# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_exp_9319
_database_code_depnum_ccdc_archive 'CCDC 2222254'
loop_
_audit_author_name
_audit_author_address
'Hanhua Xu'
;Peking University
China
;
_audit_update_record             
;
2022-11-25 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_audit_creation_date             2022-06-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C24 H31 Cl N2 O2 Ti), 0.5(C6 H6), 0.5(C4 H10 O), 0.5(C4 H8 O)'
_chemical_formula_sum            'C55 H74 Cl2 N4 O5 Ti2'
_chemical_formula_weight         1037.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Ti Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   27.7408(8)
_cell_length_b                   16.6115(4)
_cell_length_c                   24.3585(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11224.8(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16116
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.4420
_cell_measurement_theta_min      2.2270
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.919
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49340
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.088
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00   2.00   0.50    3.65    --  -15.70  57.00  30.00   60
  2  ω      7.00  57.00   0.50    3.65    --  -15.70  57.00 120.00  100
  3  ω     31.00  74.00   0.50    3.65    --  -15.70  57.00  30.00   86
  4  ω    -15.00  85.00   0.50    3.65    --   15.80  82.00 -30.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0052274000
_diffrn_orient_matrix_UB_12      0.0257465000
_diffrn_orient_matrix_UB_13      -0.0224648000
_diffrn_orient_matrix_UB_21      0.0057695000
_diffrn_orient_matrix_UB_22      -0.0314971000
_diffrn_orient_matrix_UB_23      -0.0185454000
_diffrn_orient_matrix_UB_31      -0.0243372000
_diffrn_orient_matrix_UB_32      -0.0129945000
_diffrn_orient_matrix_UB_33      0.0004677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10330
_reflns_number_total             12844
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12844
_refine_ls_number_restraints     275
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0795P)²+11.7322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1560
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C62-C56 = C56-O23 = O23-C12 = C42-C12
 1.54 with sigma of 0.01
 O57-C63 = O57-C51 = C51-C23 = C66-C23 = C66-C63
 1.54 with sigma of 0.01
 O23-C42
 2.5 with sigma of 0.01
 C62-O23
 2.5 with sigma of 0.01
 C56-C12
 2.5 with sigma of 0.01
 C23-C63
 2.5 with sigma of 0.01
 C63-C51
 2.5 with sigma of 0.01
 C66-O57
 2.5 with sigma of 0.01
 O57-C23
 2.5 with sigma of 0.01
 C51-C66
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C40 \\sim C28 \\sim C14 \\sim C2 \\sim C3: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3A
C62 \\sim C56 \\sim O23 \\sim C12 \\sim C42: within 3A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3A
C23 \\sim C66 \\sim C63 \\sim O57 \\sim C51: within 3A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3A
Uanis(C14) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O57) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(O57) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: C3(0.5) H3(0.5) C1(0.5) H1(0.5) C40(0.5) H40(0.5) C28(0.5)
 H28(0.5) C14(0.5) H14(0.5) C2(0.5) H2(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C56(0.5) H56A(0.5) H56B(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C62(0.5)
 H62A(0.5) H62B(0.5) H62C(0.5) O23(0.5) C63(0.5) H63A(0.5) H63B(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) O57(0.5) C66(0.5) H66A(0.5) H66B(0.5) C51(0.5) H51A(0.5)
 H51B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C39(H39A,H39B), C43(H43A,H43B), C12(H12A,
 H12B), C56(H56A,H56B), C63(H63A,H63B), C23(H23A,H23B), C66(H66A,H66B),
 C51(H51A,H51B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C36(H36), C34(H34), C50(H50), C8(H8), C35(H35), C49(H49),
 C48(H48), C22(H22), C21(H21), C20(H20), C3(H3), C1(H1), C40(H40), C28(H28),
 C14(H14), C2(H2)
5.c Fitted hexagon refined as free rotating group:
 C3(C1,C40,C28,C14,C2)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C30(H30A,H30B,
 H30C), C60(H60A,H60B,H60C), C31(H31A,H31B,H31C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C42(H42A,H42B,H42C), C62(H62A,H62B,
 H62C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.29156(2) 0.07488(2) 0.18223(2) 0.02202(10) Uani 1 1 d . . . . .
Ti2 Ti 0.21521(2) 0.58391(2) 0.49103(2) 0.02451(11) Uani 1 1 d . . . . .
Cl3 Cl 0.27409(2) 0.20894(3) 0.19992(3) 0.03436(15) Uani 1 1 d . . . . .
Cl4 Cl 0.24004(3) 0.71413(3) 0.47283(3) 0.03927(17) Uani 1 1 d . . . . .
O28 O 0.34890(6) 0.09359(10) 0.14784(6) 0.0277(3) Uani 1 1 d . . . . .
O1 O 0.18775(6) -0.04535(9) 0.25017(6) 0.0264(3) Uani 1 1 d . . . . .
O56 O 0.19471(6) 0.55767(9) 0.42257(6) 0.0289(4) Uani 1 1 d . . . . .
O51 O 0.34129(6) 0.39225(10) 0.52527(7) 0.0322(4) Uani 1 1 d . . . . .
N12 N 0.26460(7) 0.08101(11) 0.10298(7) 0.0228(4) Uani 1 1 d . . . . .
N42 N 0.25809(7) 0.41591(11) 0.57035(7) 0.0251(4) Uani 1 1 d . . . . .
N14 N 0.21301(7) 0.05867(11) 0.17020(7) 0.0227(4) Uani 1 1 d . . . . .
N40 N 0.20859(7) 0.44996(11) 0.50338(7) 0.0243(4) Uani 1 1 d . . . . .
C6 C 0.36441(8) 0.13373(13) 0.10256(9) 0.0252(5) Uani 1 1 d . . . . .
C5 C 0.33527(8) 0.13856(13) 0.05547(9) 0.0242(4) Uani 1 1 d . . . . .
C38 C 0.17484(9) 0.50065(13) 0.38958(9) 0.0258(5) Uani 1 1 d . . . . .
C13 C 0.21971(8) 0.08623(12) 0.11669(9) 0.0234(4) Uani 1 1 d . . . . .
C33 C 0.16169(9) 0.42841(14) 0.41484(9) 0.0279(5) Uani 1 1 d . . . . .
C37 C 0.16686(9) 0.51476(13) 0.33326(9) 0.0281(5) Uani 1 1 d . . . . .
C45 C 0.32820(9) 0.36184(14) 0.62088(10) 0.0279(5) Uani 1 1 d . . . . .
C18 C 0.17847(9) 0.01666(13) 0.28506(9) 0.0281(5) Uani 1 1 d . . . . .
C11 C 0.28614(9) 0.10014(15) 0.05037(9) 0.0290(5) Uani 1 1 d . . . . .
H11A H 0.264951 0.136446 0.030623 0.035 Uiso 1 1 calc R U . . .
H11B H 0.289011 0.051122 0.028976 0.035 Uiso 1 1 calc R U . . .
C10 C 0.35261(9) 0.17932(15) 0.00969(10) 0.0308(5) Uani 1 1 d . . . . .
H10 H 0.333554 0.183285 -0.021596 0.037 Uiso 1 1 calc R U . . .
C46 C 0.35796(9) 0.36445(14) 0.57420(10) 0.0288(5) Uani 1 1 d . . . . .
C15 C 0.17291(9) 0.09993(14) 0.19949(9) 0.0289(5) Uani 1 1 d . . . . .
H15A H 0.142558 0.077591 0.186876 0.035 Uiso 1 1 calc R U . . .
H15B H 0.173292 0.156539 0.189735 0.035 Uiso 1 1 calc R U . . .
C17 C 0.17516(10) 0.09268(14) 0.26113(10) 0.0312(5) Uani 1 1 d . . . . .
C39 C 0.16431(9) 0.41788(14) 0.47616(9) 0.0284(5) Uani 1 1 d . . . . .
H39A H 0.136485 0.444040 0.492386 0.034 Uiso 1 1 calc R U . . .
H39B H 0.161908 0.360875 0.484336 0.034 Uiso 1 1 calc R U . . .
C9 C 0.39772(10) 0.21385(18) 0.01023(11) 0.0417(6) Uani 1 1 d . . . . .
H9 H 0.409284 0.239973 -0.020865 0.050 Uiso 1 1 calc R U . . .
C57 C 0.17816(10) 0.59657(14) 0.30634(9) 0.0325(5) Uani 1 1 d . . . . .
C36 C 0.14579(10) 0.45222(15) 0.30396(10) 0.0353(6) Uani 1 1 d . . . . .
H36 H 0.139615 0.459441 0.266755 0.042 Uiso 1 1 calc R U . . .
C34 C 0.14119(10) 0.36774(14) 0.38340(10) 0.0339(5) Uani 1 1 d . . . . .
H34 H 0.132573 0.319210 0.399710 0.041 Uiso 1 1 calc R U . . .
C7 C 0.41029(9) 0.17065(15) 0.10465(10) 0.0316(5) Uani 1 1 d . . . . .
C19 C 0.17177(10) 0.00405(15) 0.34178(10) 0.0349(6) Uani 1 1 d . . . . .
