# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_compound8
_database_code_depnum_ccdc_archive 'CCDC 1877426'
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-13 downloaded from the CCDC.
;

_audit_creation_date             2019-01-25T16:34:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#


_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C42 H54 N4 Ni O11 Y Zn, 3(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H58 Cl4 F9 N4 Ni O20 S3 Y Zn'
_chemical_formula_weight         1620.94
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.9580(4)
_cell_length_b                   16.2440(4)
_cell_length_c                   24.3930(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.880(2)
_cell_angle_gamma                90
_cell_volume                     6494.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    7828
_cell_measurement_theta_min      2.8736
_cell_measurement_theta_max      29.2516

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#


_exptl_crystal_description       platelet
_exptl_crystal_colour            'pale green'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3288
_exptl_special_details           
;
 ?
;


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.7473
_exptl_absorpt_correction_T_max  0.9875

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.1978
_diffrn_orient_matrix_ub_11      0.0393582
_diffrn_orient_matrix_ub_12      0.0165373
_diffrn_orient_matrix_ub_13      0.0019597
_diffrn_orient_matrix_ub_21      -0.0180438
_diffrn_orient_matrix_ub_22      0.036275
_diffrn_orient_matrix_ub_23      -0.0139254
_diffrn_orient_matrix_ub_31      0.000233
_diffrn_orient_matrix_ub_32      0.017769
_diffrn_orient_matrix_ub_33      0.0265978
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.1617
_diffrn_reflns_number            58205
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.879
_diffrn_reflns_theta_max         29.316
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_reflns_Friedel_coverage         0
_reflns_number_total             15697
_reflns_number_gt                10102
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0498P)²+11.4687P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         15697
_refine_ls_number_parameters     839
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.059
_refine_ls_wR_factor_ref         0.1414
_refine_ls_wR_factor_gt          0.1216
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.105

