 H51A 0.9500 . ?
C52 C53 1.452(14) . ?
Cl1S O3S 1.399(9) . ?
Cl1S O2S 1.416(10) . ?
Cl1S O4S 1.418(9) . ?
Cl1S O1S 1.420(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
O3 Hf1 O2 84.7(2) . . ?
O3 Hf1 O1 83.0(3) . . ?
O2 Hf1 O1 82.8(2) . . ?
O3 Hf1 N13 73.7(3) . . ?
O2 Hf1 N13 136.3(3) . . ?
O1 Hf1 N13 129.8(3) . . ?
O3 Hf1 N7 109.9(3) . . ?
O2 Hf1 N7 148.6(3) . . ?
O1 Hf1 N7 72.1(3) . . ?
N13 Hf1 N7 75.1(3) . . ?
O3 Hf1 N9 164.3(3) . . ?
O2 Hf1 N9 82.8(3) . . ?
O1 Hf1 N9 86.0(3) . . ?
N13 Hf1 N9 122.0(3) . . ?
N7 Hf1 N9 77.0(3) . . ?
O3 Hf1 N11 109.3(3) . . ?
O2 Hf1 N11 76.3(3) . . ?
O1 Hf1 N11 154.4(3) . . ?
N13 Hf1 N11 75.8(3) . . ?
N7 Hf1 N11 121.1(3) . . ?
N9 Hf1 N11 77.0(3) . . ?
N1 Fe1 N5 91.5(3) . . ?
N1 Fe1 N3 90.4(3) . . ?
N5 Fe1 N3 88.9(3) . . ?
N1 Fe1 N2 80.4(3) . . ?
N5 Fe1 N2 168.5(3) . . ?
N3 Fe1 N2 99.2(3) . . ?
N1 Fe1 N4 168.2(3) . . ?
N5 Fe1 N4 96.0(3) . . ?
N3 Fe1 N4 80.6(3) . . ?
N2 Fe1 N4 93.4(3) . . ?
N1 Fe1 N6 98.3(3) . . ?
N5 Fe1 N6 80.5(3) . . ?
N3 Fe1 N6 166.4(3) . . ?
N2 Fe1 N6 92.6(3) . . ?
N4 Fe1 N6 92.0(3) . . ?
N1 O1 Hf1 120.7(5) . . ?
N3 O2 Hf1 119.5(5) . . ?
N5 O3 Hf1 122.1(5) . . ?
C2 N1 O1 118.0(8) . . ?
C2 N1 Fe1 119.7(6) . . ?
O1 N1 Fe1 122.3(6) . . ?
C7 N2 C3 117.5(9) . . ?
C7 N2 Fe1 129.3(7) . . ?
C3 N2 Fe1 113.0(6) . . ?
C9 N3 O2 117.6(7) . . ?
C9 N3 Fe1 119.6(6) . . ?
O2 N3 Fe1 122.3(6) . . ?
C14 N4 C10 118.7(8) . . ?
C14 N4 Fe1 128.3(7) . . ?
C10 N4 Fe1 112.9(6) . . ?
C16 N5 O3 116.2(8) . . ?
C16 N5 Fe1 119.6(7) . . ?
O3 N5 Fe1 124.0(6) . . ?
C21 N6 C17 119.0(9) . . ?
C21 N6 Fe1 129.0(7) . . ?
C17 N6 Fe1 111.6(6) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 111.3(8) . . ?
N1 C2 C1 124.1(9) . . ?
C3 C2 C1 124.5(9) . . ?
N2 C3 C4 122.4(9) . . ?
N2 C3 C2 114.3(9) . . ?
C4 C3 C2 123.1(9) . . ?
C5 C4 C3 118.3(10) . . ?
C5 C4 H4A 120.9 . . ?
C3 C4 H4A 120.9 . . ?
C6 C5 C4 119.6(10) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C7 119.3(10) . . ?
C5 C6 H6A 120.4 . . ?
C7 C6 H6A 120.4 . . ?
N2 C7 C6 123.0(9) . . ?
N2 C7 H7A 118.5 . . ?
C6 C7 H7A 118.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C8 123.8(9) . . ?
N3 C9 C10 111.8(8) . . ?
C8 C9 C10 124.2(8) . . ?
N4 C10 C11 121.3(8) . . ?
N4 C10 C9 114.8(8) . . ?
C11 C10 C9 123.8(9) . . ?
C12 C11 C10 119.7(10) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C13 C12 C11 117.4(10) . . ?
C13 C12 H12A 121.3 . . ?
C11 C12 H12A 121.3 . . ?
C12 C13 C14 121.0(11) . . ?
C12 C13 H13A 119.5 . . ?
C14 C13 H13A 119.5 . . ?
N4 C14 C13 121.8(10) . . ?
N4 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 C16 C17 111.5(9) . . ?
N5 C16 C15 123.9(10) . . ?
C17 C16 C15 124.5(9) . . ?
N6 C17 C18 120.3(10) . . ?
N6 C17 C16 115.1(8) . . ?
C18 C17 C16 124.5(10) . . ?
C19 C18 C17 118.8(11) . . ?
C19 C18 H18A 120.6 . . ?
C17 C18 H18A 120.6 . . ?
C18 C19 C20 119.8(10) . . ?
C18 C19 H19A 120.1 . . ?
C20 C19 H19A 120.1 . . ?
C21 C20 C19 117.8(11) . . ?
C21 C20 H20A 121.1 . . ?
C19 C20 H20A 121.1 . . ?
N6 C21 C20 124.2(11) . . ?
N6 C21 H21A 117.9 . . ?
C20 C21 H21A 117.9 . . ?
C22 N7 C29 107.9(8) . . ?
C22 N7 Hf1 121.7(6) . . ?
C29 N7 Hf1 122.1(6) . . ?
C30 N8 C29 122.5(8) . . ?
C30 N9 C37 108.4(8) . . ?
C30 N9 Hf1 123.7(6) . . ?
C37 N9 Hf1 124.4(6) . . ?
C38 N10 C37 124.5(8) . . ?
C45 N11 C38 107.5(8) . . ?
C45 N11 Hf1 124.4(6) . . ?
C38 N11 Hf1 122.9(6) . . ?
C46 N12 C45 123.5(9) . . ?
C53 N13 C46 107.7(8) . . ?
C53 N13 Hf1 120.0(6) . . ?
C46 N13 Hf1 122.8(6) . . ?
C53 N14 C22 122.6(9) . . ?
N14 C22 N7 126.8(9) . . ?
N14 C22 C23 124.4(9) . . ?
N7 C22 C23 108.8(9) . . ?
C28 C23 C24 121.4(9) . . ?
C28 C23 C22 107.0(8) . . ?
C24 C23 C22 131.6(10) . . ?
C25 C24 C23 116.7(10) . . ?
C25 C24 H24A 121.6 . . ?
C23 C24 H24A 121.6 . . ?
C24 C25 C26 121.6(10) . . ?
C24 C25 H25A 119.2 . . ?
C26 C25 H25A 119.2 . . ?
C27 C26 C25 122.3(10) . . ?
C27 C26 H26A 118.9 . . ?
C25 C26 H26A 118.9 . . ?
C26 C27 C28 117.3(11) . . ?
C26 C27 H27A 121.4 . . ?
C28 C27 H27A 121.4 . . ?
C23 C28 C27 120.6(9) . . ?
C23 C28 C29 106.4(9) . . ?
C27 C28 C29 132.9(10) . . ?
N8 C29 N7 128.4(9) . . ?
N8 C29 C28 121.7(9) . . ?
N7 C29 C28 109.9(9) . . ?
N8 C30 N9 127.7(9) . . ?
N8 C30 C31 122.8(9) . . ?
N9 C30 C31 109.3(8) . . ?
C36 C31 C32 122.2(10) . . ?
C36 C31 C30 105.8(9) . . ?
C32 C31 C30 131.9(10) . . ?
C31 C32 C33 116.5(10) . . ?
C31 C32 H32A 121.7 . . ?
C33 C32 H32A 121.7 . . ?
C34 C33 C32 121.2(10) . . ?
C34 C33 H33A 119.4 . . ?
C32 C33 H33A 119.4 . . ?
C33 C34 C35 123.1(10) . . ?
C33 C34 H34A 118.5 . . ?
C35 C34 H34A 118.5 . . ?
C34 C35 C36 115.8(10) . . ?
C34 C35 H35A 122.1 . . ?
C36 C35 H35A 122.1 . . ?
C31 C36 C35 121.1(10) . . ?
C31 C36 C37 108.0(9) . . ?
C35 C36 C37 130.8(10) . . ?
N10 C37 N9 127.3(8) . . ?
N10 C37 C36 124.3(9) . . ?
N9 C37 C36 108.4(8) . . ?
N10 C38 N11 127.0(9) . . ?
N10 C38 C39 123.5(9) . . ?
N11 C38 C39 109.5(9) . . ?
C40 C39 C38 133.2(11) . . ?
C40 C39 C44 119.7(10) . . ?
C38 C39 C44 107.0(9) . . ?
C41 C40 C39 117.7(11) . . ?
C41 C40 H40A 121.1 . . ?
C39 C40 H40A 121.1 . . ?
C40 C41 C42 121.6(11) . . ?
C40 C41 H41A 119.2 . . ?
C42 C41 H41A 119.2 . . ?
C43 C42 C41 121.9(11) . . ?
C43 C42 H42A 119.0 . . ?
C41 C42 H42A 119.0 . . ?
C44 C43 C42 117.2(11) . . ?
C44 C43 H43A 121.4 . . ?
C42 C43 H43A 121.4 . . ?
C43 C44 C39 121.8(10) . . ?
C43 C44 C45 132.8(10) . . ?
C39 C44 C45 105.4(9) . . ?
N12 C45 N11 126.8(9) . . ?
N12 C45 C44 122.7(9) . . ?
N11 C45 C44 110.5(9) . . ?
N12 C46 N13 127.6(9) . . ?
N12 C46 C47 123.9(10) . . ?
N13 C46 C47 108.5(8) . . ?
C52 C47 C48 121.6(9) . . ?
C52 C47 C46 107.1(9) . . ?
C48 C47 C46 131.3(10) . . ?
C49 C48 C47 116.3(11) . . ?
C49 C48 H48A 121.9 . . ?
C47 C48 H48A 121.9 . . ?
C50 C49 C48 121.9(11) . . ?
C50 C49 H49A 119.1 . . ?
C48 C49 H49A 119.1 . . ?
C49 C50 C51 123.2(11) . . ?
C49 C50 H50A 118.4 . . ?
C51 C50 H50A 118.4 . . ?
C50 C51 C52 115.2(10) . . ?
C50 C51 H51A 122.4 . . ?
C52 C51 H51A 122.4 . . ?
C47 C52 C51 121.7(9) . . ?
C47 C52 C53 107.1(9) . . ?
C51 C52 C53 131.2(10) . . ?