C43 C 0.27658(9) 0.38955(18) 0.62293(10) 0.0357(6) Uani 1 1 d . . . . .
H43A H 0.256684 0.345725 0.636320 0.043 Uiso 1 1 calc R U . . .
H43B H 0.273978 0.433573 0.648920 0.043 Uiso 1 1 calc R U . . .
C50 C 0.34655(10) 0.33097(17) 0.66968(11) 0.0367(6) Uani 1 1 d . . . . .
H50 H 0.327219 0.329361 0.700855 0.044 Uiso 1 1 calc R U . . .
C8 C 0.42600(10) 0.20967(18) 0.05729(11) 0.0418(6) Uani 1 1 d . . . . .
H8 H 0.456297 0.233632 0.057134 0.050 Uiso 1 1 calc R U . . .
C24 C 0.16871(12) -0.07991(15) 0.36765(10) 0.0407(7) Uani 1 1 d . . . . .
C35 C 0.13361(11) 0.37928(15) 0.32818(11) 0.0388(6) Uani 1 1 d . . . . .
H35 H 0.120332 0.338268 0.307050 0.047 Uiso 1 1 calc R U . . .
C16 C 0.17957(10) 0.12011(19) 0.08284(10) 0.0407(6) Uani 1 1 d . . . . .
H16A H 0.170575 0.171923 0.096968 0.061 Uiso 1 1 calc R U . . .
H16B H 0.152328 0.084539 0.084362 0.061 Uiso 1 1 calc R U . . .
H16C H 0.190042 0.125602 0.045464 0.061 Uiso 1 1 calc R U . . .
C47 C 0.40630(10) 0.33767(17) 0.57603(11) 0.0382(6) Uani 1 1 d . . . . .
C58 C 0.16941(13) 0.59327(17) 0.24430(11) 0.0471(8) Uani 1 1 d . . . . .
H58A H 0.189980 0.553221 0.228213 0.071 Uiso 1 1 calc R U . . .
H58B H 0.176438 0.644843 0.228420 0.071 Uiso 1 1 calc R U . . .
H58C H 0.136331 0.579666 0.237366 0.071 Uiso 1 1 calc R U . . .
C29 C 0.44104(10) 0.17132(19) 0.15746(11) 0.0420(6) Uani 1 1 d . . . . .
C49 C 0.39327(11) 0.3027(2) 0.67208(13) 0.0501(8) Uani 1 1 d . . . . .
H49 H 0.405190 0.281316 0.704632 0.060 Uiso 1 1 calc R U . . .
C48 C 0.42247(11) 0.3063(2) 0.62590(13) 0.0523(8) Uani 1 1 d . . . . .
H48 H 0.453914 0.287220 0.628265 0.063 Uiso 1 1 calc R U . . .
C22 C 0.16898(13) 0.15989(16) 0.29428(11) 0.0476(8) Uani 1 1 d . . . . .
H22 H 0.167884 0.211110 0.278913 0.057 Uiso 1 1 calc R U . . .
C59 C 0.14419(13) 0.65996(17) 0.33038(12) 0.0475(7) Uani 1 1 d . . . . .
H59A H 0.111384 0.644269 0.323821 0.071 Uiso 1 1 calc R U . . .
H59B H 0.150250 0.710992 0.313224 0.071 Uiso 1 1 calc R U . . .
H59C H 0.149612 0.664400 0.369187 0.071 Uiso 1 1 calc R U . . .
C30 C 0.41487(12) 0.2207(2) 0.20120(12) 0.0543(8) Uani 1 1 d . . . . .
H30A H 0.383845 0.197277 0.208260 0.081 Uiso 1 1 calc R U . . .
H30B H 0.410822 0.274936 0.188427 0.081 Uiso 1 1 calc R U . . .
H30C H 0.433512 0.220864 0.234411 0.081 Uiso 1 1 calc R U . . .
C60 C 0.23027(11) 0.62223(18) 0.31539(12) 0.0473(7) Uani 1 1 d . . . . .
H60A H 0.236146 0.628525 0.353987 0.071 Uiso 1 1 calc R U . . .
H60B H 0.236010 0.672466 0.297030 0.071 Uiso 1 1 calc R U . . .
H60C H 0.251495 0.581878 0.300841 0.071 Uiso 1 1 calc R U . . .
C31 C 0.49035(11) 0.2105(3) 0.14748(14) 0.0636(10) Uani 1 1 d . . . . .
H31A H 0.485861 0.264310 0.134023 0.095 Uiso 1 1 calc R U . . .
H31B H 0.507951 0.179609 0.120888 0.095 Uiso 1 1 calc R U . . .
H31C H 0.508102 0.212149 0.181299 0.095 Uiso 1 1 calc R U . . .
C21 C 0.16448(16) 0.14981(18) 0.35034(12) 0.0624(10) Uani 1 1 d . . . . .
H21 H 0.161376 0.194577 0.372995 0.075 Uiso 1 1 calc R U . . .
C20 C 0.16457(15) 0.07366(17) 0.37285(11) 0.0549(9) Uani 1 1 d . . . . .
H20 H 0.159601 0.068412 0.410440 0.066 Uiso 1 1 calc R U . . .
C52 C 0.43916(11) 0.3407(2) 0.52490(13) 0.0518(8) Uani 1 1 d . . . . .
C25 C 0.20998(14) -0.13439(18) 0.34974(13) 0.0552(8) Uani 1 1 d . . . . .
H25A H 0.240139 -0.107739 0.356291 0.083 Uiso 1 1 calc R U . . .
H25B H 0.206903 -0.146131 0.311305 0.083 Uiso 1 1 calc R U . . .
H25C H 0.208900 -0.183644 0.370317 0.083 Uiso 1 1 calc R U . . .
C26 C 0.1709(2) -0.0757(2) 0.43051(12) 0.0768(14) Uani 1 1 d . . . . .
H26A H 0.143406 -0.046668 0.444001 0.115 Uiso 1 1 calc R U . . .
H26B H 0.199864 -0.048568 0.441532 0.115 Uiso 1 1 calc R U . . .
H26C H 0.170737 -0.129246 0.445347 0.115 Uiso 1 1 calc R U . . .
C27 C 0.12044(15) -0.1167(2) 0.35055(17) 0.0667(10) Uani 1 1 d . . . . .
H27A H 0.119226 -0.121181 0.311279 0.100 Uiso 1 1 calc R U . . .
H27B H 0.094618 -0.082793 0.362962 0.100 Uiso 1 1 calc R U . . .
H27C H 0.117191 -0.169139 0.366659 0.100 Uiso 1 1 calc R U . . .
C32 C 0.45042(13) 0.0856(2) 0.17815(15) 0.0631(10) Uani 1 1 d . . . . .
H32A H 0.468747 0.056478 0.151247 0.095 Uiso 1 1 calc R U . . .
H32B H 0.420226 0.058769 0.184202 0.095 Uiso 1 1 calc R U . . .
H32C H 0.468159 0.087795 0.211955 0.095 Uiso 1 1 calc R U . . .
C53 C 0.49145(12) 0.3190(3) 0.53989(17) 0.0822(14) Uani 1 1 d . . . . .
H53A H 0.502929 0.355228 0.567676 0.123 Uiso 1 1 calc R U . . .
H53B H 0.511429 0.323468 0.507849 0.123 Uiso 1 1 calc R U . . .
H53C H 0.492625 0.264800 0.553486 0.123 Uiso 1 1 calc R U . . .
C54 C 0.42046(14) 0.2786(2) 0.48277(14) 0.0685(11) Uani 1 1 d . . . . .
H54A H 0.420777 0.225863 0.498940 0.103 Uiso 1 1 calc R U . . .
H54B H 0.440847 0.279026 0.450928 0.103 Uiso 1 1 calc R U . . .
H54C H 0.388117 0.292203 0.472261 0.103 Uiso 1 1 calc R U . . .
C55 C 0.43959(14) 0.4252(3) 0.49771(18) 0.0742(12) Uani 1 1 d . . . . .
H55A H 0.408442 0.436229 0.482296 0.111 Uiso 1 1 calc R U . . .
H55B H 0.463451 0.426367 0.469175 0.111 Uiso 1 1 calc R U . . .
H55C H 0.447152 0.465124 0.524843 0.111 Uiso 1 1 calc R U . . .