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Y1 Y 0.38527(2) 0.31778(3) 0.33539(2) 0.01842(10) Uani 1 1 d . . . . .
NI1 Ni 0.57699(3) 0.23777(3) 0.41185(2) 0.01696(12) Uani 1 1 d . . . . .
O3 O 0.45777(17) 0.20861(18) 0.39218(12) 0.0216(6) Uani 1 1 d . . . . .
C4 C 0.4267(3) 0.1345(3) 0.39896(17) 0.0208(9) Uani 1 1 d . . . . .
C5 C 0.4733(3) 0.0642(3) 0.41973(17) 0.0237(10) Uani 1 1 d . . . . .
C6 C 0.5622(3) 0.0633(3) 0.43975(17) 0.0242(10) Uani 1 1 d . . . . .
H6 H 0.585895 0.012031 0.453756 0.029 Uiso 1 1 calc R U . . .
N7 N 0.6121(2) 0.1224(2) 0.44090(14) 0.0241(8) Uani 1 1 d . . . . .
C8 C 0.6984(3) 0.1052(3) 0.47053(19) 0.0312(11) Uani 1 1 d . . . . .
H8A H 0.705711 0.04477 0.474116 0.037 Uiso 1 1 calc R U . . .
H8B H 0.709446 0.128121 0.509365 0.037 Uiso 1 1 calc R U . . .
C9 C 0.7616(3) 0.1395(3) 0.44201(18) 0.0265(10) Uani 1 1 d . . . . .
C10 C 0.7606(3) 0.2338(3) 0.44188(19) 0.0267(10) Uani 1 1 d . . . . .
H10A H 0.761905 0.253676 0.480466 0.032 Uiso 1 1 calc R U . . .
H10B H 0.810353 0.254266 0.432172 0.032 Uiso 1 1 calc R U . . .
N11 N 0.6882(2) 0.2681(2) 0.40128(15) 0.0228(8) Uani 1 1 d . . . . .
C12 C 0.7023(3) 0.3056(3) 0.35868(19) 0.0250(10) Uani 1 1 d . . . . .
H12 H 0.758046 0.310163 0.358407 0.03 Uiso 1 1 calc R U . . .
C13 C 0.6436(3) 0.3421(3) 0.31050(18) 0.0232(9) Uani 1 1 d . . . . .
C14 C 0.5591(2) 0.3447(3) 0.30466(17) 0.0194(9) Uani 1 1 d . . . . .
O15 O 0.52308(17) 0.31304(18) 0.34266(11) 0.0214(6) Uani 1 1 d . . . . .
C16 C 0.5102(3) 0.3805(3) 0.25489(17) 0.0201(9) Uani 1 1 d . . . . .
O17 O 0.42717(18) 0.37912(18) 0.25267(12) 0.0245(7) Uani 1 1 d . . . . .
C18 C 0.3731(3) 0.4180(3) 0.20316(18) 0.0300(11) Uani 1 1 d . . . . .
H18A H 0.385221 0.476977 0.203337 0.045 Uiso 1 1 calc R U . . .
H18B H 0.31629 0.410112 0.204319 0.045 Uiso 1 1 calc R U . . .
H18C H 0.381601 0.392908 0.168573 0.045 Uiso 1 1 calc R U . . .
C19 C 0.5424(3) 0.4109(3) 0.21302(19) 0.0279(10) Uani 1 1 d . . . . .
H19 H 0.507735 0.434278 0.179773 0.033 Uiso 1 1 calc R U . . .
C20 C 0.6263(3) 0.4074(3) 0.2195(2) 0.0326(11) Uani 1 1 d . . . . .
H20 H 0.648916 0.427742 0.190289 0.039 Uiso 1 1 calc R U . . .
C21 C 0.6762(3) 0.3748(3) 0.26764(19) 0.0284(10) Uani 1 1 d . . . . .
H21 H 0.733594 0.374301 0.272243 0.034 Uiso 1 1 calc R U . . .
C22 C 0.8464(3) 0.1139(3) 0.4795(2) 0.0401(13) Uani 1 1 d . . . . .
H22A H 0.853723 0.136475 0.517772 0.06 Uiso 1 1 calc R U . . .
H22B H 0.88915 0.135377 0.462965 0.06 Uiso 1 1 calc R U . . .
H22C H 0.849956 0.053743 0.481568 0.06 Uiso 1 1 calc R U . . .
C23 C 0.7501(3) 0.1047(3) 0.3829(2) 0.0382(12) Uani 1 1 d . . . . .
H23A H 0.753284 0.044451 0.384973 0.057 Uiso 1 1 calc R U . . .
H23B H 0.793042 0.125756 0.366398 0.057 Uiso 1 1 calc R U . . .
H23C H 0.696648 0.121182 0.359202 0.057 Uiso 1 1 calc R U . . .
C24 C 0.4339(3) -0.0101(3) 0.42462(18) 0.0282(10) Uani 1 1 d . . . . .
H24 H 0.465513 -0.057562 0.438455 0.034 Uiso 1 1 calc R U . . .
C25 C 0.3505(3) -0.0157(3) 0.40984(19) 0.0313(11) Uani 1 1 d . . . . .
H25 H 0.324939 -0.06663 0.413781 0.038 Uiso 1 1 calc R U . . .
C26 C 0.3032(3) 0.0529(3) 0.38907(18) 0.0264(10) Uani 1 1 d . . . . .
H26 H 0.245395 0.049254 0.378814 0.032 Uiso 1 1 calc R U . . .
C27 C 0.3415(3) 0.1264(3) 0.38352(17) 0.0232(9) Uani 1 1 d . . . . .
O28 O 0.30064(17) 0.19865(18) 0.36309(13) 0.0254(7) Uani 1 1 d . . . . .
C29 C 0.2145(3) 0.1998(4) 0.3596(2) 0.0398(13) Uani 1 1 d . . . . .
H29A H 0.185344 0.166864 0.327056 0.06 Uiso 1 1 calc R U . . .
H29B H 0.194583 0.256673 0.354951 0.06 Uiso 1 1 calc R U . . .
H29C H 0.205054 0.176713 0.394495 0.06 Uiso 1 1 calc R U . . .
O31 O 0.5740(2) 0.2932(2) 0.48511(15) 0.0341(9) Uani 1 1 d . . . . .
H31A H 0.542(3) 0.280(3) 0.500(2) 0.041 Uiso 1 1 d . U . . .
H31B H 0.603(4) 0.320(4) 0.503(2) 0.041 Uiso 1 1 d . U . . .
ZN1 Zn 0.19200(3) 0.39758(3) 0.26649(2) 0.02750(14) Uani 1 1 d . . . . .
O33 O 0.26695(17) 0.29929(17) 0.26501(12) 0.0223(6) Uani 1 1 d . . . . .
C34 C 0.2486(3) 0.2295(3) 0.23523(18) 0.0239(10) Uani 1 1 d . . . . .
C35 C 0.3119(3) 0.1722(3) 0.23799(18) 0.0246(10) Uani 1 1 d . . . . .
O36 O 0.38720(17) 0.19809(18) 0.27110(12) 0.0238(7) Uani 1 1 d . . . . .
C37 C 0.2980(3) 0.0984(3) 0.2096(2) 0.0351(12) Uani 1 1 d . . . . .
H37 H 0.341458 0.060566 0.212106 0.042 Uiso 1 1 calc R U . . .
C38 C 0.2202(4) 0.0794(3) 0.1773(2) 0.0472(14) Uani 1 1 d . . . . .
H38 H 0.209964 0.028228 0.157915 0.057 Uiso 1 1 calc R U . . .
C39 C 0.1578(3) 0.1351(3) 0.1734(2) 0.0415(13) Uani 1 1 d . . . . .
H39 H 0.104675 0.121763 0.151072 0.05 Uiso 1 1 calc R U . . .
C40 C 0.1707(3) 0.2110(3) 0.20148(19) 0.0286(10) Uani 1 1 d . . . . .
C41 C 0.1016(3) 0.2663(3) 0.1925(2) 0.0331(11) Uani 1 1 d . . . . .
H41 H 0.051906 0.245978 0.168918 0.04 Uiso 1 1 calc R U . . .
N42 N 0.0988(2) 0.3391(2) 0.21231(15) 0.0271(9) Uani 1 1 d . . . . .
C43 C 0.0191(3) 0.3820(3) 0.1965(2) 0.0321(11) Uani 1 1 d . . . . .
H43A H -0.002203 0.386535 0.230548 0.038 Uiso 1 1 calc R U . . .
H43B H -0.019901 0.34808 0.168263 0.038 Uiso 1 1 calc R U . . .
C44 C 0.0226(3) 0.4677(3) 0.1719(2) 0.0329(11) Uani 1 1 d . . . . .
C45 C 0.0613(3) 0.4663(4) 0.1220(2) 0.0453(14) Uani 1 1 d . . . . .
H45A H 0.118566 0.449541 0.135273 0.068 Uiso 1 1 calc R U . . .
H45B H 0.058234 0.52136 0.105173 0.068 Uiso 1 1 calc R U . . .
H45C H 0.031972 0.427062 0.093449 0.068 Uiso 1 1 calc R U . . .
C46 C 0.0663(3) 0.5292(3) 0.2168(2) 0.0367(12) Uani 1 1 d . . . . .
H46A H 0.060492 0.584818 0.199522 0.044 Uiso 1 1 calc R U . . .
H46B H 0.038503 0.52987 0.247804 0.044 Uiso 1 1 calc R U . . .
N47 N 0.1542(2) 0.5131(2) 0.24162(15) 0.0265(8) Uani 1 1 d . . . . .
C48 C 0.2005(3) 0.5769(3) 0.25085(18) 0.0262(10) Uani 1 1 d . . . . .
H48 H 0.176456 0.627168 0.234935 0.031 Uiso 1 1 calc R U . . .
C49 C 0.2856(3) 0.5811(3) 0.28284(18) 0.0232(9) Uani 1 1 d . . . . .
C50 C 0.3301(3) 0.5134(3) 0.31136(17) 0.0210(9) Uani 1 1 d . . . . .
O51 O 0.30347(17) 0.43687(17) 0.30820(12) 0.0205(6) Uani 1 1 d . . . . .
C52 C 0.4093(3) 0.5297(3) 0.34528(18) 0.0236(9) Uani 1 1 d . . . . .
O53 O 0.44877(17) 0.45906(18) 0.37084(12) 0.0250(7) Uani 1 1 d . . . . .
C54 C 0.5213(3) 0.4728(3) 0.4157(2) 0.0403(13) Uani 1 1 d . . . . .
H54A H 0.564841 0.493357 0.399605 0.06 Uiso 1 1 calc R U . . .
H54B H 0.538517 0.420969 0.435742 0.06 Uiso 1 1 calc R U . . .
H54C H 0.509865 0.513498 0.442326 0.06 Uiso 1 1 calc R U . . .
C55 C 0.4429(3) 0.6068(3) 0.3516(2) 0.0312(11) Uani 1 1 d . . . . .
H55 H 0.49624 0.615377 0.375205 0.037 Uiso 1 1 calc R U . . .
C56 C 0.3973(3) 0.6732(3) 0.3226(2) 0.0371(12) Uani 1 1 d . . . . .
H56 H 0.419766 0.727136 0.326391 0.044 Uiso 1 1 calc R U . . .