N14 C53 N13 127.7(9) . . ?
N14 C53 C52 122.7(9) . . ?
N13 C53 C52 109.6(8) . . ?
O3S Cl1S O2S 110.5(6) . . ?
O3S Cl1S O4S 109.2(6) . . ?
O2S Cl1S O4S 109.2(7) . . ?
O3S Cl1S O1S 109.5(6) . . ?
O2S Cl1S O1S 108.8(7) . . ?
O4S Cl1S O1S 109.6(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
Hf1 O1 N1 C2 -133.7(7) . . . . ?
Hf1 O1 N1 Fe1 45.7(8) . . . . ?
N5 Fe1 N1 C2 -161.9(7) . . . . ?
N3 Fe1 N1 C2 109.3(7) . . . . ?
N2 Fe1 N1 C2 10.0(7) . . . . ?
N4 Fe1 N1 C2 68.9(18) . . . . ?
N6 Fe1 N1 C2 -81.3(7) . . . . ?
N5 Fe1 N1 O1 18.7(6) . . . . ?
N3 Fe1 N1 O1 -70.2(6) . . . . ?
N2 Fe1 N1 O1 -169.5(6) . . . . ?
N4 Fe1 N1 O1 -110.5(16) . . . . ?
N6 Fe1 N1 O1 99.3(6) . . . . ?
Hf1 O2 N3 C9 -122.8(7) . . . . ?
Hf1 O2 N3 Fe1 48.8(8) . . . . ?
N1 Fe1 N3 C9 -170.8(7) . . . . ?
N5 Fe1 N3 C9 97.7(7) . . . . ?
N2 Fe1 N3 C9 -90.5(7) . . . . ?
N4 Fe1 N3 C9 1.5(7) . . . . ?
N6 Fe1 N3 C9 59.2(17) . . . . ?
N1 Fe1 N3 O2 17.8(6) . . . . ?
N5 Fe1 N3 O2 -73.7(6) . . . . ?
N2 Fe1 N3 O2 98.1(6) . . . . ?
N4 Fe1 N3 O2 -169.9(7) . . . . ?
N6 Fe1 N3 O2 -112.2(13) . . . . ?
Hf1 O3 N5 C16 -135.0(7) . . . . ?
Hf1 O3 N5 Fe1 39.5(9) . . . . ?
N1 Fe1 N5 C16 107.9(8) . . . . ?
N3 Fe1 N5 C16 -161.7(8) . . . . ?
N2 Fe1 N5 C16 63.4(19) . . . . ?
N4 Fe1 N5 C16 -81.2(8) . . . . ?
N6 Fe1 N5 C16 9.8(8) . . . . ?
N1 Fe1 N5 O3 -66.4(7) . . . . ?
N3 Fe1 N5 O3 24.0(7) . . . . ?
N2 Fe1 N5 O3 -110.9(16) . . . . ?
N4 Fe1 N5 O3 104.4(7) . . . . ?
N6 Fe1 N5 O3 -164.6(7) . . . . ?
O1 N1 C2 C3 171.7(7) . . . . ?
Fe1 N1 C2 C3 -7.7(10) . . . . ?
O1 N1 C2 C1 -4.5(13) . . . . ?
Fe1 N1 C2 C1 176.0(7) . . . . ?
C7 N2 C3 C4 -1.0(13) . . . . ?
Fe1 N2 C3 C4 -175.8(7) . . . . ?
C7 N2 C3 C2 -176.6(8) . . . . ?
Fe1 N2 C3 C2 8.7(10) . . . . ?
N1 C2 C3 N2 -1.1(11) . . . . ?
C1 C2 C3 N2 175.1(8) . . . . ?
N1 C2 C3 C4 -176.7(9) . . . . ?
C1 C2 C3 C4 -0.4(15) . . . . ?
N2 C3 C4 C5 1.1(14) . . . . ?
C2 C3 C4 C5 176.3(9) . . . . ?
C3 C4 C5 C6 -0.7(14) . . . . ?
C4 C5 C6 C7 0.2(14) . . . . ?
C3 N2 C7 C6 0.5(13) . . . . ?
Fe1 N2 C7 C6 174.2(7) . . . . ?
C5 C6 C7 N2 -0.1(14) . . . . ?
O2 N3 C9 C8 -2.6(13) . . . . ?
Fe1 N3 C9 C8 -174.4(7) . . . . ?
O2 N3 C9 C10 173.1(7) . . . . ?
Fe1 N3 C9 C10 1.3(10) . . . . ?
C14 N4 C10 C11 0.5(14) . . . . ?
Fe1 N4 C10 C11 -175.9(7) . . . . ?
C14 N4 C10 C9 -177.6(9) . . . . ?
Fe1 N4 C10 C9 6.0(10) . . . . ?
N3 C9 C10 N4 -4.9(12) . . . . ?
C8 C9 C10 N4 170.8(9) . . . . ?
N3 C9 C10 C11 177.1(9) . . . . ?
C8 C9 C10 C11 -7.2(15) . . . . ?
N4 C10 C11 C12 0.3(15) . . . . ?
C9 C10 C11 C12 178.2(10) . . . . ?
C10 C11 C12 C13 -0.3(17) . . . . ?
C11 C12 C13 C14 -0.6(18) . . . . ?
C10 N4 C14 C13 -1.4(16) . . . . ?
Fe1 N4 C14 C13 174.4(9) . . . . ?
C12 C13 C14 N4 1.5(19) . . . . ?
O3 N5 C16 C17 169.5(8) . . . . ?
Fe1 N5 C16 C17 -5.3(12) . . . . ?
O3 N5 C16 C15 -9.5(15) . . . . ?
Fe1 N5 C16 C15 175.7(8) . . . . ?
C21 N6 C17 C18 2.6(14) . . . . ?
Fe1 N6 C17 C18 -171.3(8) . . . . ?
C21 N6 C17 C16 -173.5(9) . . . . ?
Fe1 N6 C17 C16 12.6(11) . . . . ?
N5 C16 C17 N6 -5.4(13) . . . . ?
C15 C16 C17 N6 173.6(10) . . . . ?
N5 C16 C17 C18 178.8(10) . . . . ?
C15 C16 C17 C18 -2.3(17) . . . . ?
N6 C17 C18 C19 -1.6(15) . . . . ?
C16 C17 C18 C19 174.0(10) . . . . ?
C17 C18 C19 C20 -1.4(16) . . . . ?
C18 C19 C20 C21 3.5(16) . . . . ?
C17 N6 C21 C20 -0.4(15) . . . . ?
Fe1 N6 C21 C20 172.3(8) . . . . ?
C19 C20 C21 N6 -2.7(16) . . . . ?
C53 N14 C22 N7 7.0(14) . . . . ?
C53 N14 C22 C23 -176.2(9) . . . . ?
C29 N7 C22 N14 179.1(9) . . . . ?
Hf1 N7 C22 N14 30.2(13) . . . . ?
C29 N7 C22 C23 1.9(10) . . . . ?
Hf1 N7 C22 C23 -147.0(6) . . . . ?
N14 C22 C23 C28 -178.5(8) . . . . ?
N7 C22 C23 C28 -1.2(10) . . . . ?
N14 C22 C23 C24 0.8(16) . . . . ?
N7 C22 C23 C24 178.1(10) . . . . ?
C28 C23 C24 C25 2.6(15) . . . . ?
C22 C23 C24 C25 -176.6(10) . . . . ?
C23 C24 C25 C26 -0.5(16) . . . . ?
C24 C25 C26 C27 -1.9(18) . . . . ?
C25 C26 C27 C28 2.2(17) . . . . ?
C24 C23 C28 C27 -2.3(15) . . . . ?
C22 C23 C28 C27 177.1(9) . . . . ?
C24 C23 C28 C29 -179.3(9) . . . . ?
C22 C23 C28 C29 0.0(10) . . . . ?
C26 C27 C28 C23 -0.1(15) . . . . ?
C26 C27 C28 C29 176.0(10) . . . . ?
C30 N8 C29 N7 0.6(14) . . . . ?
C30 N8 C29 C28 -178.8(8) . . . . ?
C22 N7 C29 N8 178.7(9) . . . . ?
Hf1 N7 C29 N8 -32.5(12) . . . . ?
C22 N7 C29 C28 -1.9(10) . . . . ?
Hf1 N7 C29 C28 146.9(6) . . . . ?
C23 C28 C29 N8 -179.4(8) . . . . ?
C27 C28 C29 N8 4.1(16) . . . . ?
C23 C28 C29 N7 1.2(10) . . . . ?
C27 C28 C29 N7 -175.4(10) . . . . ?
C29 N8 C30 N9 1.6(15) . . . . ?
C29 N8 C30 C31 -173.6(8) . . . . ?
C37 N9 C30 N8 -171.6(9) . . . . ?
Hf1 N9 C30 N8 28.9(13) . . . . ?
C37 N9 C30 C31 4.2(10) . . . . ?
Hf1 N9 C30 C31 -155.3(6) . . . . ?
N8 C30 C31 C36 171.9(9) . . . . ?
N9 C30 C31 C36 -4.1(11) . . . . ?
N8 C30 C31 C32 -11.3(16) . . . . ?
N9 C30 C31 C32 172.7(10) . . . . ?
C36 C31 C32 C33 -1.2(15) . . . . ?
C30 C31 C32 C33 -177.6(10) . . . . ?
C31 C32 C33 C34 -0.8(15) . . . . ?
C32 C33 C34 C35 2.2(17) . . . . ?
C33 C34 C35 C36 -1.3(15) . . . . ?
C32 C31 C36 C35 2.1(15) . . . . ?
C30 C31 C36 C35 179.3(9) . . . . ?
C32 C31 C36 C37 -174.8(9) . . . . ?
C30 C31 C36 C37 2.4(11) . . . . ?
C34 C35 C36 C31 -0.8(14) . . . . ?
C34 C35 C36 C37 175.3(10) . . . . ?
C38 N10 C37 N9 -6.2(15) . . . . ?
C38 N10 C37 C36 173.1(9) . . . . ?
C30 N9 C37 N10 176.7(9) . . . . ?
Hf1 N9 C37 N10 -24.0(13) . . . . ?
C30 N9 C37 C36 -2.6(10) . . . . ?
Hf1 N9 C37 C36 156.7(6) . . . . ?
C31 C36 C37 N10 -179.4(9) . . . . ?
C35 C36 C37 N10 4.2(17) . . . . ?
C31 C36 C37 N9 0.0(11) . . . . ?
C35 C36 C37 N9 -176.4(10) . . . . ?
C37 N10 C38 N11 1.8(15) . . . . ?
C37 N10 C38 C39 -174.6(9) . . . . ?
C45 N11 C38 N10 -173.0(9) . . . . ?
Hf1 N11 C38 N10 31.5(13) . . . . ?
C45 N11 C38 C39 3.8(10) . . . . ?
