# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_try1_b_pl
_database_code_depnum_ccdc_archive 'CCDC 1993768'
loop_
_audit_author_name
_audit_author_address
'Justin M. Burroughs'
;University of Tennessee, Knoxville 
United States of America
;
_audit_update_record             
;
2020-03-30 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35.46 H50.41 Fe N2 O3.98 Ti'
_chemical_formula_sum            'C70.98 H100.97 Fe2 N4 O7.98 Ti2'
_chemical_formula_weight         1345.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   22.6283(13)
_cell_length_b                   8.7736(5)
_cell_length_c                   18.5643(10)
_cell_angle_alpha                90
_cell_angle_beta                 105.170(2)
_cell_angle_gamma                90
_cell_volume                     3557.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      31.49

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_F_000             1429
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.828
_exptl_crystal_size_mid          0.488
_exptl_crystal_size_min          0.304
_exptl_absorpt_coefficient_mu    0.670
_shelx_estimated_absorpt_T_min   0.607
_shelx_estimated_absorpt_T_max   0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            44451
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.220
_diffrn_reflns_theta_max         31.517
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11829
_reflns_number_gt                10017
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Apex3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0754P)²+2.4803P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11829
_refine_ls_number_parameters     506
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1468
_refine_ls_wR_factor_gt          0.1381
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001

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
O4'_2 O -0.1341(3) 0.2358(8) -0.1081(4) 0.0257(14) Uani 0.257(11) 1 d . U P A 2
C34'_2 C -0.0875(6) 0.223(4) -0.0472(7) 0.083(6) Uani 0.257(11) 1 d . U P A 2
H34'_2 H -0.089460 0.334572 -0.037940 0.099 Uiso 0.257(11) 1 calc R U P A 2
C36'_2 C -0.1044(6) 0.1907(19) 0.0234(7) 0.042(3) Uani 0.257(11) 1 d . U P A 2
H36A_2 H -0.134344 0.266202 0.030270 0.063 Uiso 0.257(11) 1 calc R U P A 2
H36B_2 H -0.067692 0.196347 0.065419 0.063 Uiso 0.257(11) 1 calc R U P A 2
H36C_2 H -0.122182 0.088431 0.021191 0.063 Uiso 0.257(11) 1 calc R U P A 2
C35'_2 C -0.0252(10) 0.236(4) -0.0445(16) 0.075(9) Uani 0.257(11) 1 d . U P A 2
H35A_2 H -0.016876 0.182674 -0.087154 0.113 Uiso 0.257(11) 1 calc R U P A 2
H35B_2 H -0.000496 0.191014 0.002001 0.113 Uiso 0.257(11) 1 calc R U P A 2
H35C_2 H -0.014549 0.344083 -0.046353 0.113 Uiso 0.257(11) 1 calc R U P A 2
Fe1 Fe -0.52811(2) 0.27813(3) 0.12549(2) 0.03290(8) Uani 1 1 d . . . . .
Ti1 Ti -0.18379(2) 0.38742(4) -0.18640(2) 0.03032(8) Uani 1 1 d . . . . .
O1 O -0.20598(5) 0.48788(14) -0.10413(7) 0.0290(2) Uani 1 1 d . . . . .
N1 N -0.25127(7) 0.21716(16) -0.17011(8) 0.0312(3) Uani 1 1 d . . . . .
C1 C -0.52264(10) 0.1433(2) 0.03908(11) 0.0415(4) Uani 1 1 d . . . . .
H1 H -0.489737 0.146535 0.012138 0.050 Uiso 1 1 calc R U . . .
O2 O -0.25004(7) 0.46894(16) -0.25627(8) 0.0408(3) Uani 1 1 d . . . . .
N2 N -0.18292(9) 0.2062(2) -0.27503(11) 0.0425(4) Uani 1 1 d . . . . .
C2 C -0.57802(10) 0.2262(2) 0.01999(13) 0.0441(4) Uani 1 1 d . . . . .
H2 H -0.590798 0.299720 -0.022402 0.053 Uiso 1 1 calc R U . . .
C3 C -0.61173(10) 0.1907(3) 0.07252(14) 0.0485(5) Uani 1 1 d . . . . .
H3 H -0.652339 0.234466 0.073420 0.058 Uiso 1 1 calc R U . . .
C4 C -0.57718(10) 0.0829(3) 0.12411(14) 0.0473(5) Uani 1 1 d . . . . .
H4 H -0.589278 0.037289 0.167513 0.057 Uiso 1 1 calc R U . . .
C5 C -0.52226(10) 0.0524(2) 0.10294(13) 0.0430(4) Uani 1 1 d . . . . .
H5 H -0.488874 -0.018591 0.128913 0.052 Uiso 1 1 calc R U . . .
C6 C -0.51124(9) 0.5059(2) 0.12752(14) 0.0442(5) Uani 1 1 d . . . . .
H6 H -0.525466 0.578983 0.085181 0.053 Uiso 1 1 calc R U . . .
C7 C -0.54302(12) 0.4657(3) 0.18172(17) 0.0605(7) Uani 1 1 d . . . . .
H7 H -0.584083 0.505233 0.183380 0.073 Uiso 1 1 calc R U . . .
C8 C -0.50795(12) 0.3564(4) 0.23147(13) 0.0573(7) Uani 1 1 d . . . . .
H8 H -0.519897 0.307195 0.274154 0.069 Uiso 1 1 calc R U . . .
C9 C -0.45311(10) 0.3278(3) 0.20957(11) 0.0448(5) Uani 1 1 d . . . . .
H9 H -0.419778 0.255312 0.234026 0.054 Uiso 1 1 calc R U . . .
C10 C -0.45479(8) 0.4215(2) 0.14540(10) 0.0355(4) Uani 1 1 d . . . . .
C11 C -0.40957(7) 0.4255(2) 0.10427(10) 0.0320(3) Uani 1 1 d . . . . .
C12 C -0.37204(7) 0.4298(2) 0.06890(10) 0.0312(3) Uani 1 1 d . . . . .
C13 C -0.32834(7) 0.4391(2) 0.02536(9) 0.0285(3) Uani 1 1 d . . . . .
C14 C -0.28670(7) 0.5623(2) 0.03561(10) 0.0303(3) Uani 1 1 d . . . . .
H14 H -0.287855 0.636093 0.072645 0.036 Uiso 1 1 calc R U . . .
C15 C -0.24429(7) 0.5807(2) -0.00563(10) 0.0293(3) Uani 1 1 d . . . . .
C16 C -0.24366(6) 0.47099(18) -0.06220(9) 0.0253(3) Uani 1 1 d . . . . .
C17 C -0.28433(6) 0.34391(18) -0.07144(8) 0.0246(3) Uani 1 1 d . . . . .
C18 C -0.32595(6) 0.33078(19) -0.02763(9) 0.0267(3) Uani 1 1 d . . . . .
H18 H -0.352948 0.245951 -0.034522 0.032 Uiso 1 1 calc R U . . .
C19 C -0.19918(8) 0.7146(2) 0.00875(12) 0.0396(4) Uani 1 1 d . . . . .
C20 C -0.20847(12) 0.8186(3) 0.07140(18) 0.0636(8) Uani 1 1 d . . . . .
H20A H -0.179780 0.904294 0.078021 0.095 Uiso 1 1 calc R U . . .
H20B H -0.201006 0.760426 0.117991 0.095 Uiso 1 1 calc R U . . .
H20C H -0.250549 0.857346 0.058188 0.095 Uiso 1 1 calc R U . . .
C21 C -0.20742(10) 0.8134(2) -0.06139(15) 0.0485(5) Uani 1 1 d . . . . .
H21A H -0.199322 0.751916 -0.101828 0.073 Uiso 1 1 calc R U . . .
H21B H -0.178741 0.899252 -0.050582 0.073 Uiso 1 1 calc R U . . .
H21C H -0.249479 0.852208 -0.076560 0.073 Uiso 1 1 calc R U . . .
C22 C -0.13312(8) 0.6529(3) 0.03282(13) 0.0455(5) Uani 1 1 d . . . . .
H22A H -0.126070 0.584732 -0.005922 0.068 Uiso 1 1 calc R U . . .
H22B H -0.127121 0.596512 0.079759 0.068 Uiso 1 1 calc R U . . .
H22C H -0.104201 0.738166 0.039927 0.068 Uiso 1 1 calc R U . . .
C23 C -0.28531(7) 0.22416(18) -0.12503(9) 0.0274(3) Uani 1 1 d . . . . .
H23 H -0.313709 0.143540 -0.126979 0.033 Uiso 1 1 calc R U . . .
C26 C -0.19710(14) 0.2692(4) -0.34952(14) 0.0652(8) Uani 1 1 d . . . . .
H26A H -0.196000 0.187990 -0.385395 0.098 Uiso 1 1 calc R U . . .
H26B H -0.166871 0.347523 -0.352178 0.098 Uiso 1 1 calc R U . . .
H26C H -0.238054 0.314793 -0.361496 0.098 Uiso 1 1 calc R U . . .
C27 C -0.12296(19) 0.1312(5) -0.26166(16) 0.0906(14) Uani 1 1 d . . . . .
H27A H -0.123134 0.061311 -0.302914 0.136 Uiso 1 1 calc R U . . .
H27B H -0.114696 0.073760 -0.214794 0.136 Uiso 1 1 calc R U . . .
H27C H -0.091064 0.208359 -0.258361 0.136 Uiso 1 1 calc R U . . .
O3 O -0.13553(12) 0.5271(4) -0.22272(15) 0.0234(6) Uani 0.490(3) 1 d . U P A 1
C25 C -0.2076(2) 0.0617(5) -0.2475(2) 0.0417(11) Uani 0.486(6) 1 d . . P B 1
H25A H -0.213645 -0.019342 -0.285892 0.050 Uiso 0.486(6) 1 calc R U P B 1
H25B H -0.178649 0.024063 -0.201323 0.050 Uiso 0.486(6) 1 calc R U P B 1
C24 C -0.2679(3) 0.1041(7) -0.2326(4) 0.0388(12) Uani 0.486(6) 1 d . U P B 1
H24A H -0.295868 0.150176 -0.277388 0.047 Uiso 0.486(6) 1 calc R U P B 1
H24B H -0.287970 0.013498 -0.217669 0.047 Uiso 0.486(6) 1 calc R U P B 1
C31 C -0.07068(14) 0.5565(5) -0.1975(2) 0.0398(9) Uani 0.510(3) 1 d . U P A 1
H31 H -0.053940 0.472238 -0.161757 0.048 Uiso 0.510(3) 1 calc R U P A 1
C32 C -0.0574(6) 0.6961(17) -0.1533(8) 0.105(5) Uani 0.510(3) 1 d . U P A 1
H32A H -0.076905 0.782914 -0.183525 0.157 Uiso 0.510(3) 1 calc R U P A 1
H32B H -0.013040 0.712139 -0.137319 0.157 Uiso 0.510(3) 1 calc R U P A 1
H32C H -0.073433 0.686863 -0.109247 0.157 Uiso 0.510(3) 1 calc R U P A 1
C33 C -0.0425(4) 0.5356(16) -0.2589(8) 0.130(6) Uani 0.510(3) 1 d . U P A 1
H33A H -0.044506 0.427777 -0.273030 0.195 Uiso 0.510(3) 1 calc R U P A 1
H33B H 0.000354 0.568206 -0.243185 0.195 Uiso 0.510(3) 1 calc R U P A 1
H33C H -0.064480 0.596816 -0.301692 0.195 Uiso 0.510(3) 1 calc R U P A 1
C34 C -0.09433(16) 0.1796(3) -0.0704(3) 0.0334(8) Uani 0.725(12) 1 d . U P A 1
H34 H -0.106392 0.073351 -0.087572 0.040 Uiso 0.725(12) 1 calc R U P A 1
C35 C -0.0266(4) 0.1943(11) -0.0580(5) 0.0560(19) Uani 0.725(12) 1 d . U P A 1
H35A H -0.016009 0.181230 -0.105537 0.084 Uiso 0.725(12) 1 calc R U P A 1
H35B H -0.005913 0.115836 -0.022724 0.084 Uiso 0.725(12) 1 calc R U P A 1
H35C H -0.013401 0.295371 -0.037534 0.084 Uiso 0.725(12) 1 calc R U P A 1
C36 C -0.1151(2) 0.2090(6) -0.0007(3) 0.0411(9) Uani 0.725(12) 1 d . U P A 1
H36A H -0.104413 0.313519 0.016531 0.062 Uiso 0.725(12) 1 calc R U P A 1
H36B H -0.094800 0.137120 0.038394 0.062 Uiso 0.725(12) 1 calc R U P A 1
H36C H -0.159561 0.195528 -0.011671 0.062 Uiso 0.725(12) 1 calc R U P A 1
O4 O -0.12333(10) 0.2811(4) -0.12787(18) 0.0326(7) Uani 0.743(11) 1 d . U P A 1
C24' C -0.2502(3) 0.0734(6) -0.2105(3) 0.0322(9) Uani 0.514(6) 1 d . U P B 2
H24C H -0.288752 0.016222 -0.215300 0.039 Uiso 0.514(6) 1 calc R U P B 2
H24D H -0.215511 0.008981 -0.183568 0.039 Uiso 0.514(6) 1 calc R U P B 2
C28 C -0.31174(11) 0.5143(3) -0.27075(12) 0.0468(5) Uani 1 1 d . . . C 2
H28 H -0.332114 0.452337 -0.238907 0.056 Uiso 1 1 calc R U . C 2
C29 C -0.31494(17) 0.6810(4) -0.25079(18) 0.0556(8) Uani 0.756 1 d . . P C 2
H29A H -0.291144 0.741705 -0.277537 0.083 Uiso 0.756 1 calc R U P C 2
H29B H -0.298037 0.694210 -0.196900 0.083 Uiso 0.756 1 calc R U P C 2
H29C H -0.357700 0.714776 -0.265024 0.083 Uiso 0.756 1 calc R U P C 2
C30 C -0.34467(11) 0.4877(3) -0.35186(14) 0.0371(5) Uani 0.756 1 d . . P C 2
H30A H -0.324791 0.546979 -0.383653 0.056 Uiso 0.756 1 calc R U P C 2
H30B H -0.387472 0.519730 -0.360894 0.056 Uiso 0.756 1 calc R U P C 2
H30C H -0.343064 0.379075 -0.363553 0.056 Uiso 0.756 1 calc R U P C 2
C25' C -0.24301(16) 0.1166(4) -0.28688(17) 0.0289(8) Uani 0.514(6) 1 d . . P B
2
H25C H -0.278002 0.180068 -0.313815 0.035 Uiso 0.514(6) 1 calc R U P B 2
H25D H -0.241680 0.023798 -0.316772 0.035 Uiso 0.514(6) 1 calc R U P B 2
O3'_1 O -0.11916(18) 0.4959(5) -0.1949(2) 0.0480(10) Uani 0.490(3) 1 d . U P A
2
C31'_1 C -0.1017(3) 0.6209(8) -0.2217(3) 0.0633(16) Uani 0.490(3) 1 d . U P A 2
H31'_1 H -0.139816 0.670576 -0.252406 0.076 Uiso 0.490(3) 1 calc R U P A 2
C32'_1 C -0.0704(5) 0.7344(10) -0.1692(8) 0.063(3) Uani 0.490(3) 1 d . U P A 2
H32A_1 H -0.063098 0.825266 -0.196377 0.095 Uiso 0.490(3) 1 calc R U P A 2
H32B_1 H -0.031219 0.693320 -0.139989 0.095 Uiso 0.490(3) 1 calc R U P A 2
H32C_1 H -0.095753 0.761818 -0.135686 0.095 Uiso 0.490(3) 1 calc R U P A 2
C33'_1 C -0.0597(4) 0.5935(11) -0.2753(3) 0.062(2) Uani 0.490(3) 1 d . U P A 2
H33A_1 H -0.077421 0.512948 -0.311018 0.093 Uiso 0.490(3) 1 calc R U P A 2
H33B_1 H -0.018885 0.562492 -0.246079 0.093 Uiso 0.490(3) 1 calc R U P A 2
H33C_1 H -0.056611 0.687787 -0.302328 0.093 Uiso 0.490(3) 1 calc R U P A 2


_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
O4'_2 C34'_2 1.332(12) . ?
O4'_2 Ti1 2.072(6) . ?
C34'_2 C35'_2 1.40(2) . ?
C34'_2 C36'_2 1.485(17) . ?
C34'_2 H34'_2 1.0000 . ?
C36'_2 H36A_2 0.9800 . ?
C36'_2 H36B_2 0.9800 . ?
C36'_2 H36C_2 0.9800 . ?
C35'_2 H35A_2 0.9800 . ?
C35'_2 H35B_2 0.9800 . ?
C35'_2 H35C_2 0.9800 . ?
Fe1 C8 2.020(2) . ?
Fe1 C1 2.023(2) . ?
Fe1 C7 2.024(2) . ?
Fe1 C9 2.030(2) . ?
Fe1 C6 2.033(2) . ?
Fe1 C5 2.036(2) . ?
Fe1 C10 2.0369(18) . ?
Fe1 C4 2.038(2) . ?
Fe1 C2 2.040(2) . ?
Fe1 C3 2.040(2) . ?
Ti1 O4 1.773(3) . ?
Ti1 O3'_1 1.786(3) . ?
Ti1 O2 1.8503(15) . ?
Ti1 O3 1.880(3) . ?
Ti1 O1 1.9398(12) . ?
Ti1 N1 2.2126(14) . ?
Ti1 N2 2.2922(17) . ?
O1 C16 1.3045(17) . ?
N1 C23 1.279(2) . ?
N1 C24' 1.470(5) . ?
N1 C24 1.497(6) . ?
C1 C2 1.412(3) . ?
C1 C5 1.427(3) . ?
C1 H1 1.0000 . ?
O2 C28 1.408(3) . ?
N2 C26 1.445(3) . ?
N2 C27 1.469(3) . ?
N2 C25 1.527(5) . ?
N2 C25' 1.536(4) . ?
C2 C3 1.421(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.425(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.424(3) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
C6 C7 1.426(3) . ?
C6 C10 1.438(3) . ?
C6 H6 1.0000 . ?
C7 C8 1.420(4) . ?
C7 H7 1.0000 . ?
C8 C9 1.426(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.440(3) . ?
C9 H9 1.0000 . ?
C10 C11 1.429(2) . ?
C11 C12 1.202(2) . ?
C12 C13 1.434(2) . ?
C13 C18 1.379(2) . ?
C13 C14 1.413(2) . ?
C14 C15 1.385(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.427(2) . ?
C15 C19 1.534(2) . ?
C16 C17 1.427(2) . ?
C17 C18 1.401(2) . ?
C17 C23 1.443(2) . ?
C18 H18 0.9500 . ?
C19 C21 1.534(3) . ?
C19 C20 1.535(3) . ?
C19 C22 1.542(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O3 C31 1.442(4) . ?
C25 C24 1.508(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C31 C33 1.454(12) . ?
C31 C32 1.462(14) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 O4 1.413(4) . ?
C34 C35 1.495(9) . ?
C34 C36 1.510(5) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C24' C25' 1.517(6) . ?
C24' H24C 0.9900 . ?
C24' H24D 0.9900 . ?
C28 C30 1.513(4) . ?
C28 C29 1.515(4) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C25' H25C 0.9900 . ?
C25' H25D 0.9900 . ?
O3'_1 C31'_1 1.307(7) . ?
C31'_1 C32'_1 1.443(13) . ?
C31'_1 C33'_1 1.563(8) . ?
C31'_1 H31'_1 1.0000 . ?
C32'_1 H32A_1 0.9800 . ?
C32'_1 H32B_1 0.9800 . ?
C32'_1 H32C_1 0.9800 . ?
C33'_1 H33A_1 0.9800 . ?
C33'_1 H33B_1 0.9800 . ?
C33'_1 H33C_1 0.9800 . ?