C57 C 0.3215(3) 0.6599(3) 0.2893(2) 0.0314(11) Uani 1 1 d . . . . .
H57 H 0.291408 0.70505 0.269586 0.038 Uiso 1 1 calc R U . . .
C59 C -0.0667(3) 0.4979(4) 0.1522(2) 0.0494(15) Uani 1 1 d . . . . .
H59A H -0.097585 0.461454 0.122249 0.074 Uiso 1 1 calc R U . . .
H59B H -0.067748 0.554097 0.137384 0.074 Uiso 1 1 calc R U . . .
H59C H -0.091445 0.497267 0.184324 0.074 Uiso 1 1 calc R U . . .
O60 O 0.1499(2) 0.3919(2) 0.33585(16) 0.0397(9) Uani 1 1 d D . . . .
H60A H 0.160(3) 0.436(2) 0.356(2) 0.048 Uiso 1 1 d D U . . .
H60B H 0.1035(16) 0.393(4) 0.343(2) 0.048 Uiso 1 1 d D U . . .
O61 O 0.3589(2) 0.3460(2) 0.42034(13) 0.0303(7) Uani 1 1 d D . . . .
H61A H 0.354(3) 0.3922(15) 0.4354(19) 0.036 Uiso 1 1 d D U . . .
H61B H 0.356(3) 0.311(2) 0.4453(16) 0.036 Uiso 1 1 d D U . . .
S62 S 0.27062(7) 0.54281(8) 0.45393(5) 0.0303(3) Uani 1 1 d . . . . .
O63 O 0.3425(2) 0.4921(2) 0.46779(15) 0.0414(9) Uani 1 1 d . . . . .
O64 O 0.2868(2) 0.6295(2) 0.46208(14) 0.0372(8) Uani 1 1 d . . . . .
O65 O 0.2117(2) 0.5227(2) 0.40134(14) 0.0413(9) Uani 1 1 d . . . . .
C66 C 0.2184(3) 0.5164(4) 0.5078(2) 0.0459(14) Uani 1 1 d . . . . .
F67 F 0.1983(2) 0.4374(2) 0.50491(17) 0.0768(12) Uani 1 1 d . . . . .
F68 F 0.1508(2) 0.5601(3) 0.50188(16) 0.0774(12) Uani 1 1 d . . . . .
F69 F 0.2663(2) 0.5307(3) 0.55972(14) 0.0703(11) Uani 1 1 d . . . . .
S70 S -0.05141(8) 0.28436(8) 0.33605(6) 0.0362(3) Uani 1 1 d . . . . .
O71 O 0.0278(3) 0.2806(3) 0.3273(2) 0.0635(12) Uani 1 1 d . . . . .
O72 O -0.0640(3) 0.2300(3) 0.3794(2) 0.0742(14) Uani 1 1 d . . . . .
O73 O -0.1176(3) 0.2866(3) 0.2871(2) 0.0807(15) Uani 1 1 d . . . . .
C74 C -0.0519(4) 0.3857(4) 0.3669(3) 0.0546(16) Uani 1 1 d . . . . .
F75 F -0.1202(2) 0.4015(2) 0.38269(19) 0.0792(12) Uani 1 1 d . . . . .
F76 F -0.0448(3) 0.4444(2) 0.3309(2) 0.0953(15) Uani 1 1 d . . . . .
F77 F 0.0107(3) 0.3955(3) 0.4124(2) 0.0932(15) Uani 1 1 d . . . . .
S78 S 0.38677(8) 0.20846(8) 0.54300(5) 0.0302(3) Uani 1 1 d . . . . .
O79 O 0.3266(2) 0.2285(2) 0.49083(13) 0.0375(8) Uani 1 1 d . . . . .
O80 O 0.3835(3) 0.1263(2) 0.56274(16) 0.0508(10) Uani 1 1 d . . . . .
O81 O 0.4671(2) 0.2398(3) 0.54651(16) 0.0548(11) Uani 1 1 d . . . . .
C82 C 0.3532(3) 0.2692(3) 0.5950(2) 0.0323(11) Uani 1 1 d . . . . .
F83 F 0.3514(2) 0.34894(19) 0.58309(14) 0.0572(9) Uani 1 1 d . . . . .
F84 F 0.40422(18) 0.26028(19) 0.64696(11) 0.0442(8) Uani 1 1 d . . . . .
F85 F 0.27974(18) 0.2466(2) 0.59906(13) 0.0532(9) Uani 1 1 d . . . . .
CL88 Cl 0.78193(13) 0.30810(13) 0.13395(9) 0.0851(6) Uani 1 1 d . . . . .
CL89 Cl 0.12985(19) 0.11797(14) 0.49292(11) 0.1131(9) Uani 1 1 d . . . . .
CL90 Cl 0.06122(17) 0.25791(17) 0.53599(10) 0.1129(9) Uani 1 1 d . . . . .
C91 C 0.8401(4) 0.2180(4) 0.1465(2) 0.0498(15) Uani 1 1 d . . . . .
H91A H 0.803444 0.169785 0.14309 0.06 Uiso 1 1 calc R U . . .
H91B H 0.875886 0.219012 0.185599 0.06 Uiso 1 1 calc R U . . .
C92 C 0.1123(5) 0.2244(4) 0.4872(3) 0.0676(19) Uani 1 1 d . . . . .
H92A H 0.165077 0.253673 0.49366 0.081 Uiso 1 1 calc R U . . .
H92B H 0.079544 0.237675 0.448438 0.081 Uiso 1 1 calc R U . . .
CL1 Cl 0.90025(10) 0.20894(13) 0.09744(7) 0.0684(5) Uani 1 1 d . . . . .
C100 C 0.4562(3) 0.1472(3) 0.2699(2) 0.0309(11) Uani 1 1 d . . . . .
H10C H 0.452191 0.094893 0.289029 0.046 Uiso 1 1 calc R U . . .
H10D H 0.506593 0.175517 0.289494 0.046 Uiso 1 1 calc R U . . .
H10E H 0.456728 0.136617 0.230485 0.046 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Y1 O61 2.276(3) . ?
Y1 O15 2.299(3) . ?
Y1 O33 2.301(3) . ?
Y1 O51 2.374(3) . ?
Y1 O3 2.388(3) . ?
Y1 O36 2.503(3) . ?
Y1 O17 2.511(3) . ?
Y1 O53 2.588(3) . ?
Y1 O28 2.600(3) . ?
Y1 ZN1 3.5238(7) . ?
NI1 O3 2.011(3) . ?
NI1 O31 2.013(4) . ?
NI1 N11 2.028(4) . ?
NI1 N7 2.037(4) . ?
NI1 O15 2.094(3) . ?
O3 C4 1.341(5) . ?
C4 C27 1.403(6) . ?
C4 C5 1.407(6) . ?
C5 C24 1.401(6) . ?
C5 C6 1.459(6) . ?
C6 N7 1.276(6) . ?
C6 H6 0.95 . ?
N7 C8 1.483(6) . ?
C8 C9 1.526(6) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 C23 1.514(6) . ?
C9 C10 1.532(7) . ?
C9 C22 1.550(6) . ?
C10 N11 1.475(5) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
N11 C12 1.279(5) . ?
C12 C13 1.457(6) . ?
C12 H12 0.95 . ?
C13 C14 1.403(6) . ?
C13 C21 1.407(6) . ?
C14 O15 1.338(5) . ?
C14 C16 1.408(6) . ?
C16 C19 1.369(6) . ?
C16 O17 1.395(5) . ?
O17 C18 1.459(5) . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 C20 1.392(7) . ?
C19 H19 0.95 . ?
C20 C21 1.366(6) . ?
C20 H20 0.95 . ?
C21 H21 0.95 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 C25 1.369(7) . ?
C24 H24 0.95 . ?
C25 C26 1.390(7) . ?
C25 H25 0.95 . ?
C26 C27 1.382(6) . ?
C26 H26 0.95 . ?
C27 O28 1.388(5) . ?
O28 C29 1.441(5) . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
O31 H31A 0.76(6) . ?
O31 H31B 0.72(6) . ?
ZN1 O60 2.000(4) . ?
ZN1 O51 2.007(3) . ?
ZN1 N42 2.019(4) . ?
ZN1 N47 2.025(4) . ?
ZN1 O33 2.047(3) . ?
O33 C34 1.339(5) . ?
C34 C40 1.398(6) . ?
C34 C35 1.410(6) . ?
C35 C37 1.373(6) . ?
C35 O36 1.389(5) . ?
O36 C100 1.438(5) . ?
C37 C38 1.387(7) . ?
C37 H37 0.95 . ?
C38 C39 1.377(7) . ?
C38 H38 0.95 . ?
C39 C40 1.400(7) . ?
C39 H39 0.95 . ?
C40 C41 1.448(7) . ?
C41 N42 1.283(6) . ?
C41 H41 0.95 . ?
N42 C43 1.481(6) . ?
C43 C44 1.523(7) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 C45 1.524(7) . ?
C44 C46 1.526(7) . ?
C44 C59 1.547(6) . ?
C45 H45A 0.98 . ?
C45 H45B 0.98 . ?
C45 H45C 0.98 . ?
C46 N47 1.480(6) . ?
C46 H46A 0.99 . ?
C46 H46B 0.99 . ?
N47 C48 1.285(6) . ?
C48 C49 1.455(6) . ?
C48 H48 0.95 . ?
C49 C57 1.408(6) . ?
C49 C50 1.412(6) . ?
C50 O51 1.318(5) . ?
C50 C52 1.410(6) . ?
C52 C55 1.368(6) . ?
C52 O53 1.392(5) . ?
O53 C54 1.438(5) . ?
C54 H54A 0.98 . ?
C54 H54B 0.98 . ?
C54 H54C 0.98 . ?
C55 C56 1.408(7) . ?
C55 H55 0.95 . ?
C56 C57 1.350(7) . ?
C56 H56 0.95 . ?
C57 H57 0.95 . ?
C59 H59A 0.98 . ?
C59 H59B 0.98 . ?
C59 H59C 0.98 . ?
O60 H60A 0.848(10) . ?
O60 H60B 0.847(10) . ?
O61 H61A 0.848(10) . ?
O61 H61B 0.843(10) . ?
S62 O63 1.438(4) . ?
S62 O64 1.439(4) . ?
S62 O65 1.447(3) . ?
S62 C66 1.814(6) . ?
C66 F68 1.324(6) . ?
C66 F67 1.325(7) . ?
C66 F69 1.338(6) . ?
S70 O73 1.413(4) . ?
S70 O71 1.415(4) . ?
S70 O72 1.436(4) . ?
S70 C74 1.810(7) . ?
C74 F76 1.324(7) . ?
C74 F77 1.334(7) . ?
C74 F75 1.335(6) . ?
S78 O80 1.425(4) . ?
S78 O81 1.436(4) . ?
S78 O79 1.449(3) . ?
S78 C82 1.811(5) . ?
C82 F83 1.326(6) . ?
C82 F85 1.327(5) . ?
C82 F84 1.345(5) . ?
CL88 C91 1.747(6) . ?
CL89 C92 1.754(7) . ?
CL90 C92 1.729(7) . ?
C91 CL1 1.768(6) . ?
C91 H91A 0.99 . ?
C91 H91B 0.99 . ?
C92 H92A 0.99 . ?
C92 H92B 0.99 . ?
C100 H10C 0.98 . ?
C100 H10D 0.98 . ?
C100 H10E 0.98 . ?