Hf1 N11 C38 C39 -151.7(6) . . . . ?
N10 C38 C39 C40 -4.5(18) . . . . ?
N11 C38 C39 C40 178.5(11) . . . . ?
N10 C38 C39 C44 173.8(9) . . . . ?
N11 C38 C39 C44 -3.2(11) . . . . ?
C38 C39 C40 C41 177.9(11) . . . . ?
C44 C39 C40 C41 -0.2(16) . . . . ?
C39 C40 C41 C42 -0.4(19) . . . . ?
C40 C41 C42 C43 0(2) . . . . ?
C41 C42 C43 C44 0.7(19) . . . . ?
C42 C43 C44 C39 -1.3(16) . . . . ?
C42 C43 C44 C45 -179.8(11) . . . . ?
C40 C39 C44 C43 1.1(16) . . . . ?
C38 C39 C44 C43 -177.5(9) . . . . ?
C40 C39 C44 C45 179.9(9) . . . . ?
C38 C39 C44 C45 1.3(11) . . . . ?
C46 N12 C45 N11 -2.3(16) . . . . ?
C46 N12 C45 C44 176.7(9) . . . . ?
C38 N11 C45 N12 176.2(9) . . . . ?
Hf1 N11 C45 N12 -28.9(13) . . . . ?
C38 N11 C45 C44 -2.9(10) . . . . ?
Hf1 N11 C45 C44 152.0(6) . . . . ?
C43 C44 C45 N12 0.5(18) . . . . ?
C39 C44 C45 N12 -178.2(9) . . . . ?
C43 C44 C45 N11 179.6(11) . . . . ?
C39 C44 C45 N11 1.0(11) . . . . ?
C45 N12 C46 N13 -0.1(16) . . . . ?
C45 N12 C46 C47 179.7(9) . . . . ?
C53 N13 C46 N12 179.4(10) . . . . ?
Hf1 N13 C46 N12 33.2(13) . . . . ?
C53 N13 C46 C47 -0.5(10) . . . . ?
Hf1 N13 C46 C47 -146.6(6) . . . . ?
N12 C46 C47 C52 -177.4(9) . . . . ?
N13 C46 C47 C52 2.4(11) . . . . ?
N12 C46 C47 C48 0.2(17) . . . . ?
N13 C46 C47 C48 -180.0(10) . . . . ?
C52 C47 C48 C49 -1.0(15) . . . . ?
C46 C47 C48 C49 -178.3(10) . . . . ?
C47 C48 C49 C50 3.2(16) . . . . ?
C48 C49 C50 C51 -5.0(17) . . . . ?
C49 C50 C51 C52 4.0(16) . . . . ?
C48 C47 C52 C51 0.4(15) . . . . ?
C46 C47 C52 C51 178.2(9) . . . . ?
C48 C47 C52 C53 178.8(9) . . . . ?
C46 C47 C52 C53 -3.3(10) . . . . ?
C50 C51 C52 C47 -1.8(15) . . . . ?
C50 C51 C52 C53 -179.8(10) . . . . ?
C22 N14 C53 N13 -3.2(15) . . . . ?
C22 N14 C53 C52 174.1(8) . . . . ?
C46 N13 C53 N14 176.0(9) . . . . ?
Hf1 N13 C53 N14 -36.8(12) . . . . ?
C46 N13 C53 C52 -1.6(10) . . . . ?
Hf1 N13 C53 C52 145.6(6) . . . . ?
C47 C52 C53 N14 -174.6(9) . . . . ?
C51 C52 C53 N14 3.7(16) . . . . ?
C47 C52 C53 N13 3.1(11) . . . . ?
C51 C52 C53 N13 -178.6(10) . . . . ?

_refine_diff_density_max         2.945
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.184

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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_NiZr
_database_code_depnum_ccdc_archive 'CCDC 1503091'
_audit_update_record             
;
2016-09-06 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H37 N14 Ni O3 Zr, Cl O4'
_chemical_formula_sum            'C53 H37 Cl N14 Ni O7 Zr'
_chemical_formula_weight         1167.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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                   12.3075(16)
_cell_length_b                   13.6996(18)
_cell_length_c                   16.041(2)
_cell_angle_alpha                76.481(3)
_cell_angle_beta                 79.763(3)
_cell_angle_gamma                87.948(3)
_cell_volume                     2587.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4056
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_F_000             1188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.684
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3629
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX2 DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45611
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.777
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11305
_reflns_number_gt                7901
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0835P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11305
_refine_ls_number_parameters     697
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1487
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.029
_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
Zr1 Zr 0.41314(3) 0.62370(3) 0.83971(2) 0.01720(11) Uani 1 1 d . . . . .
Ni1 Ni 0.29588(4) 0.67025(4) 0.62993(3) 0.02378(14) Uani 1 1 d . . . . .
O1 O 0.3594(2) 0.5175(2) 0.77584(17) 0.0240(6) Uani 1 1 d . . . . .
O2 O 0.2735(2) 0.70863(19) 0.80725(16) 0.0195(6) Uani 1 1 d . . . . .
O3 O 0.4916(2) 0.6953(3) 0.71282(18) 0.0351(8) Uani 1 1 d . . . . .
N1 N 0.2842(3) 0.5414(3) 0.7220(2) 0.0231(7) Uani 1 1 d . . . . .
N2 N 0.1438(3) 0.6106(3) 0.6218(2) 0.0252(8) Uani 1 1 d . . . . .
N3 N 0.2569(3) 0.7466(2) 0.7243(2) 0.0194(7) Uani 1 1 d . . . . .
N4 N 0.2620(3) 0.8122(3) 0.5589(2) 0.0294(8) Uani 1 1 d . . . . .
N5 N 0.4572(3) 0.6834(3) 0.6394(2) 0.0359(9) Uani 1 1 d . . . . .
N6 N 0.3815(4) 0.6272(4) 0.5192(2) 0.0477(12) Uani 1 1 d . . . . .
C1 C 0.1995(4) 0.3734(3) 0.7850(3) 0.0352(11) Uani 1 1 d . . . . .
H1A H 0.2680 0.3567 0.8082 0.053 Uiso 1 1 calc R U . . .
H1B H 0.1868 0.3251 0.7513 0.053 Uiso 1 1 calc R U . . .
H1C H 0.1375 0.3707 0.8332 0.053 Uiso 1 1 calc R U . . .
C2 C 0.2088(4) 0.4766(3) 0.7276(3) 0.0262(9) Uani 1 1 d . . . . .
C3 C 0.1258(4) 0.5157(3) 0.6707(3) 0.0248(9) Uani 1 1 d . . . . .
C4 C 0.0347(4) 0.4601(3) 0.6697(3) 0.0318(10) Uani 1 1 d . . . . .
H4A H 0.0229 0.3943 0.7056 0.038 Uiso 1 1 calc R U . . .
C5 C -0.0386(4) 0.5019(3) 0.6158(3) 0.0311(10) Uani 1 1 d . . . . .
H5A H -0.1007 0.4644 0.6130 0.037 Uiso 1 1 calc R U . . .
C6 C -0.0211(4) 0.5985(3) 0.5659(3) 0.0291(10) Uani 1 1 d . . . . .
H6A H -0.0713 0.6289 0.5290 0.035 Uiso 1 1 calc R U . . .
C7 C 0.0704(4) 0.6495(3) 0.5709(3) 0.0281(9) Uani 1 1 d . . . . .
H7A H 0.0824 0.7160 0.5364 0.034 Uiso 1 1 calc R U . . .
C8 C 0.1998(4) 0.9034(3) 0.7665(3) 0.0369(11) Uani 1 1 d . . . . .
H8A H 0.2016 0.8635 0.8255 0.055 Uiso 1 1 calc R U . . .
H8B H 0.1261 0.9323 0.7638 0.055 Uiso 1 1 calc R U . . .
H8C H 0.2547 0.9576 0.7518 0.055 Uiso 1 1 calc R U . . .
C9 C 0.2252(3) 0.8387(3) 0.7042(3) 0.0240(9) Uani 1 1 d . . . . .
C10 C 0.2210(3) 0.8743(3) 0.6104(3) 0.0288(10) Uani 1 1 d . . . . .
C11 C 0.1776(4) 0.9666(3) 0.5761(3) 0.0397(11) Uani 1 1 d . . . . .
H11A H 0.1485 1.0097 0.6130 0.048 Uiso 1 1 calc R U . . .
C12 C 0.1770(5) 0.9955(4) 0.4876(4) 0.0552(16) Uani 1 1 d . . . . .
H12A H 0.1479 1.0588 0.4631 0.066 Uiso 1 1 calc R U . . .
C13 C 0.2193(5) 0.9311(4) 0.4355(3) 0.0502(14) Uani 1 1 d . . . . .
H13A H 0.2195 0.9486 0.3746 0.060 Uiso 1 1 calc R U . . .
C14 C 0.2610(4) 0.8415(4) 0.4741(3) 0.0398(12) Uani 1 1 d . . . . .
H14A H 0.2910 0.7976 0.4382 0.048 Uiso 1 1 calc R U . . .
C15 C 0.6515(4) 0.6988(7) 0.5708(4) 0.084(3) Uani 1 1 d . U . . .
H15A H 0.6906 0.6346 0.5781 0.127 Uiso 1 1 calc R U . . .
H15B H 0.6601 0.7309 0.6178 0.127 Uiso 1 1 calc R U . . .
H15C H 0.6823 0.7427 0.5146 0.127 Uiso 1 1 calc R U . . .
C16 C 0.5328(4) 0.6809(5) 0.5739(3) 0.0560(17) Uani 1 1 d . . . . .
C17 C 0.4906(4) 0.6515(5) 0.5023(3) 0.0547(17) Uani 1 1 d . . . . .
C18 C 0.5572(6) 0.6426(7) 0.4251(4) 0.087(3) Uani 1 1 d . . . . .
H18A H 0.6329 0.6615 0.4132 0.105 Uiso 1 1 calc R U . . .
C19 C 0.5122(6) 0.6062(6) 0.3665(4) 0.084(2) Uani 1 1 d . U . . .
H19A H 0.5566 0.6002 0.3131 0.100 Uiso 1 1 calc R U . . .
C20 C 0.4025(7) 0.5781(6) 0.3844(4) 0.076(2) Uani 1 1 d . U . . .
H20A H 0.3713 0.5501 0.3450 0.091 Uiso 1 1 calc R U . . .
C21 C 0.3389(5) 0.5915(5) 0.4614(3) 0.0622(19) Uani 1 1 d . . . . .
H21A H 0.2626 0.5748 0.4734 0.075 Uiso 1 1 calc R U . . .
N7 N 0.5105(3) 0.4823(2) 0.8733(2) 0.0204(7) Uani 1 1 d . . . . .
N8 N 0.3609(3) 0.3617(3) 0.9388(2) 0.0231(7) Uani 1 1 d . . . . .