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
C34'_2 O4'_2 Ti1 144.5(16) . . ?
O4'_2 C34'_2 C35'_2 126.0(16) . . ?
O4'_2 C34'_2 C36'_2 115.9(11) . . ?
C35'_2 C34'_2 C36'_2 118.1(14) . . ?
O4'_2 C34'_2 H34'_2 90.0 . . ?
C35'_2 C34'_2 H34'_2 90.0 . . ?
C36'_2 C34'_2 H34'_2 90.0 . . ?
C34'_2 C36'_2 H36A_2 109.5 . . ?
C34'_2 C36'_2 H36B_2 109.5 . . ?
H36A_2 C36'_2 H36B_2 109.5 . . ?
C34'_2 C36'_2 H36C_2 109.5 . . ?
H36A_2 C36'_2 H36C_2 109.5 . . ?
H36B_2 C36'_2 H36C_2 109.5 . . ?
C34'_2 C35'_2 H35A_2 109.5 . . ?
C34'_2 C35'_2 H35B_2 109.5 . . ?
H35A_2 C35'_2 H35B_2 109.5 . . ?
C34'_2 C35'_2 H35C_2 109.5 . . ?
H35A_2 C35'_2 H35C_2 109.5 . . ?
H35B_2 C35'_2 H35C_2 109.5 . . ?
C8 Fe1 C1 157.83(11) . . ?
C8 Fe1 C7 41.12(13) . . ?
C1 Fe1 C7 159.66(11) . . ?
C8 Fe1 C9 41.22(9) . . ?
C1 Fe1 C9 121.53(9) . . ?
C7 Fe1 C9 69.36(11) . . ?
C8 Fe1 C6 69.77(11) . . ?
C1 Fe1 C6 122.64(9) . . ?
C7 Fe1 C6 41.16(9) . . ?
C9 Fe1 C6 70.11(10) . . ?
C8 Fe1 C5 121.39(11) . . ?
C1 Fe1 C5 41.17(8) . . ?
C7 Fe1 C5 157.77(10) . . ?
C9 Fe1 C5 106.30(10) . . ?
C6 Fe1 C5 159.74(8) . . ?
C8 Fe1 C10 69.37(8) . . ?
C1 Fe1 C10 106.80(8) . . ?
C7 Fe1 C10 69.04(8) . . ?
C9 Fe1 C10 41.46(8) . . ?
C6 Fe1 C10 41.39(8) . . ?
C5 Fe1 C10 122.97(8) . . ?
C8 Fe1 C4 106.35(11) . . ?
C1 Fe1 C4 69.19(10) . . ?
C7 Fe1 C4 121.73(10) . . ?
C9 Fe1 C4 122.23(10) . . ?
C6 Fe1 C4 157.74(9) . . ?
C5 Fe1 C4 40.91(9) . . ?
C10 Fe1 C4 159.47(9) . . ?
C8 Fe1 C2 159.75(10) . . ?
C1 Fe1 C2 40.66(9) . . ?
C7 Fe1 C2 123.49(12) . . ?
C9 Fe1 C2 158.08(9) . . ?
C6 Fe1 C2 106.95(10) . . ?
C5 Fe1 C2 68.57(9) . . ?
C10 Fe1 C2 122.15(8) . . ?
C4 Fe1 C2 68.72(9) . . ?
C8 Fe1 C3 122.81(10) . . ?
C1 Fe1 C3 68.86(10) . . ?
C7 Fe1 C3 107.18(11) . . ?
C9 Fe1 C3 159.19(9) . . ?
C6 Fe1 C3 121.62(10) . . ?
C5 Fe1 C3 68.73(10) . . ?
C10 Fe1 C3 158.15(9) . . ?
C4 Fe1 C3 40.91(9) . . ?
C2 Fe1 C3 40.76(10) . . ?
O4 Ti1 O2 170.59(9) . . ?
O3'_1 Ti1 O2 105.30(17) . . ?
O4 Ti1 O3 97.77(16) . . ?
O2 Ti1 O3 86.36(9) . . ?
O4 Ti1 O1 94.23(9) . . ?
O3'_1 Ti1 O1 102.35(13) . . ?
O2 Ti1 O1 92.71(6) . . ?
O3 Ti1 O1 106.29(11) . . ?
O3'_1 Ti1 O4'_2 95.6(3) . . ?
O2 Ti1 O4'_2 158.7(2) . . ?
O1 Ti1 O4'_2 86.79(17) . . ?
O4 Ti1 N1 90.61(15) . . ?
O3'_1 Ti1 N1 169.13(17) . . ?
O2 Ti1 N1 84.00(6) . . ?
O3 Ti1 N1 167.28(9) . . ?
O1 Ti1 N1 82.48(5) . . ?
O4'_2 Ti1 N1 74.8(3) . . ?
O4 Ti1 N2 85.68(8) . . ?
O3'_1 Ti1 N2 98.35(13) . . ?
O2 Ti1 N2 85.55(7) . . ?
O3 Ti1 N2 94.58(11) . . ?
O1 Ti1 N2 158.92(6) . . ?
O4'_2 Ti1 N2 87.33(16) . . ?
N1 Ti1 N2 76.44(6) . . ?
C16 O1 Ti1 139.67(10) . . ?
C23 N1 C24' 117.9(2) . . ?
C23 N1 C24 117.8(3) . . ?
C23 N1 Ti1 127.76(11) . . ?
C24' N1 Ti1 113.9(2) . . ?
C24 N1 Ti1 112.6(3) . . ?
C2 C1 C5 107.97(19) . . ?
C2 C1 Fe1 70.32(12) . . ?
C5 C1 Fe1 69.90(12) . . ?
C2 C1 H1 126.0 . . ?
C5 C1 H1 126.0 . . ?
Fe1 C1 H1 126.0 . . ?
C28 O2 Ti1 145.46(12) . . ?
C26 N2 C27 107.3(2) . . ?
C26 N2 C25 129.0(3) . . ?
C27 N2 C25 88.5(3) . . ?
C26 N2 C25' 95.3(2) . . ?
C27 N2 C25' 122.6(3) . . ?
C26 N2 Ti1 112.33(15) . . ?
C27 N2 Ti1 111.75(17) . . ?
C25 N2 Ti1 105.27(18) . . ?
C25' N2 Ti1 106.51(14) . . ?
C1 C2 C3 108.4(2) . . ?
C1 C2 Fe1 69.02(12) . . ?
C3 C2 Fe1 69.62(13) . . ?
C1 C2 H2 125.8 . . ?
C3 C2 H2 125.8 . . ?
Fe1 C2 H2 125.8 . . ?
C2 C3 C4 107.9(2) . . ?
C2 C3 Fe1 69.62(12) . . ?
C4 C3 Fe1 69.45(12) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
Fe1 C3 H3 126.0 . . ?
C5 C4 C3 107.7(2) . . ?
C5 C4 Fe1 69.48(12) . . ?
C3 C4 Fe1 69.64(13) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
Fe1 C4 H4 126.1 . . ?
C4 C5 C1 107.94(19) . . ?
C4 C5 Fe1 69.60(13) . . ?
C1 C5 Fe1 68.93(12) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Fe1 C5 H5 126.0 . . ?
C7 C6 C10 106.9(2) . . ?
C7 C6 Fe1 69.06(13) . . ?
C10 C6 Fe1 69.45(12) . . ?
C7 C6 H6 126.5 . . ?
C10 C6 H6 126.5 . . ?
Fe1 C6 H6 126.5 . . ?
C8 C7 C6 109.07(19) . . ?
C8 C7 Fe1 69.31(13) . . ?
C6 C7 Fe1 69.78(12) . . ?
C8 C7 H7 125.4 . . ?
C6 C7 H7 125.4 . . ?
Fe1 C7 H7 125.4 . . ?
C7 C8 C9 108.3(2) . . ?
C7 C8 Fe1 69.57(14) . . ?
C9 C8 Fe1 69.75(11) . . ?
C7 C8 H8 125.9 . . ?
C9 C8 H8 125.9 . . ?
Fe1 C8 H8 125.9 . . ?
C8 C9 C10 107.4(2) . . ?
C8 C9 Fe1 69.03(13) . . ?
C10 C9 Fe1 69.54(11) . . ?
C8 C9 H9 126.3 . . ?
C10 C9 H9 126.3 . . ?
Fe1 C9 H9 126.3 . . ?
C11 C10 C6 125.53(19) . . ?
C11 C10 C9 126.07(18) . . ?
C6 C10 C9 108.34(17) . . ?
C11 C10 Fe1 125.56(13) . . ?
C6 C10 Fe1 69.16(11) . . ?
C9 C10 Fe1 69.00(11) . . ?
C12 C11 C10 179.1(2) . . ?
C11 C12 C13 178.1(2) . . ?
C18 C13 C14 118.28(14) . . ?
C18 C13 C12 121.59(15) . . ?
C14 C13 C12 120.12(15) . . ?
C15 C14 C13 123.29(15) . . ?
C15 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
C14 C15 C16 118.03(14) . . ?
C14 C15 C19 121.29(15) . . ?
C16 C15 C19 120.69(14) . . ?
O1 C16 C17 121.24(14) . . ?
O1 C16 C15 119.76(13) . . ?
C17 C16 C15 119.01(13) . . ?
C18 C17 C16 120.31(14) . . ?
C18 C17 C23 116.68(13) . . ?
C16 C17 C23 123.01(13) . . ?
C13 C18 C17 121.00(14) . . ?
C13 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C15 C19 C21 110.95(17) . . ?
C15 C19 C20 111.72(15) . . ?
C21 C19 C20 107.3(2) . . ?
C15 C19 C22 109.38(16) . . ?
C21 C19 C22 109.75(16) . . ?
C20 C19 C22 107.68(19) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 C17 125.66(14) . . ?
N1 C23 H23 117.2 . . ?
C17 C23 H23 117.2 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C31 O3 Ti1 129.6(2) . . ?
C24 C25 N2 106.5(4) . . ?
C24 C25 H25A 110.4 . . ?
N2 C25 H25A 110.4 . . ?
C24 C25 H25B 110.4 . . ?
N2 C25 H25B 110.4 . . ?
H25A C25 H25B 108.6 . . ?
N1 C24 C25 104.5(4) . . ?
N1 C24 H24A 110.9 . . ?
C25 C24 H24A 110.9 . . ?
N1 C24 H24B 110.9 . . ?
C25 C24 H24B 110.9 . . ?
H24A C24 H24B 108.9 . . ?
O3 C31 C33 109.9(5) . . ?
O3 C31 C32 111.9(6) . . ?
C33 C31 C32 118.6(7) . . ?
O3 C31 H31 105.0 . . ?
C33 C31 H31 105.0 . . ?
C32 C31 H31 105.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O4 C34 C35 108.5(4) . . ?
O4 C34 C36 110.6(3) . . ?
C35 C34 C36 112.9(4) . . ?
O4 C34 H34 108.2 . . ?
C35 C34 H34 108.2 . . ?
C36 C34 H34 108.2 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 O4 Ti1 157.8(3) . . ?
N1 C24' C25' 106.4(3) . . ?
N1 C24' H24C 110.4 . . ?
C25' C24' H24C 110.4 . . ?
N1 C24' H24D 110.4 . . ?
C25' C24' H24D 110.4 . . ?
H24C C24' H24D 108.6 . . ?
O2 C28 C30 110.59(17) . . ?
O2 C28 C29 109.5(2) . . ?
C30 C28 C29 110.5(2) . . ?
O2 C28 H28 108.7 . . ?
C30 C28 H28 108.7 . . ?
C29 C28 H28 108.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24' C25' N2 107.5(3) . . ?
C24' C25' H25C 110.2 . . ?
N2 C25' H25C 110.2 . . ?
C24' C25' H25D 110.2 . . ?
N2 C25' H25D 110.2 . . ?
H25C C25' H25D 108.5 . . ?
C31'_1 O3'_1 Ti1 144.7(5) . . ?
O3'_1 C31'_1 C32'_1 117.7(7) . . ?
O3'_1 C31'_1 C33'_1 114.0(6) . . ?
C32'_1 C31'_1 C33'_1 105.3(7) . . ?
O3'_1 C31'_1 H31'_1 106.3 . . ?
C32'_1 C31'_1 H31'_1 106.3 . . ?
C33'_1 C31'_1 H31'_1 106.3 . . ?
C31'_1 C32'_1 H32A_1 109.5 . . ?
C31'_1 C32'_1 H32B_1 109.5 . . ?
H32A_1 C32'_1 H32B_1 109.5 . . ?
C31'_1 C32'_1 H32C_1 109.5 . . ?
H32A_1 C32'_1 H32C_1 109.5 . . ?
H32B_1 C32'_1 H32C_1 109.5 . . ?
C31'_1 C33'_1 H33A_1 109.5 . . ?
C31'_1 C33'_1 H33B_1 109.5 . . ?
H33A_1 C33'_1 H33B_1 109.5 . . ?
C31'_1 C33'_1 H33C_1 109.5 . . ?
H33A_1 C33'_1 H33C_1 109.5 . . ?
H33B_1 C33'_1 H33C_1 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 O4'_2 C34'_2 C35'_2 -71(3) . . . . ?
Ti1 O4'_2 C34'_2 C36'_2 109(2) . . . . ?
O3'_1 Ti1 O2 C28 -138.4(3) . . . . ?
O1 Ti1 O2 C28 -34.8(3) . . . . ?
O4'_2 Ti1 O2 C28 53.3(6) . . . . ?
N1 Ti1 O2 C28 47.3(3) . . . . ?
N2 Ti1 O2 C28 124.1(3) . . . . ?
C5 C1 C2 C3 1.4(2) . . . . ?
Fe1 C1 C2 C3 -58.62(16) . . . . ?
C5 C1 C2 Fe1 60.03(14) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
Fe1 C2 C3 C4 -59.08(17) . . . . ?
C1 C2 C3 Fe1 58.26(15) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
Fe1 C3 C4 C5 -59.26(16) . . . . ?
C2 C3 C4 Fe1 59.19(16) . . . . ?
C3 C4 C5 C1 0.9(3) . . . . ?
Fe1 C4 C5 C1 -58.42(15) . . . . ?
C3 C4 C5 Fe1 59.36(17) . . . . ?
C2 C1 C5 C4 -1.4(2) . . . . ?
Fe1 C1 C5 C4 58.84(16) . . . . ?
C2 C1 C5 Fe1 -60.29(14) . . . . ?
C10 C6 C7 C8 -1.1(3) . . . . ?
Fe1 C6 C7 C8 58.28(17) . . . . ?
C10 C6 C7 Fe1 -59.40(14) . . . . ?
C6 C7 C8 C9 0.6(3) . . . . ?
Fe1 C7 C8 C9 59.20(16) . . . . ?
C6 C7 C8 Fe1 -58.56(16) . . . . ?
C7 C8 C9 C10 0.1(3) . . . . ?
Fe1 C8 C9 C10 59.19(14) . . . . ?
C7 C8 C9 Fe1 -59.09(17) . . . . ?
C7 C6 C10 C11 178.67(19) . . . . ?
Fe1 C6 C10 C11 119.52(18) . . . . ?
C7 C6 C10 C9 1.2(2) . . . . ?
Fe1 C6 C10 C9 -57.98(14) . . . . ?
C7 C6 C10 Fe1 59.15(15) . . . . ?
C8 C9 C10 C11 -178.28(19) . . . . ?
Fe1 C9 C10 C11 -119.41(19) . . . . ?
C8 C9 C10 C6 -0.8(2) . . . . ?
Fe1 C9 C10 C6 58.08(14) . . . . ?
C8 C9 C10 Fe1 -58.87(15) . . . . ?
C18 C13 C14 C15 1.0(3) . . . . ?
C12 C13 C14 C15 -178.39(17) . . . . ?
C13 C14 C15 C16 1.2(3) . . . . ?
C13 C14 C15 C19 -178.73(18) . . . . ?
Ti1 O1 C16 C17 1.0(3) . . . . ?
Ti1 O1 C16 C15 -179.38(13) . . . . ?
C14 C15 C16 O1 177.33(15) . . . . ?
C19 C15 C16 O1 -2.7(3) . . . . ?
C14 C15 C16 C17 -3.0(2) . . . . ?
C19 C15 C16 C17 176.96(16) . . . . ?
O1 C16 C17 C18 -177.71(14) . . . . ?
C15 C16 C17 C18 2.6(2) . . . . ?
O1 C16 C17 C23 2.2(2) . . . . ?
C15 C16 C17 C23 -177.46(15) . . . . ?
C14 C13 C18 C17 -1.4(2) . . . . ?
C12 C13 C18 C17 177.94(15) . . . . ?
C16 C17 C18 C13 -0.4(2) . . . . ?
C23 C17 C18 C13 179.72(15) . . . . ?
C14 C15 C19 C21 -120.19(19) . . . . ?
C16 C15 C19 C21 59.8(2) . . . . ?
C14 C15 C19 C20 -0.5(3) . . . . ?
C16 C15 C19 C20 179.5(2) . . . . ?
C14 C15 C19 C22 118.59(19) . . . . ?
C16 C15 C19 C22 -61.4(2) . . . . ?
C24' N1 C23 C17 168.5(3) . . . . ?
C24 N1 C23 C17 -166.8(3) . . . . ?
Ti1 N1 C23 C17 -3.6(3) . . . . ?
C18 C17 C23 N1 179.38(16) . . . . ?
C16 C17 C23 N1 -0.5(3) . . . . ?
O4 Ti1 O3 C31 -11.7(4) . . . . ?
O2 Ti1 O3 C31 176.8(4) . . . . ?
O1 Ti1 O3 C31 85.0(4) . . . . ?
N1 Ti1 O3 C31 -142.5(4) . . . . ?
N2 Ti1 O3 C31 -98.0(4) . . . . ?
C26 N2 C25 C24 -83.6(4) . . . . ?
C27 N2 C25 C24 165.2(4) . . . . ?
Ti1 N2 C25 C24 53.0(4) . . . . ?
C23 N1 C24 C25 -150.4(3) . . . . ?
Ti1 N1 C24 C25 43.9(5) . . . . ?
N2 C25 C24 N1 -64.3(5) . . . . ?
Ti1 O3 C31 C33 123.1(7) . . . . ?
Ti1 O3 C31 C32 -102.9(7) . . . . ?
C35 C34 O4 Ti1 -168.5(6) . . . . ?
C36 C34 O4 Ti1 -44.1(7) . . . . ?
O3 Ti1 O4 C34 162.9(6) . . . . ?
O1 Ti1 O4 C34 55.8(6) . . . . ?
N1 Ti1 O4 C34 -26.7(6) . . . . ?
N2 Ti1 O4 C34 -103.0(6) . . . . ?
C23 N1 C24' C25' 145.4(3) . . . . ?
Ti1 N1 C24' C25' -41.4(4) . . . . ?
Ti1 O2 C28 C30 -147.2(2) . . . . ?
Ti1 O2 C28 C29 90.9(3) . . . . ?
N1 C24' C25' N2 59.4(4) . . . . ?
C26 N2 C25' C24' -163.6(3) . . . . ?
C27 N2 C25' C24' 82.0(3) . . . . ?
Ti1 N2 C25' C24' -48.4(3) . . . . ?
O2 Ti1 O3'_1 C31'_1 15.5(7) . . . . ?
O1 Ti1 O3'_1 C31'_1 -80.8(7) . . . . ?
O4'_2 Ti1 O3'_1 C31'_1 -168.8(7) . . . . ?
N1 Ti1 O3'_1 C31'_1 163.7(6) . . . . ?
N2 Ti1 O3'_1 C31'_1 103.1(6) . . . . ?
Ti1 O3'_1 C31'_1 C32'_1 112.6(8) . . . . ?
Ti1 O3'_1 C31'_1 C33'_1 -123.3(6) . . . . ?