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
O61 Y1 O15 111.71(11) . . ?
O61 Y1 O33 111.60(12) . . ?
O15 Y1 O33 136.68(10) . . ?
O61 Y1 O51 81.54(11) . . ?
O15 Y1 O51 123.94(10) . . ?
O33 Y1 O51 64.08(10) . . ?
O61 Y1 O3 79.26(11) . . ?
O15 Y1 O3 64.44(10) . . ?
O33 Y1 O3 123.80(10) . . ?
O51 Y1 O3 160.80(10) . . ?
O61 Y1 O36 139.83(11) . . ?
O15 Y1 O36 81.13(10) . . ?
O33 Y1 O36 65.19(10) . . ?
O51 Y1 O36 123.96(10) . . ?
O3 Y1 O36 72.48(10) . . ?
O61 Y1 O17 144.48(11) . . ?
O15 Y1 O17 65.39(9) . . ?
O33 Y1 O17 79.91(10) . . ?
O51 Y1 O17 73.60(10) . . ?
O3 Y1 O17 123.44(10) . . ?
O36 Y1 O17 75.69(10) . . ?
O61 Y1 O53 71.29(11) . . ?
O15 Y1 O53 71.12(10) . . ?
O33 Y1 O53 124.99(10) . . ?
O51 Y1 O53 62.21(9) . . ?
O3 Y1 O53 110.90(9) . . ?
O36 Y1 O53 145.78(10) . . ?
O17 Y1 O53 74.77(10) . . ?
O61 Y1 O28 70.29(11) . . ?
O15 Y1 O28 124.96(10) . . ?
O33 Y1 O28 70.30(10) . . ?
O51 Y1 O28 110.93(9) . . ?
O3 Y1 O28 62.14(9) . . ?
O36 Y1 O28 71.43(10) . . ?
O17 Y1 O28 142.48(10) . . ?
O53 Y1 O28 141.57(10) . . ?
O61 Y1 ZN1 89.08(9) . . ?
O15 Y1 ZN1 148.39(7) . . ?
O33 Y1 ZN1 33.50(7) . . ?
O51 Y1 ZN1 33.04(7) . . ?
O3 Y1 ZN1 145.81(7) . . ?
O36 Y1 ZN1 98.46(7) . . ?
O17 Y1 ZN1 83.76(7) . . ?
O53 Y1 ZN1 95.13(6) . . ?
O28 Y1 ZN1 83.68(7) . . ?
O3 NI1 O31 93.70(14) . . ?
O3 NI1 N11 159.61(13) . . ?
O31 NI1 N11 103.89(15) . . ?
O3 NI1 N7 93.01(13) . . ?
O31 NI1 N7 100.03(15) . . ?
N11 NI1 N7 93.98(15) . . ?
O3 NI1 O15 75.00(11) . . ?
O31 NI1 O15 110.44(14) . . ?
N11 NI1 O15 89.05(13) . . ?
N7 NI1 O15 147.70(13) . . ?
C4 O3 NI1 125.8(3) . . ?
C4 O3 Y1 125.3(2) . . ?
NI1 O3 Y1 107.44(12) . . ?
O3 C4 C27 117.5(4) . . ?
O3 C4 C5 124.7(4) . . ?
C27 C4 C5 117.8(4) . . ?
C24 C5 C4 119.6(4) . . ?
C24 C5 C6 116.0(4) . . ?
C4 C5 C6 124.4(4) . . ?
N7 C6 C5 128.5(4) . . ?
N7 C6 H6 115.8 . . ?
C5 C6 H6 115.8 . . ?
C6 N7 C8 115.8(4) . . ?
C6 N7 NI1 123.5(3) . . ?
C8 N7 NI1 120.5(3) . . ?
N7 C8 C9 115.4(4) . . ?
N7 C8 H8A 108.4 . . ?
C9 C8 H8A 108.4 . . ?
N7 C8 H8B 108.4 . . ?
C9 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C23 C9 C8 111.3(4) . . ?
C23 C9 C10 111.9(4) . . ?
C8 C9 C10 111.0(4) . . ?
C23 C9 C22 109.6(4) . . ?
C8 C9 C22 106.6(4) . . ?
C10 C9 C22 106.1(4) . . ?
N11 C10 C9 112.7(4) . . ?
N11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
N11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C12 N11 C10 115.3(4) . . ?
C12 N11 NI1 126.4(3) . . ?
C10 N11 NI1 117.6(3) . . ?
N11 C12 C13 128.1(4) . . ?
N11 C12 H12 115.9 . . ?
C13 C12 H12 115.9 . . ?
C14 C13 C21 119.9(4) . . ?
C14 C13 C12 124.2(4) . . ?
C21 C13 C12 115.8(4) . . ?
O15 C14 C13 123.7(4) . . ?
O15 C14 C16 118.9(4) . . ?
C13 C14 C16 117.4(4) . . ?
C14 O15 NI1 126.9(3) . . ?
C14 O15 Y1 124.8(2) . . ?
NI1 O15 Y1 107.84(11) . . ?
C19 C16 O17 124.7(4) . . ?
C19 C16 C14 122.2(4) . . ?
O17 C16 C14 113.1(3) . . ?
C16 O17 C18 116.0(3) . . ?
C16 O17 Y1 117.8(2) . . ?
C18 O17 Y1 126.1(3) . . ?
O17 C18 H18A 109.5 . . ?
O17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 C20 119.6(4) . . ?
C16 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C21 C20 C19 120.2(4) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C13 120.7(4) . . ?
C20 C21 H21 119.7 . . ?
C13 C21 H21 119.7 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C9 C23 H23A 109.5 . . ?
C9 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C9 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C5 121.2(4) . . ?
C25 C24 H24 119.4 . . ?
C5 C24 H24 119.4 . . ?
C24 C25 C26 120.2(4) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C27 C26 C25 119.2(4) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 O28 124.2(4) . . ?
C26 C27 C4 122.1(4) . . ?
O28 C27 C4 113.7(4) . . ?
C27 O28 C29 115.9(4) . . ?
C27 O28 Y1 117.7(2) . . ?
C29 O28 Y1 126.4(3) . . ?
O28 C29 H29A 109.5 . . ?
O28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
NI1 O31 H31A 119(4) . . ?
NI1 O31 H31B 130(5) . . ?
H31A O31 H31B 110(6) . . ?
O60 ZN1 O51 94.60(13) . . ?
O60 ZN1 N42 98.20(15) . . ?
O51 ZN1 N42 163.49(14) . . ?
O60 ZN1 N47 98.14(16) . . ?
O51 ZN1 N47 92.39(13) . . ?
N42 ZN1 N47 96.05(15) . . ?
O60 ZN1 O33 109.72(14) . . ?
O51 ZN1 O33 75.45(11) . . ?
N42 ZN1 O33 90.39(14) . . ?
N47 ZN1 O33 150.21(14) . . ?
O60 ZN1 Y1 94.02(12) . . ?
O51 ZN1 Y1 40.15(8) . . ?
N42 ZN1 Y1 127.97(11) . . ?
N47 ZN1 Y1 131.91(10) . . ?
O33 ZN1 Y1 38.35(8) . . ?
C34 O33 ZN1 127.7(3) . . ?
C34 O33 Y1 123.5(3) . . ?
ZN1 O33 Y1 108.15(12) . . ?
O33 C34 C40 123.7(4) . . ?
O33 C34 C35 117.8(4) . . ?
C40 C34 C35 118.6(4) . . ?
C37 C35 O36 124.8(4) . . ?
C37 C35 C34 121.5(4) . . ?
O36 C35 C34 113.7(4) . . ?
C35 O36 C100 116.4(3) . . ?
C35 O36 Y1 116.2(2) . . ?
C100 O36 Y1 126.9(3) . . ?
C35 C37 C38 119.8(5) . . ?
C35 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C39 C38 C37 119.7(5) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C38 C39 C40 121.6(5) . . ?
C38 C39 H39 119.2 . . ?
C40 C39 H39 119.2 . . ?
C34 C40 C39 118.9(4) . . ?
C34 C40 C41 124.1(4) . . ?
C39 C40 C41 116.9(4) . . ?
N42 C41 C40 128.5(4) . . ?
N42 C41 H41 115.7 . . ?
C40 C41 H41 115.7 . . ?
C41 N42 C43 117.1(4) . . ?
C41 N42 ZN1 125.5(3) . . ?
C43 N42 ZN1 117.3(3) . . ?
N42 C43 C44 114.0(4) . . ?
N42 C43 H43A 108.8 . . ?
C44 C43 H43A 108.8 . . ?
N42 C43 H43B 108.8 . . ?
C44 C43 H43B 108.8 . . ?
H43A C43 H43B 107.6 . . ?
C43 C44 C45 111.7(4) . . ?
C43 C44 C46 112.2(4) . . ?
C45 C44 C46 110.7(4) . . ?
C43 C44 C59 106.1(4) . . ?
C45 C44 C59 110.1(4) . . ?
C46 C44 C59 105.8(4) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N47 C46 C44 115.5(4) . . ?
N47 C46 H46A 108.4 . . ?
C44 C46 H46A 108.4 . . ?
N47 C46 H46B 108.4 . . ?
C44 C46 H46B 108.4 . . ?
H46A C46 H46B 107.5 . . ?
C48 N47 C46 115.8(4) . . ?
C48 N47 ZN1 124.2(3) . . ?
C46 N47 ZN1 119.6(3) . . ?
N47 C48 C49 127.6(4) . . ?
N47 C48 H48 116.2 . . ?
C49 C48 H48 116.2 . . ?
C57 C49 C50 119.5(4) . . ?
C57 C49 C48 116.3(4) . . ?
C50 C49 C48 123.9(4) . . ?
O51 C50 C52 118.2(4) . . ?
O51 C50 C49 125.0(4) . . ?
C52 C50 C49 116.8(4) . . ?
C50 O51 ZN1 126.4(3) . . ?
C50 O51 Y1 125.8(2) . . ?
ZN1 O51 Y1 106.81(12) . . ?
C55 C52 O53 124.5(4) . . ?
C55 C52 C50 123.0(4) . . ?
O53 C52 C50 112.6(4) . . ?
C52 O53 C54 115.5(3) . . ?
C52 O53 Y1 118.1(2) . . ?
C54 O53 Y1 126.4(3) . . ?
O53 C54 H54A 109.5 . . ?
O53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 C56 119.1(4) . . ?
C52 C55 H55 120.4 . . ?
C56 C55 H55 120.4 . . ?
C57 C56 C55 119.6(5) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C56 C57 C49 122.0(4) . . ?
C56 C57 H57 119 . . ?
C49 C57 H57 119 . . ?
C44 C59 H59A 109.5 . . ?
C44 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C44 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
ZN1 O60 H60A 112(4) . . ?
ZN1 O60 H60B 136(4) . . ?
H60A O60 H60B 86(5) . . ?
Y1 O61 H61A 129(3) . . ?
Y1 O61 H61B 125(4) . . ?
H61A O61 H61B 105(5) . . ?
O63 S62 O64 114.1(2) . . ?
O63 S62 O65 115.5(2) . . ?
O64 S62 O65 114.1(2) . . ?
O63 S62 C66 103.7(2) . . ?
O64 S62 C66 104.0(3) . . ?
O65 S62 C66 103.5(2) . . ?
F68 C66 F67 108.1(5) . . ?
F68 C66 F69 107.9(5) . . ?
F67 C66 F69 107.7(5) . . ?
F68 C66 S62 111.4(4) . . ?
F67 C66 S62 110.9(4) . . ?
F69 C66 S62 110.7(4) . . ?
O73 S70 O71 116.9(3) . . ?
O73 S70 O72 113.7(3) . . ?
O71 S70 O72 114.3(3) . . ?
O73 S70 C74 103.9(3) . . ?
O71 S70 C74 102.0(3) . . ?
O72 S70 C74 103.6(3) . . ?
F76 C74 F77 106.0(5) . . ?
F76 C74 F75 106.6(5) . . ?
F77 C74 F75 107.5(6) . . ?
F76 C74 S70 111.6(5) . . ?
F77 C74 S70 111.5(5) . . ?
F75 C74 S70 113.1(4) . . ?
O80 S78 O81 115.5(3) . . ?
O80 S78 O79 115.3(2) . . ?
O81 S78 O79 114.6(2) . . ?
O80 S78 C82 103.1(2) . . ?
O81 S78 C82 103.2(2) . . ?
O79 S78 C82 102.5(2) . . ?
F83 C82 F85 108.5(4) . . ?
F83 C82 F84 106.6(4) . . ?
F85 C82 F84 106.8(4) . . ?
F83 C82 S78 111.9(3) . . ?
F85 C82 S78 111.8(3) . . ?
F84 C82 S78 111.1(3) . . ?
CL88 C91 CL1 110.4(3) . . ?
CL88 C91 H91A 109.6 . . ?
CL1 C91 H91A 109.6 . . ?
CL88 C91 H91B 109.6 . . ?
CL1 C91 H91B 109.6 . . ?
H91A C91 H91B 108.1 . . ?
CL90 C92 CL89 111.1(4) . . ?
CL90 C92 H92A 109.4 . . ?
CL89 C92 H92A 109.4 . . ?
CL90 C92 H92B 109.4 . . ?
CL89 C92 H92B 109.4 . . ?
H92A C92 H92B 108 . . ?
O36 C100 H10C 109.5 . . ?
O36 C100 H10D 109.5 . . ?
H10C C100 H10D 109.5 . . ?
O36 C100 H10E 109.5 . . ?
H10C C100 H10E 109.5 . . ?
H10D C100 H10E 109.5 . . ?