N9 N 0.3058(3) 0.5281(2) 0.9571(2) 0.0202(7) Uani 1 1 d . . . . .
N10 N 0.1994(3) 0.6564(3) 1.0175(2) 0.0259(8) Uani 1 1 d . . . . .
N11 N 0.3777(3) 0.7222(3) 0.9359(2) 0.0224(7) Uani 1 1 d . . . . .
N12 N 0.5317(3) 0.8387(3) 0.8820(2) 0.0239(7) Uani 1 1 d . . . . .
N13 N 0.5792(3) 0.6757(2) 0.8506(2) 0.0206(7) Uani 1 1 d . . . . .
N14 N 0.6921(3) 0.5448(3) 0.8004(2) 0.0219(7) Uani 1 1 d . . . . .
C22 C 0.6170(3) 0.4732(3) 0.8320(2) 0.0204(8) Uani 1 1 d . . . . .
C23 C 0.6365(3) 0.3690(3) 0.8256(3) 0.0223(8) Uani 1 1 d . . . . .
C24 C 0.7270(3) 0.3215(3) 0.7865(3) 0.0268(9) Uani 1 1 d . . . . .
H24A H 0.7949 0.3560 0.7617 0.032 Uiso 1 1 calc R U . . .
C25 C 0.7137(4) 0.2227(3) 0.7852(3) 0.0328(10) Uani 1 1 d . . . . .
H25A H 0.7736 0.1883 0.7588 0.039 Uiso 1 1 calc R U . . .
C26 C 0.6132(4) 0.1713(3) 0.8221(3) 0.0351(11) Uani 1 1 d . . . . .
H26A H 0.6062 0.1034 0.8191 0.042 Uiso 1 1 calc R U . . .
C27 C 0.5252(4) 0.2175(3) 0.8624(3) 0.0283(9) Uani 1 1 d . . . . .
H27A H 0.4578 0.1826 0.8882 0.034 Uiso 1 1 calc R U . . .
C28 C 0.5389(3) 0.3174(3) 0.8636(3) 0.0245(9) Uani 1 1 d . . . . .
C29 C 0.4614(3) 0.3883(3) 0.8959(2) 0.0229(8) Uani 1 1 d . . . . .
C30 C 0.2904(3) 0.4269(3) 0.9683(2) 0.0213(8) Uani 1 1 d . . . . .
C31 C 0.1834(3) 0.3972(3) 1.0206(3) 0.0250(9) Uani 1 1 d . . . . .
C32 C 0.1239(3) 0.3072(3) 1.0432(3) 0.0303(10) Uani 1 1 d . . . . .
H32A H 0.1537 0.2489 1.0255 0.036 Uiso 1 1 calc R U . . .
C33 C 0.0198(4) 0.3069(4) 1.0926(3) 0.0350(11) Uani 1 1 d . . . . .
H33A H -0.0238 0.2475 1.1075 0.042 Uiso 1 1 calc R U . . .
C34 C -0.0233(4) 0.3912(4) 1.1211(3) 0.0346(11) Uani 1 1 d . . . . .
H34A H -0.0946 0.3875 1.1560 0.041 Uiso 1 1 calc R U . . .
C35 C 0.0351(3) 0.4789(3) 1.0997(3) 0.0299(10) Uani 1 1 d . . . . .
H35A H 0.0062 0.5360 1.1201 0.036 Uiso 1 1 calc R U . . .
C36 C 0.1386(3) 0.4818(3) 1.0470(3) 0.0261(9) Uani 1 1 d . . . . .
C37 C 0.2163(3) 0.5631(3) 1.0068(2) 0.0222(8) Uani 1 1 d . . . . .
C38 C 0.2741(3) 0.7282(3) 0.9852(3) 0.0242(9) Uani 1 1 d . . . . .
C39 C 0.2583(3) 0.8285(3) 0.9998(3) 0.0267(9) Uani 1 1 d . . . . .
C40 C 0.1688(4) 0.8730(4) 1.0438(3) 0.0331(10) Uani 1 1 d . . . . .
H40A H 0.1023 0.8369 1.0704 0.040 Uiso 1 1 calc R U . . .
C41 C 0.1820(4) 0.9723(4) 1.0465(3) 0.0410(12) Uani 1 1 d . . . . .
H41A H 0.1227 1.0055 1.0749 0.049 Uiso 1 1 calc R U . . .
C42 C 0.2807(4) 1.0248(4) 1.0081(3) 0.0418(12) Uani 1 1 d . . . . .
H42A H 0.2869 1.0926 1.0116 0.050 Uiso 1 1 calc R U . . .
C43 C 0.3690(4) 0.9805(3) 0.9655(3) 0.0329(10) Uani 1 1 d . . . . .
H43A H 0.4361 1.0162 0.9401 0.039 Uiso 1 1 calc R U . . .
C44 C 0.3557(3) 0.8815(3) 0.9612(3) 0.0267(9) Uani 1 1 d . . . . .
C45 C 0.4293(3) 0.8136(3) 0.9225(3) 0.0231(8) Uani 1 1 d . . . . .
C46 C 0.6001(3) 0.7747(3) 0.8496(2) 0.0235(9) Uani 1 1 d . . . . .
C47 C 0.7122(3) 0.8017(3) 0.8049(2) 0.0231(8) Uani 1 1 d . . . . .
C48 C 0.7721(3) 0.8903(3) 0.7854(3) 0.0283(9) Uani 1 1 d . . . . .
H48A H 0.7418 0.9479 0.8042 0.034 Uiso 1 1 calc R U . . .
C49 C 0.8784(4) 0.8922(3) 0.7372(3) 0.0303(10) Uani 1 1 d . . . . .
H49A H 0.9211 0.9522 0.7219 0.036 Uiso 1 1 calc R U . . .
C50 C 0.9224(3) 0.8069(3) 0.7114(3) 0.0315(10) Uani 1 1 d . . . . .
H50A H 0.9947 0.8100 0.6781 0.038 Uiso 1 1 calc R U . . .
C51 C 0.8639(3) 0.7175(3) 0.7328(3) 0.0266(9) Uani 1 1 d . . . . .
H51A H 0.8953 0.6592 0.7158 0.032 Uiso 1 1 calc R U . . .
C52 C 0.7579(3) 0.7163(3) 0.7798(3) 0.0233(8) Uani 1 1 d . . . . .
C53 C 0.6747(3) 0.6381(3) 0.8106(2) 0.0206(8) Uani 1 1 d . . . . .
Cl1S Cl -0.03417(13) 0.80038(9) 0.36695(10) 0.0522(4) Uani 1 1 d . . . . .
O1S O 0.0610(3) 0.7378(3) 0.3586(3) 0.0513(10) Uani 1 1 d . . . . .
O3S O -0.0427(5) 0.8325(3) 0.4490(3) 0.0842(16) Uani 1 1 d . . . . .
O4S O -0.1316(3) 0.7461(3) 0.3775(3) 0.0707(12) Uani 1 1 d . . . . .
O2S O -0.0272(6) 0.8865(4) 0.2980(3) 0.106(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O2 2.114(3) . ?
Zr1 O3 2.115(3) . ?
Zr1 O1 2.147(3) . ?
Zr1 N13 2.237(3) . ?
Zr1 N7 2.248(3) . ?
Zr1 N11 2.254(3) . ?
Zr1 N9 2.257(3) . ?
Ni1 N1 2.010(3) . ?
Ni1 N3 2.014(3) . ?
Ni1 N5 2.036(4) . ?
Ni1 N4 2.081(4) . ?
Ni1 N6 2.097(4) . ?
Ni1 N2 2.105(4) . ?
O1 N1 1.357(4) . ?
O2 N3 1.360(4) . ?
O3 N5 1.365(4) . ?
N1 C2 1.284(5) . ?
N2 C7 1.339(5) . ?
N2 C3 1.355(5) . ?
N3 C9 1.292(5) . ?
N4 C14 1.327(5) . ?
N4 C10 1.346(6) . ?
N5 C16 1.280(6) . ?
N6 C21 1.332(7) . ?
N6 C17 1.359(7) . ?
C1 C2 1.492(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.492(6) . ?
C3 C4 1.382(6) . ?
C4 C5 1.378(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.379(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.371(6) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.472(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.478(6) . ?
C10 C11 1.385(6) . ?
C11 C12 1.382(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.380(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.366(7) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.480(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.481(8) . ?
C17 C18 1.387(7) . ?
C18 C19 1.366(10) . ?
C18 H18A 0.9500 . ?
C19 C20 1.378(11) . ?
C19 H19A 0.9500 . ?
C20 C21 1.388(8) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
N7 C22 1.376(5) . ?
N7 C29 1.383(5) . ?
N8 C29 1.323(5) . ?
N8 C30 1.331(5) . ?
N9 C30 1.371(5) . ?
N9 C37 1.381(5) . ?
N10 C38 1.319(5) . ?
N10 C37 1.334(5) . ?
N11 C45 1.378(5) . ?
N11 C38 1.387(5) . ?
N12 C46 1.325(5) . ?
N12 C45 1.327(5) . ?
N13 C53 1.379(5) . ?
N13 C46 1.385(5) . ?
N14 C22 1.319(5) . ?
N14 C53 1.331(5) . ?
C22 C23 1.463(5) . ?
C23 C28 1.383(6) . ?
C23 C24 1.397(6) . ?
C24 C25 1.375(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.408(6) . ?
C25 H25A 0.9500 . ?
C26 C27 1.373(6) . ?
C26 H26A 0.9500 . ?
C27 C28 1.390(6) . ?
C27 H27A 0.9500 . ?
C28 C29 1.454(6) . ?
C30 C31 1.446(5) . ?
C31 C36 1.388(6) . ?
C31 C32 1.396(6) . ?
C32 C33 1.381(6) . ?
C32 H32A 0.9500 . ?
C33 C34 1.393(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.363(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.395(6) . ?
C35 H35A 0.9500 . ?
C36 C37 1.446(6) . ?
C38 C39 1.448(6) . ?
C39 C44 1.392(6) . ?
C39 C40 1.399(6) . ?
C40 C41 1.388(7) . ?
C40 H40A 0.9500 . ?
C41 C42 1.400(7) . ?
C41 H41A 0.9500 . ?
C42 C43 1.378(6) . ?
C42 H42A 0.9500 . ?
C43 C44 1.391(6) . ?
C43 H43A 0.9500 . ?
C44 C45 1.444(5) . ?
C46 C47 1.455(5) . ?
C47 C48 1.386(6) . ?
C47 C52 1.392(6) . ?
C48 C49 1.394(6) . ?
C48 H48A 0.9500 . ?
C49 C50 1.390(6) . ?
C49 H49A 0.9500 . ?
C50 C51 1.383(6) . ?
C50 H50A 0.9500 . ?
C51 C52 1.386(6) . ?
C51 H51A 0.9500 . ?
C52 C53 1.445(6) . ?
Cl1S O4S 1.396(4) . ?