_refine_diff_density_max         0.942
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.069

# start Validation Reply Form
_vrf_PLAT412_try1_b_pl           
;
PROBLEM: Short Intra XH3 .. XHn     H27B     ..H25B     .       1.59 Ang.  
RESPONSE:  This disorder is due to the ethylene diamine component of the ligand.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_try1_c_pl
_database_code_depnum_ccdc_archive 'CCDC 1993769'
loop_
_audit_author_name
_audit_author_address
'Justin M. Burroughs'
;University of Tennessee, Knoxville 
United States of America
;
_audit_update_record             
;
2020-03-30 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H57.62 Fe N2 O4 Zr'
_chemical_formula_sum            'C39 H57.63 Fe N2 O4 Zr'
_chemical_formula_weight         765.57

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   22.8642(12)
_cell_length_b                   9.1582(5)
_cell_length_c                   19.4463(10)
_cell_angle_alpha                90
_cell_angle_beta                 106.4470(10)
_cell_angle_gamma                90
_cell_volume                     3905.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2.184
_cell_measurement_theta_max      31.5415

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_F_000             1615
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.677
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            51591
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.184
_diffrn_reflns_theta_max         31.553
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13066
_reflns_number_gt                11296
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Apex3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+3.4445P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13066
_refine_ls_number_parameters     457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0888
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.18450(2) 0.39448(2) 0.20547(2) 0.01224(4) Uani 1 1 d . . . . .
Fe1 Fe 0.51485(2) 0.29566(3) -0.12383(2) 0.01666(5) Uani 1 1 d . . . . .
O1 O 0.12376(5) 0.26569(14) 0.14029(6) 0.0218(2) Uani 1 1 d . . . . .
O2 O 0.25865(5) 0.48304(13) 0.27213(6) 0.0183(2) Uani 1 1 d . . . . .
O3 O 0.12546(6) 0.52246(15) 0.22987(7) 0.0255(3) Uani 1 1 d . . . . .
O4 O 0.20778(5) 0.48047(13) 0.11937(6) 0.0166(2) Uani 1 1 d . . . . .
N3 N 0.19385(7) 0.21427(16) 0.29734(7) 0.0212(3) Uani 1 1 d . . . . .
N4 N 0.25431(6) 0.21975(15) 0.18618(7) 0.0169(2) Uani 1 1 d . . . . .
C1 C 0.51455(8) 0.0743(2) -0.11061(10) 0.0265(3) Uani 1 1 d . . . . .
H1 H 0.481563 0.005747 -0.136353 0.032 Uiso 1 1 calc R U . . .
C2 C 0.51822(9) 0.1473(2) -0.04489(10) 0.0260(3) Uani 1 1 d . . . . .
H2 H 0.488291 0.138712 -0.016268 0.031 Uiso 1 1 calc R U . . .
C3 C 0.57181(8) 0.2348(2) -0.02705(10) 0.0261(3) Uani 1 1 d . . . . .
H3 H 0.586092 0.298567 0.016211 0.031 Uiso 1 1 calc R U . . .
C4 C 0.60123(8) 0.2168(2) -0.08199(10) 0.0259(3) Uani 1 1 d . . . . .
H4 H 0.639716 0.266070 -0.084120 0.031 Uiso 1 1 calc R U . . .
C5 C 0.56611(8) 0.1173(2) -0.13356(11) 0.0269(4) Uani 1 1 d . . . . .
H5 H 0.575490 0.084599 -0.178338 0.032 Uiso 1 1 calc R U . . .
C6 C 0.49662(7) 0.51220(19) -0.11542(10) 0.0221(3) Uani 1 1 d . . . . .
H6 H 0.513685 0.575690 -0.072591 0.027 Uiso 1 1 calc R U . . .
C7 C 0.52253(9) 0.4890(2) -0.17296(11) 0.0300(4) Uani 1 1 d . . . . .
H7 H 0.561387 0.532867 -0.177257 0.036 Uiso 1 1 calc R U . . .
C8 C 0.48483(9) 0.3896(2) -0.22233(10) 0.0312(4) Uani 1 1 d . . . . .
H8 H 0.492484 0.352581 -0.267379 0.037 Uiso 1 1 calc R U . . .
C9 C 0.43464(8) 0.3506(2) -0.19620(8) 0.0241(3) Uani 1 1 d . . . . .
H9 H 0.400797 0.282218 -0.219702 0.029 Uiso 1 1 calc R U . . .
C10 C 0.44166(7) 0.42704(18) -0.12978(8) 0.0181(3) Uani 1 1 d . . . . .
C11 C 0.40188(7) 0.41980(18) -0.08486(8) 0.0180(3) Uani 1 1 d . . . . .
C12 C 0.36878(7) 0.41885(18) -0.04670(8) 0.0182(3) Uani 1 1 d . . . . .
C13 C 0.32752(7) 0.42981(18) -0.00324(8) 0.0166(3) Uani 1 1 d . . . . .
C14 C 0.28909(7) 0.55243(18) -0.01095(8) 0.0161(3) Uani 1 1 d . . . . .
H14 H 0.290847 0.623979 -0.045682 0.019 Uiso 1 1 calc R U . . .
C15 C 0.24877(6) 0.57397(17) 0.02965(7) 0.0148(3) Uani 1 1 d . . . . .
C16 C 0.24583(6) 0.46429(17) 0.08086(7) 0.0141(3) Uani 1 1 d . . . . .
C17 C 0.28435(7) 0.33921(17) 0.08905(8) 0.0151(3) Uani 1 1 d . . . . .
C18 C 0.32460(7) 0.32431(18) 0.04678(8) 0.0171(3) Uani 1 1 d . . . . .
H18 H 0.350189 0.240802 0.052534 0.021 Uiso 1 1 calc R U . . .
C19 C 0.20931(7) 0.71222(18) 0.02208(8) 0.0178(3) Uani 1 1 d . . . . .
C20 C 0.22188(9) 0.8188(2) -0.03276(10) 0.0273(4) Uani 1 1 d . . . . .
H20A H 0.212469 0.771489 -0.079821 0.041 Uiso 1 1 calc R U . . .
H20B H 0.264937 0.847441 -0.017719 0.041 Uiso 1 1 calc R U . . .
H20C H 0.196271 0.905753 -0.035811 0.041 Uiso 1 1 calc R U . . .
C21 C 0.14111(7) 0.6720(2) -0.00299(9) 0.0251(3) Uani 1 1 d . . . . .
H21A H 0.116513 0.761105 -0.008094 0.038 Uiso 1 1 calc R U . . .
H21B H 0.131324 0.607628 0.032462 0.038 Uiso 1 1 calc R U . . .
H21C H 0.132119 0.621703 -0.049297 0.038 Uiso 1 1 calc R U . . .
C22 C 0.22364(8) 0.79418(19) 0.09413(9) 0.0218(3) Uani 1 1 d . . . . .
H22A H 0.267272 0.816987 0.110459 0.033 Uiso 1 1 calc R U . . .
H22B H 0.212704 0.732694 0.129846 0.033 Uiso 1 1 calc R U . . .
H22C H 0.200048 0.885006 0.087905 0.033 Uiso 1 1 calc R U . . .
C23 C 0.28539(7) 0.22387(17) 0.14070(8) 0.0168(3) Uani 1 1 d . . . . .
H23 H 0.311701 0.143553 0.140788 0.020 Uiso 1 1 calc R U . . .
C24 C 0.25965(10) 0.0912(2) 0.23224(10) 0.0292(4) Uani 1 1 d . . . . .
H24A H 0.299955 0.044790 0.238652 0.035 Uiso 1 1 calc R U . . .
H24B H 0.227783 0.019243 0.209249 0.035 Uiso 1 1 calc R U . . .
C25 C 0.25274(9) 0.1336(2) 0.30314(10) 0.0304(4) Uani 1 1 d . . . . .
H25A H 0.287480 0.196536 0.328105 0.036 Uiso 1 1 calc R U . . .
H25B H 0.254089 0.044738 0.332516 0.036 Uiso 1 1 calc R U . . .
C26 C 0.20308(11) 0.2860(3) 0.36831(10) 0.0376(5) Uani 1 1 d . . . . .
H26A H 0.237591 0.353748 0.376894 0.056 Uiso 1 1 calc R U . . .
H26B H 0.211573 0.211606 0.406054 0.056 Uiso 1 1 calc R U . . .
H26C H 0.166162 0.339986 0.368692 0.056 Uiso 1 1 calc R U . . .
C27 C 0.14130(12) 0.1193(3) 0.28570(12) 0.0483(7) Uani 1 1 d . . . . .
H27A H 0.104714 0.178234 0.281728 0.072 Uiso 1 1 calc R U . . .
H27B H 0.147269 0.051654 0.326160 0.072 Uiso 1 1 calc R U . . .
H27C H 0.136348 0.063715 0.241354 0.072 Uiso 1 1 calc R U . . .
C28 C 0.31147(7) 0.56690(18) 0.29998(8) 0.0173(3) Uani 1 1 d . . . . .
C29 C 0.29263(8) 0.72487(19) 0.30676(9) 0.0236(3) Uani 1 1 d . . . . .
H29A H 0.270707 0.762477 0.259281 0.035 Uiso 1 1 calc R U . . .
H29B H 0.329065 0.784369 0.327036 0.035 Uiso 1 1 calc R U . . .
H29C H 0.266013 0.729219 0.338335 0.035 Uiso 1 1 calc R U . . .
C30 C 0.34699(8) 0.5078(2) 0.37357(9) 0.0237(3) Uani 1 1 d . . . . .
H30A H 0.358511 0.406068 0.368798 0.035 Uiso 1 1 calc R U . . .
H30B H 0.321379 0.512994 0.406271 0.035 Uiso 1 1 calc R U . . .
H30C H 0.383827 0.566606 0.392765 0.035 Uiso 1 1 calc R U . . .
C31 C 0.35132(8) 0.5605(2) 0.24880(9) 0.0241(3) Uani 1 1 d . . . . .
H31A H 0.328235 0.597587 0.201655 0.036 Uiso 1 1 calc R U . . .
H31B H 0.363462 0.459180 0.244135 0.036 Uiso 1 1 calc R U . . .
H31C H 0.387790 0.620580 0.267797 0.036 Uiso 1 1 calc R U . . .
C32 C 0.08769(7) 0.20206(19) 0.07613(9) 0.0214(3) Uani 1 1 d . . . . .
C33 C 0.07171(9) 0.0460(2) 0.09128(11) 0.0322(4) Uani 1 1 d . . . . .
H33A H 0.048091 0.000053 0.046524 0.048 Uiso 1 1 calc R U . . .
H33B H 0.047483 0.047273 0.125552 0.048 Uiso 1 1 calc R U . . .
H33C H 0.109294 -0.009503 0.111497 0.048 Uiso 1 1 calc R U . . .
C34 C 0.12334(9) 0.2015(2) 0.02033(10) 0.0316(4) Uani 1 1 d . . . . .
H34A H 0.098759 0.154994 -0.023784 0.047 Uiso 1 1 calc R U . . .
H34B H 0.161433 0.147091 0.039076 0.047 Uiso 1 1 calc R U . . .
H34C H 0.132653 0.302219 0.009955 0.047 Uiso 1 1 calc R U . . .
C35 C 0.02985(8) 0.2927(2) 0.04852(11) 0.0320(4) Uani 1 1 d . . . . .
H35A H 0.040734 0.392422 0.038677 0.048 Uiso 1 1 calc R U . . .
H35B H 0.007602 0.294906 0.084809 0.048 Uiso 1 1 calc R U . . .
H35C H 0.004031 0.248878 0.004334 0.048 Uiso 1 1 calc R U . . .
C36 C 0.0777(4) 0.6093(12) 0.2362(6) 0.0158(17) Uani 0.623(5) 1 d . . P A 1
C37 C 0.0543(2) 0.5641(5) 0.2971(3) 0.0508(12) Uani 0.623(5) 1 d . . P A 1
H37A H 0.023427 0.634166 0.302433 0.076 Uiso 0.623(5) 1 calc R U P A 1
H37B H 0.088001 0.561647 0.341360 0.076 Uiso 0.623(5) 1 calc R U P A 1
H37C H 0.035911 0.466787 0.287599 0.076 Uiso 0.623(5) 1 calc R U P A 1
C38 C 0.10762(17) 0.7637(4) 0.2548(3) 0.0444(10) Uani 0.623(5) 1 d . . P A 1
H38A H 0.121470 0.799104 0.214453 0.067 Uiso 0.623(5) 1 calc R U P A 1
H38B H 0.142522 0.756637 0.297677 0.067 Uiso 0.623(5) 1 calc R U P A 1
H38C H 0.077572 0.831906 0.263741 0.067 Uiso 0.623(5) 1 calc R U P A 1
C39 C 0.0274(2) 0.6224(7) 0.1661(2) 0.0539(15) Uani 0.623(5) 1 d . . P A 1
H39A H 0.044804 0.656909 0.128421 0.081 Uiso 0.623(5) 1 calc R U P A 1
H39B H -0.003366 0.691982 0.171959 0.081 Uiso 0.623(5) 1 calc R U P A 1
H39C H 0.008429 0.526677 0.152757 0.081 Uiso 0.623(5) 1 calc R U P A 1
C1_1 C 0.0744(10) 0.609(3) 0.2319(13) 0.036(6) Uiso 0.377(5) 1 d . . P A 2
C2_1 C 0.0484(4) 0.6757(8) 0.1628(4) 0.0384(16) Uiso 0.377(5) 1 d . . P A 2
H2A_1 H 0.039159 0.600006 0.125671 0.058 Uiso 0.377(5) 1 calc R U P A 2
H2B_1 H 0.077514 0.745428 0.152983 0.058 Uiso 0.377(5) 1 calc R U P A 2
H2C_1 H 0.010733 0.726977 0.162785 0.058 Uiso 0.377(5) 1 calc R U P A 2
C3_1 C 0.0879(3) 0.7086(8) 0.2949(4) 0.0463(17) Uiso 0.377(5) 1 d . . P A 2
H3A_1 H 0.127314 0.709048 0.328250 0.056 Uiso 0.377(5) 1 calc R U P A 2
H3B_1 H 0.057053 0.771782 0.301794 0.056 Uiso 0.377(5) 1 calc R U P A 2
C4_1 C 0.0306(3) 0.4853(7) 0.2453(3) 0.0370(14) Uiso 0.377(5) 1 d . . P A 2
H4A_1 H -0.006744 0.529666 0.250876 0.055 Uiso 0.377(5) 1 calc R U P A 2
H4B_1 H 0.051229 0.431249 0.288897 0.055 Uiso 0.377(5) 1 calc R U P A 2
H4C_1 H 0.020338 0.418321 0.204303 0.055 Uiso 0.377(5) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O3 1.9452(12) . ?
Zr1 O1 1.9823(12) . ?
Zr1 O2 1.9919(11) . ?
Zr1 O4 2.0522(10) . ?
Zr1 N4 2.3638(13) . ?
Zr1 N3 2.3968(14) . ?
Fe1 C8 2.0339(18) . ?
Fe1 C9 2.0337(17) . ?
Fe1 C2 2.0349(18) . ?
Fe1 C10 2.0377(16) . ?
Fe1 C3 2.0398(17) . ?
Fe1 C6 2.0425(18) . ?
Fe1 C7 2.0427(19) . ?
Fe1 C4 2.0428(17) . ?
Fe1 C1 2.0437(19) . ?
Fe1 C5 2.0498(18) . ?
O1 C32 1.4120(19) . ?
O2 C28 1.4041(18) . ?
O3 C36 1.385(8) . ?
O3 C1_1 1.42(2) . ?
O4 C16 1.3071(17) . ?
N3 C27 1.448(3) . ?
N3 C26 1.489(2) . ?
N3 C25 1.512(2) . ?
N4 C23 1.282(2) . ?
N4 C24 1.464(2) . ?
C1 C2 1.424(3) . ?
C1 C5 1.429(3) . ?
C1 H1 1.0000 . ?
C2 C3 1.422(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.424(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.423(2) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
C6 C7 1.422(2) . ?
C6 C10 1.438(2) . ?
C6 H6 1.0000 . ?
C7 C8 1.423(3) . ?
C7 H7 1.0000 . ?
C8 C9 1.426(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.437(2) . ?
C9 H9 1.0000 . ?
C10 C11 1.430(2) . ?
C11 C12 1.201(2) . ?
C12 C13 1.437(2) . ?
C13 C18 1.386(2) . ?
C13 C14 1.408(2) . ?
C14 C15 1.387(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.429(2) . ?
C15 C19 1.537(2) . ?
C16 C17 1.426(2) . ?
C17 C18 1.403(2) . ?
C17 C23 1.453(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.532(2) . ?
C19 C22 1.541(2) . ?
C19 C21 1.541(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 0.9500 . ?
C24 C25 1.484(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.526(2) . ?
C28 C31 1.529(2) . ?
C28 C30 1.530(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.524(3) . ?
C32 C35 1.524(2) . ?
C32 C34 1.531(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.490(10) . ?
C36 C39 1.518(12) . ?
C36 C38 1.568(12) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C1_1 C2_1 1.44(3) . ?
C1_1 C3_1 1.49(3) . ?
C1_1 C4_1 1.58(3) . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
C3_1 H3A_1 0.9500 . ?
C3_1 H3B_1 0.9500 . ?
C4_1 H4A_1 0.9800 . ?
C4_1 H4B_1 0.9800 . ?
C4_1 H4C_1 0.9800 . ?