####################################################################### 
# 
# 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1877427'
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-13 downloaded from the CCDC.
;

_audit_creation_date             2019-02-11T14:47:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C21 H34 Er N3 Ni O12, 2(N O3), H2 O'
_chemical_formula_sum            'C21 H36 Er N5 Ni O19'
_chemical_formula_weight         888.52
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8381(11)
_cell_length_b                   12.6145(16)
_cell_length_c                   12.8061(15)
_cell_angle_alpha                89.022(15)
_cell_angle_beta                 86.952(14)
_cell_angle_gamma                73.975(14)
_cell_volume                     1525.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      26.05
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             890
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.442
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_T_max  0.499

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_diffrn_standards_number         200
_diffrn_standards_interval_time  4
_diffrn_standards_decay_%        0.1
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_number            15153
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.157
_diffrn_reflns_theta_max         26.099
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.94
_diffrn_measured_fraction_theta_max 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.922
_reflns_Friedel_coverage         0
_reflns_number_total             5588
_reflns_number_gt                5185
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0586P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5588
_refine_ls_number_parameters     460
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.55
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.171

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1333(4) 0.5665(3) 0.1450(3) 0.0138(8) Uani 1 1 d . . . . .
C2 C -0.0663(4) 0.4543(3) 0.1251(3) 0.0161(8) Uani 1 1 d . . . . .
C3 C -0.1444(5) 0.3873(4) 0.0868(4) 0.0218(9) Uani 1 1 d . . . . .
H3 H -0.099204 0.313699 0.071802 0.026 Uiso 1 1 calc R U . . .
C4 C -0.2866(5) 0.4280(4) 0.0708(4) 0.0242(10) Uani 1 1 d . . . . .
H4 H -0.337408 0.381348 0.048042 0.029 Uiso 1 1 calc R U . . .
C5 C -0.3548(4) 0.5398(4) 0.0887(3) 0.0202(9) Uani 1 1 d . . . . .
H5 H -0.450782 0.568085 0.077891 0.024 Uiso 1 1 calc R U . . .
C6 C -0.2773(4) 0.6070(4) 0.1227(3) 0.0161(8) Uani 1 1 d . . . . .
C7 C -0.4669(4) 0.7723(4) 0.0971(4) 0.0220(9) Uani 1 1 d . . . . .
H7A H -0.46214 0.753453 0.024393 0.033 Uiso 1 1 calc R U . . .
H7B H -0.486706 0.850803 0.10397 0.033 Uiso 1 1 calc R U . . .
H7C H -0.54082 0.747748 0.133173 0.033 Uiso 1 1 calc R U . . .
C8 C 0.0176(4) 0.7492(3) 0.4420(3) 0.0130(8) Uani 1 1 d . . . . .
C9 C 0.1314(4) 0.6896(3) 0.5019(3) 0.0163(8) Uani 1 1 d . . . . .
C10 C 0.1401(5) 0.7244(4) 0.6047(4) 0.0233(10) Uani 1 1 d . . . . .
H10 H 0.21414 0.685175 0.644385 0.028 Uiso 1 1 calc R U . . .
C11 C 0.0432(5) 0.8139(4) 0.6477(4) 0.0271(10) Uani 1 1 d . . . . .
H11 H 0.051634 0.835113 0.715688 0.032 Uiso 1 1 calc R U . . .
C12 C -0.0692(5) 0.8739(4) 0.5892(3) 0.0209(9) Uani 1 1 d . . . . .
H12 H -0.134863 0.935935 0.617349 0.025 Uiso 1 1 calc R U . . .
C13 C -0.0809(4) 0.8395(3) 0.4889(3) 0.0157(8) Uani 1 1 d . . . . .
C14 C -0.2853(5) 0.9912(4) 0.4608(4) 0.0307(11) Uani 1 1 d . . . . .
H14A H -0.335266 0.979994 0.524652 0.046 Uiso 1 1 calc R U . . .
H14B H -0.351983 1.02071 0.408476 0.046 Uiso 1 1 calc R U . . .
H14C H -0.230969 1.041996 0.472853 0.046 Uiso 1 1 calc R U . . .
C15 C 0.0839(4) 0.4035(3) 0.1374(3) 0.0176(8) Uani 1 1 d . . . . .
H15 H 0.123476 0.33544 0.105562 0.021 Uiso 1 1 calc R U . . .
C16 C 0.3171(4) 0.3826(4) 0.1869(3) 0.0179(9) Uani 1 1 d . . . . .
H16A H 0.371995 0.425522 0.149318 0.021 Uiso 1 1 calc R U . . .
H16B H 0.330331 0.314307 0.148998 0.021 Uiso 1 1 calc R U . . .
C17 C 0.3742(4) 0.3555(4) 0.2966(4) 0.0190(9) Uani 1 1 d . . . . .
C18 C 0.2814(5) 0.2963(4) 0.3623(4) 0.0207(9) Uani 1 1 d . . . . .
H18A H 0.187429 0.344622 0.372366 0.031 Uiso 1 1 calc R U . . .
H18B H 0.321295 0.276341 0.429065 0.031 Uiso 1 1 calc R U . . .
H18C H 0.277632 0.231004 0.326513 0.031 Uiso 1 1 calc R U . . .
C19 C 0.5235(5) 0.2768(4) 0.2817(4) 0.0274(11) Uani 1 1 d . . . . .
H19A H 0.519004 0.211948 0.245426 0.041 Uiso 1 1 calc R U . . .
H19B H 0.561999 0.256146 0.348811 0.041 Uiso 1 1 calc R U . . .
H19C H 0.583071 0.312858 0.241608 0.041 Uiso 1 1 calc R U . . .
C20 C 0.3879(4) 0.4582(3) 0.3520(4) 0.0189(9) Uani 1 1 d . . . . .
H20A H 0.435136 0.435143 0.416561 0.023 Uiso 1 1 calc R U . . .
H20B H 0.44846 0.491527 0.308255 0.023 Uiso 1 1 calc R U . . .
C21 C 0.2443(4) 0.5954(3) 0.4639(3) 0.0166(8) Uani 1 1 d . . . . .
H21 H 0.318873 0.569837 0.507788 0.02 Uiso 1 1 calc R U . . .
N1 N 0.1670(3) 0.4441(3) 0.1883(3) 0.0160(7) Uani 1 1 d . . . . .
N2 N 0.2541(3) 0.5431(3) 0.3772(3) 0.0143(7) Uani 1 1 d . . . . .
N3 N 0.1882(4) 0.8774(3) -0.0322(3) 0.0189(8) Uani 1 1 d . . . . .
N4 N 0.2962(4) 1.0636(3) 0.1609(3) 0.0204(8) Uani 1 1 d . . . . .
N5 N -0.4042(4) 0.7351(3) 0.3716(3) 0.0181(7) Uani 1 1 d . . . . .
O1 O -0.0698(3) 0.6364(2) 0.1848(2) 0.0140(6) Uani 1 1 d . . . . .
O2 O -0.0009(3) 0.7239(2) 0.3444(2) 0.0140(6) Uani 1 1 d . . . . .
O3 O -0.3332(3) 0.7194(2) 0.1417(2) 0.0194(6) Uani 1 1 d . . . . .
O4 O -0.1930(3) 0.8888(2) 0.4259(2) 0.0198(6) Uani 1 1 d . . . . .
O5 O 0.2301(3) 0.6593(3) 0.1859(2) 0.0209(6) Uani 1 1 d D . . . .
HO5A H 0.240(5) 0.718(2) 0.214(3) 0.025 Uiso 1 1 d D U . . .
HO5B H 0.199(5) 0.678(3) 0.1256(18) 0.025 Uiso 1 1 d D U . . .
O6 O -0.0317(3) 0.5095(2) 0.3830(3) 0.0206(6) Uani 1 1 d D . . . .
HO6A H -0.11372 0.55073 0.39516 0.025 Uiso 1 1 d D U . . .
HO6B H -0.02604 0.44505 0.40288 0.025 Uiso 1 1 d D U . . .
O7 O -0.0393(3) 0.9229(3) 0.2371(3) 0.0209(6) Uani 1 1 d D . . . .
HO7A H 0.0476(18) 0.907(4) 0.251(4) 0.025 Uiso 1 1 d D U . . .
HO7B H -0.057(4) 0.979(3) 0.198(4) 0.025 Uiso 1 1 d D U . . .
O8 O -0.1396(4) 0.8392(3) 0.0654(3) 0.0239(7) Uani 1 1 d . . . . .
H1O8 H -0.077(7) 0.848(5) 0.048(5) 0.029 Uiso 1 1 d . U . . .
H2O8 H -0.192(6) 0.857(5) 0.020(5) 0.029 Uiso 1 1 d . U . . .
O9 O -0.3464(3) 0.9754(3) 0.2068(3) 0.0216(7) Uani 1 1 d D . . . .
HO9A H -0.329(4) 1.021(3) 0.162(3) 0.026 Uiso 1 1 d D U . . .
HO9B H -0.4345(14) 0.993(4) 0.221(4) 0.026 Uiso 1 1 d D U . . .
O10 O -0.4293(3) 0.8330(3) 0.3359(3) 0.0212(6) Uani 1 1 d . . . . .
O11 O -0.2761(3) 0.6765(3) 0.3588(3) 0.0209(6) Uani 1 1 d . . . . .
O12 O -0.4965(3) 0.6999(3) 0.4150(3) 0.0347(9) Uani 1 1 d . . . . .
O13 O 0.2484(3) 0.8417(3) 0.3003(3) 0.0242(7) Uani 1 1 d D . . . .
HO3A H 0.285(5) 0.820(4) 0.358(2) 0.029 Uiso 1 1 d D U . . .
HO3B H 0.294(5) 0.883(4) 0.270(3) 0.029 Uiso 1 1 d D U . . .
O15A O 0.1579(4) 0.8297(3) 0.0470(3) 0.0381(9) Uani 1 1 d . . . . .
O14A O 0.3014(17) 0.8855(14) -0.0588(12) 0.0356(16) Uani 0.44 1 d . . P A 1
O16A O 0.0761(9) 0.9241(9) -0.0759(8) 0.0356(16) Uani 0.44 1 d . . P A 1
O14B O 0.3065(13) 0.9022(10) -0.0324(9) 0.0356(16) Uani 0.56 1 d . . P A 2
O16B O 0.1232(7) 0.8934(7) -0.1150(6) 0.0356(16) Uani 0.56 1 d . . P A 2
O17 O 0.1714(4) 1.0650(4) 0.1588(3) 0.0497(11) Uani 1 1 d . . . . .
O18 O 0.3695(3) 1.0101(3) 0.2339(3) 0.0227(7) Uani 1 1 d . . . . .
O19 O 0.3508(4) 1.1127(3) 0.0941(3) 0.0376(9) Uani 1 1 d . . . . .
NI1 Ni 0.09995(5) 0.58174(4) 0.27377(4) 0.01177(12) Uani 1 1 d . . . . .
ER1 Er -0.18887(2) 0.80879(2) 0.24510(2) 0.01155(8) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.335(5) . ?
C1 C2 1.407(6) . ?
C1 C6 1.410(5) . ?
C2 C3 1.400(6) . ?
C2 C15 1.456(6) . ?
C3 C4 1.376(6) . ?
C3 H3 0.93 . ?
C4 C5 1.402(7) . ?
C4 H4 0.93 . ?
C5 C6 1.376(6) . ?
C5 H5 0.93 . ?
C6 O3 1.392(5) . ?
C7 O3 1.444(5) . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
C8 O2 1.329(5) . ?
C8 C13 1.396(6) . ?
C8 C9 1.419(5) . ?
C9 C10 1.410(6) . ?
C9 C21 1.455(6) . ?
C10 C11 1.363(7) . ?
C10 H10 0.93 . ?
C11 C12 1.401(7) . ?
C11 H11 0.93 . ?
C12 C13 1.383(6) . ?
C12 H12 0.93 . ?
C13 O4 1.398(5) . ?
C14 O4 1.422(6) . ?
C14 H14A 0.96 . ?
C14 H14B 0.96 . ?
C14 H14C 0.96 . ?
C15 N1 1.287(5) . ?
C15 H15 0.93 . ?
C16 N1 1.465(5) . ?
C16 C17 1.539(6) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 C20 1.529(6) . ?
C17 C19 1.534(6) . ?
C17 C18 1.541(6) . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C20 N2 1.474(5) . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C21 N2 1.287(6) . ?
C21 H21 0.93 . ?
N1 NI1 2.001(4) . ?
N2 NI1 2.019(3) . ?
N3 O14A 1.178(17) . ?
N3 O15A 1.236(5) . ?
N3 O16B 1.252(8) . ?
N3 O16A 1.254(10) . ?
N3 O14B 1.285(11) . ?
N4 O17 1.225(5) . ?
N4 O19 1.233(5) . ?
N4 O18 1.277(5) . ?
N5 O12 1.222(5) . ?
N5 O10 1.272(5) . ?
N5 O11 1.276(5) . ?
O1 NI1 2.025(3) . ?
O1 ER1 2.291(3) . ?
O2 NI1 1.999(3) . ?
O2 ER1 2.301(3) . ?
O3 ER1 2.485(3) . ?
O4 ER1 2.536(3) . ?
O5 NI1 2.089(3) . ?
O5 HO5A 0.857(10) . ?
O5 HO5B 0.852(10) . ?
O6 NI1 2.209(3) . ?
O6 HO6A 0.8387 . ?
O6 HO6B 0.8356 . ?
O7 ER1 2.323(3) . ?
O7 HO7A 0.850(10) . ?
O7 HO7B 0.849(10) . ?
O8 ER1 2.373(4) . ?
O8 H1O8 0.68(6) . ?
O8 H2O8 0.79(6) . ?
O9 ER1 2.304(3) . ?
O9 HO9A 0.851(10) . ?
O9 HO9B 0.843(10) . ?
O10 ER1 2.522(3) . ?
O11 ER1 2.493(3) . ?
O13 HO3A 0.849(10) . ?
O13 HO3B 0.846(10) . ?
NI1 ER1 3.4632(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 124.3(3) . . ?
O1 C1 C6 118.0(4) . . ?
C2 C1 C6 117.8(3) . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 C15 116.9(4) . . ?
C1 C2 C15 123.5(4) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
C6 C5 C4 118.9(4) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 O3 123.9(4) . . ?
C5 C6 C1 122.4(4) . . ?
O3 C6 C1 113.7(3) . . ?
O3 C7 H7A 109.5 . . ?
O3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 C13 118.3(3) . . ?
O2 C8 C9 123.9(4) . . ?
C13 C8 C9 117.8(4) . . ?
C10 C9 C8 118.8(4) . . ?
C10 C9 C21 116.5(4) . . ?
C8 C9 C21 124.6(4) . . ?
C11 C10 C9 121.9(4) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 118.9(4) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C8 122.7(4) . . ?
C12 C13 O4 123.9(4) . . ?
C8 C13 O4 113.4(3) . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C2 125.9(4) . . ?
N1 C15 H15 117 . . ?
C2 C15 H15 117 . . ?
N1 C16 C17 113.6(3) . . ?
N1 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
N1 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C20 C17 C19 107.3(3) . . ?
C20 C17 C16 111.9(4) . . ?
C19 C17 C16 106.9(4) . . ?
C20 C17 C18 111.6(4) . . ?
C19 C17 C18 108.5(4) . . ?
C16 C17 C18 110.5(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C17 115.8(3) . . ?
N2 C20 H20A 108.3 . . ?
C17 C20 H20A 108.3 . . ?
N2 C20 H20B 108.3 . . ?
C17 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
N2 C21 C9 128.2(4) . . ?
N2 C21 H21 115.9 . . ?
C9 C21 H21 115.9 . . ?
C15 N1 C16 117.6(3) . . ?
C15 N1 NI1 123.4(3) . . ?
C16 N1 NI1 119.0(3) . . ?
C21 N2 C20 117.2(3) . . ?
C21 N2 NI1 122.1(3) . . ?
C20 N2 NI1 120.5(3) . . ?
O14Aa N3 O15A 126.3(8) . . ?
O15A N3 O16B 126.4(5) . . ?
O14Aa N3 O16A 124.9(8) . . ?
O15A N3 O16A 108.5(5) . . ?
O15A N3 O14B 115.7(6) . . ?
O16Bb N3 O14B 117.4(6) . . ?
O17 N4 O19 121.0(4) . . ?
O17 N4 O18 118.8(4) . . ?
O19 N4 O18 120.2(4) . . ?
O12 N5 O10 122.2(4) . . ?
O12 N5 O11 122.5(4) . . ?
O10 N5 O11 115.4(3) . . ?
C1 O1 NI1 121.1(2) . . ?
C1 O1 ER1 123.7(2) . . ?
NI1 O1 ER1 106.54(11) . . ?
C8 O2 NI1 124.7(2) . . ?
C8 O2 ER1 126.3(2) . . ?
NI1 O2 ER1 107.08(11) . . ?
C6 O3 C7 116.7(3) . . ?
C6 O3 ER1 116.4(2) . . ?
C7 O3 ER1 126.8(2) . . ?
C13 O4 C14 116.8(3) . . ?
C13 O4 ER1 117.5(2) . . ?
C14 O4 ER1 124.7(3) . . ?
NI1 O5 HO5A 115(3) . . ?
NI1 O5 HO5B 112(3) . . ?
HO5A O5 HO5B 106.6(17) . . ?
NI1 O6 HO6A 113.7 . . ?
NI1 O6 HO6B 133.2 . . ?
HO6A O6 HO6B 110.9 . . ?
ER1 O7 HO7A 128(3) . . ?
ER1 O7 HO7B 120(3) . . ?
HO7A O7 HO7B 107.6(17) . . ?
ER1 O8 H1O8 121(5) . . ?
ER1 O8 H2O8 129(4) . . ?
H1O8 O8 H2O8 107(7) . . ?
ER1 O9 HO9A 124(3) . . ?
ER1 O9 HO9B 126(3) . . ?
HO9A O9 HO9B 108.2(17) . . ?
N5 O10 ER1 96.0(2) . . ?
N5 O11 ER1 97.2(2) . . ?
HO3A O13 HO3B 108.2(17) . . ?
O2 NI1 N1 169.06(12) . . ?
O2 NI1 N2 93.69(13) . . ?
N1 NI1 N2 96.97(14) . . ?
O2 NI1 O1 78.56(11) . . ?
N1 NI1 O1 90.69(12) . . ?
N2 NI1 O1 171.98(13) . . ?
O2 NI1 O5 90.89(12) . . ?
N1 NI1 O5 92.15(14) . . ?
N2 NI1 O5 86.70(13) . . ?
O1 NI1 O5 95.42(12) . . ?
O2 NI1 O6 84.58(11) . . ?
N1 NI1 O6 93.24(13) . . ?
N2 NI1 O6 88.52(13) . . ?
O1 NI1 O6 88.67(11) . . ?
O5 NI1 O6 173.19(12) . . ?
O2 NI1 ER1 39.43(8) . . ?
N1 NI1 ER1 129.98(9) . . ?
N2 NI1 ER1 133.05(10) . . ?
O1 NI1 ER1 39.37(8) . . ?
O5 NI1 ER1 90.74(9) . . ?
O6 NI1 ER1 88.99(7) . . ?
O1 ER1 O2 67.39(9) . . ?
O1 ER1 O9 145.95(11) . . ?
O2 ER1 O9 144.36(10) . . ?
O1 ER1 O7 110.09(11) . . ?
O2 ER1 O7 74.02(10) . . ?
O9 ER1 O7 79.36(10) . . ?
O1 ER1 O8 76.60(11) . . ?
O2 ER1 O8 117.61(11) . . ?
O9 ER1 O8 75.26(12) . . ?
O7 ER1 O8 73.03(12) . . ?
O1 ER1 O3 65.76(9) . . ?
O2 ER1 O3 127.54(10) . . ?
O9 ER1 O3 87.54(10) . . ?
O7 ER1 O3 144.96(11) . . ?
O8 ER1 O3 72.24(12) . . ?
O1 ER1 O11 74.05(10) . . ?
O2 ER1 O11 75.10(10) . . ?
O9 ER1 O11 118.11(10) . . ?
O7 ER1 O11 143.83(10) . . ?
O8 ER1 O11 139.57(11) . . ?
O3 ER1 O11 70.63(11) . . ?
O1 ER1 O10 117.74(10) . . ?
O2 ER1 O10 114.73(10) . . ?
O9 ER1 O10 67.33(10) . . ?
O7 ER1 O10 131.01(11) . . ?
O8 ER1 O10 126.98(11) . . ?
O3 ER1 O10 70.01(10) . . ?
O11 ER1 O10 50.85(10) . . ?
O1 ER1 O4 128.68(9) . . ?
O2 ER1 O4 64.40(9) . . ?
O9 ER1 O4 85.31(11) . . ?
O7 ER1 O4 72.34(11) . . ?
O8 ER1 O4 142.76(11) . . ?
O3 ER1 O4 139.17(10) . . ?
O11 ER1 O4 77.65(10) . . ?
O10 ER1 O4 70.15(10) . . ?
O1 ER1 NI1 34.10(6) . . ?
O2 ER1 NI1 33.49(7) . . ?
O9 ER1 NI1 167.76(7) . . ?
O7 ER1 NI1 89.91(8) . . ?
O8 ER1 NI1 96.08(9) . . ?
O3 ER1 NI1 98.17(7) . . ?
O11 ER1 NI1 74.09(7) . . ?
O10 ER1 NI1 124.79(7) . . ?
O4 ER1 NI1 97.12(7) . . ?