Cl1S O2S 1.410(5) . ?
Cl1S O1S 1.432(4) . ?
Cl1S O3S 1.468(4) . ?

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 Zr1 O3 85.12(11) . . ?
O2 Zr1 O1 86.06(10) . . ?
O3 Zr1 O1 84.10(12) . . ?
O2 Zr1 N13 129.61(11) . . ?
O3 Zr1 N13 72.71(11) . . ?
O1 Zr1 N13 133.59(11) . . ?
O2 Zr1 N7 155.27(11) . . ?
O3 Zr1 N7 104.12(12) . . ?
O1 Zr1 N7 72.42(11) . . ?
N13 Zr1 N7 75.08(12) . . ?
O2 Zr1 N11 74.93(11) . . ?
O3 Zr1 N11 115.74(13) . . ?
O1 Zr1 N11 150.54(11) . . ?
N13 Zr1 N11 75.23(11) . . ?
N7 Zr1 N11 119.05(12) . . ?
O2 Zr1 N9 89.86(11) . . ?
O3 Zr1 N9 165.87(12) . . ?
O1 Zr1 N9 82.39(11) . . ?
N13 Zr1 N9 120.10(11) . . ?
N7 Zr1 N9 75.62(11) . . ?
N11 Zr1 N9 75.39(12) . . ?
N1 Ni1 N3 89.22(12) . . ?
N1 Ni1 N5 89.86(15) . . ?
N3 Ni1 N5 87.77(14) . . ?
N1 Ni1 N4 161.99(13) . . ?
N3 Ni1 N4 78.24(14) . . ?
N5 Ni1 N4 102.37(15) . . ?
N1 Ni1 N6 102.98(15) . . ?
N3 Ni1 N6 160.02(17) . . ?
N5 Ni1 N6 76.64(16) . . ?
N4 Ni1 N6 92.78(16) . . ?
N1 Ni1 N2 77.35(14) . . ?
N3 Ni1 N2 103.94(13) . . ?
N5 Ni1 N2 162.36(15) . . ?
N4 Ni1 N2 93.02(13) . . ?
N6 Ni1 N2 94.25(16) . . ?
N1 O1 Zr1 122.1(2) . . ?
N3 O2 Zr1 124.0(2) . . ?
N5 O3 Zr1 122.8(2) . . ?
C2 N1 O1 118.2(3) . . ?
C2 N1 Ni1 120.4(3) . . ?
O1 N1 Ni1 121.2(3) . . ?
C7 N2 C3 117.7(4) . . ?
C7 N2 Ni1 129.3(3) . . ?
C3 N2 Ni1 112.7(3) . . ?
C9 N3 O2 117.8(3) . . ?
C9 N3 Ni1 119.3(3) . . ?
O2 N3 Ni1 122.5(2) . . ?
C14 N4 C10 118.7(4) . . ?
C14 N4 Ni1 128.2(3) . . ?
C10 N4 Ni1 112.3(3) . . ?
C16 N5 O3 116.5(4) . . ?
C16 N5 Ni1 119.8(3) . . ?
O3 N5 Ni1 123.8(2) . . ?
C21 N6 C17 119.2(4) . . ?
C21 N6 Ni1 127.4(4) . . ?
C17 N6 Ni1 112.9(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 125.8(4) . . ?
N1 C2 C3 112.7(4) . . ?
C1 C2 C3 121.5(4) . . ?
N2 C3 C4 122.1(4) . . ?
N2 C3 C2 115.6(4) . . ?
C4 C3 C2 122.3(4) . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.6 . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C7 C6 C5 118.4(4) . . ?
C7 C6 H6A 120.8 . . ?
C5 C6 H6A 120.8 . . ?
N2 C7 C6 123.4(4) . . ?
N2 C7 H7A 118.3 . . ?
C6 C7 H7A 118.3 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C8 124.2(4) . . ?
N3 C9 C10 112.7(4) . . ?
C8 C9 C10 123.0(4) . . ?
N4 C10 C11 120.8(4) . . ?
N4 C10 C9 116.6(4) . . ?
C11 C10 C9 122.6(4) . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C13 C12 C11 119.0(5) . . ?
C13 C12 H12A 120.5 . . ?
C11 C12 H12A 120.5 . . ?
C14 C13 C12 118.1(5) . . ?
C14 C13 H13A 121.0 . . ?
C12 C13 H13A 121.0 . . ?
N4 C14 C13 123.9(5) . . ?
N4 C14 H14A 118.1 . . ?
C13 C14 H14A 118.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 C16 C15 124.3(5) . . ?
N5 C16 C17 113.0(5) . . ?
C15 C16 C17 122.6(5) . . ?
N6 C17 C18 121.2(6) . . ?
N6 C17 C16 115.3(4) . . ?
C18 C17 C16 123.4(6) . . ?
C19 C18 C17 118.9(7) . . ?
C19 C18 H18A 120.6 . . ?
C17 C18 H18A 120.6 . . ?
C18 C19 C20 120.3(5) . . ?
C18 C19 H19A 119.8 . . ?
C20 C19 H19A 119.8 . . ?
C19 C20 C21 118.3(6) . . ?
C19 C20 H20A 120.8 . . ?
C21 C20 H20A 120.8 . . ?
N6 C21 C20 122.0(7) . . ?
N6 C21 H21A 119.0 . . ?
C20 C21 H21A 119.0 . . ?
C22 N7 C29 107.9(3) . . ?
C22 N7 Zr1 121.8(2) . . ?
C29 N7 Zr1 122.0(2) . . ?
C29 N8 C30 122.2(4) . . ?
C30 N9 C37 107.2(3) . . ?
C30 N9 Zr1 123.5(2) . . ?
C37 N9 Zr1 124.6(3) . . ?
C38 N10 C37 122.5(3) . . ?
C45 N11 C38 107.2(3) . . ?
C45 N11 Zr1 122.4(3) . . ?
C38 N11 Zr1 122.8(3) . . ?
C46 N12 C45 122.5(4) . . ?
C53 N13 C46 107.3(3) . . ?
C53 N13 Zr1 121.1(2) . . ?
C46 N13 Zr1 122.1(2) . . ?
C22 N14 C53 122.4(3) . . ?
N14 C22 N7 127.4(4) . . ?
N14 C22 C23 123.3(3) . . ?
N7 C22 C23 109.2(3) . . ?
C28 C23 C24 121.0(4) . . ?
C28 C23 C22 106.5(3) . . ?
C24 C23 C22 132.3(4) . . ?
C25 C24 C23 117.2(4) . . ?
C25 C24 H24A 121.4 . . ?
C23 C24 H24A 121.4 . . ?
C24 C25 C26 121.5(4) . . ?
C24 C25 H25A 119.2 . . ?
C26 C25 H25A 119.2 . . ?
C27 C26 C25 121.2(4) . . ?
C27 C26 H26A 119.4 . . ?
C25 C26 H26A 119.4 . . ?
C26 C27 C28 117.2(4) . . ?
C26 C27 H27A 121.4 . . ?
C28 C27 H27A 121.4 . . ?
C23 C28 C27 121.9(4) . . ?
C23 C28 C29 107.2(4) . . ?
C27 C28 C29 130.8(4) . . ?
N8 C29 N7 128.5(4) . . ?
N8 C29 C28 122.5(4) . . ?
N7 C29 C28 109.0(3) . . ?
N8 C30 N9 127.6(4) . . ?
N8 C30 C31 122.6(4) . . ?
N9 C30 C31 109.8(3) . . ?
C36 C31 C32 120.8(4) . . ?
C36 C31 C30 106.5(4) . . ?
C32 C31 C30 132.7(4) . . ?
C33 C32 C31 116.9(4) . . ?
C33 C32 H32A 121.5 . . ?
C31 C32 H32A 121.5 . . ?
C32 C33 C34 121.9(4) . . ?
C32 C33 H33A 119.0 . . ?
C34 C33 H33A 119.0 . . ?
C35 C34 C33 121.2(4) . . ?
C35 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
C34 C35 C36 117.6(4) . . ?
C34 C35 H35A 121.2 . . ?
C36 C35 H35A 121.2 . . ?
C31 C36 C35 121.4(4) . . ?
C31 C36 C37 106.7(4) . . ?
C35 C36 C37 131.8(4) . . ?
N10 C37 N9 127.4(4) . . ?
N10 C37 C36 123.1(4) . . ?
N9 C37 C36 109.5(4) . . ?
N10 C38 N11 128.0(4) . . ?
N10 C38 C39 122.8(4) . . ?
N11 C38 C39 109.2(4) . . ?
C44 C39 C40 121.4(4) . . ?
C44 C39 C38 106.9(3) . . ?
C40 C39 C38 131.7(4) . . ?
C41 C40 C39 116.7(4) . . ?
C41 C40 H40A 121.6 . . ?
C39 C40 H40A 121.6 . . ?
C40 C41 C42 121.5(4) . . ?
C40 C41 H41A 119.3 . . ?
C42 C41 H41A 119.3 . . ?
C43 C42 C41 121.7(4) . . ?
C43 C42 H42A 119.2 . . ?
C41 C42 H42A 119.2 . . ?
C42 C43 C44 117.2(4) . . ?
C42 C43 H43A 121.4 . . ?
C44 C43 H43A 121.4 . . ?
C43 C44 C39 121.6(4) . . ?
C43 C44 C45 131.8(4) . . ?
C39 C44 C45 106.6(4) . . ?
N12 C45 N11 127.2(4) . . ?
N12 C45 C44 122.9(4) . . ?
N11 C45 C44 109.9(4) . . ?
N12 C46 N13 127.6(4) . . ?
N12 C46 C47 122.8(4) . . ?
N13 C46 C47 109.5(3) . . ?
C48 C47 C52 121.2(4) . . ?
C48 C47 C46 132.5(4) . . ?
C52 C47 C46 106.4(4) . . ?
C47 C48 C49 117.8(4) . . ?
C47 C48 H48A 121.1 . . ?
C49 C48 H48A 121.1 . . ?
C50 C49 C48 120.4(4) . . ?
C50 C49 H49A 119.8 . . ?
C48 C49 H49A 119.8 . . ?
C51 C50 C49 122.0(4) . . ?
C51 C50 H50A 119.0 . . ?
C49 C50 H50A 119.0 . . ?
C50 C51 C52 117.4(4) . . ?
C50 C51 H51A 121.3 . . ?
C52 C51 H51A 121.3 . . ?
C51 C52 C47 121.2(4) . . ?
C51 C52 C53 131.7(4) . . ?
C47 C52 C53 107.0(3) . . ?
N14 C53 N13 127.2(4) . . ?
N14 C53 C52 123.1(3) . . ?
N13 C53 C52 109.8(3) . . ?
O4S Cl1S O2S 112.2(4) . . ?
O4S Cl1S O1S 111.5(2) . . ?
O2S Cl1S O1S 112.2(3) . . ?