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 Zr1 O1 96.06(6) . . ?
O3 Zr1 O2 96.74(5) . . ?
O1 Zr1 O2 166.28(5) . . ?
O3 Zr1 O4 109.03(5) . . ?
O1 Zr1 O4 90.19(5) . . ?
O2 Zr1 O4 90.29(5) . . ?
O3 Zr1 N4 173.20(5) . . ?
O1 Zr1 N4 83.00(5) . . ?
O2 Zr1 N4 83.71(5) . . ?
O4 Zr1 N4 77.73(4) . . ?
O3 Zr1 N3 98.90(5) . . ?
O1 Zr1 N3 88.02(5) . . ?
O2 Zr1 N3 85.15(5) . . ?
O4 Zr1 N3 152.05(5) . . ?
N4 Zr1 N3 74.36(5) . . ?
C8 Fe1 C9 41.04(7) . . ?
C8 Fe1 C2 157.45(9) . . ?
C9 Fe1 C2 121.42(8) . . ?
C8 Fe1 C10 69.14(7) . . ?
C9 Fe1 C10 41.35(6) . . ?
C2 Fe1 C10 106.98(7) . . ?
C8 Fe1 C3 160.33(8) . . ?
C9 Fe1 C3 157.10(7) . . ?
C2 Fe1 C3 40.86(8) . . ?
C10 Fe1 C3 120.89(7) . . ?
C8 Fe1 C6 69.05(8) . . ?
C9 Fe1 C6 69.54(8) . . ?
C2 Fe1 C6 123.56(7) . . ?
C10 Fe1 C6 41.26(6) . . ?
C3 Fe1 C6 106.44(7) . . ?
C8 Fe1 C7 40.85(9) . . ?
C9 Fe1 C7 69.02(8) . . ?
C2 Fe1 C7 160.30(8) . . ?
C10 Fe1 C7 68.88(7) . . ?
C3 Fe1 C7 123.47(8) . . ?
C6 Fe1 C7 40.75(7) . . ?
C8 Fe1 C4 123.71(8) . . ?
C9 Fe1 C4 160.69(7) . . ?
C2 Fe1 C4 68.77(8) . . ?
C10 Fe1 C4 156.50(7) . . ?
C3 Fe1 C4 40.83(8) . . ?
C6 Fe1 C4 120.49(7) . . ?
C7 Fe1 C4 106.93(8) . . ?
C8 Fe1 C1 121.73(9) . . ?
C9 Fe1 C1 107.34(8) . . ?
C2 Fe1 C1 40.86(8) . . ?
C10 Fe1 C1 124.12(7) . . ?
C3 Fe1 C1 68.71(8) . . ?
C6 Fe1 C1 160.90(7) . . ?
C7 Fe1 C1 157.27(8) . . ?
C4 Fe1 C1 68.70(7) . . ?
C8 Fe1 C5 107.43(8) . . ?
C9 Fe1 C5 124.09(7) . . ?
C2 Fe1 C5 68.73(8) . . ?
C10 Fe1 C5 161.26(7) . . ?
C3 Fe1 C5 68.59(8) . . ?
C6 Fe1 C5 156.34(7) . . ?
C7 Fe1 C5 121.35(8) . . ?
C4 Fe1 C5 40.69(7) . . ?
C1 Fe1 C5 40.86(7) . . ?
C32 O1 Zr1 159.83(11) . . ?
C28 O2 Zr1 162.62(10) . . ?
C36 O3 Zr1 170.8(5) . . ?
C1_1 O3 Zr1 167.3(10) . . ?
C16 O4 Zr1 142.42(10) . . ?
C27 N3 C26 107.67(16) . . ?
C27 N3 C25 113.60(18) . . ?
C26 N3 C25 104.89(15) . . ?
C27 N3 Zr1 113.71(12) . . ?
C26 N3 Zr1 110.26(12) . . ?
C25 N3 Zr1 106.36(10) . . ?
C23 N4 C24 118.63(14) . . ?
C23 N4 Zr1 128.35(11) . . ?
C24 N4 Zr1 113.00(10) . . ?
C2 C1 C5 107.85(16) . . ?
C2 C1 Fe1 69.24(10) . . ?
C5 C1 Fe1 69.80(11) . . ?
C2 C1 H1 126.1 . . ?
C5 C1 H1 126.1 . . ?
Fe1 C1 H1 126.1 . . ?
C3 C2 C1 108.13(16) . . ?
C3 C2 Fe1 69.76(10) . . ?
C1 C2 Fe1 69.90(11) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
Fe1 C2 H2 125.9 . . ?
C2 C3 C4 108.02(16) . . ?
C2 C3 Fe1 69.39(10) . . ?
C4 C3 Fe1 69.70(10) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
Fe1 C3 H3 126.0 . . ?
C5 C4 C3 108.09(16) . . ?
C5 C4 Fe1 69.92(10) . . ?
C3 C4 Fe1 69.47(10) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
Fe1 C4 H4 126.0 . . ?
C4 C5 C1 107.90(16) . . ?
C4 C5 Fe1 69.39(10) . . ?
C1 C5 Fe1 69.34(10) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Fe1 C5 H5 126.0 . . ?
C7 C6 C10 107.57(16) . . ?
C7 C6 Fe1 69.63(11) . . ?
C10 C6 Fe1 69.19(10) . . ?
C7 C6 H6 126.2 . . ?
C10 C6 H6 126.2 . . ?
Fe1 C6 H6 126.2 . . ?
C6 C7 C8 108.59(16) . . ?
C6 C7 Fe1 69.61(10) . . ?
C8 C7 Fe1 69.24(11) . . ?
C6 C7 H7 125.7 . . ?
C8 C7 H7 125.7 . . ?
Fe1 C7 H7 125.7 . . ?
C7 C8 C9 108.34(15) . . ?
C7 C8 Fe1 69.91(11) . . ?
C9 C8 Fe1 69.47(10) . . ?
C7 C8 H8 125.8 . . ?
C9 C8 H8 125.8 . . ?
Fe1 C8 H8 125.8 . . ?
C8 C9 C10 107.58(17) . . ?
C8 C9 Fe1 69.49(10) . . ?
C10 C9 Fe1 69.47(9) . . ?
C8 C9 H9 126.2 . . ?
C10 C9 H9 126.2 . . ?
Fe1 C9 H9 126.2 . . ?
C11 C10 C6 125.36(15) . . ?
C11 C10 C9 126.71(15) . . ?
C6 C10 C9 107.92(14) . . ?
C11 C10 Fe1 126.31(12) . . ?
C6 C10 Fe1 69.55(9) . . ?
C9 C10 Fe1 69.18(9) . . ?
C12 C11 C10 177.71(18) . . ?
C11 C12 C13 175.17(18) . . ?
C18 C13 C14 118.57(13) . . ?
C18 C13 C12 122.28(15) . . ?
C14 C13 C12 119.15(14) . . ?
C15 C14 C13 123.26(14) . . ?
C15 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
C14 C15 C16 117.81(14) . . ?
C14 C15 C19 121.95(13) . . ?
C16 C15 C19 120.22(12) . . ?
O4 C16 C17 121.14(13) . . ?
O4 C16 C15 119.33(13) . . ?
C17 C16 C15 119.53(13) . . ?
C18 C17 C16 119.96(14) . . ?
C18 C17 C23 116.69(14) . . ?
C16 C17 C23 123.35(13) . . ?
C13 C18 C17 120.87(14) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C15 111.77(13) . . ?
C20 C19 C22 106.80(14) . . ?
C15 C19 C22 110.26(12) . . ?
C20 C19 C21 107.73(13) . . ?
C15 C19 C21 110.32(14) . . ?
C22 C19 C21 109.86(13) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 C17 126.47(14) . . ?
N4 C23 H23 116.8 . . ?
C17 C23 H23 116.8 . . ?
N4 C24 C25 110.21(16) . . ?
N4 C24 H24A 109.6 . . ?
C25 C24 H24A 109.6 . . ?
N4 C24 H24B 109.6 . . ?
C25 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C24 C25 N3 112.69(15) . . ?
C24 C25 H25A 109.1 . . ?
N3 C25 H25A 109.1 . . ?
C24 C25 H25B 109.1 . . ?
N3 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
N3 C26 H26A 109.5 . . ?
N3 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N3 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C27 H27A 109.5 . . ?
N3 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N3 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O2 C28 C29 108.60(13) . . ?
O2 C28 C31 109.51(13) . . ?
C29 C28 C31 109.12(14) . . ?
O2 C28 C30 109.76(13) . . ?
C29 C28 C30 110.02(13) . . ?
C31 C28 C30 109.81(13) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O1 C32 C33 109.15(14) . . ?
O1 C32 C35 108.54(14) . . ?
C33 C32 C35 110.29(15) . . ?
O1 C32 C34 109.44(14) . . ?
C33 C32 C34 109.82(16) . . ?
C35 C32 C34 109.57(16) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O3 C36 C37 112.5(7) . . ?
O3 C36 C39 112.4(7) . . ?
C37 C36 C39 112.6(6) . . ?
O3 C36 C38 103.5(6) . . ?
C37 C36 C38 107.4(7) . . ?
C39 C36 C38 107.8(7) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O3 C1_1 C2_1 109.6(15) . . ?
O3 C1_1 C3_1 112.6(16) . . ?
C2_1 C1_1 C3_1 116.3(17) . . ?
O3 C1_1 C4_1 99.6(15) . . ?
C2_1 C1_1 C4_1 110.1(16) . . ?
C3_1 C1_1 C4_1 107.3(14) . . ?
C1_1 C2_1 H2A_1 109.5 . . ?
C1_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
C1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
C1_1 C3_1 H3A_1 120.0 . . ?
C1_1 C3_1 H3B_1 120.0 . . ?
H3A_1 C3_1 H3B_1 120.0 . . ?
C1_1 C4_1 H4A_1 109.5 . . ?
C1_1 C4_1 H4B_1 109.5 . . ?
H4A_1 C4_1 H4B_1 109.5 . . ?
C1_1 C4_1 H4C_1 109.5 . . ?
H4A_1 C4_1 H4C_1 109.5 . . ?
H4B_1 C4_1 H4C_1 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 -0.2(2) . . . . ?
Fe1 C1 C2 C3 -59.50(12) . . . . ?
C5 C1 C2 Fe1 59.33(13) . . . . ?
C1 C2 C3 C4 0.4(2) . . . . ?
Fe1 C2 C3 C4 -59.20(13) . . . . ?
C1 C2 C3 Fe1 59.59(13) . . . . ?
C2 C3 C4 C5 -0.5(2) . . . . ?
Fe1 C3 C4 C5 -59.47(13) . . . . ?
C2 C3 C4 Fe1 59.00(12) . . . . ?
C3 C4 C5 C1 0.4(2) . . . . ?
Fe1 C4 C5 C1 -58.83(13) . . . . ?
C3 C4 C5 Fe1 59.19(13) . . . . ?
C2 C1 C5 C4 -0.1(2) . . . . ?
Fe1 C1 C5 C4 58.86(13) . . . . ?
C2 C1 C5 Fe1 -58.98(13) . . . . ?
C10 C6 C7 C8 -0.6(2) . . . . ?
Fe1 C6 C7 C8 58.40(14) . . . . ?
C10 C6 C7 Fe1 -59.00(12) . . . . ?
C6 C7 C8 C9 0.4(2) . . . . ?
Fe1 C7 C8 C9 59.03(13) . . . . ?
C6 C7 C8 Fe1 -58.63(13) . . . . ?
C7 C8 C9 C10 0.0(2) . . . . ?
Fe1 C8 C9 C10 59.26(12) . . . . ?
C7 C8 C9 Fe1 -59.30(13) . . . . ?
C7 C6 C10 C11 179.96(16) . . . . ?
Fe1 C6 C10 C11 120.69(16) . . . . ?
C7 C6 C10 C9 0.56(19) . . . . ?
Fe1 C6 C10 C9 -58.71(12) . . . . ?
C7 C6 C10 Fe1 59.27(12) . . . . ?
C8 C9 C10 C11 -179.71(16) . . . . ?
Fe1 C9 C10 C11 -120.44(17) . . . . ?
C8 C9 C10 C6 -0.3(2) . . . . ?
Fe1 C9 C10 C6 58.95(12) . . . . ?
C8 C9 C10 Fe1 -59.26(13) . . . . ?
C18 C13 C14 C15 0.7(2) . . . . ?
C12 C13 C14 C15 -178.60(14) . . . . ?
C13 C14 C15 C16 -1.0(2) . . . . ?
C13 C14 C15 C19 177.41(14) . . . . ?
Zr1 O4 C16 C17 9.7(2) . . . . ?
Zr1 O4 C16 C15 -170.31(12) . . . . ?
C14 C15 C16 O4 -179.20(13) . . . . ?
C19 C15 C16 O4 2.3(2) . . . . ?
C14 C15 C16 C17 0.8(2) . . . . ?
C19 C15 C16 C17 -177.72(13) . . . . ?
O4 C16 C17 C18 179.73(13) . . . . ?
C15 C16 C17 C18 -0.2(2) . . . . ?
O4 C16 C17 C23 -1.3(2) . . . . ?
C15 C16 C17 C23 178.69(14) . . . . ?
C14 C13 C18 C17 -0.1(2) . . . . ?
C12 C13 C18 C17 179.16(14) . . . . ?
C16 C17 C18 C13 -0.1(2) . . . . ?
C23 C17 C18 C13 -179.07(14) . . . . ?
C14 C15 C19 C20 -1.5(2) . . . . ?
C16 C15 C19 C20 176.95(14) . . . . ?
C14 C15 C19 C22 -120.09(15) . . . . ?
C16 C15 C19 C22 58.32(18) . . . . ?
C14 C15 C19 C21 118.38(16) . . . . ?
C16 C15 C19 C21 -63.21(18) . . . . ?
C24 N4 C23 C17 177.64(16) . . . . ?
Zr1 N4 C23 C17 -0.5(2) . . . . ?
C18 C17 C23 N4 176.88(15) . . . . ?
C16 C17 C23 N4 -2.1(2) . . . . ?
C23 N4 C24 C25 147.33(16) . . . . ?
Zr1 N4 C24 C25 -34.22(19) . . . . ?
N4 C24 C25 N3 55.5(2) . . . . ?
C27 N3 C25 C24 79.4(2) . . . . ?
C26 N3 C25 C24 -163.25(16) . . . . ?
Zr1 N3 C25 C24 -46.42(18) . . . . ?
Zr1 O2 C28 C29 75.4(4) . . . . ?
Zr1 O2 C28 C31 -43.6(4) . . . . ?
Zr1 O2 C28 C30 -164.2(3) . . . . ?
Zr1 O1 C32 C33 152.6(3) . . . . ?
Zr1 O1 C32 C35 -87.2(3) . . . . ?
Zr1 O1 C32 C34 32.4(4) . . . . ?
Zr1 O3 C1_1 C2_1 -36(6) . . . . ?
Zr1 O3 C1_1 C3_1 -167(3) . . . . ?
Zr1 O3 C1_1 C4_1 79(5) . . . . ?