####################################################################### 
# 
# 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_complex3
_database_code_depnum_ccdc_archive 'CCDC 1877429'
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-13 downloaded from the CCDC.
;

_audit_creation_date             2019-02-11T16:52:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C21 H36 Cl3 N2 Ni1 O10 Y'
_chemical_formula_sum            'C21 H36 Cl3 N2 Ni O10 Y'
_chemical_formula_weight         730.49
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_Int_Tables_number      29
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   8.8025(2)
_cell_length_b                   16.3713(4)
_cell_length_c                   20.1951(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2910.28(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    14016
_cell_measurement_theta_min      3.0199
_cell_measurement_theta_max      31.2971
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.4495
_exptl_absorpt_correction_T_max  0.8742

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 8.2632
_diffrn_orient_matrix_ub_11      -0.0013773
_diffrn_orient_matrix_ub_12      -0.015735
_diffrn_orient_matrix_ub_13      -0.0327185
_diffrn_orient_matrix_ub_21      -0.0372475
_diffrn_orient_matrix_ub_22      0.0358892
_diffrn_orient_matrix_ub_23      -0.0110514
_diffrn_orient_matrix_ub_31      0.0714322
_diffrn_orient_matrix_ub_32      0.0184921
_diffrn_orient_matrix_ub_33      -0.0063918
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.056
_diffrn_reflns_number            20707
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.204
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_coverage         0.94
_reflns_number_total             5928
_reflns_number_gt                5337
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.468(4) ref 1 0 0 0 1 0 0 0 1
2 0.532(4) mt_II -1 0 0 0 -1 0 0 0 -1
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0175P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5928
_refine_ls_number_parameters     384
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.024
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.038
_refine_ls_wR_factor_gt          0.0377
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.049

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6921(4) 0.2275(2) 0.42633(18) 0.0239(8) Uani 1 1 d . . . . .
H1A H 0.596882 0.237667 0.401583 0.029 Uiso 1 1 calc R U . . .
H1B H 0.682296 0.254908 0.469804 0.029 Uiso 1 1 calc R U . . .
C2 C 0.7051(3) 0.1352(2) 0.43855(17) 0.0203(8) Uani 1 1 d . . . . .
C3 C 0.5613(4) 0.1113(2) 0.47705(19) 0.0314(10) Uani 1 1 d . . . . .
H3A H 0.562351 0.052441 0.485698 0.047 Uiso 1 1 calc R U . . .
H3B H 0.471326 0.12532 0.450841 0.047 Uiso 1 1 calc R U . . .
H3C H 0.55862 0.141018 0.519177 0.047 Uiso 1 1 calc R U . . .
C4 C 0.8431(4) 0.1150(3) 0.47964(19) 0.0351(10) Uani 1 1 d . . . . .
H4A H 0.934963 0.132163 0.456016 0.053 Uiso 1 1 calc R U . . .
H4B H 0.846955 0.055917 0.487442 0.053 Uiso 1 1 calc R U . . .
H4C H 0.837127 0.143631 0.522156 0.053 Uiso 1 1 calc R U . . .
C5 C 0.6996(4) 0.0882(2) 0.37405(17) 0.0214(8) Uani 1 1 d . . . . .
H5A H 0.690299 0.029371 0.384639 0.026 Uiso 1 1 calc R U . . .
H5B H 0.606243 0.104401 0.350057 0.026 Uiso 1 1 calc R U . . .
C6 C 0.8281(4) 0.3433(2) 0.40020(16) 0.0175(7) Uani 1 1 d . . . . .
H6 H 0.766994 0.364453 0.434994 0.021 Uiso 1 1 calc R U . . .
C7 C 0.9215(4) 0.40255(19) 0.36538(16) 0.0158(7) Uani 1 1 d . . . . .
C8 C 0.9092(4) 0.4840(2) 0.38656(17) 0.0249(9) Uani 1 1 d . . . . .
H8 H 0.848296 0.496564 0.424048 0.03 Uiso 1 1 calc R U . . .
C9 C 0.9829(5) 0.5454(2) 0.35434(19) 0.0304(9) Uani 1 1 d . . . . .
H9 H 0.975635 0.59981 0.370363 0.036 Uiso 1 1 calc R U . . .
C10 C 1.0686(4) 0.52898(19) 0.29835(17) 0.0242(9) Uani 1 1 d . . . . .
H10 H 1.118315 0.571796 0.275156 0.029 Uiso 1 1 calc R U . . .
C11 C 1.0802(4) 0.4493(2) 0.27697(16) 0.0171(7) Uani 1 1 d . . . . .
C12 C 1.0085(3) 0.38488(18) 0.30934(17) 0.0140(7) Uani 1 1 d . . . . .
C13 C 1.2309(4) 0.4884(2) 0.1827(2) 0.0310(9) Uani 1 1 d . . . . .
H13A H 1.154509 0.529523 0.171 0.046 Uiso 1 1 calc R U . . .
H13B H 1.274352 0.465214 0.142136 0.046 Uiso 1 1 calc R U . . .
H13C H 1.311588 0.513997 0.208861 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8712(4) 0.03522(19) 0.29685(16) 0.0153(7) Uani 1 1 d . . . . .
H14 H 0.822101 -0.014345 0.308714 0.018 Uiso 1 1 calc R U . . .
C15 C 0.9836(4) 0.02959(18) 0.24467(15) 0.0140(7) Uani 1 1 d . . . . .
C16 C 1.0199(4) -0.0491(2) 0.22157(17) 0.0201(8) Uani 1 1 d . . . . .
H16 H 0.972851 -0.095165 0.241551 0.024 Uiso 1 1 calc R U . . .
C17 C 1.1213(4) -0.0611(2) 0.17100(17) 0.0242(9) Uani 1 1 d . . . . .
H17 H 1.147234 -0.114953 0.157717 0.029 Uiso 1 1 calc R U . . .
C18 C 1.1861(4) 0.0055(2) 0.13919(17) 0.0221(8) Uani 1 1 d . . . . .
H18 H 1.254296 -0.002266 0.103296 0.026 Uiso 1 1 calc R U . . .
C19 C 1.1501(4) 0.0826(2) 0.16031(17) 0.0176(8) Uani 1 1 d . . . . .
C20 C 1.0519(4) 0.09696(19) 0.21335(15) 0.0135(7) Uani 1 1 d . . . . .
C21 C 1.3024(4) 0.1444(2) 0.07444(18) 0.0274(9) Uani 1 1 d . . . . .
H21A H 1.389763 0.109975 0.085647 0.041 Uiso 1 1 calc R U . . .
H21B H 1.338179 0.19798 0.059487 0.041 Uiso 1 1 calc R U . . .
H21C H 1.243632 0.118403 0.039001 0.041 Uiso 1 1 calc R U . . .
N1 N 0.8174(3) 0.26632(16) 0.39007(13) 0.0151(6) Uani 1 1 d . . . . .
N2 N 0.8301(3) 0.09877(16) 0.32885(13) 0.0152(6) Uani 1 1 d . . . . .
O1 O 1.0263(2) 0.31064(12) 0.28438(10) 0.0141(5) Uani 1 1 d . . . . .
O2 O 1.0257(2) 0.17379(13) 0.23071(10) 0.0143(5) Uani 1 1 d . . . . .
O3 O 1.1608(2) 0.42468(13) 0.22070(11) 0.0214(6) Uani 1 1 d . . . . .
O4 O 1.2075(2) 0.15438(14) 0.13207(11) 0.0191(5) Uani 1 1 d . . . . .
O5 O 1.3231(2) 0.24118(17) 0.26780(12) 0.0283(6) Uani 1 1 d D . . . .
H5C H 1.4193(15) 0.244(2) 0.2705(16) 0.034 Uiso 1 1 d D U . . .
H5D H 1.286(3) 0.222(2) 0.3022(12) 0.034 Uiso 1 1 d D U . . .
O6 O 1.4048(3) 0.31055(16) 0.15315(12) 0.0266(6) Uani 1 1 d D . . . .
H6A H 1.417(4) 0.336(2) 0.1154(10) 0.032 Uiso 1 1 d D U . . .
H6B H 1.478(3) 0.2957(19) 0.1799(13) 0.032 Uiso 1 1 d D U . . .
O7 O 1.1518(3) 0.33382(17) 0.07952(12) 0.0284(6) Uani 1 1 d D . . . .
H7A H 1.060(3) 0.364(2) 0.0647(18) 0.034 Uiso 1 1 d D U . . .
H7B H 1.201(3) 0.322(2) 0.0441(11) 0.034 Uiso 1 1 d D U . . .
O8 O 0.9069(3) 0.3015(2) 0.15112(14) 0.0467(9) Uani 1 1 d D . . . .
H8A H 0.843(3) 0.286(2) 0.1811(15) 0.056 Uiso 1 1 d D U . . .
H8B H 0.894(4) 0.336(2) 0.1187(15) 0.056 Uiso 1 1 d D U . . .
O20 O 0.5110(3) 0.40085(16) 0.05208(13) 0.0280(6) Uani 1 1 d D . . . .
H20A H 0.473(3) 0.4501(12) 0.0480(19) 0.034 Uiso 1 1 d D U . . .
H20B H 0.6104(16) 0.3987(19) 0.053(2) 0.034 Uiso 1 1 d D U . . .
O21 O 0.2976(3) 0.32127(19) 0.96755(15) 0.0475(8) Uani 1 1 d D . . . .
H21D H 0.380(3) 0.346(2) 0.974(2) 0.057 Uiso 1 1 d D U . . .
H21E H 0.311(4) 0.2758(15) 0.948(2) 0.057 Uiso 1 1 d D U . . .
CL1 Cl 1.15651(9) 0.16447(5) 0.37867(4) 0.02124(19) Uani 1 1 d . . . . .
CL2 Cl 0.66639(8) 0.25758(5) 0.24979(4) 0.01974(18) Uani 1 1 d . . . . .
CL3 Cl 0.86307(10) 0.42649(5) 0.04176(4) 0.02202(19) Uani 1 1 d . . . . .
NI1 Ni 0.92590(4) 0.20828(2) 0.31594(2) 0.01413(9) Uani 1 1 d . . . . .
Y1 Y 1.15312(3) 0.28298(2) 0.18734(2) 0.01356(7) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.469(4) . ?
C1 C2 1.534(5) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C4 1.508(5) . ?
C2 C5 1.514(5) . ?
C2 C3 1.536(4) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 N2 1.477(4) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 N1 1.280(4) . ?
C6 C7 1.453(5) . ?
C6 H6 0.95 . ?
C7 C12 1.397(5) . ?
C7 C8 1.405(5) . ?
C8 C9 1.361(5) . ?
C8 H8 0.95 . ?
C9 C10 1.385(5) . ?
C9 H9 0.95 . ?
C10 C11 1.378(5) . ?
C10 H10 0.95 . ?
C11 C12 1.392(4) . ?
C11 O3 1.399(4) . ?
C12 O1 1.325(3) . ?
C13 O3 1.435(4) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 N2 1.277(4) . ?
C14 C15 1.448(4) . ?
C14 H14 0.95 . ?
C15 C20 1.407(4) . ?
C15 C16 1.407(4) . ?
C16 C17 1.370(5) . ?
C16 H16 0.95 . ?
C17 C18 1.388(5) . ?
C17 H17 0.95 . ?
C18 C19 1.370(5) . ?
C18 H18 0.95 . ?
C19 C20 1.397(4) . ?
C19 O4 1.400(4) . ?
C20 O2 1.326(4) . ?
C21 O4 1.442(4) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
N1 NI1 2.014(3) . ?
N2 NI1 1.998(3) . ?
O1 NI1 1.999(2) . ?
O1 Y1 2.301(2) . ?
O2 NI1 2.013(2) . ?
O2 Y1 2.285(2) . ?
O3 Y1 2.417(2) . ?
O4 Y1 2.430(2) . ?
O5 Y1 2.313(2) . ?
O5 H5C 0.849(13) . ?
O5 H5D 0.830(13) . ?
O6 Y1 2.364(2) . ?
O6 H6A 0.873(13) . ?
O6 H6B 0.873(13) . ?
O7 Y1 2.331(2) . ?
O7 H7A 1.00(3) . ?
O7 H7B 0.858(14) . ?
O8 Y1 2.307(3) . ?
O8 H8A 0.862(13) . ?
O8 H8B 0.870(13) . ?
O20 H20A 0.876(13) . ?
O20 H20B 0.876(13) . ?
O21 H21D 0.836(14) . ?
O21 H21E 0.849(14) . ?
CL1 NI1 2.4980(9) . ?
NI1 Y1 3.4988(5) . ?