C3 C 0.4602(5) -0.0656(7) 0.0587(5) 0.174(4) Uani 0.5 1 d G U P A -1
H3 H 0.439883 -0.094201 0.081956 0.208 Uiso 0.5 1 calc R U P A -1
C1 C 0.5099(6) -0.0731(6) 0.0638(4) 0.181(4) Uani 0.5 1 d G U P A -1
H1 H 0.522834 -0.106824 0.090483 0.217 Uiso 0.5 1 calc R U P A -1
C40 C 0.5402(4) -0.0303(9) 0.0290(6) 0.184(4) Uani 0.5 1 d G U P A -1
H40 H 0.573491 -0.035370 0.032444 0.221 Uiso 0.5 1 calc R U P A -1
C28 C 0.5209(5) 0.0201(10) -0.0109(6) 0.184(4) Uani 0.5 1 d G U P A -1
H28 H 0.541197 0.048707 -0.034123 0.221 Uiso 0.5 1 calc R U P A -1
C14 C 0.4712(6) 0.0276(9) -0.0160(6) 0.182(4) Uani 0.5 1 d G U P A -1
H14 H 0.458246 0.061331 -0.042651 0.218 Uiso 0.5 1 calc R U P A -1
C2 C 0.4408(4) -0.0152(8) 0.0188(6) 0.171(4) Uani 0.5 1 d G U P A -1
H2 H 0.407588 -0.010123 0.015388 0.206 Uiso 0.5 1 calc R U P A -1
C12 C 0.4961(6) 0.4898(13) 0.1728(6) 0.185(5) Uani 0.5 1 d D U P B -1
H12A H 0.505694 0.542463 0.159546 0.223 Uiso 0.5 1 calc R U P B -1
H12B H 0.523404 0.453622 0.169186 0.223 Uiso 0.5 1 calc R U P B -1
C56 C 0.5133(7) 0.4431(10) 0.2684(6) 0.188(5) Uani 0.5 1 d D U P B -1
H56A H 0.546647 0.455419 0.259799 0.226 Uiso 0.5 1 calc R U P B -1
H56B H 0.507681 0.386865 0.259767 0.226 Uiso 0.5 1 calc R U P B -1
C42 C 0.4536(4) 0.4582(6) 0.1391(4) 0.104(3) Uani 0.5 1 d D U P B -1
H42A H 0.460405 0.464619 0.100666 0.156 Uiso 0.5 1 calc R U P B -1
H42B H 0.425073 0.488072 0.148280 0.156 Uiso 0.5 1 calc R U P B -1
H42C H 0.448599 0.402283 0.147078 0.156 Uiso 0.5 1 calc R U P B -1
C62 C 0.5042(6) 0.4575(9) 0.3306(6) 0.133(5) Uani 0.5 1 d D U P B -1
H62A H 0.496002 0.407429 0.347913 0.200 Uiso 0.5 1 calc R U P B -1
H62B H 0.478104 0.494937 0.335060 0.200 Uiso 0.5 1 calc R U P B -1
H62C H 0.532783 0.479069 0.347195 0.200 Uiso 0.5 1 calc R U P B -1
O23 O 0.4804(5) 0.4953(8) 0.2339(5) 0.206(4) Uani 0.5 1 d D U P B -1
C63 C 0.5388(4) -0.2098(7) 0.1901(4) 0.135(3) Uani 0.5 1 d D U P C -1
H63A H 0.573304 -0.218728 0.188205 0.162 Uiso 0.5 1 calc R U P C -1
H63B H 0.526083 -0.211036 0.153030 0.162 Uiso 0.5 1 calc R U P C -1
C23 C 0.4878(5) -0.2352(7) 0.2730(5) 0.150(3) Uani 0.5 1 d D U P C -1
H23A H 0.453413 -0.245488 0.270236 0.180 Uiso 0.5 1 calc R U P C -1
H23B H 0.499126 -0.255864 0.307883 0.180 Uiso 0.5 1 calc R U P C -1
O57 O 0.5288(3) -0.1278(5) 0.2158(5) 0.174(3) Uani 0.5 1 d D U P C -1
C66 C 0.5151(4) -0.2773(5) 0.2244(5) 0.134(3) Uani 0.5 1 d D U P C -1
H66A H 0.539534 -0.313672 0.238544 0.161 Uiso 0.5 1 calc R U P C -1
H66B H 0.492799 -0.307932 0.202018 0.161 Uiso 0.5 1 calc R U P C -1
C51 C 0.4979(5) -0.1434(7) 0.2688(5) 0.150(3) Uani 0.5 1 d D U P C -1
H51A H 0.515217 -0.125187 0.301080 0.180 Uiso 0.5 1 calc R U P C -1
H51B H 0.467717 -0.113953 0.266625 0.180 Uiso 0.5 1 calc R U P C -1
C41 C 0.21328(8) 0.42165(13) 0.55683(9) 0.0257(5) Uani 1 1 d . . . . .
C4 C 0.17137(10) 0.3984(2) 0.59197(10) 0.0433(7) Uani 1 1 d . . . . .
H4A H 0.160255 0.345881 0.581564 0.065 Uiso 1 1 calc R U . . .
H4B H 0.145811 0.436753 0.587136 0.065 Uiso 1 1 calc R U . . .
H4C H 0.181119 0.397778 0.629781 0.065 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
Ti1 Ti1 3.3920(8) 2 ?
Ti1 Cl3 2.3194(7) . ?
Ti1 O28 1.8243(17) . ?
Ti1 O1 1.8191(15) 2 ?
Ti1 N12 2.0726(18) . ?
Ti1 N14 2.2151(19) . ?
Ti1 N14 2.2414(18) 2 ?
Ti1 C13 2.561(2) . ?
Ti2 Ti2 3.3905(8) 2_565 ?
Ti2 Cl4 2.3131(7) . ?
Ti2 O56 1.8150(15) . ?
Ti2 O51 1.8192(18) 2_565 ?
Ti2 N42 2.0692(18) 2_565 ?
Ti2 N40 2.2527(19) . ?
Ti2 N40 2.208(2) 2_565 ?
Ti2 C41 2.552(2) 2_565 ?
O28 C6 1.359(3) . ?
O1 C18 1.360(3) . ?
O56 C38 1.359(3) . ?
O51 C46 1.359(3) . ?
N12 C13 1.292(3) . ?
N12 C11 1.449(3) . ?
N42 C43 1.448(3) . ?
N42 C41 1.290(3) . ?
N14 C13 1.394(3) . ?
N14 C15 1.489(3) . ?
N40 C39 1.494(3) . ?
N40 C41 1.391(3) . ?
C6 C5 1.405(3) . ?
C6 C7 1.414(3) . ?
C5 C11 1.510(3) . ?
C5 C10 1.390(3) . ?
C38 C33 1.397(3) . ?
C38 C37 1.409(3) . ?
C13 C16 1.496(3) . ?
C33 C39 1.506(3) . ?
C33 C34 1.388(3) . ?
C37 C57 1.541(3) . ?
C37 C36 1.389(3) . ?
C45 C46 1.406(3) . ?
C45 C43 1.505(3) . ?
C45 C50 1.391(3) . ?
C18 C17 1.394(3) . ?
C18 C19 1.410(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10 H10 0.9300 . ?
C10 C9 1.377(4) . ?
C46 C47 1.414(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C17 1.508(3) . ?
C17 C22 1.388(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C9 H9 0.9300 . ?
C9 C8 1.391(4) . ?
C57 C58 1.532(3) . ?
C57 C59 1.530(4) . ?
C57 C60 1.523(4) . ?
C36 H36 0.9300 . ?
C36 C35 1.389(4) . ?
C34 H34 0.9300 . ?
C34 C35 1.375(3) . ?
C7 C8 1.393(3) . ?
C7 C29 1.544(3) . ?
C19 C24 1.533(3) . ?
C19 C20 1.396(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C50 H50 0.9300 . ?
C50 C49 1.380(4) . ?
C8 H8 0.9300 . ?
C24 C25 1.523(4) . ?
C24 C26 1.534(4) . ?
C24 C27 1.530(5) . ?
C35 H35 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C47 C48 1.396(4) . ?
C47 C52 1.544(4) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C29 C30 1.528(4) . ?
C29 C31 1.534(4) . ?
C29 C32 1.533(5) . ?
C49 H49 0.9300 . ?
C49 C48 1.387(5) . ?
C48 H48 0.9300 . ?
C22 H22 0.9300 . ?
C22 C21 1.382(4) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C21 H21 0.9300 . ?
C21 C20 1.379(4) . ?
C20 H20 0.9300 . ?
C52 C53 1.538(4) . ?
C52 C54 1.545(5) . ?
C52 C55 1.552(5) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C3 H3 0.9300 . ?
C3 C1 1.3900 . ?
C3 C2 1.3900 . ?
C1 H1 0.9300 . ?
C1 C40 1.3900 . ?
C40 H40 0.9300 . ?
C40 C28 1.3900 . ?
C28 H28 0.9300 . ?
C28 C14 1.3900 . ?
C14 H14 0.9300 . ?
C14 C2 1.3900 . ?
C2 H2 0.9300 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C42 1.530(9) . ?
C12 O23 1.554(9) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C62 1.554(9) . ?
C56 O23 1.514(9) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 O57 1.525(8) . ?
C63 C66 1.544(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C66 1.570(8) . ?
C23 C51 1.554(8) . ?
O57 C51 1.573(8) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C41 C4 1.494(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 Ti1 Ti1 124.20(3) . 2 ?
Cl3 Ti1 C13 83.25(5) . . ?
O28 Ti1 Ti1 135.86(5) . 2 ?
O28 Ti1 Cl3 95.97(6) . . ?
O28 Ti1 N12 83.03(7) . . ?
O28 Ti1 N14 144.85(7) . . ?
O28 Ti1 N14 99.09(7) . 2 ?
O28 Ti1 C13 112.33(7) . . ?