O4S Cl1S O3S 103.8(3) . . ?
O2S Cl1S O3S 108.6(3) . . ?
O1S Cl1S O3S 108.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 N1 C2 -138.1(3) . . . . ?
Zr1 O1 N1 Ni1 46.3(3) . . . . ?
Zr1 O2 N3 C9 -134.1(3) . . . . ?
Zr1 O2 N3 Ni1 38.9(3) . . . . ?
Zr1 O3 N5 C16 -143.6(4) . . . . ?
Zr1 O3 N5 Ni1 36.5(4) . . . . ?
O1 N1 C2 C1 -3.8(6) . . . . ?
Ni1 N1 C2 C1 171.9(3) . . . . ?
O1 N1 C2 C3 174.8(3) . . . . ?
Ni1 N1 C2 C3 -9.5(4) . . . . ?
C7 N2 C3 C4 -0.8(6) . . . . ?
Ni1 N2 C3 C4 -175.2(3) . . . . ?
C7 N2 C3 C2 -178.9(3) . . . . ?
Ni1 N2 C3 C2 6.7(4) . . . . ?
N1 C2 C3 N2 1.2(5) . . . . ?
C1 C2 C3 N2 179.9(4) . . . . ?
N1 C2 C3 C4 -176.9(4) . . . . ?
C1 C2 C3 C4 1.8(6) . . . . ?
N2 C3 C4 C5 1.5(6) . . . . ?
C2 C3 C4 C5 179.5(4) . . . . ?
C3 C4 C5 C6 -1.6(6) . . . . ?
C4 C5 C6 C7 0.9(6) . . . . ?
C3 N2 C7 C6 0.0(6) . . . . ?
Ni1 N2 C7 C6 173.5(3) . . . . ?
C5 C6 C7 N2 -0.1(6) . . . . ?
O2 N3 C9 C8 -3.6(6) . . . . ?
Ni1 N3 C9 C8 -176.9(3) . . . . ?
O2 N3 C9 C10 174.2(3) . . . . ?
Ni1 N3 C9 C10 0.9(4) . . . . ?
C14 N4 C10 C11 0.6(6) . . . . ?
Ni1 N4 C10 C11 -170.0(3) . . . . ?
C14 N4 C10 C9 -179.3(4) . . . . ?
Ni1 N4 C10 C9 10.1(4) . . . . ?
N3 C9 C10 N4 -7.5(5) . . . . ?
C8 C9 C10 N4 170.3(4) . . . . ?
N3 C9 C10 C11 172.6(4) . . . . ?
C8 C9 C10 C11 -9.6(6) . . . . ?
N4 C10 C11 C12 -0.3(7) . . . . ?
C9 C10 C11 C12 179.5(4) . . . . ?
C10 C11 C12 C13 0.3(8) . . . . ?
C11 C12 C13 C14 -0.5(8) . . . . ?
C10 N4 C14 C13 -0.9(7) . . . . ?
Ni1 N4 C14 C13 168.1(4) . . . . ?
C12 C13 C14 N4 0.8(8) . . . . ?
O3 N5 C16 C15 -5.6(9) . . . . ?
Ni1 N5 C16 C15 174.3(5) . . . . ?
O3 N5 C16 C17 170.6(4) . . . . ?
Ni1 N5 C16 C17 -9.5(7) . . . . ?
C21 N6 C17 C18 2.0(9) . . . . ?
Ni1 N6 C17 C18 -170.4(5) . . . . ?
C21 N6 C17 C16 -174.2(5) . . . . ?
Ni1 N6 C17 C16 13.4(6) . . . . ?
N5 C16 C17 N6 -3.2(8) . . . . ?
C15 C16 C17 N6 173.1(6) . . . . ?
N5 C16 C17 C18 -179.3(6) . . . . ?
C15 C16 C17 C18 -3.0(10) . . . . ?
N6 C17 C18 C19 -1.7(10) . . . . ?
C16 C17 C18 C19 174.1(6) . . . . ?
C17 C18 C19 C20 -0.6(10) . . . . ?
C18 C19 C20 C21 2.6(10) . . . . ?
C17 N6 C21 C20 0.1(8) . . . . ?
Ni1 N6 C21 C20 171.3(4) . . . . ?
C19 C20 C21 N6 -2.4(9) . . . . ?
C53 N14 C22 N7 5.0(6) . . . . ?
C53 N14 C22 C23 -176.6(3) . . . . ?
C29 N7 C22 N14 -179.8(4) . . . . ?
Zr1 N7 C22 N14 31.5(5) . . . . ?
C29 N7 C22 C23 1.6(4) . . . . ?
Zr1 N7 C22 C23 -147.1(3) . . . . ?
N14 C22 C23 C28 -178.4(4) . . . . ?
N7 C22 C23 C28 0.3(4) . . . . ?
N14 C22 C23 C24 -2.4(7) . . . . ?
N7 C22 C23 C24 176.2(4) . . . . ?
C28 C23 C24 C25 1.8(6) . . . . ?
C22 C23 C24 C25 -173.6(4) . . . . ?
C23 C24 C25 C26 -0.2(6) . . . . ?
C24 C25 C26 C27 -1.3(7) . . . . ?
C25 C26 C27 C28 1.2(7) . . . . ?
C24 C23 C28 C27 -2.0(6) . . . . ?
C22 C23 C28 C27 174.5(4) . . . . ?
C24 C23 C28 C29 -178.5(3) . . . . ?
C22 C23 C28 C29 -2.0(4) . . . . ?
C26 C27 C28 C23 0.4(6) . . . . ?
C26 C27 C28 C29 176.0(4) . . . . ?
C30 N8 C29 N7 -0.7(6) . . . . ?
C30 N8 C29 C28 179.9(3) . . . . ?
C22 N7 C29 N8 177.7(4) . . . . ?
Zr1 N7 C29 N8 -33.7(5) . . . . ?
C22 N7 C29 C28 -2.9(4) . . . . ?
Zr1 N7 C29 C28 145.8(3) . . . . ?
C23 C28 C29 N8 -177.5(4) . . . . ?
C27 C28 C29 N8 6.5(7) . . . . ?
C23 C28 C29 N7 3.0(4) . . . . ?
C27 C28 C29 N7 -173.0(4) . . . . ?
C29 N8 C30 N9 2.9(6) . . . . ?
C29 N8 C30 C31 -175.5(4) . . . . ?
C37 N9 C30 N8 -173.5(4) . . . . ?
Zr1 N9 C30 N8 29.9(5) . . . . ?
C37 N9 C30 C31 5.1(4) . . . . ?
Zr1 N9 C30 C31 -151.5(3) . . . . ?
N8 C30 C31 C36 173.6(3) . . . . ?
N9 C30 C31 C36 -5.1(4) . . . . ?
N8 C30 C31 C32 -8.8(7) . . . . ?
N9 C30 C31 C32 172.6(4) . . . . ?
C36 C31 C32 C33 0.0(6) . . . . ?
C30 C31 C32 C33 -177.4(4) . . . . ?
C31 C32 C33 C34 -2.0(6) . . . . ?
C32 C33 C34 C35 1.4(7) . . . . ?
C33 C34 C35 C36 1.1(6) . . . . ?
C32 C31 C36 C35 2.6(6) . . . . ?
C30 C31 C36 C35 -179.4(4) . . . . ?
C32 C31 C36 C37 -175.1(4) . . . . ?
C30 C31 C36 C37 2.9(4) . . . . ?
C34 C35 C36 C31 -3.1(6) . . . . ?
C34 C35 C36 C37 173.9(4) . . . . ?
C38 N10 C37 N9 -5.4(6) . . . . ?
C38 N10 C37 C36 175.3(4) . . . . ?
C30 N9 C37 N10 177.4(4) . . . . ?
Zr1 N9 C37 N10 -26.3(5) . . . . ?
C30 N9 C37 C36 -3.2(4) . . . . ?
Zr1 N9 C37 C36 153.1(3) . . . . ?
C31 C36 C37 N10 179.5(3) . . . . ?
C35 C36 C37 N10 2.2(7) . . . . ?
C31 C36 C37 N9 0.1(4) . . . . ?
C35 C36 C37 N9 -177.2(4) . . . . ?
C37 N10 C38 N11 1.0(6) . . . . ?
C37 N10 C38 C39 -177.2(4) . . . . ?
C45 N11 C38 N10 -175.6(4) . . . . ?
Zr1 N11 C38 N10 34.1(5) . . . . ?
C45 N11 C38 C39 2.7(4) . . . . ?
Zr1 N11 C38 C39 -147.5(3) . . . . ?
N10 C38 C39 C44 176.3(4) . . . . ?
N11 C38 C39 C44 -2.2(5) . . . . ?
N10 C38 C39 C40 -2.7(7) . . . . ?
N11 C38 C39 C40 178.9(4) . . . . ?
C44 C39 C40 C41 0.3(6) . . . . ?
C38 C39 C40 C41 179.1(4) . . . . ?
C39 C40 C41 C42 -0.9(7) . . . . ?
C40 C41 C42 C43 0.4(8) . . . . ?
C41 C42 C43 C44 0.7(7) . . . . ?
C42 C43 C44 C39 -1.3(7) . . . . ?
C42 C43 C44 C45 180.0(4) . . . . ?
C40 C39 C44 C43 0.8(7) . . . . ?
C38 C39 C44 C43 -178.2(4) . . . . ?
C40 C39 C44 C45 179.8(4) . . . . ?
C38 C39 C44 C45 0.7(4) . . . . ?
C46 N12 C45 N11 -1.3(6) . . . . ?
C46 N12 C45 C44 177.4(4) . . . . ?
C38 N11 C45 N12 176.6(4) . . . . ?
Zr1 N11 C45 N12 -33.1(5) . . . . ?
C38 N11 C45 C44 -2.3(4) . . . . ?
Zr1 N11 C45 C44 148.1(3) . . . . ?
C43 C44 C45 N12 0.8(7) . . . . ?
C39 C44 C45 N12 -178.0(4) . . . . ?
C43 C44 C45 N11 179.8(4) . . . . ?
C39 C44 C45 N11 0.9(5) . . . . ?
C45 N12 C46 N13 0.7(6) . . . . ?
C45 N12 C46 C47 179.8(4) . . . . ?
C53 N13 C46 N12 -179.1(4) . . . . ?
Zr1 N13 C46 N12 34.4(5) . . . . ?
C53 N13 C46 C47 1.7(4) . . . . ?
Zr1 N13 C46 C47 -144.8(3) . . . . ?
N12 C46 C47 C48 -0.3(7) . . . . ?
N13 C46 C47 C48 178.9(4) . . . . ?
N12 C46 C47 C52 -179.6(4) . . . . ?
N13 C46 C47 C52 -0.4(4) . . . . ?
C52 C47 C48 C49 2.2(6) . . . . ?
C46 C47 C48 C49 -177.0(4) . . . . ?