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 C1 C2 116.8(3) . . ?
N1 C1 H1A 108.1 . . ?
C2 C1 H1A 108.1 . . ?
N1 C1 H1B 108.1 . . ?
C2 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C4 C2 C5 112.8(3) . . ?
C4 C2 C1 111.4(3) . . ?
C5 C2 C1 111.1(3) . . ?
C4 C2 C3 109.2(3) . . ?
C5 C2 C3 106.2(3) . . ?
C1 C2 C3 105.7(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C2 116.5(3) . . ?
N2 C5 H5A 108.2 . . ?
C2 C5 H5A 108.2 . . ?
N2 C5 H5B 108.2 . . ?
C2 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
N1 C6 C7 128.4(3) . . ?
N1 C6 H6 115.8 . . ?
C7 C6 H6 115.8 . . ?
C12 C7 C8 119.0(3) . . ?
C12 C7 C6 124.3(3) . . ?
C8 C7 C6 116.3(3) . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 120.4(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 122.5(3) . . ?
C10 C11 O3 124.4(3) . . ?
C12 C11 O3 113.1(3) . . ?
O1 C12 C11 117.6(3) . . ?
O1 C12 C7 124.3(3) . . ?
C11 C12 C7 118.2(3) . . ?
O3 C13 H13A 109.5 . . ?
O3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 C15 127.8(3) . . ?
N2 C14 H14 116.1 . . ?
C15 C14 H14 116.1 . . ?
C20 C15 C16 118.2(3) . . ?
C20 C15 C14 124.7(3) . . ?
C16 C15 C14 117.0(3) . . ?
C17 C16 C15 121.7(3) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 120.0(3) . . ?
C16 C17 H17 120 . . ?
C18 C17 H17 120 . . ?
C19 C18 C17 119.0(3) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 122.5(3) . . ?
C18 C19 O4 124.3(3) . . ?
C20 C19 O4 113.3(3) . . ?
O2 C20 C19 118.0(3) . . ?
O2 C20 C15 123.4(3) . . ?
C19 C20 C15 118.6(3) . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C6 N1 C1 113.7(3) . . ?
C6 N1 NI1 123.3(2) . . ?
C1 N1 NI1 121.5(2) . . ?
C14 N2 C5 115.9(3) . . ?
C14 N2 NI1 123.1(2) . . ?
C5 N2 NI1 120.9(2) . . ?
C12 O1 NI1 126.54(19) . . ?
C12 O1 Y1 124.19(19) . . ?
NI1 O1 Y1 108.73(9) . . ?
C20 O2 NI1 124.59(19) . . ?
C20 O2 Y1 123.76(19) . . ?
NI1 O2 Y1 108.82(9) . . ?
C11 O3 C13 116.3(3) . . ?
C11 O3 Y1 119.26(18) . . ?
C13 O3 Y1 124.1(2) . . ?
C19 O4 C21 116.3(3) . . ?
C19 O4 Y1 117.94(18) . . ?
C21 O4 Y1 125.7(2) . . ?
Y1 O5 H5C 132(2) . . ?
Y1 O5 H5D 116(2) . . ?
H5C O5 H5D 111(2) . . ?
Y1 O6 H6A 118(2) . . ?
Y1 O6 H6B 117(2) . . ?
H6A O6 H6B 125(2) . . ?
Y1 O7 H7A 117.6(19) . . ?
Y1 O7 H7B 134(2) . . ?
H7A O7 H7B 106(2) . . ?
Y1 O8 H8A 110(3) . . ?
Y1 O8 H8B 117(3) . . ?
H8A O8 H8B 129(3) . . ?
H20A O20 H20B 115(2) . . ?
H21D O21 H21E 111(2) . . ?
N2 NI1 O1 168.61(10) . . ?
N2 NI1 O2 92.53(10) . . ?
O1 NI1 O2 76.67(8) . . ?
N2 NI1 N1 97.25(11) . . ?
O1 NI1 N1 92.93(10) . . ?
O2 NI1 N1 167.09(10) . . ?
N2 NI1 CL1 91.10(7) . . ?
O1 NI1 CL1 92.48(7) . . ?
O2 NI1 CL1 89.91(6) . . ?
N1 NI1 CL1 98.28(8) . . ?
N2 NI1 Y1 130.67(8) . . ?
O1 NI1 Y1 38.51(6) . . ?
O2 NI1 Y1 38.17(6) . . ?
N1 NI1 Y1 131.14(8) . . ?
CL1 NI1 Y1 90.70(2) . . ?
O2 Y1 O1 65.75(7) . . ?
O2 Y1 O8 76.30(9) . . ?
O1 Y1 O8 77.79(9) . . ?
O2 Y1 O5 79.44(8) . . ?
O1 Y1 O5 76.92(8) . . ?
O8 Y1 O5 150.39(9) . . ?
O2 Y1 O7 129.43(9) . . ?
O1 Y1 O7 136.31(8) . . ?
O8 Y1 O7 69.67(9) . . ?
O5 Y1 O7 139.91(8) . . ?
O2 Y1 O6 136.16(8) . . ?
O1 Y1 O6 131.76(8) . . ?
O8 Y1 O6 139.70(8) . . ?
O5 Y1 O6 69.83(8) . . ?
O7 Y1 O6 70.34(8) . . ?
O2 Y1 O3 131.14(7) . . ?
O1 Y1 O3 65.61(7) . . ?
O8 Y1 O3 89.36(10) . . ?
O5 Y1 O3 94.01(9) . . ?
O7 Y1 O3 85.29(9) . . ?
O6 Y1 O3 82.64(8) . . ?
O2 Y1 O4 66.11(7) . . ?
O1 Y1 O4 131.10(7) . . ?
O8 Y1 O4 98.81(10) . . ?
O5 Y1 O4 86.49(9) . . ?
O7 Y1 O4 83.18(9) . . ?
O6 Y1 O4 81.17(8) . . ?
O3 Y1 O4 162.56(7) . . ?
O2 Y1 NI1 33.00(5) . . ?
O1 Y1 NI1 32.75(5) . . ?
O8 Y1 NI1 75.18(6) . . ?
O5 Y1 NI1 75.22(6) . . ?
O7 Y1 NI1 144.63(6) . . ?
O6 Y1 NI1 145.01(6) . . ?
O3 Y1 NI1 98.31(5) . . ?
O4 Y1 NI1 98.67(5) . . ?

####################################################################### 
# 
# 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_complex2
_database_code_depnum_ccdc_archive 'CCDC 1877430'
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-13 downloaded from the CCDC.
;

_audit_creation_date             2019-02-11T14:56:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C21 H36 Cl3 Gd1 N2 Ni1 O10'
_chemical_formula_sum            'C21 H36 Cl3 Gd N2 Ni O10'
_chemical_formula_weight         798.83
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_Int_Tables_number      29
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   8.8734(3)
_cell_length_b                   16.4237(7)
_cell_length_c                   20.2362(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2949.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9068
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      40.38
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.7985
_exptl_absorpt_correction_T_max  0.9921

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#


_diffrn_ambient_temperature      180(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       ω-φ
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_number            112448
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.013
_diffrn_reflns_theta_max         40.561
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.93
_diffrn_measured_fraction_theta_max 0.697
_diffrn_reflns_Laue_measured_fraction_max 0.697
_diffrn_reflns_point_group_measured_fraction_max 0.689
_reflns_Friedel_fraction_full    0.92
_reflns_Friedel_fraction_max     0.68
_reflns_Friedel_coverage         0.935
_reflns_number_total             13037
_reflns_number_gt                12081
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0153P)²+0.5061P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.00209(8)
_refine_ls_number_reflns         13037
_refine_ls_number_parameters     384
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0372
_refine_ls_wR_factor_gt          0.0363
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_restrained_S_all      1.05
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 5346 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0022(19)
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.069