_refine_diff_density_max         2.396
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.073

# start Validation Reply Form
_vrf_PLAT230_try1_c_pl           
;
PROBLEM: Hirshfeld Test Diff for    N3       --C25      .        9.2 s.u.  
RESPONSE: This disorder is due to the ethylene diamine portion of the ligand. Attempts to model this disorder were not successful.  
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_try3_A
_database_code_depnum_ccdc_archive 'CCDC 1993771'
loop_
_audit_author_name
_audit_author_address
'Justin M. Burroughs'
;University of Tennessee, Knoxville 
United States of America
;
_audit_update_record             
;
2020-03-30 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31.52 H58.94 N2 O4 Zr'
_chemical_formula_sum            'C31.51 H58.93 N2 O4 Zr'
_chemical_formula_weight         621.07

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

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0808(8)
_cell_length_b                   9.9464(8)
_cell_length_c                   21.5037(18)
_cell_angle_alpha                93.147(3)
_cell_angle_beta                 91.175(3)
_cell_angle_gamma                115.995(2)
_cell_volume                     1741.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9846
_cell_measurement_theta_min      2.4105
_cell_measurement_theta_max      30.387

_exptl_crystal_description       Block
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.349
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            60166
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.284
_diffrn_reflns_theta_max         30.571
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10664
_reflns_number_gt                9406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Apex3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+4.0565P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10664
_refine_ls_number_parameters     475
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1102
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001

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
C3'_6 C 0.235(2) 0.079(2) 0.5844(11) 0.047(6) Uani 0.174(4) 1 d . U P A 2
H3'A_6 H 0.161940 0.001204 0.553466 0.071 Uiso 0.174(4) 1 calc R U P A 2
H3'B_6 H 0.169213 0.107279 0.613332 0.071 Uiso 0.174(4) 1 calc R U P A 2
H3'C_6 H 0.301158 0.041579 0.607667 0.071 Uiso 0.174(4) 1 calc R U P A 2
C1'_6 C 0.486(3) 0.168(3) 0.5114(10) 0.063(8) Uani 0.174(4) 1 d . U P A 2
H1'A_6 H 0.423253 0.087885 0.479158 0.095 Uiso 0.174(4) 1 calc R U P A 2
H1'B_6 H 0.538567 0.130102 0.541426 0.095 Uiso 0.174(4) 1 calc R U P A 2
H1'C_6 H 0.569354 0.253117 0.491979 0.095 Uiso 0.174(4) 1 calc R U P A 2
C2'_6 C 0.267(3) 0.286(2) 0.5144(9) 0.047(6) Uani 0.174(4) 1 d . U P A 2
H2'A_6 H 0.345944 0.378207 0.496917 0.070 Uiso 0.174(4) 1 calc R U P A 2
H2'B_6 H 0.195373 0.310231 0.541517 0.070 Uiso 0.174(4) 1 calc R U P A 2
H2'C_6 H 0.201263 0.213764 0.480383 0.070 Uiso 0.174(4) 1 calc R U P A 2
C1"_6 C 0.466(3) 0.229(3) 0.4915(12) 0.055(6) Uiso 0.174(4) 1 d . U P A 3
H1"A_6 H 0.396920 0.163175 0.456453 0.082 Uiso 0.174(4) 1 calc R U P A 3
H1"B_6 H 0.548411 0.195788 0.504079 0.082 Uiso 0.174(4) 1 calc R U P A 3
H1"C_6 H 0.521778 0.332247 0.478742 0.082 Uiso 0.174(4) 1 calc R U P A 3
C3"_6 C 0.275(2) 0.0821(18) 0.5728(7) 0.019(3) Uiso 0.174(4) 1 d . U P A 3
H3"A_6 H 0.197087 0.082929 0.603569 0.029 Uiso 0.174(4) 1 calc R U P A 3
H3"B_6 H 0.356591 0.056636 0.592616 0.029 Uiso 0.174(4) 1 calc R U P A 3
H3"C_6 H 0.215729 0.007399 0.538425 0.029 Uiso 0.174(4) 1 calc R U P A 3
C2"_6 C 0.217(3) 0.273(3) 0.5293(11) 0.040(5) Uiso 0.174(4) 1 d . U P A 3
H2"A_6 H 0.268126 0.370420 0.511537 0.059 Uiso 0.174(4) 1 calc R U P A 3
H2"B_6 H 0.157028 0.279602 0.565811 0.059 Uiso 0.174(4) 1 calc R U P A 3
H2"C_6 H 0.140472 0.197870 0.498040 0.059 Uiso 0.174(4) 1 calc R U P A 3
N1 N 0.4598(2) 0.6204(2) 0.79383(9) 0.0239(4) Uani 1 1 d . . . . .
O1 O 0.75493(18) 0.66015(18) 0.74168(7) 0.0206(3) Uani 1 1 d . . . . .
Zr1 Zr 0.73539(2) 0.79539(2) 0.81278(2) 0.01396(5) Uani 1 1 d . . . . .
N2 N 0.5754(3) 0.8635(2) 0.88684(9) 0.0240(4) Uani 1 1 d . . . . .
O2 O 0.9540(2) 0.95232(18) 0.83650(8) 0.0268(3) Uani 1 1 d . . . . .
O4 O 0.6786(2) 0.9176(2) 0.75617(7) 0.0256(3) Uani 1 1 d . . . . .
C1 C 0.3796(8) 0.0861(6) 0.5469(3) 0.077(2) Uani 0.826(4) 1 d . . P A 1
H1A H 0.309412 0.015792 0.513013 0.115 Uiso 0.826(4) 1 calc R U P A 1
H1B H 0.351523 0.039058 0.586599 0.115 Uiso 0.826(4) 1 calc R U P A 1
H1C H 0.494778 0.112496 0.539346 0.115 Uiso 0.826(4) 1 calc R U P A 1
C2 C 0.3815(9) 0.2961(6) 0.4889(2) 0.082(2) Uani 0.826(4) 1 d . . P A 1
H2A H 0.305147 0.225329 0.456469 0.123 Uiso 0.826(4) 1 calc R U P A 1
H2B H 0.494520 0.323947 0.477268 0.123 Uiso 0.826(4) 1 calc R U P A 1
H2C H 0.363156 0.386114 0.493079 0.123 Uiso 0.826(4) 1 calc R U P A 1
C3 C 0.1609(6) 0.1647(8) 0.5595(3) 0.083(2) Uani 0.826(4) 1 d . . P A 1
H3A H 0.133546 0.249751 0.562003 0.125 Uiso 0.826(4) 1 calc R U P A 1
H3B H 0.133292 0.113283 0.598184 0.125 Uiso 0.826(4) 1 calc R U P A 1
H3C H 0.098186 0.094639 0.524214 0.125 Uiso 0.826(4) 1 calc R U P A 1
C4 C 0.3538(4) 0.2242(3) 0.54958(11) 0.0330(6) Uani 1 1 d . . . . .
C5 C 0.4601(3) 0.3381(3) 0.60248(10) 0.0258(5) Uani 1 1 d . . . . .
C6 C 0.3917(3) 0.3793(2) 0.65224(10) 0.0235(4) Uani 1 1 d . . . . .
H6 H 0.275827 0.334156 0.654562 0.028 Uiso 1 1 calc R U . . .
C7 C 0.4895(3) 0.4865(2) 0.69970(10) 0.0191(4) Uani 1 1 d . . . . .
C8 C 0.6633(3) 0.5559(2) 0.69797(9) 0.0179(4) Uani 1 1 d . . . . .
C9 C 0.7362(3) 0.5106(3) 0.64814(10) 0.0209(4) Uani 1 1 d . . . . .
C10 C 0.6320(3) 0.4049(3) 0.60260(10) 0.0256(5) Uani 1 1 d . . . . .
H10 H 0.680918 0.375806 0.569098 0.031 Uiso 1 1 calc R U . . .
C11 C 0.9238(3) 0.5778(3) 0.64497(11) 0.0254(5) Uani 1 1 d . . . . .
C12 C 0.9970(3) 0.7478(3) 0.63892(13) 0.0331(5) Uani 1 1 d . . . . .
H12A H 1.116416 0.788745 0.637007 0.050 Uiso 1 1 calc R U . . .
H12B H 0.970029 0.795551 0.675126 0.050 Uiso 1 1 calc R U . . .
H12C H 0.951151 0.767620 0.600775 0.050 Uiso 1 1 calc R U . . .
C13 C 1.0000(3) 0.5474(3) 0.70376(12) 0.0316(5) Uani 1 1 d . . . . .
H13A H 0.953964 0.438988 0.707689 0.047 Uiso 1 1 calc R U . . .
H13B H 0.975429 0.595279 0.740514 0.047 Uiso 1 1 calc R U . . .
H13C H 1.119080 0.588402 0.700590 0.047 Uiso 1 1 calc R U . . .
C14 C 0.9753(4) 0.5092(4) 0.58865(14) 0.0443(7) Uani 1 1 d . . . . .
H14A H 0.930886 0.528813 0.550104 0.066 Uiso 1 1 calc R U . . .
H14B H 0.932535 0.400761 0.591635 0.066 Uiso 1 1 calc R U . . .
H14C H 1.095257 0.554415 0.588304 0.066 Uiso 1 1 calc R U . . .
C15 C 0.4002(3) 0.5203(2) 0.74812(10) 0.0215(4) Uani 1 1 d . . . . .
H15 H 0.284604 0.461860 0.745878 0.026 Uiso 1 1 calc R U . . .
C16 C 0.3476(8) 0.6278(7) 0.8403(3) 0.0254(10) Uani 0.737(7) 1 d . U P B 1
H16A H 0.353078 0.574155 0.877098 0.030 Uiso 0.737(7) 1 calc R U P B 1
H16B H 0.233467 0.580820 0.822468 0.030 Uiso 0.737(7) 1 calc R U P B 1
C17 C 0.4009(4) 0.7926(4) 0.85913(15) 0.0249(8) Uani 0.737(7) 1 d . . P B 1
H17A H 0.394183 0.845092 0.822148 0.030 Uiso 0.737(7) 1 calc R U P B 1
H17B H 0.326514 0.802555 0.890145 0.030 Uiso 0.737(7) 1 calc R U P B 1
C18 C 0.5794(8) 0.8199(6) 0.94979(16) 0.0344(12) Uani 0.740(12) 1 d . U P B 1
H18A H 0.535213 0.710514 0.949212 0.052 Uiso 0.740(12) 1 calc R U P B 1
H18B H 0.512841 0.853574 0.975769 0.052 Uiso 0.740(12) 1 calc R U P B 1
H18C H 0.692885 0.866089 0.966986 0.052 Uiso 0.740(12) 1 calc R U P B 1
C19 C 0.6291(8) 1.0296(5) 0.8893(3) 0.0323(10) Uani 0.740(12) 1 d . U P B 1
H19A H 0.631031 1.061199 0.846849 0.048 Uiso 0.740(12) 1 calc R U P B 1
H19B H 0.739181 1.082001 0.909530 0.048 Uiso 0.740(12) 1 calc R U P B 1
H19C H 0.552178 1.054038 0.913187 0.048 Uiso 0.740(12) 1 calc R U P B 1
C16' C 0.340(2) 0.663(2) 0.8290(8) 0.022(3) Uani 0.263(7) 1 d . U P B 2
H16C H 0.320885 0.740541 0.807755 0.027 Uiso 0.263(7) 1 calc R U P B 2
H16D H 0.233526 0.574686 0.832351 0.027 Uiso 0.263(7) 1 calc R U P B 2
C17' C 0.4248(11) 0.7248(10) 0.8930(4) 0.025(2) Uani 0.263(7) 1 d . . P B 2
H17C H 0.350415 0.745798 0.920690 0.030 Uiso 0.263(7) 1 calc R U P B 2
H17D H 0.452454 0.649615 0.911914 0.030 Uiso 0.263(7) 1 calc R U P B 2
C18' C 0.675(2) 0.8926(18) 0.9521(4) 0.030(3) Uani 0.260(12) 1 d . U P B 2
H18D H 0.694761 0.805459 0.959887 0.045 Uiso 0.260(12) 1 calc R U P B 2
H18E H 0.611650 0.908616 0.985571 0.045 Uiso 0.260(12) 1 calc R U P B 2
H18F H 0.780542 0.981676 0.951027 0.045 Uiso 0.260(12) 1 calc R U P B 2
C19' C 0.557(2) 0.9915(17) 0.8761(6) 0.029(3) Uani 0.260(12) 1 d . U P B 2
H19D H 0.449921 0.987004 0.873157 0.035 Uiso 0.260(12) 1 calc R U P B 2
H19E H 0.650280 1.083740 0.871824 0.035 Uiso 0.260(12) 1 calc R U P B 2
C20 C 0.6450(3) 0.9766(3) 0.70206(11) 0.0267(5) Uani 1 1 d . . . . .
C21 C 0.7944(4) 1.0279(4) 0.66221(12) 0.0368(6) Uani 1 1 d . . . . .
H21A H 0.815588 0.942054 0.649718 0.055 Uiso 1 1 calc R U . . .
H21B H 0.890062 1.104182 0.686352 0.055 Uiso 1 1 calc R U . . .
H21C H 0.773468 1.070631 0.624936 0.055 Uiso 1 1 calc R U . . .
C22 C 0.6149(4) 1.1119(4) 0.72138(15) 0.0450(7) Uani 1 1 d . . . . .
H22A H 0.599260 1.157382 0.684061 0.068 Uiso 1 1 calc R U . . .
H22B H 0.709563 1.185567 0.746839 0.068 Uiso 1 1 calc R U . . .
H22C H 0.516462 1.079672 0.745659 0.068 Uiso 1 1 calc R U . . .
C23 C 0.4953(4) 0.8551(4) 0.66642(16) 0.0536(10) Uani 1 1 d . . . . .
H23A H 0.474718 0.893034 0.627706 0.080 Uiso 1 1 calc R U . . .
H23B H 0.399682 0.826738 0.692091 0.080 Uiso 1 1 calc R U . . .
H23C H 0.515031 0.767193 0.656485 0.080 Uiso 1 1 calc R U . . .
C24 C 1.1049(3) 1.0809(3) 0.84202(12) 0.0271(5) Uani 1 1 d . . . . .
C25 C 1.0742(4) 1.2197(3) 0.84364(17) 0.0467(7) Uani 1 1 d . . . . .
H25A H 1.179325 1.309663 0.845297 0.070 Uiso 1 1 calc R U . . .
H25B H 1.013972 1.222451 0.880610 0.070 Uiso 1 1 calc R U . . .
H25C H 1.009391 1.216192 0.806039 0.070 Uiso 1 1 calc R U . . .
C26 C 1.1933(4) 1.0791(4) 0.90278(16) 0.0506(8) Uani 1 1 d . . . . .
H26A H 1.207132 0.986701 0.902555 0.076 Uiso 1 1 calc R U . . .
H26B H 1.128374 1.083315 0.938025 0.076 Uiso 1 1 calc R U . . .
H26C H 1.301151 1.165969 0.906813 0.076 Uiso 1 1 calc R U . . .
C27 C 1.2031(4) 1.0776(4) 0.78614(16) 0.0460(7) Uani 1 1 d . . . . .
H27A H 1.143609 1.079049 0.747826 0.069 Uiso 1 1 calc R U . . .
H27B H 1.218893 0.986178 0.784698 0.069 Uiso 1 1 calc R U . . .
H27C H 1.310162 1.165567 0.789815 0.069 Uiso 1 1 calc R U . . .
O3 O 0.7383(2) 0.65984(18) 0.87751(7) 0.0233(3) Uani 1 1 d . . . . .
C28 C 0.7741(3) 0.5527(3) 0.90467(12) 0.0270(5) Uani 1 1 d . . . . .
C29 C 0.6988(7) 0.5092(6) 0.9639(2) 0.0451(14) Uani 0.634(6) 1 d . . P C 1
H29A H 0.579167 0.465675 0.957644 0.068 Uiso 0.634(6) 1 calc R U P C 1
H29B H 0.736668 0.597762 0.993449 0.068 Uiso 0.634(6) 1 calc R U P C 1
H29C H 0.729691 0.434995 0.980668 0.068 Uiso 0.634(6) 1 calc R U P C 1
C30 C 0.7150(9) 0.4137(5) 0.8555(3) 0.0571(17) Uani 0.634(6) 1 d . . P C 1
H30A H 0.769414 0.445555 0.816450 0.086 Uiso 0.634(6) 1 calc R U P C 1
H30B H 0.595945 0.371810 0.847868 0.086 Uiso 0.634(6) 1 calc R U P C 1
H30C H 0.742996 0.337143 0.871767 0.086 Uiso 0.634(6) 1 calc R U P C 1
C31 C 0.9621(6) 0.6191(8) 0.9098(3) 0.0519(16) Uani 0.634(6) 1 d . . P C 1
H31A H 1.005870 0.647329 0.868770 0.078 Uiso 0.634(6) 1 calc R U P C 1
H31B H 0.994658 0.544242 0.924773 0.078 Uiso 0.634(6) 1 calc R U P C 1
H31C H 1.005612 0.708013 0.939231 0.078 Uiso 0.634(6) 1 calc R U P C 1
C30' C 0.6075(11) 0.4109(9) 0.9047(6) 0.053(3) Uani 0.366(6) 1 d . . P C 2
H30D H 0.569553 0.370578 0.861661 0.080 Uiso 0.366(6) 1 calc R U P C 2
H30E H 0.526385 0.437466 0.924275 0.080 Uiso 0.366(6) 1 calc R U P C 2
H30F H 0.621198 0.335047 0.928129 0.080 Uiso 0.366(6) 1 calc R U P C 2
C29' C 0.8199(15) 0.6069(12) 0.9779(4) 0.047(3) Uani 0.366(6) 1 d . . P C 2
H29D H 0.922698 0.699390 0.982226 0.071 Uiso 0.366(6) 1 calc R U P C 2
H29E H 0.832840 0.528641 0.999788 0.071 Uiso 0.366(6) 1 calc R U P C 2
H29F H 0.731780 0.625624 0.995966 0.071 Uiso 0.366(6) 1 calc R U P C 2
C31' C 0.9011(12) 0.5230(11) 0.8785(5) 0.044(2) Uani 0.366(6) 1 d . . P C 2
H31D H 0.957019 0.575357 0.844095 0.052 Uiso 0.366(6) 1 calc R U P C 2
H31E H 0.929534 0.450871 0.895489 0.052 Uiso 0.366(6) 1 calc R U P C 2