O1 Ti1 Ti1 90.95(5) 2 2 ?
O1 Ti1 Cl3 98.96(5) 2 . ?
O1 Ti1 O28 100.88(7) 2 . ?
O1 Ti1 N12 167.01(7) 2 . ?
O1 Ti1 N14 113.44(7) 2 . ?
O1 Ti1 N14 82.52(7) 2 2 ?
O1 Ti1 C13 146.37(8) 2 . ?
N12 Ti1 Ti1 77.92(5) . 2 ?
N12 Ti1 Cl3 92.89(5) . . ?
N12 Ti1 N14 61.82(7) . . ?
N12 Ti1 N14 84.63(7) . 2 ?
N12 Ti1 C13 30.10(7) . . ?
N14 Ti1 Ti1 40.15(5) 2 2 ?
N14 Ti1 Ti1 40.72(5) . 2 ?
N14 Ti1 Cl3 86.31(5) . . ?
N14 Ti1 Cl3 164.32(6) 2 . ?
N14 Ti1 N14 78.86(8) . 2 ?
N14 Ti1 C13 86.98(7) 2 . ?
N14 Ti1 C13 32.94(7) . . ?
C13 Ti1 Ti1 61.63(5) . 2 ?
Cl4 Ti2 Ti2 126.83(3) . 2_565 ?
Cl4 Ti2 C41 85.57(5) . 2_565 ?
O56 Ti2 Ti2 88.91(5) . 2_565 ?
O56 Ti2 Cl4 98.15(5) . . ?
O56 Ti2 O51 101.74(8) . 2_565 ?
O56 Ti2 N42 166.03(7) . 2_565 ?
O56 Ti2 N40 111.35(8) . 2_565 ?
O56 Ti2 N40 81.95(7) . . ?
O56 Ti2 C41 144.29(8) . 2_565 ?
O51 Ti2 Ti2 132.03(6) 2_565 2_565 ?
O51 Ti2 Cl4 98.09(6) 2_565 . ?
O51 Ti2 N42 83.11(7) 2_565 2_565 ?
O51 Ti2 N40 94.79(8) 2_565 . ?
O51 Ti2 N40 144.87(7) 2_565 2_565 ?
O51 Ti2 C41 112.93(7) 2_565 2_565 ?
N42 Ti2 Ti2 78.32(5) 2_565 2_565 ?
N42 Ti2 Cl4 94.07(6) 2_565 . ?
N42 Ti2 N40 62.00(7) 2_565 2_565 ?
N42 Ti2 N40 84.61(7) 2_565 . ?
N42 Ti2 C41 30.16(7) 2_565 2_565 ?
N40 Ti2 Ti2 40.04(5) . 2_565 ?
N40 Ti2 Ti2 41.02(5) 2_565 2_565 ?
N40 Ti2 Cl4 88.82(5) 2_565 . ?
N40 Ti2 Cl4 166.80(6) . . ?
N40 Ti2 N40 78.95(8) 2_565 . ?
N40 Ti2 C41 86.78(7) . 2_565 ?
N40 Ti2 C41 32.97(7) 2_565 2_565 ?
C41 Ti2 Ti2 61.82(5) 2_565 2_565 ?
C6 O28 Ti1 137.08(15) . . ?
C18 O1 Ti1 146.36(14) . 2 ?
C38 O56 Ti2 146.90(14) . . ?
C46 O51 Ti2 140.28(15) . 2_565 ?
C13 N12 Ti1 96.34(13) . . ?
C13 N12 C11 127.68(19) . . ?
C11 N12 Ti1 133.27(15) . . ?
C43 N42 Ti2 134.41(15) . 2_565 ?
C41 N42 Ti2 96.12(14) . 2_565 ?
C41 N42 C43 126.1(2) . . ?
Ti1 N14 Ti1 99.13(7) . 2 ?
C13 N14 Ti1 87.28(13) . . ?
C13 N14 Ti1 117.05(13) . 2 ?
C13 N14 C15 113.37(18) . . ?
C15 N14 Ti1 110.54(13) . 2 ?
C15 N14 Ti1 128.01(14) . . ?
Ti2 N40 Ti2 98.93(8) 2_565 . ?
C39 N40 Ti2 111.11(13) . . ?
C39 N40 Ti2 129.47(14) . 2_565 ?
C41 N40 Ti2 116.84(14) . . ?
C41 N40 Ti2 87.24(13) . 2_565 ?
C41 N40 C39 111.83(18) . . ?
O28 C6 C5 120.6(2) . . ?
O28 C6 C7 117.9(2) . . ?
C5 C6 C7 121.5(2) . . ?
C6 C5 C11 124.20(19) . . ?
C10 C5 C6 118.9(2) . . ?
C10 C5 C11 116.9(2) . . ?
O56 C38 C33 116.38(19) . . ?
O56 C38 C37 121.6(2) . . ?
C33 C38 C37 122.0(2) . . ?
N12 C13 Ti1 53.56(11) . . ?
N12 C13 N14 110.38(19) . . ?
N12 C13 C16 126.9(2) . . ?
N14 C13 Ti1 59.78(11) . . ?
N14 C13 C16 122.7(2) . . ?
C16 C13 Ti1 161.99(17) . . ?
C38 C33 C39 121.6(2) . . ?
C34 C33 C38 119.2(2) . . ?
C34 C33 C39 118.9(2) . . ?
C38 C37 C57 121.9(2) . . ?
C36 C37 C38 116.2(2) . . ?
C36 C37 C57 121.8(2) . . ?
C46 C45 C43 125.2(2) . . ?
C50 C45 C46 119.2(2) . . ?
C50 C45 C43 115.6(2) . . ?
O1 C18 C17 115.93(19) . . ?
O1 C18 C19 121.7(2) . . ?
C17 C18 C19 122.4(2) . . ?
N12 C11 C5 113.09(18) . . ?
N12 C11 H11A 109.0 . . ?
N12 C11 H11B 109.0 . . ?
C5 C11 H11A 109.0 . . ?
C5 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C5 C10 H10 119.7 . . ?
C9 C10 C5 120.7(2) . . ?
C9 C10 H10 119.7 . . ?
O51 C46 C45 121.3(2) . . ?
O51 C46 C47 117.2(2) . . ?
C45 C46 C47 121.5(2) . . ?
N14 C15 H15A 108.7 . . ?
N14 C15 H15B 108.7 . . ?
N14 C15 C17 114.18(19) . . ?
H15A C15 H15B 107.6 . . ?
C17 C15 H15A 108.7 . . ?
C17 C15 H15B 108.7 . . ?
C18 C17 C15 119.4(2) . . ?
C22 C17 C18 119.6(2) . . ?
C22 C17 C15 120.7(2) . . ?
N40 C39 C33 116.01(19) . . ?
N40 C39 H39A 108.3 . . ?
N40 C39 H39B 108.3 . . ?
C33 C39 H39A 108.3 . . ?
C33 C39 H39B 108.3 . . ?
H39A C39 H39B 107.4 . . ?
C10 C9 H9 120.0 . . ?
C10 C9 C8 120.0(2) . . ?
C8 C9 H9 120.0 . . ?
C58 C57 C37 110.9(2) . . ?
C59 C57 C37 108.6(2) . . ?
C59 C57 C58 107.8(2) . . ?
C60 C57 C37 112.2(2) . . ?
C60 C57 C58 107.6(2) . . ?
C60 C57 C59 109.7(2) . . ?
C37 C36 H36 118.8 . . ?
C37 C36 C35 122.4(2) . . ?
C35 C36 H36 118.8 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.1(2) . . ?
C35 C34 H34 120.0 . . ?
C6 C7 C29 122.0(2) . . ?
C8 C7 C6 117.0(2) . . ?
C8 C7 C29 120.9(2) . . ?
C18 C19 C24 123.1(2) . . ?
C20 C19 C18 115.3(2) . . ?
C20 C19 C24 121.5(2) . . ?
N42 C43 C45 113.60(19) . . ?
N42 C43 H43A 108.8 . . ?
N42 C43 H43B 108.8 . . ?
C45 C43 H43A 108.8 . . ?
C45 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C45 C50 H50 119.8 . . ?
C49 C50 C45 120.3(3) . . ?
C49 C50 H50 119.8 . . ?
C9 C8 C7 122.0(2) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C19 C24 C26 111.5(2) . . ?
C25 C24 C19 112.4(2) . . ?
C25 C24 C26 106.5(3) . . ?
C25 C24 C27 110.0(3) . . ?
C27 C24 C19 107.4(3) . . ?
C27 C24 C26 108.9(3) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 C36 120.0(2) . . ?
C34 C35 H35 120.0 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C46 C47 C52 121.6(2) . . ?
C48 C47 C46 116.7(3) . . ?
C48 C47 C52 121.6(3) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C30 C29 C7 108.8(2) . . ?
C30 C29 C31 107.8(3) . . ?
C30 C29 C32 110.5(3) . . ?
C31 C29 C7 111.3(2) . . ?
C32 C29 C7 111.2(2) . . ?
C32 C29 C31 107.2(3) . . ?
C50 C49 H49 120.0 . . ?