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7290(2) 0.00944(12) 1.00031(16) 0.0314(5) Uani 1 1 d . . . . .
H1A H 0.65226 -0.029962 1.014115 0.047 Uiso 1 1 calc R U . . .
H1B H 0.77726 0.032953 1.039462 0.047 Uiso 1 1 calc R U . . .
H1C H 0.805037 -0.01809 0.973208 0.047 Uiso 1 1 calc R U . . .
C3 C 0.5778(2) 0.04922(11) 0.90650(11) 0.0193(4) Uani 1 1 d . . . . .
C4 C 0.5644(3) -0.02998(12) 0.88481(13) 0.0284(5) Uani 1 1 d . . . . .
H4 H 0.614234 -0.072848 0.907532 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4771(3) -0.04654(13) 0.82923(14) 0.0322(5) Uani 1 1 d . . . . .
H5 H 0.467603 -0.100846 0.813604 0.039 Uiso 1 1 calc R U . . .
C6 C 0.4045(3) 0.01611(13) 0.79696(13) 0.0271(5) Uani 1 1 d . . . . .
H6 H 0.344065 0.004222 0.759426 0.033 Uiso 1 1 calc R U . . .
C7 C 0.4179(2) 0.09737(11) 0.81844(11) 0.0185(4) Uani 1 1 d . . . . .
C8 C 0.50664(18) 0.11471(10) 0.87420(11) 0.0165(4) Uani 1 1 d . . . . .
C9 C 0.3263(2) 0.15678(12) 0.78387(12) 0.0197(4) Uani 1 1 d . . . . .
H9 H 0.265565 0.135987 0.749067 0.024 Uiso 1 1 calc R U . . .
C10 C 0.1909(3) 0.27298(13) 0.75770(14) 0.0259(5) Uani 1 1 d . . . . .
H10A H 0.096464 0.262812 0.782389 0.031 Uiso 1 1 calc R U . . .
H10B H 0.181216 0.245768 0.71426 0.031 Uiso 1 1 calc R U . . .
C11 C 0.2046(2) 0.36484(13) 0.74584(12) 0.0226(4) Uani 1 1 d . . . . .
C12 C 0.3434(2) 0.3855(2) 0.70478(16) 0.0365(6) Uani 1 1 d . . . . .
H12A H 0.338623 0.356646 0.662457 0.055 Uiso 1 1 calc R U . . .
H12B H 0.434339 0.368885 0.728743 0.055 Uiso 1 1 calc R U . . .
H12C H 0.346609 0.444343 0.696749 0.055 Uiso 1 1 calc R U . . .
C13 C 0.0620(3) 0.38918(16) 0.70695(14) 0.0331(5) Uani 1 1 d . . . . .
H13A H 0.064385 0.447745 0.697733 0.05 Uiso 1 1 calc R U . . .
H13B H -0.027697 0.376267 0.733206 0.05 Uiso 1 1 calc R U . . .
H13C H 0.058631 0.358984 0.665203 0.05 Uiso 1 1 calc R U . . .
C14 C 0.1987(2) 0.41182(13) 0.81036(13) 0.0249(5) Uani 1 1 d . . . . .
H14A H 0.189157 0.470457 0.799849 0.03 Uiso 1 1 calc R U . . .
H14B H 0.106356 0.395455 0.834365 0.03 Uiso 1 1 calc R U . . .
C15 C 0.3698(2) 0.46506(11) 0.88689(12) 0.0194(4) Uani 1 1 d . . . . .
H15 H 0.321208 0.514407 0.87477 0.023 Uiso 1 1 calc R U . . .
C16 C 0.4826(2) 0.47096(11) 0.93951(11) 0.0182(4) Uani 1 1 d . . . . .
C17 C 0.5177(2) 0.54972(11) 0.96221(12) 0.0230(4) Uani 1 1 d . . . . .
H17 H 0.470553 0.595309 0.942035 0.028 Uiso 1 1 calc R U . . .
C18 C 0.6177(3) 0.56236(13) 1.01246(12) 0.0268(6) Uani 1 1 d . . . . .
H18 H 0.642195 0.616263 1.025699 0.032 Uiso 1 1 calc R U . . .
C19 C 0.6841(2) 0.49599(13) 1.04441(12) 0.0235(5) Uani 1 1 d . . . . .
H19 H 0.752958 0.504246 1.079729 0.028 Uiso 1 1 calc R U . . .
C20 C 0.64822(19) 0.41853(12) 1.02394(12) 0.0185(4) Uani 1 1 d . . . . .
C21 C 0.54990(19) 0.40374(11) 0.97053(11) 0.0156(4) Uani 1 1 d . . . . .
O13 O 0.82697(16) 0.25796(13) 0.91498(10) 0.0313(4) Uani 1 1 d D . . . .
H13D H 0.796(3) 0.2800(17) 0.8807(11) 0.038 Uiso 1 1 d D U . . .
H13E H 0.9203(14) 0.260(2) 0.9111(15) 0.038 Uiso 1 1 d D U . . .
C25 C 0.7994(2) 0.35821(15) 1.11018(13) 0.0293(5) Uani 1 1 d . . . . .
H25A H 0.888523 0.390559 1.098865 0.044 Uiso 1 1 calc R U . . .
H25B H 0.83107 0.304749 1.1266 0.044 Uiso 1 1 calc R U . . .
H25C H 0.741407 0.386372 1.144484 0.044 Uiso 1 1 calc R U . . .
O12 O 0.40472(19) 0.19917(17) 1.03562(12) 0.0540(7) Uani 1 1 d D . . . .
H12 H 0.327(3) 0.207(2) 1.0151(16) 0.065 Uiso 1 1 d D U . . .
H12D H 0.367(4) 0.167(2) 1.0625(16) 0.065 Uiso 1 1 d D U . . .
O14 O 0.90992(16) 0.18943(12) 1.03215(9) 0.0299(4) Uani 1 1 d D . . . .
H14D H 0.938(3) 0.1649(18) 1.0664(10) 0.036 Uiso 1 1 d D U . . .
H14E H 0.991(2) 0.1981(17) 1.0128(12) 0.036 Uiso 1 1 d D U . . .
CL2 Cl 0.65520(5) 0.33564(3) 0.80587(3) 0.02312(11) Uani 1 1 d . . . . .
N1 N 0.32890(16) 0.40130(10) 0.85535(10) 0.0184(3) Uani 1 1 d . . . . .
N2 N 0.31620(19) 0.23402(10) 0.79409(10) 0.0190(4) Uani 1 1 d . . . . .
O1 O 0.52472(15) 0.18841(8) 0.89923(7) 0.0175(3) Uani 1 1 d . . . . .
O2 O 0.52520(14) 0.32714(8) 0.95343(7) 0.0171(3) Uani 1 1 d . . . . .
O3 O 0.65902(16) 0.07329(9) 0.96226(10) 0.0238(3) Uani 1 1 d . . . . .
O4 O 0.70682(16) 0.34783(9) 1.05216(8) 0.0224(3) Uani 1 1 d . . . . .
O5 O 0.65419(16) 0.16372(13) 1.10668(9) 0.0312(4) Uani 1 1 d D . . . .
H5A H 0.701(3) 0.1679(18) 1.1433(10) 0.037 Uiso 1 1 d D U . . .
H5B H 0.577(2) 0.1375(17) 1.1209(13) 0.037 Uiso 1 1 d D U . . .
CL1 Cl 0.16914(4) 0.24234(3) 0.93437(3) 0.02099(10) Uani 1 1 d . . . . .
NI1 Ni 0.42470(3) 0.29148(2) 0.86804(2) 0.01590(5) Uani 1 1 d . . . . .
GD1 Gd 0.65445(2) 0.21640(2) 0.99671(2) 0.01559(3) Uani 1 1 d . . . . .
CL3 Cl 0.13613(5) 0.07172(3) 0.64278(3) 0.02391(11) Uani 1 1 d . . . . .
O10 O 1.01439(17) 0.09974(10) 1.13325(10) 0.0297(4) Uani 1 1 d D . . . .
H10C H 1.1080(15) 0.0945(16) 1.1378(17) 0.036 Uiso 1 1 d D U . . .
H10D H 0.985(3) 0.0511(10) 1.1332(16) 0.036 Uiso 1 1 d D U . . .
O11 O 0.8010(3) 0.17903(16) 1.21765(12) 0.0508(6) Uani 1 1 d D . . . .
H11A H 0.885(2) 0.1568(19) 1.212(2) 0.061 Uiso 1 1 d D U . . .
H11B H 0.824(4) 0.2215(16) 1.239(2) 0.061 Uiso 1 1 d D U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O3 1.442(3) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C3 C4 1.378(3) . ?
C3 O3 1.396(3) . ?
C3 C8 1.408(3) . ?
C4 C5 1.392(4) . ?
C4 H4 0.95 . ?
C5 C6 1.379(3) . ?
C5 H5 0.95 . ?
C6 C7 1.409(3) . ?
C6 H6 0.95 . ?
C7 C8 1.405(3) . ?
C7 C9 1.450(3) . ?
C8 O1 1.322(2) . ?
C9 N2 1.288(3) . ?
C9 H9 0.95 . ?
C10 N2 1.479(3) . ?
C10 C11 1.532(3) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 C14 1.517(3) . ?
C11 C12 1.524(3) . ?
C11 C13 1.543(3) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 N1 1.481(3) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 N1 1.279(3) . ?
C15 C16 1.465(3) . ?
C15 H15 0.95 . ?
C16 C21 1.404(3) . ?
C16 C17 1.408(3) . ?
C17 C18 1.366(3) . ?
C17 H17 0.95 . ?
C18 C19 1.398(3) . ?
C18 H18 0.95 . ?
C19 C20 1.375(3) . ?
C19 H19 0.95 . ?
C20 O4 1.395(3) . ?
C20 C21 1.410(3) . ?
C21 O2 1.323(2) . ?
O13 GD1 2.3548(17) . ?
O13 H13D 0.830(13) . ?
O13 H13E 0.832(13) . ?
C25 O4 1.443(3) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
O12 GD1 2.3686(18) . ?
O12 H12 0.818(13) . ?
O12 H12D 0.833(10) . ?
O14 GD1 2.4185(14) . ?
O14 H14D 0.841(13) . ?
O14 H14E 0.828(13) . ?
CL2 NI1 2.5085(6) . ?
N1 NI1 2.0104(16) . ?
N2 NI1 2.0142(19) . ?
O1 NI1 2.0130(13) . ?
O1 GD1 2.3297(14) . ?
O2 NI1 2.0307(14) . ?
O2 GD1 2.3217(13) . ?
O3 GD1 2.4520(16) . ?
O4 GD1 2.4767(15) . ?
O5 GD1 2.3876(18) . ?
O5 H5A 0.852(13) . ?
O5 H5B 0.860(13) . ?
NI1 GD1 3.5294(3) . ?
O10 H10C 0.840(13) . ?
O10 H10D 0.840(13) . ?
O11 H11A 0.838(13) . ?
O11 H11B 0.841(13) . ?

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 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C3 O3 124.70(18) . . ?
C4 C3 C8 122.3(2) . . ?
O3 C3 C8 112.98(17) . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 119.8(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 121.4(2) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 119.16(18) . . ?
C8 C7 C9 124.42(18) . . ?
C6 C7 C9 116.17(19) . . ?
O1 C8 C3 117.84(18) . . ?
O1 C8 C7 124.15(16) . . ?
C3 C8 C7 117.98(17) . . ?
N2 C9 C7 128.6(2) . . ?
N2 C9 H9 115.7 . . ?
C7 C9 H9 115.7 . . ?
N2 C10 C11 116.38(17) . . ?
N2 C10 H10A 108.2 . . ?
C11 C10 H10A 108.2 . . ?
N2 C10 H10B 108.2 . . ?
C11 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
C14 C11 C12 112.6(2) . . ?
C14 C11 C10 111.3(2) . . ?
C12 C11 C10 111.6(2) . . ?
C14 C11 C13 106.20(18) . . ?
C12 C11 C13 109.1(2) . . ?
C10 C11 C13 105.66(18) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 C11 116.29(16) . . ?
N1 C14 H14A 108.2 . . ?
C11 C14 H14A 108.2 . . ?
N1 C14 H14B 108.2 . . ?
C11 C14 H14B 108.2 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 C16 127.65(17) . . ?
N1 C15 H15 116.2 . . ?
C16 C15 H15 116.2 . . ?
C21 C16 C17 118.9(2) . . ?
C21 C16 C15 124.33(17) . . ?
C17 C16 C15 116.71(17) . . ?
C18 C17 C16 121.78(19) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 119.98(19) . . ?
C17 C18 H18 120 . . ?
C19 C18 H18 120 . . ?
C20 C19 C18 119.0(2) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C19 C20 O4 124.1(2) . . ?
C19 C20 C21 122.2(2) . . ?
O4 C20 C21 113.65(17) . . ?
O2 C21 C16 124.09(18) . . ?
O2 C21 C20 117.83(17) . . ?
C16 C21 C20 118.07(17) . . ?
GD1 O13 H13D 120(2) . . ?
GD1 O13 H13E 136(2) . . ?
H13D O13 H13E 103.7(19) . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
GD1 O12 H12 127(3) . . ?
GD1 O12 H12D 132(2) . . ?
H12 O12 H12D 95.0(13) . . ?
GD1 O14 H14D 127.9(19) . . ?
GD1 O14 H14E 129.7(19) . . ?
H14D O14 H14E 102.2(18) . . ?
C15 N1 C14 115.62(16) . . ?
C15 N1 NI1 123.43(14) . . ?
C14 N1 NI1 120.87(14) . . ?
C9 N2 C10 113.46(18) . . ?
C9 N2 NI1 123.19(15) . . ?
C10 N2 NI1 121.77(14) . . ?
C8 O1 NI1 126.61(12) . . ?
C8 O1 GD1 124.42(12) . . ?
NI1 O1 GD1 108.50(6) . . ?
C21 O2 NI1 124.72(13) . . ?
C21 O2 GD1 124.36(12) . . ?
NI1 O2 GD1 108.18(6) . . ?
C3 O3 C1 116.62(18) . . ?
C3 O3 GD1 119.52(11) . . ?
C1 O3 GD1 123.55(16) . . ?
C20 O4 C25 116.56(17) . . ?
C20 O4 GD1 118.04(12) . . ?
C25 O4 GD1 125.34(13) . . ?
GD1 O5 H5A 141.3(18) . . ?
GD1 O5 H5B 119.6(18) . . ?
H5A O5 H5B 98.0(17) . . ?
N1 NI1 N2 97.08(7) . . ?
N1 NI1 O1 168.81(7) . . ?
N2 NI1 O1 92.85(6) . . ?
N1 NI1 O2 92.05(7) . . ?
N2 NI1 O2 167.74(6) . . ?
O1 NI1 O2 77.41(6) . . ?
N1 NI1 CL2 91.22(5) . . ?
N2 NI1 CL2 98.77(6) . . ?
O1 NI1 CL2 92.34(4) . . ?
O2 NI1 CL2 89.16(4) . . ?
N1 NI1 GD1 130.69(6) . . ?
N2 NI1 GD1 131.34(5) . . ?
O1 NI1 GD1 38.75(4) . . ?
O2 NI1 GD1 38.68(4) . . ?
CL2 NI1 GD1 90.004(14) . . ?
O2 GD1 O1 65.86(5) . . ?
O2 GD1 O13 80.16(6) . . ?
O1 GD1 O13 77.51(6) . . ?
O2 GD1 O12 75.93(6) . . ?
O1 GD1 O12 78.20(7) . . ?
O13 GD1 O12 151.20(6) . . ?
O2 GD1 O5 129.42(6) . . ?
O1 GD1 O5 135.82(5) . . ?
O13 GD1 O5 139.49(5) . . ?
O12 GD1 O5 69.27(6) . . ?
O2 GD1 O14 135.92(5) . . ?
O1 GD1 O14 132.69(6) . . ?
O13 GD1 O14 69.64(6) . . ?
O12 GD1 O14 139.15(7) . . ?
O5 GD1 O14 70.01(5) . . ?
O2 GD1 O3 130.68(5) . . ?
O1 GD1 O3 65.05(5) . . ?
O13 GD1 O3 93.86(7) . . ?
O12 GD1 O3 89.74(8) . . ?
O5 GD1 O3 85.27(7) . . ?
O14 GD1 O3 83.87(6) . . ?
O2 GD1 O4 65.22(5) . . ?
O1 GD1 O4 130.42(5) . . ?
O13 GD1 O4 86.77(7) . . ?
O12 GD1 O4 97.42(8) . . ?
O5 GD1 O4 83.90(6) . . ?
O14 GD1 O4 81.34(6) . . ?
O3 GD1 O4 163.97(5) . . ?
O2 GD1 NI1 33.14(3) . . ?
O1 GD1 NI1 32.74(3) . . ?
O13 GD1 NI1 75.88(4) . . ?
O12 GD1 NI1 75.32(5) . . ?
O5 GD1 NI1 144.45(4) . . ?
O14 GD1 NI1 145.50(4) . . ?
O3 GD1 NI1 97.74(4) . . ?
O4 GD1 NI1 97.94(4) . . ?
H10C O10 H10D 102.1(17) . . ?
H11A O11 H11B 102.0(19) . . ?