_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
C3'_6 C4 1.61(2) . ?
C3'_6 H3'A_6 0.9800 . ?
C3'_6 H3'B_6 0.9800 . ?
C3'_6 H3'C_6 0.9800 . ?
C1'_6 C4 1.73(2) . ?
C1'_6 H1'A_6 0.9800 . ?
C1'_6 H1'B_6 0.9800 . ?
C1'_6 H1'C_6 0.9800 . ?
C2'_6 C4 1.42(2) . ?
C2'_6 H2'A_6 0.9800 . ?
C2'_6 H2'B_6 0.9800 . ?
C2'_6 H2'C_6 0.9800 . ?
C1"_6 C4 1.62(3) . ?
C1"_6 H1"A_6 0.9800 . ?
C1"_6 H1"B_6 0.9800 . ?
C1"_6 H1"C_6 0.9800 . ?
C3"_6 C4 1.402(16) . ?
C3"_6 H3"A_6 0.9800 . ?
C3"_6 H3"B_6 0.9800 . ?
C3"_6 H3"C_6 0.9800 . ?
C2"_6 C4 1.58(2) . ?
C2"_6 H2"A_6 0.9800 . ?
C2"_6 H2"B_6 0.9800 . ?
C2"_6 H2"C_6 0.9800 . ?
N1 C15 1.284(3) . ?
N1 C16 1.464(7) . ?
N1 C16' 1.531(18) . ?
N1 Zr1 2.3497(19) . ?
O1 C8 1.325(2) . ?
O1 Zr1 2.0428(15) . ?
Zr1 O2 1.9475(16) . ?
Zr1 O4 1.9780(15) . ?
Zr1 O3 1.9980(15) . ?
Zr1 N2 2.4384(19) . ?
N2 C19' 1.388(12) . ?
N2 C18 1.449(4) . ?
N2 C17' 1.471(10) . ?
N2 C19 1.501(5) . ?
N2 C17 1.516(4) . ?
N2 C18' 1.597(10) . ?
O2 C24 1.403(3) . ?
O4 C20 1.417(3) . ?
C1 C4 1.490(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C4 1.496(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.608(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.537(3) . ?
C5 C6 1.378(3) . ?
C5 C10 1.404(4) . ?
C6 C7 1.407(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.421(3) . ?
C7 C15 1.445(3) . ?
C8 C9 1.424(3) . ?
C9 C10 1.392(3) . ?
C9 C11 1.538(3) . ?
C10 H10 0.9500 . ?
C11 C13 1.535(3) . ?
C11 C12 1.537(4) . ?
C11 C14 1.537(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?
C16 C17 1.519(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C16' C17' 1.52(2) . ?
C16' H16C 0.9900 . ?
C16' H16D 0.9900 . ?
C17' H17C 0.9900 . ?
C17' H17D 0.9900 . ?
C18' H18D 0.9800 . ?
C18' H18E 0.9800 . ?
C18' H18F 0.9800 . ?
C19' H19D 0.9500 . ?
C19' H19E 0.9500 . ?
C20 C23 1.520(4) . ?
C20 C21 1.524(4) . ?
C20 C22 1.525(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C27 1.518(4) . ?
C24 C25 1.522(4) . ?
C24 C26 1.524(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O3 C28 1.395(3) . ?
C28 C31' 1.429(8) . ?
C28 C29 1.455(5) . ?
C28 C31 1.536(6) . ?
C28 C30' 1.552(9) . ?
C28 C30 1.575(6) . ?
C28 C29' 1.621(8) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
C29' H29D 0.9800 . ?
C29' H29E 0.9800 . ?
C29' H29F 0.9800 . ?
C31' H31D 0.9500 . ?
C31' H31E 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 C3'_6 H3'A_6 109.5 . . ?
C4 C3'_6 H3'B_6 109.5 . . ?
H3'A_6 C3'_6 H3'B_6 109.5 . . ?
C4 C3'_6 H3'C_6 109.5 . . ?
H3'A_6 C3'_6 H3'C_6 109.5 . . ?
H3'B_6 C3'_6 H3'C_6 109.5 . . ?
C4 C1'_6 H1'A_6 109.5 . . ?
C4 C1'_6 H1'B_6 109.5 . . ?
H1'A_6 C1'_6 H1'B_6 109.5 . . ?
C4 C1'_6 H1'C_6 109.5 . . ?
H1'A_6 C1'_6 H1'C_6 109.5 . . ?
H1'B_6 C1'_6 H1'C_6 109.5 . . ?
C4 C2'_6 H2'A_6 109.5 . . ?
C4 C2'_6 H2'B_6 109.5 . . ?
H2'A_6 C2'_6 H2'B_6 109.5 . . ?
C4 C2'_6 H2'C_6 109.5 . . ?
H2'A_6 C2'_6 H2'C_6 109.5 . . ?
H2'B_6 C2'_6 H2'C_6 109.5 . . ?
C4 C1"_6 H1"A_6 109.5 . . ?
C4 C1"_6 H1"B_6 109.5 . . ?
H1"A_6 C1"_6 H1"B_6 109.5 . . ?
C4 C1"_6 H1"C_6 109.5 . . ?
H1"A_6 C1"_6 H1"C_6 109.5 . . ?
H1"B_6 C1"_6 H1"C_6 109.5 . . ?
C4 C3"_6 H3"A_6 109.5 . . ?
C4 C3"_6 H3"B_6 109.5 . . ?
H3"A_6 C3"_6 H3"B_6 109.5 . . ?
C4 C3"_6 H3"C_6 109.5 . . ?
H3"A_6 C3"_6 H3"C_6 109.5 . . ?
H3"B_6 C3"_6 H3"C_6 109.5 . . ?
C4 C2"_6 H2"A_6 109.5 . . ?
C4 C2"_6 H2"B_6 109.5 . . ?
H2"A_6 C2"_6 H2"B_6 109.5 . . ?
C4 C2"_6 H2"C_6 109.5 . . ?
H2"A_6 C2"_6 H2"C_6 109.5 . . ?
H2"B_6 C2"_6 H2"C_6 109.5 . . ?
C15 N1 C16 118.0(3) . . ?
C15 N1 C16' 117.4(8) . . ?
C15 N1 Zr1 126.89(15) . . ?
C16 N1 Zr1 115.1(3) . . ?
C16' N1 Zr1 113.3(8) . . ?
C8 O1 Zr1 140.73(14) . . ?
O2 Zr1 O4 94.87(8) . . ?
O2 Zr1 O3 94.79(7) . . ?
O4 Zr1 O3 165.97(7) . . ?
O2 Zr1 O1 108.30(7) . . ?
O4 Zr1 O1 93.74(7) . . ?
O3 Zr1 O1 92.86(6) . . ?
O2 Zr1 N1 172.84(7) . . ?
O4 Zr1 N1 84.39(7) . . ?
O3 Zr1 N1 84.76(7) . . ?
O1 Zr1 N1 78.86(6) . . ?
O2 Zr1 N2 99.89(7) . . ?
O4 Zr1 N2 84.28(7) . . ?
O3 Zr1 N2 84.06(7) . . ?
O1 Zr1 N2 151.81(7) . . ?
N1 Zr1 N2 72.95(7) . . ?
C19' N2 C17' 117.0(9) . . ?
C18 N2 C19 108.7(3) . . ?
C18 N2 C17 110.4(3) . . ?
C19 N2 C17 105.5(3) . . ?
C19' N2 C18' 107.8(7) . . ?
C17' N2 C18' 104.5(7) . . ?
C19' N2 Zr1 116.4(5) . . ?
C18 N2 Zr1 116.0(2) . . ?
C17' N2 Zr1 105.5(3) . . ?
C19 N2 Zr1 109.8(2) . . ?
C17 N2 Zr1 105.94(15) . . ?
C18' N2 Zr1 104.3(4) . . ?
C24 O2 Zr1 166.99(16) . . ?
C20 O4 Zr1 162.89(16) . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 C2 112.7(4) . . ?
C2'_6 C4 C5 110.0(8) . . ?
C3"_6 C4 C5 109.1(7) . . ?
C1 C4 C5 111.7(3) . . ?
C2 C4 C5 110.5(3) . . ?
C3"_6 C4 C1"_6 113.5(12) . . ?
C5 C4 C1"_6 109.5(10) . . ?
C1 C4 C3 104.3(4) . . ?
C2 C4 C3 105.1(4) . . ?
C5 C4 C3 112.3(3) . . ?
C2'_6 C4 C3'_6 113.3(12) . . ?
C5 C4 C3'_6 104.6(8) . . ?
C3"_6 C4 C2"_6 107.5(12) . . ?
C5 C4 C2"_6 106.8(9) . . ?
C1"_6 C4 C2"_6 110.1(12) . . ?
C2'_6 C4 C1'_6 118.4(15) . . ?
C5 C4 C1'_6 105.2(7) . . ?
C3'_6 C4 C1'_6 104.2(12) . . ?
C6 C5 C10 116.6(2) . . ?
C6 C5 C4 121.9(2) . . ?
C10 C5 C4 121.5(2) . . ?
C5 C6 C7 121.6(2) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 120.8(2) . . ?
C6 C7 C15 115.3(2) . . ?
C8 C7 C15 123.94(19) . . ?
O1 C8 C7 120.70(18) . . ?
O1 C8 C9 120.96(19) . . ?
C7 C8 C9 118.34(19) . . ?
C10 C9 C8 117.7(2) . . ?
C10 C9 C11 121.6(2) . . ?
C8 C9 C11 120.7(2) . . ?
C9 C10 C5 124.9(2) . . ?
C9 C10 H10 117.6 . . ?
C5 C10 H10 117.6 . . ?
C13 C11 C12 109.2(2) . . ?
C13 C11 C14 107.3(2) . . ?
C12 C11 C14 107.4(2) . . ?
C13 C11 C9 110.37(19) . . ?
C12 C11 C9 110.58(19) . . ?
C14 C11 C9 111.9(2) . . ?
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 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C7 127.3(2) . . ?
N1 C15 H15 116.4 . . ?
C7 C15 H15 116.4 . . ?
N1 C16 C17 107.2(4) . . ?
N1 C16 H16A 110.3 . . ?
C17 C16 H16A 110.3 . . ?
N1 C16 H16B 110.3 . . ?
C17 C16 H16B 110.3 . . ?
H16A C16 H16B 108.5 . . ?
N2 C17 C16 110.0(3) . . ?
N2 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
N2 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17' C16' N1 104.2(10) . . ?
C17' C16' H16C 110.9 . . ?
N1 C16' H16C 110.9 . . ?
C17' C16' H16D 110.9 . . ?
N1 C16' H16D 110.9 . . ?
H16C C16' H16D 108.9 . . ?
N2 C17' C16' 109.4(9) . . ?
N2 C17' H17C 109.8 . . ?
C16' C17' H17C 109.8 . . ?
N2 C17' H17D 109.8 . . ?
C16' C17' H17D 109.8 . . ?
H17C C17' H17D 108.2 . . ?
N2 C18' H18D 109.5 . . ?
N2 C18' H18E 109.5 . . ?
H18D C18' H18E 109.5 . . ?
N2 C18' H18F 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
N2 C19' H19D 120.0 . . ?
N2 C19' H19E 120.0 . . ?
H19D C19' H19E 120.0 . . ?
O4 C20 C23 108.9(2) . . ?
O4 C20 C21 108.61(19) . . ?
C23 C20 C21 110.7(3) . . ?
O4 C20 C22 109.1(2) . . ?
C23 C20 C22 110.8(3) . . ?
C21 C20 C22 108.6(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 C24 C27 108.4(2) . . ?
O2 C24 C25 109.2(2) . . ?
C27 C24 C25 110.1(2) . . ?
O2 C24 C26 108.0(2) . . ?
C27 C24 C26 111.2(3) . . ?
C25 C24 C26 109.7(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 O3 Zr1 157.66(15) . . ?
O3 C28 C31' 117.1(4) . . ?
O3 C28 C29 113.6(3) . . ?
O3 C28 C31 105.8(3) . . ?
C29 C28 C31 113.1(4) . . ?
O3 C28 C30' 105.3(4) . . ?
C31' C28 C30' 113.2(6) . . ?
O3 C28 C30 106.5(3) . . ?
C29 C28 C30 111.2(4) . . ?
C31 C28 C30 106.1(4) . . ?
O3 C28 C29' 106.9(3) . . ?
C31' C28 C29' 109.6(6) . . ?
C30' C28 C29' 103.9(6) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C30' H30D 109.5 . . ?
C28 C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C28 C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
C28 C29' H29D 109.5 . . ?
C28 C29' H29E 109.5 . . ?
H29D C29' H29E 109.5 . . ?
C28 C29' H29F 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
C28 C31' H31D 120.0 . . ?
C28 C31' H31E 120.0 . . ?
H31D C31' H31E 120.0 . . ?

_refine_diff_density_max         1.091
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.084

# start Validation Reply Form
_vrf_PLAT213_try3_A              
;
PROBLEM: Atom C1'_6           has ADP max/min Ratio .....        5.9 prolat
RESPONSE: This is due to disorder in the t-butoxide groups which was modeled.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_14_a
_database_code_depnum_ccdc_archive 'CCDC 1993770'
loop_
_audit_author_name
_audit_author_address
'Justin M. Burroughs'
;University of Tennessee, Knoxville 
United States of America
;
_audit_update_record             
;
2020-03-30 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C28 H52 N2 O4 Ti), C4 H8, C H3'
_chemical_formula_sum            'C17.43 H32.86 N1.14 O2.29 Ti0.57'
_chemical_formula_weight         322.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   26.1034(16)
_cell_length_b                   13.6068(8)
_cell_length_c                   18.7389(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.427(2)
_cell_angle_gamma                90
_cell_volume                     6655.6(7)
_cell_formula_units_Z            14
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9856
_cell_measurement_theta_min      2.6855
_cell_measurement_theta_max      31.5245