C50 C49 C48 120.0(3) . . ?
C48 C49 H49 120.0 . . ?
C47 C48 H48 118.9 . . ?
C49 C48 C47 122.3(3) . . ?
C49 C48 H48 118.9 . . ?
C17 C22 H22 120.4 . . ?
C21 C22 C17 119.2(3) . . ?
C21 C22 H22 120.4 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C22 C21 H21 119.9 . . ?
C20 C21 C22 120.3(3) . . ?
C20 C21 H21 119.9 . . ?
C19 C20 H20 118.5 . . ?
C21 C20 C19 123.0(3) . . ?
C21 C20 H20 118.5 . . ?
C47 C52 C54 108.4(3) . . ?
C47 C52 C55 112.2(3) . . ?
C53 C52 C47 111.0(3) . . ?
C53 C52 C54 108.5(3) . . ?
C53 C52 C55 107.8(3) . . ?
C54 C52 C55 108.8(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C1 C3 H3 120.0 . . ?
C1 C3 C2 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C1 H1 120.0 . . ?
C3 C1 C40 120.0 . . ?
C40 C1 H1 120.0 . . ?
C1 C40 H40 120.0 . . ?
C28 C40 C1 120.0 . . ?
C28 C40 H40 120.0 . . ?
C40 C28 H28 120.0 . . ?
C40 C28 C14 120.0 . . ?
C14 C28 H28 120.0 . . ?
C28 C14 H14 120.0 . . ?
C28 C14 C2 120.0 . . ?
C2 C14 H14 120.0 . . ?
C3 C2 H2 120.0 . . ?
C14 C2 C3 120.0 . . ?
C14 C2 H2 120.0 . . ?
H12A C12 H12B 108.4 . . ?
C42 C12 H12A 110.0 . . ?
C42 C12 H12B 110.0 . . ?
C42 C12 O23 108.6(9) . . ?
O23 C12 H12A 110.0 . . ?
O23 C12 H12B 110.0 . . ?
H56A C56 H56B 108.1 . . ?
C62 C56 H56A 109.5 . . ?
C62 C56 H56B 109.5 . . ?
O23 C56 H56A 109.5 . . ?
O23 C56 H56B 109.5 . . ?
O23 C56 C62 110.8(9) . . ?
C12 C42 H42A 109.5 . . ?
C12 C42 H42B 109.5 . . ?
C12 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C56 C62 H62A 109.5 . . ?
C56 C62 H62B 109.5 . . ?
C56 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C56 O23 C12 109.2(8) . . ?
H63A C63 H63B 108.1 . . ?
O57 C63 H63A 109.5 . . ?
O57 C63 H63B 109.5 . . ?
O57 C63 C66 110.5(5) . . ?
C66 C63 H63A 109.5 . . ?
C66 C63 H63B 109.5 . . ?
H23A C23 H23B 108.5 . . ?
C66 C23 H23A 110.2 . . ?
C66 C23 H23B 110.2 . . ?
C51 C23 H23A 110.2 . . ?
C51 C23 H23B 110.2 . . ?
C51 C23 C66 107.5(5) . . ?
C63 O57 C51 106.7(5) . . ?
C63 C66 C23 106.8(5) . . ?
C63 C66 H66A 110.4 . . ?
C63 C66 H66B 110.4 . . ?
C23 C66 H66A 110.4 . . ?
C23 C66 H66B 110.4 . . ?
H66A C66 H66B 108.6 . . ?
C23 C51 O57 108.3(5) . . ?
C23 C51 H51A 110.0 . . ?
C23 C51 H51B 110.0 . . ?
O57 C51 H51A 110.0 . . ?
O57 C51 H51B 110.0 . . ?
H51A C51 H51B 108.4 . . ?
N42 C41 Ti2 53.72(11) . 2_565 ?
N42 C41 N40 110.7(2) . . ?
N42 C41 C4 125.8(2) . . ?
N40 C41 Ti2 59.79(11) . 2_565 ?
N40 C41 C4 123.4(2) . . ?
C4 C41 Ti2 162.78(19) . 2_565 ?
C41 C4 H4A 109.5 . . ?
C41 C4 H4B 109.5 . . ?
C41 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 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 Ti1 O28 C6 96.0(2) 2 . . . ?
Ti1 O28 C6 C5 -33.4(3) . . . . ?
Ti1 O28 C6 C7 146.07(19) . . . . ?
Ti1 O1 C18 C17 15.8(4) 2 . . . ?
Ti1 O1 C18 C19 -165.4(2) 2 . . . ?
Ti1 N12 C13 N14 -19.68(18) . . . . ?
Ti1 N12 C13 C16 157.5(2) . . . . ?
Ti1 N12 C11 C5 -13.8(3) . . . . ?
Ti1 N14 C13 Ti1 -98.86(12) 2 . . . ?
Ti1 N14 C13 N12 -80.59(19) 2 . . . ?
Ti1 N14 C13 N12 18.27(17) . . . . ?
Ti1 N14 C13 C16 -159.1(2) . . . . ?
Ti1 N14 C13 C16 102.1(2) 2 . . . ?
Ti1 N14 C15 C17 65.8(2) 2 . . . ?
Ti1 N14 C15 C17 -54.7(3) . . . . ?
Ti2 Ti2 O56 C38 53.3(3) 2_565 . . . ?
Ti2 O56 C38 C33 2.6(4) . . . . ?
Ti2 O56 C38 C37 -179.0(2) . . . . ?
Ti2 O51 C46 C45 -14.6(4) 2_565 . . . ?
Ti2 O51 C46 C47 164.9(2) 2_565 . . . ?
Ti2 N42 C43 C45 5.8(4) 2_565 . . . ?
Ti2 N42 C41 N40 -19.01(19) 2_565 . . . ?
Ti2 N42 C41 C4 158.7(2) 2_565 . . . ?
Ti2 N40 C39 C33 -60.8(3) 2_565 . . . ?
Ti2 N40 C39 C33 61.4(2) . . . . ?
Ti2 N40 C41 Ti2 -98.62(12) . . . 2_565 ?
Ti2 N40 C41 N42 17.69(18) 2_565 . . . ?
Ti2 N40 C41 N42 -80.9(2) . . . . ?
Ti2 N40 C41 C4 101.3(2) . . . . ?
Ti2 N40 C41 C4 -160.1(2) 2_565 . . . ?
Cl3 Ti1 O28 C6 -60.8(2) . . . . ?
Cl4 Ti2 O56 C38 -179.6(3) . . . . ?
O28 C6 C5 C11 -0.9(3) . . . . ?
O28 C6 C5 C10 -179.2(2) . . . . ?
O28 C6 C7 C8 178.4(2) . . . . ?
O28 C6 C7 C29 -4.2(4) . . . . ?
O1 Ti1 O28 C6 -161.2(2) 2 . . . ?
O1 C18 C17 C15 10.9(4) . . . . ?
O1 C18 C17 C22 -175.7(3) . . . . ?
O1 C18 C19 C24 -7.1(4) . . . . ?
O1 C18 C19 C20 177.4(3) . . . . ?
O56 C38 C33 C39 6.6(3) . . . . ?
O56 C38 C33 C34 180.0(2) . . . . ?
O56 C38 C37 C57 -2.6(4) . . . . ?
O56 C38 C37 C36 -179.2(2) . . . . ?
O51 Ti2 O56 C38 -79.5(3) 2_565 . . . ?
O51 C46 C47 C48 -177.6(2) . . . . ?
O51 C46 C47 C52 0.7(4) . . . . ?
N12 Ti1 O28 C6 31.4(2) . . . . ?
N42 Ti2 O56 C38 29.6(5) 2_565 . . . ?
N14 Ti1 O28 C6 114.8(2) 2 . . . ?
N14 Ti1 O28 C6 31.3(3) . . . . ?
N14 C15 C17 C18 -54.0(3) . . . . ?
N14 C15 C17 C22 132.7(3) . . . . ?
N40 Ti2 O56 C38 88.5(3) 2_565 . . . ?
N40 Ti2 O56 C38 13.7(3) . . . . ?
C6 C5 C11 N12 19.5(3) . . . . ?
C6 C5 C10 C9 0.5(4) . . . . ?
C6 C7 C8 C9 1.2(4) . . . . ?
C6 C7 C29 C30 -64.9(3) . . . . ?
C6 C7 C29 C31 176.4(3) . . . . ?
C6 C7 C29 C32 57.1(4) . . . . ?
C5 C6 C7 C8 -2.1(4) . . . . ?
C5 C6 C7 C29 175.3(2) . . . . ?
C5 C10 C9 C8 -1.4(4) . . . . ?
C38 C33 C39 N40 -43.5(3) . . . . ?
C38 C33 C34 C35 -0.6(4) . . . . ?
C38 C37 C57 C58 176.0(3) . . . . ?
C38 C37 C57 C59 -65.8(3) . . . . ?
C38 C37 C57 C60 55.6(3) . . . . ?
C38 C37 C36 C35 -0.7(4) . . . . ?
C13 Ti1 O28 C6 24.3(2) . . . . ?
C13 N12 C11 C5 142.9(2) . . . . ?