C47 C48 C49 C50 -1.1(6) . . . . ?
C48 C49 C50 C51 -0.6(6) . . . . ?
C49 C50 C51 C52 1.3(6) . . . . ?
C50 C51 C52 C47 -0.2(6) . . . . ?
C50 C51 C52 C53 178.4(4) . . . . ?
C48 C47 C52 C51 -1.5(6) . . . . ?
C46 C47 C52 C51 177.8(4) . . . . ?
C48 C47 C52 C53 179.6(4) . . . . ?
C46 C47 C52 C53 -1.1(4) . . . . ?
C22 N14 C53 N13 -2.8(6) . . . . ?
C22 N14 C53 C52 177.0(4) . . . . ?
C46 N13 C53 N14 177.5(4) . . . . ?
Zr1 N13 C53 N14 -35.6(5) . . . . ?
C46 N13 C53 C52 -2.4(4) . . . . ?
Zr1 N13 C53 C52 144.5(3) . . . . ?
C51 C52 C53 N14 3.6(7) . . . . ?
C47 C52 C53 N14 -177.7(3) . . . . ?
C51 C52 C53 N13 -176.6(4) . . . . ?
C47 C52 C53 N13 2.2(4) . . . . ?

_refine_diff_density_max         1.650
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.102

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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_sb
_database_code_depnum_ccdc_archive 'CCDC 1503092'
_audit_update_record             
;
2016-11-15 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H36 N6 Ni O3 Sb, Cl O4'
_chemical_formula_sum            'C27 H36 Cl N6 Ni O7 Sb'
_chemical_formula_weight         772.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   12.9295(6)
_cell_length_b                   12.9295(6)
_cell_length_c                   31.955(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4626.3(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1235
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             2352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.627
_shelx_estimated_absorpt_T_min   0.686
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3396
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX2 DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19347
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0518
_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       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.912
_diffrn_reflns_theta_max         28.972
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2743
_reflns_number_gt                2327
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0950P)²+1.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2743
_refine_ls_number_parameters     145
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1279
_refine_ls_wR_factor_gt          0.1185
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.6667 0.3333 0.02607(2) 0.01494(16) Uani 1 3 d S T P . .
Sb1 Sb 0.6667 0.3333 0.14484(2) 0.01826(14) Uani 1 3 d S T P . .
O1 O 0.73228(19) 0.24919(18) 0.10312(6) 0.0199(4) Uani 1 1 d . . . . .
N1 N 0.7639(2) 0.2870(2) 0.06322(7) 0.0172(5) Uani 1 1 d . . . . .
N2 N 0.8186(2) 0.3797(2) -0.01087(8) 0.0197(5) Uani 1 1 d . . . . .
C1 C 0.9303(3) 0.2458(3) 0.07012(10) 0.0288(7) Uani 1 1 d . . . . .
H1A H 1.0126 0.3123 0.0721 0.043 Uiso 1 1 calc R U . . .
H1B H 0.9291 0.1798 0.0547 0.043 Uiso 1 1 calc R U . . .
H1C H 0.8983 0.2188 0.0983 0.043 Uiso 1 1 calc R U . . .
C2 C 0.8555(2) 0.2863(3) 0.04771(9) 0.0196(5) Uani 1 1 d . . . . .
C3 C 0.8829(2) 0.3309(3) 0.00434(9) 0.0197(6) Uani 1 1 d . . . . .
C4 C 0.9698(3) 0.3253(3) -0.01954(10) 0.0280(7) Uani 1 1 d . . . . .
H4A H 1.0146 0.2919 -0.0083 0.034 Uiso 1 1 calc R U . . .
C5 C 0.9899(3) 0.3691(3) -0.05999(10) 0.0316(7) Uani 1 1 d . . . . .
H5A H 1.0482 0.3651 -0.0769 0.038 Uiso 1 1 calc R U . . .
C6 C 0.9249(3) 0.4186(3) -0.07566(10) 0.0295(7) Uani 1 1 d . . . . .
H6A H 0.9375 0.4491 -0.1034 0.035 Uiso 1 1 calc R U . . .
C7 C 0.8409(3) 0.4226(3) -0.04987(9) 0.0241(6) Uani 1 1 d . . . . .
H7A H 0.7968 0.4576 -0.0605 0.029 Uiso 1 1 calc R U . . .
C8 C 0.8355(3) 0.4283(3) 0.17671(12) 0.0366(8) Uani 1 1 d . . . . .
H8A H 0.8784 0.5107 0.1655 0.044 Uiso 1 1 calc R U . . .
H8B H 0.8191 0.4340 0.2066 0.044 Uiso 1 1 calc R U . . .
C9 C 0.9180(4) 0.3791(4) 0.17436(15) 0.0515(11) Uani 1 1 d . . . . .
H9A H 0.9840 0.4218 0.1941 0.077 Uiso 1 1 calc R U . . .
H9B H 0.9499 0.3891 0.1459 0.077 Uiso 1 1 calc R U . . .
H9C H 0.8743 0.2940 0.1815 0.077 Uiso 1 1 calc R U . . .
Cl1 Cl 0.0000 0.0000 0.0000 0.0328(4) Uani 1 6 d DS T P . .
Cl2 Cl 0.3333 0.6667 0.1667 0.0711(9) Uani 1 6 d DS T P . .
O1S O 0.0798(6) 0.1181(5) 0.0134(3) 0.0579(19) Uani 0.5 1 d D . P A 1
O2S O 0.0000 0.0000 0.0460(3) 0.085(5) Uani 0.5 3 d DS T P A 1
O3S O 0.3333 0.6667 0.1234(3) 0.098(6) Uani 0.5 3 d DS T P B 1
O4S O 0.2989(8) 0.7466(8) 0.1457(3) 0.076(2) Uani 0.5 1 d D . P B 1


_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 N1 2.025(2) . ?
Ni1 N1 2.025(2) 3_665 ?
Ni1 N1 2.025(2) 2_655 ?
Ni1 N2 2.106(2) 3_665 ?
Ni1 N2 2.106(2) 2_655 ?
Ni1 N2 2.106(2) . ?
Sb1 O1 2.146(2) . ?
Sb1 O1 2.146(2) 3_665 ?
Sb1 O1 2.146(2) 2_655 ?
Sb1 C8 2.152(3) 3_665 ?
Sb1 C8 2.152(3) . ?
Sb1 C8 2.152(3) 2_655 ?
O1 N1 1.353(3) . ?
N1 C2 1.288(4) . ?
N2 C7 1.336(4) . ?
N2 C3 1.360(4) . ?
C1 C2 1.493(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.475(4) . ?
C3 C4 1.389(4) . ?
C4 C5 1.383(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.380(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.385(4) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.492(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
Cl1 O1S 1.416(5) . ?
Cl1 O1S 1.417(5) 10 ?
Cl1 O1S 1.417(5) 11 ?
Cl1 O1S 1.417(5) 2 ?
Cl1 O1S 1.417(5) 12 ?
Cl1 O1S 1.417(5) 3 ?
Cl1 O2S 1.468(9) 10 ?
Cl1 O2S 1.469(9) . ?
Cl2 O3S 1.384(9) . ?
Cl2 O3S 1.384(9) 13_565 ?
Cl2 O4S 1.475(7) 3_565 ?
Cl2 O4S 1.475(7) 2_665 ?
Cl2 O4S 1.475(7) 15 ?
Cl2 O4S 1.475(7) 14_455 ?
Cl2 O4S 1.475(7) . ?
Cl2 O4S 1.475(7) 13_565 ?
O1S O1S 1.600(9) 11 ?
O1S O1S 1.600(9) 12 ?
O1S O2S 1.704(9) . ?
O2S O1S 1.704(9) 2 ?
O2S O1S 1.704(9) 3 ?
O3S O4S 1.494(11) . ?
O3S O4S 1.494(11) 3_565 ?
O3S O4S 1.494(11) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 89.10(9) . 3_665 ?
N1 Ni1 N1 89.10(9) . 2_655 ?
N1 Ni1 N1 89.10(9) 3_665 2_655 ?
N1 Ni1 N2 105.14(9) . 3_665 ?
N1 Ni1 N2 77.53(10) 3_665 3_665 ?
N1 Ni1 N2 160.11(10) 2_655 3_665 ?
N1 Ni1 N2 160.11(10) . 2_655 ?
N1 Ni1 N2 105.15(9) 3_665 2_655 ?
N1 Ni1 N2 77.53(10) 2_655 2_655 ?
N2 Ni1 N2 91.66(9) 3_665 2_655 ?
N1 Ni1 N2 77.53(10) . . ?
N1 Ni1 N2 160.11(10) 3_665 . ?
N1 Ni1 N2 105.15(9) 2_655 . ?
N2 Ni1 N2 91.66(9) 3_665 . ?
N2 Ni1 N2 91.66(9) 2_655 . ?
O1 Sb1 O1 85.46(8) . 3_665 ?
O1 Sb1 O1 85.46(8) . 2_655 ?
O1 Sb1 O1 85.46(8) 3_665 2_655 ?
O1 Sb1 C8 82.37(12) . 3_665 ?
O1 Sb1 C8 92.17(11) 3_665 3_665 ?
O1 Sb1 C8 167.75(13) 2_655 3_665 ?
O1 Sb1 C8 92.17(11) . . ?
O1 Sb1 C8 167.74(13) 3_665 . ?
O1 Sb1 C8 82.37(12) 2_655 . ?
C8 Sb1 C8 99.44(14) 3_665 . ?
O1 Sb1 C8 167.74(13) . 2_655 ?
O1 Sb1 C8 82.37(12) 3_665 2_655 ?
O1 Sb1 C8 92.17(11) 2_655 2_655 ?
C8 Sb1 C8 99.44(14) 3_665 2_655 ?
C8 Sb1 C8 99.44(14) . 2_655 ?
N1 O1 Sb1 121.77(15) . . ?
C2 N1 O1 118.2(2) . . ?
C2 N1 Ni1 119.03(19) . . ?
O1 N1 Ni1 122.64(17) . . ?
C7 N2 C3 118.1(3) . . ?
C7 N2 Ni1 128.2(2) . . ?
C3 N2 Ni1 111.55(18) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 113.7(2) . . ?
N1 C2 C1 125.3(3) . . ?
C3 C2 C1 121.1(3) . . ?
N2 C3 C4 121.7(3) . . ?
N2 C3 C2 115.7(2) . . ?
C4 C3 C2 122.6(3) . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C7 118.2(3) . . ?
C5 C6 H6A 120.9 . . ?
C7 C6 H6A 120.9 . . ?
N2 C7 C6 123.4(3) . . ?
N2 C7 H7A 118.3 . . ?
C6 C7 H7A 118.3 . . ?
C9 C8 Sb1 118.1(3) . . ?
C9 C8 H8A 107.8 . . ?
Sb1 C8 H8A 107.8 . . ?
C9 C8 H8B 107.8 . . ?