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_F_000             2468
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.290
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            202143
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.162
_diffrn_reflns_theta_max         31.541
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             22206
_reflns_number_gt                19440
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Apex3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0267P)²+11.5186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22206
_refine_ls_number_parameters     706
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1522
_refine_ls_wR_factor_gt          0.1482
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti2 Ti 0.04053(2) 0.33898(2) 0.78993(2) 0.01272(7) Uani 1 1 d . . . . .
Ti1 Ti 0.46071(2) 0.18286(2) 0.20206(2) 0.01156(6) Uani 1 1 d . . . . .
O1 O 0.41438(5) 0.18703(10) 0.28126(7) 0.0172(3) Uani 1 1 d . . . . .
N1 N 0.47781(6) 0.03394(11) 0.24346(8) 0.0141(3) Uani 1 1 d . . . . .
C1 C 0.31391(8) -0.08949(16) 0.46151(11) 0.0231(4) Uani 1 1 d . . . . .
O2 O 0.51653(5) 0.22391(10) 0.25714(7) 0.0157(2) Uani 1 1 d . . . . .
N2 N 0.51931(6) 0.11902(12) 0.12160(8) 0.0155(3) Uani 1 1 d . . . . .
C2 C 0.35066(10) -0.14344(19) 0.51239(13) 0.0324(5) Uani 1 1 d . . . . .
H2A H 0.378402 -0.173334 0.484928 0.049 Uiso 1 1 calc R U . . .
H2B H 0.331943 -0.194829 0.537939 0.049 Uiso 1 1 calc R U . . .
H2C H 0.365098 -0.096596 0.546799 0.049 Uiso 1 1 calc R U . . .
C61 C 0.3022(4) 0.9165(8) 0.7627(9) 0.289(9) Uani 1 1 d . . . . .
H61A H 0.314335 0.857462 0.738160 0.433 Uiso 1 1 calc R U . . .
H61B H 0.299567 0.903169 0.813959 0.433 Uiso 1 1 calc R U . . .
H61C H 0.326431 0.970438 0.755016 0.433 Uiso 1 1 calc R U . . .
O3 O 0.45623(5) 0.30119(10) 0.15470(7) 0.0166(2) Uani 1 1 d . . . . .
N3 N 0.02380(6) 0.48927(12) 0.75127(8) 0.0146(3) Uani 1 1 d . . . . .
C3 C 0.27094(8) -0.04377(19) 0.50594(12) 0.0280(5) Uani 1 1 d . . . . .
H3A H 0.246010 -0.012007 0.474096 0.042 Uiso 1 1 calc R U . . .
H3B H 0.285494 0.005210 0.538632 0.042 Uiso 1 1 calc R U . . .
H3C H 0.253842 -0.095297 0.533479 0.042 Uiso 1 1 calc R U . . .
C58 C 0.2522(4) 0.7683(10) 0.7215(5) 0.201(5) Uani 1 1 d D . . . .
H58A H 0.281403 0.773054 0.755395 0.241 Uiso 1 1 calc R U . . .
H58B H 0.266390 0.768741 0.672630 0.241 Uiso 1 1 calc R U . . .
C57 C 0.2216(4) 0.6591(9) 0.7350(4) 0.197(5) Uani 1 1 d . . . . .
H57A H 0.195337 0.649856 0.697969 0.296 Uiso 1 1 calc R U . . .
H57B H 0.205444 0.659551 0.782013 0.296 Uiso 1 1 calc R U . . .
H57C H 0.246480 0.605279 0.732711 0.296 Uiso 1 1 calc R U . . .
C56 C -0.09163(9) 0.24512(18) 0.67676(13) 0.0284(5) Uani 1 1 d . . . . .
H56A H -0.115759 0.260469 0.638024 0.043 Uiso 1 1 calc R U . . .
H56B H -0.109452 0.248091 0.722561 0.043 Uiso 1 1 calc R U . . .
H56C H -0.077743 0.178930 0.669782 0.043 Uiso 1 1 calc R U . . .
C55 C -0.01933(9) 0.31742(18) 0.60612(11) 0.0248(4) Uani 1 1 d . . . . .
H55A H -0.042920 0.333979 0.567004 0.037 Uiso 1 1 calc R U . . .
H55B H -0.005226 0.251574 0.598316 0.037 Uiso 1 1 calc R U . . .
H55C H 0.008637 0.365429 0.607716 0.037 Uiso 1 1 calc R U . . .
C54 C -0.04810(8) 0.31939(14) 0.67665(10) 0.0179(3) Uani 1 1 d . . . . .
H54 H -0.062849 0.386544 0.683434 0.021 Uiso 1 1 calc R U . . .
C53 C 0.17945(9) 0.4235(2) 0.83443(16) 0.0365(6) Uani 1 1 d . . . . .
H53A H 0.177527 0.394702 0.786567 0.055 Uiso 1 1 calc R U . . .
H53B H 0.187498 0.372043 0.869313 0.055 Uiso 1 1 calc R U . . .
H53C H 0.206322 0.473825 0.835689 0.055 Uiso 1 1 calc R U . . .
C52 C 0.13055(9) 0.51737(18) 0.92640(12) 0.0273(4) Uani 1 1 d . . . . .
H52A H 0.157303 0.567898 0.927216 0.041 Uiso 1 1 calc R U . . .
H52B H 0.138469 0.466999 0.962195 0.041 Uiso 1 1 calc R U . . .
H52C H 0.097404 0.547504 0.937190 0.041 Uiso 1 1 calc R U . . .
C51 C 0.12819(8) 0.47025(15) 0.85265(11) 0.0200(4) Uani 1 1 d . . . . .
H51 H 0.120563 0.522649 0.816695 0.024 Uiso 1 1 calc R U . . .
C50 C 0.12805(9) 0.15207(19) 0.86327(12) 0.0293(5) Uani 1 1 d . . . . .
H50A H 0.122936 0.098920 0.828651 0.044 Uiso 1 1 calc R U . . .
H50B H 0.149954 0.128780 0.902463 0.044 Uiso 1 1 calc R U . . .
H50C H 0.144485 0.208005 0.839748 0.044 Uiso 1 1 calc R U . . .
C39 C 0.16194(7) 0.25856(14) 0.61308(10) 0.0160(3) Uani 1 1 d . . . . .
C38 C 0.16665(7) 0.43667(15) 0.57053(10) 0.0177(3) Uani 1 1 d . . . . .
H38 H 0.192737 0.415530 0.538968 0.021 Uiso 1 1 calc R U . . .
C37 C 0.14485(7) 0.36669(14) 0.61506(9) 0.0150(3) Uani 1 1 d . . . . .
C36 C 0.10647(7) 0.39880(14) 0.66406(9) 0.0142(3) Uani 1 1 d . . . . .
C35 C 0.08994(7) 0.49796(14) 0.66030(9) 0.0154(3) Uani 1 1 d . . . . .
C34 C 0.11335(7) 0.56461(14) 0.61325(10) 0.0171(3) Uani 1 1 d . . . . .
H34 H 0.101696 0.630729 0.611938 0.021 Uiso 1 1 calc R U . . .
C33 C 0.15279(7) 0.53661(15) 0.56893(10) 0.0180(3) Uani 1 1 d . . . . .
C32 C 0.16121(9) 0.71408(16) 0.52663(13) 0.0267(4) Uani 1 1 d . . . . .
H32A H 0.181056 0.757529 0.495603 0.040 Uiso 1 1 calc R U . . .
H32B H 0.164328 0.736543 0.576165 0.040 Uiso 1 1 calc R U . . .
H32C H 0.125112 0.715421 0.511929 0.040 Uiso 1 1 calc R U . . .
C31 C 0.23832(10) 0.6077(2) 0.5412(2) 0.0558(10) Uani 1 1 d . . . . .
H31A H 0.251658 0.540540 0.537459 0.084 Uiso 1 1 calc R U . . .
H31B H 0.242398 0.631040 0.590359 0.084 Uiso 1 1 calc R U . . .
H31C H 0.257308 0.650838 0.508934 0.084 Uiso 1 1 calc R U . . .
C30 C 0.17648(13) 0.5771(2) 0.44172(14) 0.0418(7) Uani 1 1 d . . . . .
H30A H 0.140109 0.574274 0.428515 0.063 Uiso 1 1 calc R U . . .
H30B H 0.191962 0.512106 0.435268 0.063 Uiso 1 1 calc R U . . .
H30C H 0.193954 0.624929 0.411326 0.063 Uiso 1 1 calc R U . . .
O4 O 0.41280(5) 0.11963(10) 0.14326(7) 0.0177(3) Uani 1 1 d . . . . .
N4 N -0.01780(7) 0.39996(12) 0.87144(8) 0.0182(3) Uani 1 1 d . . . . .
C4 C 0.28992(11) -0.1634(2) 0.40930(15) 0.0368(6) Uani 1 1 d . . . . .
H4A H 0.266125 -0.129095 0.377185 0.055 Uiso 1 1 calc R U . . .
H4B H 0.271331 -0.213765 0.436069 0.055 Uiso 1 1 calc R U . . .
H4C H 0.316985 -0.194587 0.381269 0.055 Uiso 1 1 calc R U . . .
C59 C 0.2207(5) 0.8523(8) 0.7300(7) 0.283(10) Uani 1 1 d D . . . .
H59 H 0.185083 0.842567 0.737705 0.339 Uiso 1 1 calc R U . . .
C49 C 0.04953(9) 0.10010(17) 0.93030(11) 0.0255(4) Uani 1 1 d . . . . .
H49A H 0.015789 0.122458 0.946131 0.038 Uiso 1 1 calc R U . . .
H49B H 0.069895 0.079236 0.971754 0.038 Uiso 1 1 calc R U . . .
H49C H 0.045351 0.044672 0.897373 0.038 Uiso 1 1 calc R U . . .
C48 C 0.07677(8) 0.18372(15) 0.89252(10) 0.0198(4) Uani 1 1 d . . . . .
H48 H 0.082584 0.238130 0.927532 0.024 Uiso 1 1 calc R U . . .
C47 C -0.00327(10) 0.37136(17) 0.94506(10) 0.0257(4) Uani 1 1 d . . . . .
H47A H -0.007331 0.300194 0.950713 0.039 Uiso 1 1 calc R U . . .
H47B H -0.025382 0.405498 0.979063 0.039 Uiso 1 1 calc R U . . .
H47C H 0.032526 0.389464 0.954148 0.039 Uiso 1 1 calc R U . . .
C46 C -0.07080(8) 0.36577(16) 0.85860(12) 0.0254(4) Uani 1 1 d . . . . .
H46A H -0.082793 0.389574 0.812024 0.038 Uiso 1 1 calc R U . . .
H46B H -0.093152 0.391291 0.896081 0.038 Uiso 1 1 calc R U . . .
H46C H -0.071620 0.293768 0.859168 0.038 Uiso 1 1 calc R U . . .
C45 C -0.01571(8) 0.50885(14) 0.86619(10) 0.0179(3) Uani 1 1 d . . . . .
H45A H 0.016190 0.533026 0.889081 0.021 Uiso 1 1 calc R U . . .
H45B H -0.045109 0.537683 0.891874 0.021 Uiso 1 1 calc R U . . .
C44 C -0.01727(8) 0.54142(14) 0.78874(10) 0.0177(3) Uani 1 1 d . . . . .
H44A H -0.050927 0.525288 0.767043 0.021 Uiso 1 1 calc R U . . .
H44B H -0.011988 0.613325 0.785448 0.021 Uiso 1 1 calc R U . . .
C43 C 0.04873(7) 0.53697(14) 0.70351(9) 0.0153(3) Uani 1 1 d . . . . .
H43 H 0.039336 0.603616 0.695830 0.018 Uiso 1 1 calc R U . . .
C42 C 0.19927(8) 0.23837(16) 0.55192(11) 0.0235(4) Uani 1 1 d . . . . .
H42A H 0.183106 0.256470 0.506409 0.035 Uiso 1 1 calc R U . . .
H42B H 0.208075 0.168365 0.551287 0.035 Uiso 1 1 calc R U . . .
H42C H 0.230450 0.277381 0.558993 0.035 Uiso 1 1 calc R U . . .
C41 C 0.11566(8) 0.19004(16) 0.60192(12) 0.0230(4) Uani 1 1 d . . . . .
H41A H 0.098028 0.207364 0.557307 0.034 Uiso 1 1 calc R U . . .
H41B H 0.091988 0.197344 0.641918 0.034 Uiso 1 1 calc R U . . .
H41C H 0.127486 0.121780 0.599418 0.034 Uiso 1 1 calc R U . . .
C40 C 0.18964(9) 0.23230(17) 0.68320(11) 0.0255(4) Uani 1 1 d . . . . .
H40A H 0.200898 0.163638 0.681515 0.038 Uiso 1 1 calc R U . . .
H40B H 0.166202 0.241346 0.723271 0.038 Uiso 1 1 calc R U . . .
H40C H 0.219498 0.275191 0.689504 0.038 Uiso 1 1 calc R U . . .
C5 C 0.34315(7) -0.01241(15) 0.41787(10) 0.0178(3) Uani 1 1 d . . . . .
O5 O 0.08683(5) 0.33693(10) 0.71061(7) 0.0169(3) Uani 1 1 d . . . . .
C6 C 0.38448(7) -0.04041(14) 0.37642(10) 0.0172(3) Uani 1 1 d . . . . .
H6 H 0.396108 -0.106502 0.378709 0.021 Uiso 1 1 calc R U . . .
O6 O 0.08870(6) 0.39979(10) 0.84977(7) 0.0183(3) Uani 1 1 d . . . . .
C7 C 0.40966(7) 0.02580(14) 0.33122(9) 0.0148(3) Uani 1 1 d . . . . .
C60 C 0.2396(13) 0.9509(9) 0.7276(6) 0.70(3) Uani 1 1 d . . . . .
H60A H 0.220752 0.996222 0.759279 0.835 Uiso 1 1 calc R U . . .
H60B H 0.241014 0.977786 0.678518 0.835 Uiso 1 1 calc R U . . .
O7 O 0.04532(6) 0.21962(10) 0.83604(7) 0.0174(3) Uani 1 1 d . . . . .
C8 C 0.39295(7) 0.12516(14) 0.32648(9) 0.0144(3) Uani 1 1 d . . . . .
O8 O -0.01506(5) 0.29870(10) 0.73452(7) 0.0167(3) Uani 1 1 d . . . . .
C9 C 0.35297(7) 0.15701(14) 0.37249(9) 0.0147(3) Uani 1 1 d . . . . .
C10 C 0.32921(7) 0.08695(15) 0.41537(10) 0.0172(3) Uani 1 1 d . . . . .
H10 H 0.301818 0.107979 0.444759 0.021 Uiso 1 1 calc R U . . .
C11 C 0.33568(7) 0.26492(14) 0.37362(10) 0.0172(3) Uani 1 1 d . . . . .
C12 C 0.31074(10) 0.29233(18) 0.30194(12) 0.0293(5) Uani 1 1 d . . . . .
H12A H 0.335624 0.283522 0.263568 0.044 Uiso 1 1 calc R U . . .
H12B H 0.299640 0.361110 0.303281 0.044 Uiso 1 1 calc R U . . .
H12C H 0.281020 0.249884 0.293193 0.044 Uiso 1 1 calc R U . . .
C13 C 0.38165(8) 0.33213(16) 0.38900(12) 0.0242(4) Uani 1 1 d . . . . .
H13A H 0.406903 0.324960 0.350912 0.036 Uiso 1 1 calc R U . . .
H13B H 0.397325 0.313767 0.434773 0.036 Uiso 1 1 calc R U . . .
H13C H 0.370083 0.400575 0.391128 0.036 Uiso 1 1 calc R U . . .
C14 C 0.29611(9) 0.28452(17) 0.43208(12) 0.0257(4) Uani 1 1 d . . . . .
H14A H 0.287177 0.354476 0.432308 0.039 Uiso 1 1 calc R U . . .
H14B H 0.310601 0.266205 0.478601 0.039 Uiso 1 1 calc R U . . .
H14C H 0.265269 0.245398 0.422653 0.039 Uiso 1 1 calc R U . . .
C16 C 0.51978(7) -0.01843(14) 0.20798(10) 0.0164(3) Uani 1 1 d . . . . .
H16A H 0.515358 -0.090329 0.213165 0.020 Uiso 1 1 calc R U . . .
H16B H 0.553128 0.000366 0.229466 0.020 Uiso 1 1 calc R U . . .
C15 C 0.45247(7) -0.01342(14) 0.29090(10) 0.0151(3) Uani 1 1 d . . . . .
H15 H 0.462488 -0.079286 0.300389 0.018 Uiso 1 1 calc R U . . .
C17 C 0.51799(8) 0.01031(14) 0.12982(10) 0.0173(3) Uani 1 1 d . . . . .
H17A H 0.547587 -0.019027 0.104881 0.021 Uiso 1 1 calc R U . . .
H17B H 0.486268 -0.015802 0.107597 0.021 Uiso 1 1 calc R U . . .
C18 C 0.57197(8) 0.15591(16) 0.13305(12) 0.0238(4) Uani 1 1 d . . . . .
H18A H 0.594586 0.128321 0.096662 0.036 Uiso 1 1 calc R U . . .
H18B H 0.584143 0.136104 0.180517 0.036 Uiso 1 1 calc R U . . .
H18C H 0.572117 0.227773 0.129578 0.036 Uiso 1 1 calc R U . . .
C19 C 0.50402(9) 0.14342(17) 0.04742(10) 0.0246(4) Uani 1 1 d . . . . .
H19A H 0.527142 0.110567 0.014068 0.037 Uiso 1 1 calc R U . . .
H19B H 0.505974 0.214698 0.040435 0.037 Uiso 1 1 calc R U . . .
H19C H 0.468826 0.121151 0.038676 0.037 Uiso 1 1 calc R U . . .
C22 C 0.45800(10) 0.41679(17) 0.05773(12) 0.0276(4) Uani 1 1 d . . . . .
H22A H 0.491084 0.389688 0.043120 0.041 Uiso 1 1 calc R U . . .
H22B H 0.463694 0.472353 0.090108 0.041 Uiso 1 1 calc R U . . .
H22C H 0.438996 0.439234 0.015478 0.041 Uiso 1 1 calc R U . . .
C29 C 0.18184(8) 0.60851(16) 0.52067(12) 0.0246(4) Uani 1 1 d . . . . .
C28 C 0.37270(9) -0.00353(18) 0.07004(12) 0.0267(4) Uani 1 1 d . . . . .
H28A H 0.366050 0.044575 0.032174 0.040 Uiso 1 1 calc R U . . .
H28B H 0.345533 -0.053243 0.069798 0.040 Uiso 1 1 calc R U . . .
H28C H 0.405816 -0.035364 0.061844 0.040 Uiso 1 1 calc R U . . .
C27 C 0.32223(9) 0.0946(2) 0.15845(17) 0.0394(6) Uani 1 1 d . . . . .
H27A H 0.313844 0.143719 0.121953 0.059 Uiso 1 1 calc R U . . .
H27B H 0.323885 0.126327 0.205354 0.059 Uiso 1 1 calc R U . . .
H27C H 0.295742 0.043558 0.158752 0.059 Uiso 1 1 calc R U . . .
C26 C 0.37379(7) 0.04828(15) 0.14183(11) 0.0186(3) Uani 1 1 d . . . . .
H26 H 0.381569 -0.001675 0.179520 0.022 Uiso 1 1 calc R U . . .
C25 C 0.51866(9) 0.20663(18) 0.38534(11) 0.0255(4) Uani 1 1 d . . . . .
H25A H 0.504904 0.273032 0.391752 0.038 Uiso 1 1 calc R U . . .
H25B H 0.541583 0.190622 0.425331 0.038 Uiso 1 1 calc R U . . .
H25C H 0.490384 0.159284 0.383699 0.038 Uiso 1 1 calc R U . . .
C24 C 0.59330(9) 0.27342(19) 0.31696(13) 0.0299(5) Uani 1 1 d . . . . .
H24A H 0.611260 0.270210 0.271281 0.045 Uiso 1 1 calc R U . . .
H24B H 0.616951 0.255673 0.355715 0.045 Uiso 1 1 calc R U . . .
H24C H 0.580580 0.340344 0.324569 0.045 Uiso 1 1 calc R U . . .
C23 C 0.54831(7) 0.20189(14) 0.31588(10) 0.0174(3) Uani 1 1 d . . . . .
H23 H 0.561946 0.133726 0.309922 0.021 Uiso 1 1 calc R U . . .
C21 C 0.37604(9) 0.3765(2) 0.12157(13) 0.0319(5) Uani 1 1 d . . . . .
H21A H 0.356242 0.401492 0.080808 0.048 Uiso 1 1 calc R U . . .
H21B H 0.381851 0.429693 0.155917 0.048 Uiso 1 1 calc R U . . .
H21C H 0.356991 0.323272 0.144583 0.048 Uiso 1 1 calc R U . . .
C20 C 0.42724(8) 0.33764(15) 0.09582(10) 0.0192(4) Uani 1 1 d . . . . .
H20 H 0.420771 0.282376 0.061743 0.023 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti2 O7 1.8435(14) . ?
Ti2 O8 1.8605(14) . ?
Ti2 O6 1.8714(14) . ?
Ti2 O5 1.9230(13) . ?
Ti2 N3 2.2118(16) . ?
Ti2 N4 2.3183(16) . ?
Ti1 O3 1.8418(14) . ?
Ti1 O2 1.8650(14) . ?
Ti1 O4 1.8702(14) . ?
Ti1 O1 1.9223(13) . ?
Ti1 N1 2.2140(16) . ?
Ti1 N2 2.3243(15) . ?
O1 C8 1.322(2) . ?
N1 C15 1.285(2) . ?
N1 C16 1.470(2) . ?
C1 C4 1.534(3) . ?
C1 C3 1.534(3) . ?
C1 C2 1.534(3) . ?
C1 C5 1.536(3) . ?
O2 C23 1.406(2) . ?
N2 C18 1.478(3) . ?
N2 C19 1.481(3) . ?
N2 C17 1.488(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C61 C60 1.82(3) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
O3 C20 1.422(2) . ?
N3 C43 1.286(2) . ?
N3 C44 1.469(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C58 C59 1.419(13) . ?
C58 C57 1.707(13) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C56 C54 1.521(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C55 C54 1.525(3) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C54 O8 1.409(2) . ?
C54 H54 1.0000 . ?
C53 C51 1.522(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C52 C51 1.524(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C51 O6 1.409(2) . ?
C51 H51 1.0000 . ?
C50 C48 1.513(3) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C39 C42 1.535(3) . ?
C39 C40 1.537(3) . ?
C39 C37 1.538(3) . ?
C39 C41 1.539(3) . ?
C38 C37 1.391(3) . ?
C38 C33 1.407(3) . ?
C38 H38 0.9500 . ?
C37 C36 1.432(2) . ?
C36 O5 1.319(2) . ?
C36 C35 1.418(3) . ?
C35 C34 1.408(2) . ?
C35 C43 1.452(3) . ?
C34 C33 1.381(3) . ?
C34 H34 0.9500 . ?
C33 C29 1.536(3) . ?
C32 C29 1.538(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C31 C29 1.521(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 C29 1.545(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O4 C26 1.407(2) . ?
N4 C46 1.478(3) . ?
N4 C47 1.480(3) . ?
N4 C45 1.486(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C59 C60 1.431(16) . ?
C59 H59 0.9500 . ?
C49 C48 1.519(3) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C48 O7 1.421(2) . ?
C48 H48 1.0000 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C45 C44 1.518(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C43 H43 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C5 C6 1.388(3) . ?
C5 C10 1.401(3) . ?
C6 C7 1.403(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.423(3) . ?
C7 C15 1.455(2) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C8 C9 1.426(2) . ?
C9 C10 1.395(3) . ?
C9 C11 1.536(3) . ?
C10 H10 0.9500 . ?
C11 C13 1.534(3) . ?
C11 C12 1.534(3) . ?
C11 C14 1.535(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 C17 1.516(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C15 H15 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 C20 1.524(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C28 C26 1.519(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27 C26 1.520(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26 H26 1.0000 . ?
C25 C23 1.521(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C24 C23 1.525(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 H23 1.0000 . ?
C21 C20 1.519(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20 1.0000 . ?