C13 N14 C15 C17 -160.52(19) . . . . ?
C33 C38 C37 C57 175.7(2) . . . . ?
C33 C38 C37 C36 -0.9(4) . . . . ?
C33 C34 C35 C36 -1.0(4) . . . . ?
C37 C38 C33 C39 -171.8(2) . . . . ?
C37 C38 C33 C34 1.6(4) . . . . ?
C37 C36 C35 C34 1.7(5) . . . . ?
C45 C46 C47 C48 1.9(4) . . . . ?
C45 C46 C47 C52 -179.8(3) . . . . ?
C45 C50 C49 C48 1.1(5) . . . . ?
C18 C17 C22 C21 -2.3(5) . . . . ?
C18 C19 C24 C25 49.9(4) . . . . ?
C18 C19 C24 C26 169.4(3) . . . . ?
C18 C19 C24 C27 -71.3(4) . . . . ?
C18 C19 C20 C21 -0.7(5) . . . . ?
C11 N12 C13 Ti1 -163.2(3) . . . . ?
C11 N12 C13 N14 177.15(19) . . . . ?
C11 N12 C13 C16 -5.7(4) . . . . ?
C11 C5 C10 C9 -177.9(2) . . . . ?
C10 C5 C11 N12 -162.2(2) . . . . ?
C10 C9 C8 C7 0.5(5) . . . . ?
C46 C45 C43 N42 3.5(4) . . . . ?
C46 C45 C50 C49 -0.5(4) . . . . ?
C46 C47 C48 C49 -1.3(5) . . . . ?
C46 C47 C52 C53 172.3(3) . . . . ?
C46 C47 C52 C54 -68.6(4) . . . . ?
C46 C47 C52 C55 51.7(4) . . . . ?
C15 N14 C13 Ti1 130.62(18) . . . . ?
C15 N14 C13 N12 148.89(19) . . . . ?
C15 N14 C13 C16 -28.4(3) . . . . ?
C15 C17 C22 C21 171.0(3) . . . . ?
C17 C18 C19 C24 171.8(3) . . . . ?
C17 C18 C19 C20 -3.8(4) . . . . ?
C17 C22 C21 C20 -2.1(6) . . . . ?
C39 N40 C41 Ti2 131.78(18) . . . 2_565 ?
C39 N40 C41 N42 149.5(2) . . . . ?
C39 N40 C41 C4 -28.3(3) . . . . ?
C39 C33 C34 C35 173.0(3) . . . . ?
C57 C37 C36 C35 -177.3(3) . . . . ?
C36 C37 C57 C58 -7.5(4) . . . . ?
C36 C37 C57 C59 110.7(3) . . . . ?
C36 C37 C57 C60 -127.9(3) . . . . ?
C34 C33 C39 N40 143.1(2) . . . . ?
C7 C6 C5 C11 179.6(2) . . . . ?
C7 C6 C5 C10 1.3(3) . . . . ?
C19 C18 C17 C15 -168.0(2) . . . . ?
C19 C18 C17 C22 5.4(4) . . . . ?
C43 N42 C41 Ti2 -161.8(3) . . . 2_565 ?
C43 N42 C41 N40 179.2(2) . . . . ?
C43 N42 C41 C4 -3.1(4) . . . . ?
C43 C45 C46 O51 -1.0(4) . . . . ?
C43 C45 C46 C47 179.5(3) . . . . ?
C43 C45 C50 C49 179.0(3) . . . . ?
C50 C45 C46 O51 178.4(2) . . . . ?
C50 C45 C46 C47 -1.1(4) . . . . ?
C50 C45 C43 N42 -175.9(2) . . . . ?
C50 C49 C48 C47 -0.2(5) . . . . ?
C8 C7 C29 C30 112.5(3) . . . . ?
C8 C7 C29 C31 -6.2(4) . . . . ?
C8 C7 C29 C32 -125.6(3) . . . . ?
C24 C19 C20 C21 -176.4(4) . . . . ?
C29 C7 C8 C9 -176.2(3) . . . . ?
C48 C47 C52 C53 -9.5(5) . . . . ?
C48 C47 C52 C54 109.6(3) . . . . ?
C48 C47 C52 C55 -130.1(3) . . . . ?
C22 C21 C20 C19 3.7(7) . . . . ?
C20 C19 C24 C25 -134.8(3) . . . . ?
C20 C19 C24 C26 -15.3(5) . . . . ?
C20 C19 C24 C27 104.0(4) . . . . ?
C52 C47 C48 C49 -179.6(3) . . . . ?
C3 C1 C40 C28 0.0 . . . . ?
C1 C3 C2 C14 0.0 . . . . ?
C1 C40 C28 C14 0.0 . . . . ?
C40 C28 C14 C2 0.0 . . . . ?
C28 C14 C2 C3 0.0 . . . . ?
C2 C3 C1 C40 0.0 . . . . ?
C42 C12 O23 C56 121.1(13) . . . . ?
C62 C56 O23 C12 170.9(14) . . . . ?
C63 O57 C51 C23 -2.3(13) . . . . ?
O57 C63 C66 C23 1.7(10) . . . . ?
C66 C63 O57 C51 0.3(11) . . . . ?
C66 C23 C51 O57 3.4(13) . . . . ?
C51 C23 C66 C63 -3.1(12) . . . . ?
C41 Ti2 O56 C38 86.6(3) 2_565 . . . ?
C41 N42 C43 C45 160.0(2) . . . . ?
C41 N40 C39 C33 -166.06(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.811
####################################################################### 
# 
# 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_exp_8146
_database_code_depnum_ccdc_archive 'CCDC 2222930'
loop_
_audit_author_name
_audit_author_address
'Hanhua Xu'
;Peking University
China
;
_audit_update_record             
;
2022-11-29 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_audit_creation_date             2022-11-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H94 Li6 N8 O4'
_chemical_formula_sum            'C60 H94 Li6 N8 O4'
_chemical_formula_weight         1033.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Li'
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'
Li Li -0.0003 0.0001 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.2159(6)
_cell_length_b                   14.3624(4)
_cell_length_c                   17.5594(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.260(2)
_cell_angle_gamma                90
_cell_volume                     6357.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20582
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.3850
_cell_measurement_theta_min      2.0940
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.987
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43774
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.320
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -52.00   0.50   15.94    --  -12.90 -19.00 120.00  100
  2  ω    -45.00  76.00   0.50   15.94    --  -12.90 -19.00 120.00  242
  3  ω    -78.00  34.00   0.50   15.94    --  -12.90 -37.00  60.00  224
  4  ω    -21.00   6.00   0.50   15.94    --   12.90  77.00-120.00   54
  5  ω    -11.00  75.00   0.50   15.94    --   12.90  57.00 -60.00  172
  6  ω     -5.00  20.00   0.50   15.94    --   12.90 -77.00  90.00   50
  7  ω    -27.00  37.00   0.50   15.94    --   12.90  82.00  60.00  128
  8  ω     -6.00  98.00   0.50   15.94    --   12.90  57.00  30.00  208
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0019313000
_diffrn_orient_matrix_UB_12      0.0439223000
_diffrn_orient_matrix_UB_13      -0.0183241000
_diffrn_orient_matrix_UB_21      0.0063083000
_diffrn_orient_matrix_UB_22      -0.0211336000
_diffrn_orient_matrix_UB_23      -0.0351625000
_diffrn_orient_matrix_UB_31      -0.0273546000
_diffrn_orient_matrix_UB_32      -0.0079802000
_diffrn_orient_matrix_UB_33      -0.0077379000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6182
_reflns_number_total             7291
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0628P)²+4.4689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1413
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C32(H32A,H32B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C2(H2), C18(H18), C17(H17), C3(H3)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,
 H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N8 N 0.47441(4) 0.33456(8) 0.83956(6) 0.0278(2) Uani 1 1 d . . . . .
N10 N 0.53364(4) 0.21643(8) 0.83455(6) 0.0289(2) Uani 1 1 d . . . . .
N33 N 0.73176(5) 0.32653(9) 0.66713(7) 0.0419(3) Uani 1 1 d . . . . .
N30 N 0.73430(5) 0.24924(9) 0.82020(8) 0.0423(3) Uani 1 1 d . . . . .
C9 C 0.50620(5) 0.27542(9) 0.87664(7) 0.0268(3) Uani 1 1 d . . . . .
C6 C 0.40020(5) 0.46498(9) 0.75944(7) 0.0287(3) Uani 1 1 d . . . . .
C14 C 0.60450(5) 0.09454(9) 0.74302(8) 0.0301(3) Uani 1 1 d . . . . .
C1 C 0.42462(5) 0.47734(9) 0.83234(8) 0.0327(3) Uani 1 1 d . . . . .
C15 C 0.60559(5) 0.01912(9) 0.68954(9) 0.0345(3) Uani 1 1 d . . . . .
C5 C 0.39694(5) 0.54435(9) 0.70977(8) 0.0344(3) Uani 1 1 d . . . . .
C13 C 0.58376(6) 0.07640(10) 0.81630(8) 0.0347(3) Uani 1 1 d . . . . .