Sb1 C8 H8B 107.8 . . ?
H8A C8 H8B 107.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1S Cl1 O1S 180.0 . 10 ?
O1S Cl1 O1S 68.8(3) . 11 ?
O1S Cl1 O1S 111.2(3) 10 11 ?
O1S Cl1 O1S 111.2(3) . 2 ?
O1S Cl1 O1S 68.8(3) 10 2 ?
O1S Cl1 O1S 180.0(8) 11 2 ?
O1S Cl1 O1S 68.8(3) . 12 ?
O1S Cl1 O1S 111.2(3) 10 12 ?
O1S Cl1 O1S 111.2(3) 11 12 ?
O1S Cl1 O1S 68.8(3) 2 12 ?
O1S Cl1 O1S 111.2(3) . 3 ?
O1S Cl1 O1S 68.8(3) 10 3 ?
O1S Cl1 O1S 68.8(3) 11 3 ?
O1S Cl1 O1S 111.2(3) 2 3 ?
O1S Cl1 O1S 180.0(7) 12 3 ?
O1S Cl1 O2S 107.6(3) . 10 ?
O1S Cl1 O2S 72.4(3) 10 10 ?
O1S Cl1 O2S 72.4(3) 11 10 ?
O1S Cl1 O2S 107.6(3) 2 10 ?
O1S Cl1 O2S 72.4(3) 12 10 ?
O1S Cl1 O2S 107.6(3) 3 10 ?
O1S Cl1 O2S 72.4(3) . . ?
O1S Cl1 O2S 107.6(3) 10 . ?
O1S Cl1 O2S 107.6(3) 11 . ?
O1S Cl1 O2S 72.4(3) 2 . ?
O1S Cl1 O2S 107.6(3) 12 . ?
O1S Cl1 O2S 72.4(3) 3 . ?
O2S Cl1 O2S 180.0 10 . ?
O3S Cl2 O3S 180.0 . 13_565 ?
O3S Cl2 O4S 62.9(4) . 3_565 ?
O3S Cl2 O4S 117.1(4) 13_565 3_565 ?
O3S Cl2 O4S 62.9(4) . 2_665 ?
O3S Cl2 O4S 117.1(4) 13_565 2_665 ?
O4S Cl2 O4S 100.9(4) 3_565 2_665 ?
O3S Cl2 O4S 117.1(4) . 15 ?
O3S Cl2 O4S 62.9(4) 13_565 15 ?
O4S Cl2 O4S 180.0 3_565 15 ?
O4S Cl2 O4S 79.1(4) 2_665 15 ?
O3S Cl2 O4S 117.1(4) . 14_455 ?
O3S Cl2 O4S 62.9(4) 13_565 14_455 ?
O4S Cl2 O4S 79.1(4) 3_565 14_455 ?
O4S Cl2 O4S 180.0 2_665 14_455 ?
O4S Cl2 O4S 100.9(4) 15 14_455 ?
O3S Cl2 O4S 62.9(4) . . ?
O3S Cl2 O4S 117.1(4) 13_565 . ?
O4S Cl2 O4S 100.9(4) 3_565 . ?
O4S Cl2 O4S 100.9(4) 2_665 . ?
O4S Cl2 O4S 79.1(4) 15 . ?
O4S Cl2 O4S 79.1(4) 14_455 . ?
O3S Cl2 O4S 117.1(4) . 13_565 ?
O3S Cl2 O4S 62.9(4) 13_565 13_565 ?
O4S Cl2 O4S 79.1(4) 3_565 13_565 ?
O4S Cl2 O4S 79.1(4) 2_665 13_565 ?
O4S Cl2 O4S 100.9(4) 15 13_565 ?
O4S Cl2 O4S 100.9(4) 14_455 13_565 ?
O4S Cl2 O4S 180.0(6) . 13_565 ?
Cl1 O1S O1S 55.62(16) . 11 ?
Cl1 O1S O1S 55.62(16) . 12 ?
O1S O1S O1S 93.9(7) 11 12 ?
Cl1 O1S O2S 55.2(3) . . ?
O1S O1S O2S 89.6(3) 11 . ?
O1S O1S O2S 89.6(3) 12 . ?
Cl1 O2S O1S 52.4(3) . 2 ?
Cl1 O2S O1S 52.4(3) . 3 ?
O1S O2S O1S 86.7(4) 2 3 ?
Cl1 O2S O1S 52.4(3) . . ?
O1S O2S O1S 86.7(4) 2 . ?
O1S O2S O1S 86.7(4) 3 . ?
Cl2 O3S O4S 61.5(3) . . ?
Cl2 O3S O4S 61.5(3) . 3_565 ?
O4S O3S O4S 99.1(4) . 3_565 ?
Cl2 O3S O4S 61.5(3) . 2_665 ?
O4S O3S O4S 99.1(4) . 2_665 ?
O4S O3S O4S 99.1(4) 3_565 2_665 ?
Cl2 O4S O3S 55.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sb1 O1 N1 C2 142.2(2) . . . . ?
Sb1 O1 N1 Ni1 -42.2(3) . . . . ?
O1 N1 C2 C3 -179.1(2) . . . . ?
Ni1 N1 C2 C3 5.0(3) . . . . ?
O1 N1 C2 C1 0.6(4) . . . . ?
Ni1 N1 C2 C1 -175.3(2) . . . . ?
C7 N2 C3 C4 0.1(4) . . . . ?
Ni1 N2 C3 C4 164.7(2) . . . . ?
C7 N2 C3 C2 179.3(3) . . . . ?
Ni1 N2 C3 C2 -16.1(3) . . . . ?
N1 C2 C3 N2 8.0(4) . . . . ?
C1 C2 C3 N2 -171.7(3) . . . . ?
N1 C2 C3 C4 -172.8(3) . . . . ?
C1 C2 C3 C4 7.5(4) . . . . ?
N2 C3 C4 C5 -0.9(5) . . . . ?
C2 C3 C4 C5 180.0(3) . . . . ?
C3 C4 C5 C6 0.8(5) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C3 N2 C7 C6 0.7(4) . . . . ?
Ni1 N2 C7 C6 -160.9(2) . . . . ?
C5 C6 C7 N2 -0.8(5) . . . . ?
O1S Cl1 O1S O1S 180.0 2 . . 11 ?
O1S Cl1 O1S O1S -124.6(9) 12 . . 11 ?
O1S Cl1 O1S O1S 55.4(9) 3 . . 11 ?
O2S Cl1 O1S O1S -62.3(4) 10 . . 11 ?
O2S Cl1 O1S O1S 117.7(4) . . . 11 ?
O1S Cl1 O1S O1S 124.6(9) 11 . . 12 ?
O1S Cl1 O1S O1S -55.4(9) 2 . . 12 ?
O1S Cl1 O1S O1S 180.0 3 . . 12 ?
O2S Cl1 O1S O1S 62.3(4) 10 . . 12 ?
O2S Cl1 O1S O1S -117.7(4) . . . 12 ?
O1S Cl1 O1S O2S -117.7(4) 11 . . . ?
O1S Cl1 O1S O2S 62.3(4) 2 . . . ?
O1S Cl1 O1S O2S 117.7(4) 12 . . . ?
O1S Cl1 O1S O2S -62.3(4) 3 . . . ?
O2S Cl1 O1S O2S 180.000(0) 10 . . . ?
O1S Cl1 O2S O1S 120.001(0) . . . 2 ?
O1S Cl1 O2S O1S -60.000(0) 10 . . 2 ?
O1S Cl1 O2S O1S 180.0 11 . . 2 ?
O1S Cl1 O2S O1S 60.000(1) 12 . . 2 ?
O1S Cl1 O2S O1S -120.000(1) 3 . . 2 ?
O1S Cl1 O2S O1S -119.999(1) . . . 3 ?
O1S Cl1 O2S O1S 60.000(0) 10 . . 3 ?
O1S Cl1 O2S O1S -60.000(0) 11 . . 3 ?
O1S Cl1 O2S O1S 120.000(1) 2 . . 3 ?
O1S Cl1 O2S O1S 180.0 12 . . 3 ?
O1S Cl1 O2S O1S 179.999(0) 10 . . . ?
O1S Cl1 O2S O1S 59.999(0) 11 . . . ?
O1S Cl1 O2S O1S -120.001(0) 2 . . . ?
O1S Cl1 O2S O1S -60.001(1) 12 . . . ?
O1S Cl1 O2S O1S 119.999(1) 3 . . . ?
O1S O1S O2S Cl1 -47.0(4) 11 . . . ?
O1S O1S O2S Cl1 47.0(4) 12 . . . ?
Cl1 O1S O2S O1S -43.42(18) . . . 2 ?
O1S O1S O2S O1S -90.4(3) 11 . . 2 ?
O1S O1S O2S O1S 3.5(5) 12 . . 2 ?
Cl1 O1S O2S O1S 43.42(18) . . . 3 ?
O1S O1S O2S O1S -3.5(5) 11 . . 3 ?
O1S O1S O2S O1S 90.4(3) 12 . . 3 ?
O4S Cl2 O3S O4S -119.999(4) 3_565 . . . ?
O4S Cl2 O3S O4S 119.997(4) 2_665 . . . ?
O4S Cl2 O3S O4S 59.999(4) 15 . . . ?
O4S Cl2 O3S O4S -60.001(4) 14_455 . . . ?
O4S Cl2 O3S O4S 179.999(4) 13_565 . . . ?
O4S Cl2 O3S O4S -120.004(1) 2_665 . . 3_565 ?
O4S Cl2 O3S O4S 179.998(1) 15 . . 3_565 ?
O4S Cl2 O3S O4S 59.998(2) 14_455 . . 3_565 ?
O4S Cl2 O3S O4S 119.999(1) . . . 3_565 ?
O4S Cl2 O3S O4S -60.002(1) 13_565 . . 3_565 ?
O4S Cl2 O3S O4S 120.004(1) 3_565 . . 2_665 ?
O4S Cl2 O3S O4S -59.998(1) 15 . . 2_665 ?
O4S Cl2 O3S O4S 180.002(1) 14_455 . . 2_665 ?
O4S Cl2 O3S O4S -119.997(0) . . . 2_665 ?
O4S Cl2 O3S O4S 60.002(1) 13_565 . . 2_665 ?
O3S Cl2 O4S O3S 180.001(4) 13_565 . . . ?
O4S Cl2 O4S O3S 51.8(3) 3_565 . . . ?
O4S Cl2 O4S O3S -51.8(3) 2_665 . . . ?
O4S Cl2 O4S O3S -128.2(3) 15 . . . ?
O4S Cl2 O4S O3S 128.2(3) 14_455 . . . ?
O4S O3S O4S Cl2 -50.4(3) 3_565 . . . ?
O4S O3S O4S Cl2 50.4(3) 2_665 . . . ?

_refine_diff_density_max         1.764
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.114

_shelxl_version_number           2014/6