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
O7 Ti2 O8 92.98(6) . . ?
O7 Ti2 O6 93.76(6) . . ?
O8 Ti2 O6 169.24(6) . . ?
O7 Ti2 O5 107.98(6) . . ?
O8 Ti2 O5 93.23(6) . . ?
O6 Ti2 O5 92.65(6) . . ?
O7 Ti2 N3 168.69(6) . . ?
O8 Ti2 N3 86.47(6) . . ?
O6 Ti2 N3 85.27(6) . . ?
O5 Ti2 N3 83.33(6) . . ?
O7 Ti2 N4 92.81(6) . . ?
O8 Ti2 N4 87.70(6) . . ?
O6 Ti2 N4 83.60(6) . . ?
O5 Ti2 N4 159.09(6) . . ?
N3 Ti2 N4 75.87(6) . . ?
O3 Ti1 O2 92.95(6) . . ?
O3 Ti1 O4 94.50(6) . . ?
O2 Ti1 O4 168.55(6) . . ?
O3 Ti1 O1 107.95(6) . . ?
O2 Ti1 O1 93.28(6) . . ?
O4 Ti1 O1 92.68(6) . . ?
O3 Ti1 N1 168.77(6) . . ?
O2 Ti1 N1 85.73(6) . . ?
O4 Ti1 N1 85.27(6) . . ?
O1 Ti1 N1 83.27(6) . . ?
O3 Ti1 N2 93.09(6) . . ?
O2 Ti1 N2 87.46(6) . . ?
O4 Ti1 N2 83.47(6) . . ?
O1 Ti1 N2 158.87(6) . . ?
N1 Ti1 N2 75.72(6) . . ?
C8 O1 Ti1 138.41(12) . . ?
C15 N1 C16 117.31(16) . . ?
C15 N1 Ti1 126.71(13) . . ?
C16 N1 Ti1 115.74(11) . . ?
C4 C1 C3 108.39(19) . . ?
C4 C1 C2 109.5(2) . . ?
C3 C1 C2 108.25(18) . . ?
C4 C1 C5 108.07(17) . . ?
C3 C1 C5 112.35(18) . . ?
C2 C1 C5 110.28(17) . . ?
C23 O2 Ti1 145.46(12) . . ?
C18 N2 C19 107.70(16) . . ?
C18 N2 C17 110.18(16) . . ?
C19 N2 C17 108.29(15) . . ?
C18 N2 Ti1 113.26(12) . . ?
C19 N2 Ti1 110.55(12) . . ?
C17 N2 Ti1 106.77(11) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C20 O3 Ti1 135.24(13) . . ?
C43 N3 C44 117.62(16) . . ?
C43 N3 Ti2 126.51(13) . . ?
C44 N3 Ti2 115.67(11) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C59 C58 C57 114.3(8) . . ?
C59 C58 H58A 108.7 . . ?
C57 C58 H58A 108.7 . . ?
C59 C58 H58B 108.7 . . ?
C57 C58 H58B 108.7 . . ?
H58A C58 H58B 107.6 . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C58 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O8 C54 C56 108.62(16) . . ?
O8 C54 C55 111.15(16) . . ?
C56 C54 C55 111.24(18) . . ?
O8 C54 H54 108.6 . . ?
C56 C54 H54 108.6 . . ?
C55 C54 H54 108.6 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C51 C53 110.58(17) . . ?
O6 C51 C52 110.22(17) . . ?
C53 C51 C52 110.44(19) . . ?
O6 C51 H51 108.5 . . ?
C53 C51 H51 108.5 . . ?
C52 C51 H51 108.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C42 C39 C40 107.43(16) . . ?
C42 C39 C37 112.04(16) . . ?
C40 C39 C37 109.66(16) . . ?
C42 C39 C41 106.99(16) . . ?
C40 C39 C41 109.83(17) . . ?
C37 C39 C41 110.81(16) . . ?
C37 C38 C33 124.62(18) . . ?
C37 C38 H38 117.7 . . ?
C33 C38 H38 117.7 . . ?
C38 C37 C36 117.84(17) . . ?
C38 C37 C39 121.37(16) . . ?
C36 C37 C39 120.78(16) . . ?
O5 C36 C35 121.38(16) . . ?
O5 C36 C37 120.43(17) . . ?
C35 C36 C37 118.19(16) . . ?
C34 C35 C36 120.71(17) . . ?
C34 C35 C43 116.15(17) . . ?
C36 C35 C43 123.13(16) . . ?
C33 C34 C35 121.87(18) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 H34 119.1 . . ?
C34 C33 C38 116.51(17) . . ?
C34 C33 C29 123.48(18) . . ?
C38 C33 C29 119.99(18) . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 O4 Ti1 144.03(13) . . ?
C46 N4 C47 107.59(17) . . ?
C46 N4 C45 109.76(17) . . ?
C47 N4 C45 108.33(16) . . ?
C46 N4 Ti2 113.50(12) . . ?
C47 N4 Ti2 110.79(13) . . ?
C45 N4 Ti2 106.77(11) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C58 C59 C60 123.4(18) . . ?
C58 C59 H59 118.3 . . ?
C60 C59 H59 118.3 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O7 C48 C50 109.61(16) . . ?
O7 C48 C49 109.56(17) . . ?
C50 C48 C49 111.96(18) . . ?
O7 C48 H48 108.5 . . ?
C50 C48 H48 108.5 . . ?
C49 C48 H48 108.5 . . ?
N4 C47 H47A 109.5 . . ?
N4 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N4 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N4 C46 H46A 109.5 . . ?
N4 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N4 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N4 C45 C44 110.71(15) . . ?
N4 C45 H45A 109.5 . . ?
C44 C45 H45A 109.5 . . ?
N4 C45 H45B 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 108.1 . . ?
N3 C44 C45 107.55(15) . . ?
N3 C44 H44A 110.2 . . ?
C45 C44 H44A 110.2 . . ?
N3 C44 H44B 110.2 . . ?
C45 C44 H44B 110.2 . . ?
H44A C44 H44B 108.5 . . ?
N3 C43 C35 125.75(17) . . ?
N3 C43 H43 117.1 . . ?
C35 C43 H43 117.1 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C6 C5 C10 116.69(17) . . ?
C6 C5 C1 120.13(18) . . ?
C10 C5 C1 123.15(18) . . ?
C36 O5 Ti2 138.73(12) . . ?
C5 C6 C7 122.09(18) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C51 O6 Ti2 144.31(13) . . ?
C6 C7 C8 120.19(17) . . ?
C6 C7 C15 116.29(17) . . ?
C8 C7 C15 123.52(16) . . ?
C59 C60 C61 93.3(14) . . ?
C59 C60 H60A 113.1 . . ?
C61 C60 H60A 113.1 . . ?
C59 C60 H60B 113.1 . . ?
C61 C60 H60B 113.1 . . ?
H60A C60 H60B 110.4 . . ?
C48 O7 Ti2 133.53(12) . . ?
O1 C8 C7 120.94(16) . . ?
O1 C8 C9 120.61(17) . . ?
C7 C8 C9 118.44(16) . . ?
C54 O8 Ti2 147.25(12) . . ?
C10 C9 C8 118.10(17) . . ?
C10 C9 C11 120.88(16) . . ?
C8 C9 C11 121.01(16) . . ?
C9 C10 C5 124.22(17) . . ?
C9 C10 H10 117.9 . . ?
C5 C10 H10 117.9 . . ?
C13 C11 C12 110.22(18) . . ?
C13 C11 C14 106.98(16) . . ?
C12 C11 C14 107.41(17) . . ?
C13 C11 C9 110.04(16) . . ?
C12 C11 C9 110.07(16) . . ?
C14 C11 C9 112.04(16) . . ?
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 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C16 C17 107.10(15) . . ?
N1 C16 H16A 110.3 . . ?
C17 C16 H16A 110.3 . . ?
N1 C16 H16B 110.3 . . ?
C17 C16 H16B 110.3 . . ?
H16A C16 H16B 108.5 . . ?
N1 C15 C7 125.20(17) . . ?
N1 C15 H15 117.4 . . ?
C7 C15 H15 117.4 . . ?
N2 C17 C16 110.85(15) . . ?
N2 C17 H17A 109.5 . . ?
C16 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C31 C29 C33 109.16(19) . . ?
C31 C29 C32 109.1(2) . . ?
C33 C29 C32 112.16(17) . . ?
C31 C29 C30 108.7(2) . . ?
C33 C29 C30 110.22(19) . . ?
C32 C29 C30 107.38(19) . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 C26 C28 110.24(17) . . ?
O4 C26 C27 110.59(18) . . ?
C28 C26 C27 111.29(18) . . ?
O4 C26 H26 108.2 . . ?
C28 C26 H26 108.2 . . ?
C27 C26 H26 108.2 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C23 C25 111.10(16) . . ?
O2 C23 C24 108.92(16) . . ?
C25 C23 C24 111.00(18) . . ?
O2 C23 H23 108.6 . . ?
C25 C23 H23 108.6 . . ?
C24 C23 H23 108.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C20 C21 109.82(16) . . ?
O3 C20 C22 109.30(17) . . ?
C21 C20 C22 111.76(18) . . ?
O3 C20 H20 108.6 . . ?
C21 C20 H20 108.6 . . ?
C22 C20 H20 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Ti1 O2 C23 169.2(2) . . . . ?
O4 Ti1 O2 C23 -60.3(4) . . . . ?
O1 Ti1 O2 C23 61.0(2) . . . . ?
N1 Ti1 O2 C23 -22.0(2) . . . . ?
N2 Ti1 O2 C23 -97.8(2) . . . . ?
O2 Ti1 O3 C20 172.53(17) . . . . ?
O4 Ti1 O3 C20 1.23(18) . . . . ?
O1 Ti1 O3 C20 -93.06(17) . . . . ?
N1 Ti1 O3 C20 89.6(4) . . . . ?
N2 Ti1 O3 C20 84.91(17) . . . . ?
C33 C38 C37 C36 -1.6(3) . . . . ?
C33 C38 C37 C39 179.54(18) . . . . ?
C42 C39 C37 C38 -6.9(3) . . . . ?
C40 C39 C37 C38 112.3(2) . . . . ?
C41 C39 C37 C38 -126.32(19) . . . . ?
C42 C39 C37 C36 174.29(17) . . . . ?
C40 C39 C37 C36 -66.5(2) . . . . ?
C41 C39 C37 C36 54.9(2) . . . . ?
C38 C37 C36 O5 -175.69(17) . . . . ?
C39 C37 C36 O5 3.1(3) . . . . ?
C38 C37 C36 C35 5.1(3) . . . . ?
C39 C37 C36 C35 -176.05(16) . . . . ?
O5 C36 C35 C34 176.23(17) . . . . ?
C37 C36 C35 C34 -4.6(3) . . . . ?
O5 C36 C35 C43 -3.8(3) . . . . ?
C37 C36 C35 C43 175.35(17) . . . . ?
C36 C35 C34 C33 0.3(3) . . . . ?
C43 C35 C34 C33 -179.60(18) . . . . ?
C35 C34 C33 C38 3.2(3) . . . . ?
C35 C34 C33 C29 -175.59(19) . . . . ?
C37 C38 C33 C34 -2.5(3) . . . . ?
C37 C38 C33 C29 176.27(19) . . . . ?
O3 Ti1 O4 C26 -146.3(2) . . . . ?
O2 Ti1 O4 C26 83.3(4) . . . . ?
O1 Ti1 O4 C26 -38.0(2) . . . . ?
N1 Ti1 O4 C26 45.0(2) . . . . ?
N2 Ti1 O4 C26 121.1(2) . . . . ?
C57 C58 C59 C60 174.1(10) . . . . ?
C46 N4 C45 C44 -76.7(2) . . . . ?
C47 N4 C45 C44 166.04(17) . . . . ?
Ti2 N4 C45 C44 46.67(18) . . . . ?
C43 N3 C44 C45 -141.68(17) . . . . ?
Ti2 N3 C44 C45 33.38(19) . . . . ?
N4 C45 C44 N3 -53.6(2) . . . . ?
C44 N3 C43 C35 -179.12(17) . . . . ?
Ti2 N3 C43 C35 6.4(3) . . . . ?
C34 C35 C43 N3 -177.41(18) . . . . ?
C36 C35 C43 N3 2.7(3) . . . . ?
C4 C1 C5 C6 -62.7(3) . . . . ?
C3 C1 C5 C6 177.79(19) . . . . ?
C2 C1 C5 C6 56.9(3) . . . . ?
C4 C1 C5 C10 115.1(2) . . . . ?
C3 C1 C5 C10 -4.5(3) . . . . ?
C2 C1 C5 C10 -125.3(2) . . . . ?
C35 C36 O5 Ti2 -6.5(3) . . . . ?
C37 C36 O5 Ti2 174.37(14) . . . . ?
C10 C5 C6 C7 -3.2(3) . . . . ?
C1 C5 C6 C7 174.67(18) . . . . ?
C53 C51 O6 Ti2 -88.2(3) . . . . ?
C52 C51 O6 Ti2 149.36(18) . . . . ?
O7 Ti2 O6 C51 145.7(2) . . . . ?
O8 Ti2 O6 C51 -85.6(4) . . . . ?
O5 Ti2 O6 C51 37.5(2) . . . . ?
N3 Ti2 O6 C51 -45.6(2) . . . . ?
N4 Ti2 O6 C51 -121.8(2) . . . . ?
C5 C6 C7 C8 -0.3(3) . . . . ?
C5 C6 C7 C15 179.91(18) . . . . ?
C58 C59 C60 C61 -30.4(16) . . . . ?
C50 C48 O7 Ti2 -82.2(2) . . . . ?
C49 C48 O7 Ti2 154.61(14) . . . . ?
O8 Ti2 O7 C48 -176.02(17) . . . . ?
O6 Ti2 O7 C48 -4.41(18) . . . . ?
O5 Ti2 O7 C48 89.60(17) . . . . ?
N3 Ti2 O7 C48 -89.1(4) . . . . ?
N4 Ti2 O7 C48 -88.18(17) . . . . ?
Ti1 O1 C8 C7 11.1(3) . . . . ?
Ti1 O1 C8 C9 -169.86(14) . . . . ?
C6 C7 C8 O1 -176.19(17) . . . . ?
C15 C7 C8 O1 3.6(3) . . . . ?
C6 C7 C8 C9 4.7(3) . . . . ?
C15 C7 C8 C9 -175.44(17) . . . . ?
C56 C54 O8 Ti2 -170.86(18) . . . . ?
C55 C54 O8 Ti2 66.4(3) . . . . ?
O7 Ti2 O8 C54 -170.1(2) . . . . ?
O6 Ti2 O8 C54 61.2(4) . . . . ?
O5 Ti2 O8 C54 -61.9(2) . . . . ?
N3 Ti2 O8 C54 21.2(2) . . . . ?
N4 Ti2 O8 C54 97.2(2) . . . . ?
O1 C8 C9 C10 175.39(17) . . . . ?
C7 C8 C9 C10 -5.5(3) . . . . ?
O1 C8 C9 C11 -3.2(3) . . . . ?
C7 C8 C9 C11 175.84(17) . . . . ?
C8 C9 C10 C5 2.1(3) . . . . ?
C11 C9 C10 C5 -179.28(18) . . . . ?
C6 C5 C10 C9 2.3(3) . . . . ?
C1 C5 C10 C9 -175.52(18) . . . . ?
C10 C9 C11 C13 125.98(19) . . . . ?
C8 C9 C11 C13 -55.4(2) . . . . ?
C10 C9 C11 C12 -112.4(2) . . . . ?
C8 C9 C11 C12 66.2(2) . . . . ?
C10 C9 C11 C14 7.1(3) . . . . ?
C8 C9 C11 C14 -174.34(17) . . . . ?
C15 N1 C16 C17 139.96(17) . . . . ?
Ti1 N1 C16 C17 -34.81(18) . . . . ?
C16 N1 C15 C7 -179.66(17) . . . . ?
Ti1 N1 C15 C7 -5.5(3) . . . . ?
C6 C7 C15 N1 175.00(18) . . . . ?
C8 C7 C15 N1 -4.8(3) . . . . ?
C18 N2 C17 C16 76.99(19) . . . . ?
C19 N2 C17 C16 -165.45(16) . . . . ?
Ti1 N2 C17 C16 -46.39(17) . . . . ?
N1 C16 C17 N2 54.2(2) . . . . ?
C34 C33 C29 C31 120.1(3) . . . . ?
C38 C33 C29 C31 -58.7(3) . . . . ?
C34 C33 C29 C32 -1.0(3) . . . . ?
C38 C33 C29 C32 -179.77(19) . . . . ?
C34 C33 C29 C30 -120.6(2) . . . . ?
C38 C33 C29 C30 60.7(3) . . . . ?
Ti1 O4 C26 C28 -147.23(18) . . . . ?
Ti1 O4 C26 C27 89.3(3) . . . . ?
Ti1 O2 C23 C25 -66.5(3) . . . . ?
Ti1 O2 C23 C24 170.90(18) . . . . ?
Ti1 O3 C20 C21 86.8(2) . . . . ?
Ti1 O3 C20 C22 -150.25(15) . . . . ?

_refine_diff_density_max         1.778
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.074


# start Validation Reply Form
_vrf_PLAT413_14_a                
;
PROBLEM: Short Inter XH3 .. XHn     H58A     ..H61A     .       1.47 Ang.  
RESPONSE: Due to the disordered of co-crystalized pentane solvent.
;
_vrf_PLAT260_14_a                
;
PROBLEM: Large Average Ueq of Residue Including       C57      0.344 Check 
RESPONSE: Due to the disordered of co-crystalized pentane solvent.
;
# end Validation Reply Form