C7 C 0.43669(6) 0.39303(10) 0.88083(7) 0.0328(3) Uani 1 1 d . . . . .
C25 C 0.37652(6) 0.53564(11) 0.62757(8) 0.0390(3) Uani 1 1 d . . . . .
C20 C 0.62334(6) 0.03422(10) 0.60779(9) 0.0392(3) Uani 1 1 d . . . . .
C12 C 0.51145(6) 0.27467(11) 0.96290(7) 0.0367(3) Uani 1 1 d . . . . .
H12A H 0.493468 0.329301 0.983587 0.055 Uiso 1 1 calc R U . . .
H12B H 0.549074 0.276294 0.978049 0.055 Uiso 1 1 calc R U . . .
H12C H 0.495187 0.217921 0.982778 0.055 Uiso 1 1 calc R U . . .
C11 C 0.57474(6) 0.15645(10) 0.86965(8) 0.0366(3) Uani 1 1 d . . . . .
H11A H 0.562910 0.133132 0.919539 0.044 Uiso 1 1 calc R U . . .
H11B H 0.608015 0.191999 0.877813 0.044 Uiso 1 1 calc R U . . .
C4 C 0.41305(7) 0.63035(11) 0.73908(11) 0.0496(4) Uani 1 1 d . . . . .
H4 H 0.409584 0.683617 0.707279 0.060 Uiso 1 1 calc R U . . .
C16 C 0.58935(6) -0.06842(11) 0.71382(11) 0.0471(4) Uani 1 1 d . . . . .
H16 H 0.590775 -0.118850 0.678919 0.057 Uiso 1 1 calc R U . . .
C2 C 0.44032(7) 0.56507(11) 0.85759(10) 0.0465(4) Uani 1 1 d . . . . .
H2 H 0.455776 0.572006 0.907090 0.056 Uiso 1 1 calc R U . . .
C26 C 0.31778(6) 0.51040(13) 0.62655(10) 0.0477(4) Uani 1 1 d . . . . .
H26A H 0.312863 0.451337 0.653429 0.072 Uiso 1 1 calc R U . . .
H26B H 0.304961 0.504091 0.573708 0.072 Uiso 1 1 calc R U . . .
H26C H 0.297763 0.559555 0.651847 0.072 Uiso 1 1 calc R U . . .
C27 C 0.40756(7) 0.46050(12) 0.58539(9) 0.0473(4) Uani 1 1 d . . . . .
H27A H 0.445442 0.475833 0.587249 0.071 Uiso 1 1 calc R U . . .
H27B H 0.395090 0.457648 0.532187 0.071 Uiso 1 1 calc R U . . .
H27C H 0.402002 0.400014 0.609771 0.071 Uiso 1 1 calc R U . . .
C18 C 0.56770(7) -0.01281(11) 0.83660(10) 0.0472(4) Uani 1 1 d . . . . .
H18 H 0.554140 -0.023447 0.885891 0.057 Uiso 1 1 calc R U . . .
C21 C 0.68142(6) 0.06360(12) 0.60868(10) 0.0475(4) Uani 1 1 d . . . . .
H21A H 0.685636 0.121458 0.637782 0.071 Uiso 1 1 calc R U . . .
H21B H 0.692840 0.073661 0.556334 0.071 Uiso 1 1 calc R U . . .
H21C H 0.703137 0.014588 0.632507 0.071 Uiso 1 1 calc R U . . .
C28 C 0.38260(8) 0.62649(13) 0.58248(11) 0.0579(5) Uani 1 1 d . . . . .
H28A H 0.361658 0.675694 0.606135 0.087 Uiso 1 1 calc R U . . .
H28B H 0.369972 0.616962 0.529873 0.087 Uiso 1 1 calc R U . . .
H28C H 0.420040 0.644786 0.582652 0.087 Uiso 1 1 calc R U . . .
C17 C 0.57122(8) -0.08557(11) 0.78629(12) 0.0559(5) Uani 1 1 d . . . . .
H17 H 0.561379 -0.146719 0.800995 0.067 Uiso 1 1 calc R U . . .
C32 C 0.78092(7) 0.29114(14) 0.70356(12) 0.0560(5) Uani 1 1 d . . . . .
H32A H 0.811289 0.328002 0.685322 0.067 Uiso 1 1 calc R U . . .
H32B H 0.786294 0.225724 0.687725 0.067 Uiso 1 1 calc R U . . .
C3 C 0.43367(8) 0.64205(11) 0.81153(12) 0.0583(5) Uani 1 1 d . . . . .
H3 H 0.443200 0.702259 0.829585 0.070 Uiso 1 1 calc R U . . .
C29 C 0.73742(8) 0.14816(12) 0.81070(12) 0.0559(5) Uani 1 1 d . . . . .
H29A H 0.735531 0.132762 0.756340 0.084 Uiso 1 1 calc R U . . .
H29B H 0.707794 0.118601 0.836620 0.084 Uiso 1 1 calc R U . . .
H29C H 0.771024 0.125450 0.832786 0.084 Uiso 1 1 calc R U . . .
C22 C 0.58886(8) 0.10926(13) 0.56886(10) 0.0533(4) Uani 1 1 d . . . . .
H22A H 0.551692 0.089273 0.567968 0.080 Uiso 1 1 calc R U . . .
H22B H 0.600592 0.118583 0.516572 0.080 Uiso 1 1 calc R U . . .
H22C H 0.592296 0.167814 0.597198 0.080 Uiso 1 1 calc R U . . .
C23 C 0.61882(8) -0.05434(13) 0.55895(11) 0.0580(5) Uani 1 1 d . . . . .
H23A H 0.642631 -0.102230 0.579983 0.087 Uiso 1 1 calc R U . . .
H23B H 0.628740 -0.040073 0.506581 0.087 Uiso 1 1 calc R U . . .
H23C H 0.582197 -0.077174 0.559150 0.087 Uiso 1 1 calc R U . . .
C31 C 0.78038(7) 0.29551(14) 0.78848(12) 0.0577(5) Uani 1 1 d . . . . .
H31A H 0.813045 0.265939 0.809363 0.069 Uiso 1 1 calc R U . . .
H31B H 0.780588 0.361556 0.804624 0.069 Uiso 1 1 calc R U . . .
C35 C 0.72879(9) 0.42708(12) 0.67191(13) 0.0621(5) Uani 1 1 d . . . . .
H35A H 0.728781 0.445999 0.725535 0.093 Uiso 1 1 calc R U . . .
H35B H 0.696105 0.448699 0.646397 0.093 Uiso 1 1 calc R U . . .
H35C H 0.759491 0.454553 0.647048 0.093 Uiso 1 1 calc R U . . .
C34 C 0.73202(10) 0.30000(15) 0.58688(11) 0.0669(6) Uani 1 1 d . . . . .
H34A H 0.762247 0.329405 0.562268 0.100 Uiso 1 1 calc R U . . .
H34B H 0.698973 0.320622 0.561779 0.100 Uiso 1 1 calc R U . . .
H34C H 0.735031 0.232172 0.582722 0.100 Uiso 1 1 calc R U . . .
C36 C 0.73314(10) 0.26813(16) 0.90249(11) 0.0681(6) Uani 1 1 d . . . . .
H36A H 0.701392 0.239795 0.923851 0.102 Uiso 1 1 calc R U . . .
H36B H 0.732409 0.335539 0.911033 0.102 Uiso 1 1 calc R U . . .
H36C H 0.764854 0.241625 0.927408 0.102 Uiso 1 1 calc R U . . .
Li37 Li 0.57119(9) 0.27716(15) 0.74529(13) 0.0312(5) Uani 1 1 d . . . . .
Li38 Li 0.66822(9) 0.28332(16) 0.74350(13) 0.0339(5) Uani 1 1 d . . . . .
Li39 Li 0.500000 0.4102(3) 0.750000 0.0403(8) Uani 1 2 d S T P . .
O19 O 0.62037(4) 0.17985(6) 0.72634(5) 0.0312(2) Uani 1 1 d . . . . .
O24 O 0.38301(4) 0.38123(6) 0.73890(5) 0.0306(2) Uani 1 1 d . . . . .
Li1 Li 0.500000 0.1399(2) 0.750000 0.0384(7) Uani 1 2 d S T P . .
H7A H 0.4507(6) 0.4148(11) 0.9288(9) 0.034(4) Uiso 1 1 d . . . . .
H7B H 0.4031(7) 0.3583(12) 0.8909(9) 0.041(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N8 C9 1.3284(17) . ?
N8 C7 1.4717(17) . ?
N8 Li37 2.036(2) 2_656 ?
N8 Li39 2.028(2) . ?
N10 C9 1.3286(17) . ?
N10 C11 1.4723(17) . ?
N10 Li37 2.044(2) . ?
N10 Li1 2.019(2) . ?
N33 C32 1.473(2) . ?
N33 C35 1.449(2) . ?
N33 C34 1.460(2) . ?
N33 Li38 2.201(3) . ?
N30 C29 1.464(2) . ?
N30 C31 1.460(2) . ?
N30 C36 1.471(2) . ?
N30 Li38 2.175(3) . ?
C9 C12 1.5177(17) . ?
C6 C1 1.4194(19) . ?
C6 C5 1.4366(18) . ?
C6 Li39 2.6456(17) . ?
C6 O24 1.3258(15) . ?
C14 C15 1.4343(18) . ?
C14 C13 1.424(2) . ?
C14 Li37 2.755(3) . ?
C14 O19 1.3238(16) . ?
C14 Li1 2.7200(15) . ?
C1 C7 1.5075(19) . ?
C1 C2 1.390(2) . ?
C1 Li39 2.5990(19) . ?
C15 C20 1.529(2) . ?
C15 C16 1.392(2) . ?
C5 C25 1.527(2) . ?
C5 C4 1.395(2) . ?
C13 C11 1.503(2) . ?
C13 C18 1.392(2) . ?
C13 Li1 2.5575(18) . ?
C7 H7A 0.958(16) . ?
C7 H7B 1.002(17) . ?
C25 C26 1.525(2) . ?
C25 C27 1.534(2) . ?
C25 C28 1.536(2) . ?
C20 C21 1.524(2) . ?
C20 C22 1.536(2) . ?
C20 C23 1.537(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C4 H4 0.9500 . ?
C4 C3 1.374(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.378(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C17 1.372(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C17 H17 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.493(3) . ?
C3 H3 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
Li37 Li39 2.624(3) . ?
Li37 O19 1.903(2) . ?
Li37 O24 1.905(2) 2_656 ?
Li37 Li1 2.668(3) . ?
Li38 O19 1.934(2) . ?
Li38 O24 1.939(3) 2_656 ?

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
C9 N8 C7 120.87(11) . . ?
C9 N8 Li37 115.13(10) . 2_656 ?
C9 N8 Li39 121.57(10) . . ?
C7 N8 Li37 103.33(10) . 2_656 ?
C7 N8 Li39 107.24(11) . . ?
Li39 N8 Li37 80.42(9) . 2_656 ?
C9 N10 C11 120.71(11) . . ?
C9 N10 Li37 114.21(10) . . ?
C9 N10 Li1 122.72(10) . . ?
C11 N10 Li37 103.71(11) . . ?
C11 N10 Li1 105.66(11) . . ?
Li1 N10 Li37 82.10(9) . . ?
C32 N33 Li38 104.78(12) . . ?
C35 N33 C32 111.27(15) . . ?
C35 N33 C34 108.51(16) . . ?
C35 N33 Li38 101.92(12) . . ?
C34 N33 C32 107.91(15) . . ?
C34 N33 Li38 122.23(13) . . ?
C29 N30 C36 107.28(15) . . ?
C29 N30 Li38 101.25(11) . . ?
C31 N30 C29 111.27(15) . . ?
C31 N30 C36 108.91(15) . . ?
C31 N30 Li38 105.47(12) . . ?
C36 N30 Li38 122.36(13) . . ?
N8 C9 N10 116.82(11) . . ?
N8 C9 C12 122.14(12) . . ?
N10 C9 C12 121.04(12) . . ?
C1 C6 C5 117.78(12) . . ?
C1 C6 Li39 72.50(8) . . ?
C5 C6 Li39 103.88(10) . . ?
O24 C6 C1 119.44(11) . . ?
O24 C6 C5 122.74(12) . . ?
O24 C6 Li39 91.07(10) . . ?
C15 C14 Li37 137.63(10) . . ?
C15 C14 Li1 104.06(10) . . ?
C13 C14 C15 117.79(13) . . ?
C13 C14 Li37 92.46(9) . . ?
C13 C14 Li1 68.13(8) . . ?
O19 C14 C15 122.96(13) . . ?
O19 C14 C13 119.23(12) . . ?
O19 C14 Li37 38.33(7) . . ?
O19 C14 Li1 94.92(10) . . ?
Li1 C14 Li37 58.33(9) . . ?
C6 C1 C7 119.16(12) . . ?
C6 C1 Li39 76.11(7) . . ?
C7 C1 Li39 82.82(10) . . ?
C2 C1 C6 121.05(13) . . ?
C2 C1 C7 119.69(13) . . ?
C2 C1 Li39 107.89(12) . . ?
C14 C15 C20 121.19(13) . . ?
C16 C15 C14 118.14(14) . . ?
C16 C15 C20 120.66(13) . . ?
C6 C5 C25 121.50(13) . . ?
C4 C5 C6 117.79(14) . . ?
C4 C5 C25 120.71(13) . . ?
C14 C13 C11 119.13(12) . . ?
C14 C13 Li1 80.76(7) . . ?
C11 C13 Li1 82.88(10) . . ?
C18 C13 C14 120.96(14) . . ?
C18 C13 C11 119.69(14) . . ?
C18 C13 Li1 101.72(12) . . ?
N8 C7 C1 107.75(10) . . ?
N8 C7 H7A 112.9(9) . . ?
N8 C7 H7B 111.2(10) . . ?
C1 C7 H7A 107.4(10) . . ?
C1 C7 H7B 109.8(10) . . ?
H7A C7 H7B 107.8(13) . . ?
C5 C25 C27 110.43(12) . . ?
C5 C25 C28 112.48(14) . . ?
C26 C25 C5 109.76(12) . . ?
C26 C25 C27 109.46(14) . . ?
C26 C25 C28 107.69(13) . . ?
C27 C25 C28 106.92(12) . . ?
C15 C20 C22 110.07(12) . . ?
C15 C20 C23 112.77(14) . . ?
C21 C20 C15 109.32(12) . . ?
C21 C20 C22 110.17(15) . . ?
C21 C20 C23 107.12(13) . . ?
C22 C20 C23 107.34(13) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N10 C11 C13 107.54(11) . . ?
N10 C11 H11A 110.2 . . ?
N10 C11 H11B 110.2 . . ?
C13 C11 H11A 110.2 . . ?
C13 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C5 C4 H4 118.3 . . ?
C3 C4 C5 123.44(15) . . ?
C3 C4 H4 118.3 . . ?
C15 C16 H16 118.4 . . ?
C17 C16 C15 123.21(15) . . ?
C17 C16 H16 118.4 . . ?
C1 C2 H2 119.7 . . ?
C3 C2 C1 120.66(16) . . ?
C3 C2 H2 119.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C13 C18 H18 119.6 . . ?
C17 C18 C13 120.83(16) . . ?
C17 C18 H18 119.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C16 C17 H17 120.5 . . ?
C18 C17 C16 118.93(15) . . ?
C18 C17 H17 120.5 . . ?
N33 C32 H32A 108.9 . . ?
N33 C32 H32B 108.9 . . ?
N33 C32 C31 113.16(14) . . ?
H32A C32 H32B 107.8 . . ?
C31 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
C4 C3 C2 118.94(15) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
N30 C29 H29A 109.5 . . ?
N30 C29 H29B 109.5 . . ?
N30 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N30 C31 C32 112.76(14) . . ?
N30 C31 H31A 109.0 . . ?
N30 C31 H31B 109.0 . . ?
C32 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
N33 C35 H35A 109.5 . . ?
N33 C35 H35B 109.5 . . ?
N33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N33 C34 H34A 109.5 . . ?
N33 C34 H34B 109.5 . . ?
N33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N30 C36 H36A 109.5 . . ?
N30 C36 H36B 109.5 . . ?
N30 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N8 Li37 N10 118.04(12) 2_656 . ?
N8 Li37 C14 122.84(10) 2_656 . ?
N8 Li37 C7 31.08(5) 2_656 2_656 ?
N8 Li37 Li39 49.65(6) 2_656 . ?
N8 Li37 Li1 87.26(9) 2_656 . ?
N10 Li37 C14 75.60(8) . . ?
N10 Li37 C7 147.34(11) . 2_656 ?
N10 Li37 Li39 87.58(9) . . ?
N10 Li37 Li1 48.54(6) . . ?
C14 Li37 C7 125.18(9) . 2_656 ?
Li39 Li37 C14 154.52(11) . . ?
Li39 Li37 C7 63.34(6) . 2_656 ?
Li39 Li37 Li1 94.33(10) . . ?
O19 Li37 N8 121.95(12) . 2_656 ?
O19 Li37 N10 97.78(10) . . ?
O19 Li37 C14 25.57(5) . . ?
O19 Li37 C7 109.67(10) . 2_656 ?
O19 Li37 Li39 171.60(12) . . ?
O19 Li37 O24 101.92(11) . 2_656 ?
O19 Li37 Li1 84.51(10) . . ?
O24 Li37 N8 96.88(10) 2_656 2_656 ?
O24 Li37 N10 120.83(12) 2_656 . ?
O24 Li37 C14 124.40(11) 2_656 . ?
O24 Li37 C7 71.23(8) 2_656 2_656 ?
O24 Li37 Li39 80.63(10) 2_656 . ?
O24 Li37 Li1 168.77(12) 2_656 . ?
Li1 Li37 C14 60.18(7) . . ?
Li1 Li37 C7 115.56(9) . 2_656 ?
N30 Li38 N33 83.27(10) . . ?
O19 Li38 N33 125.58(12) . . ?
O19 Li38 N30 112.98(12) . . ?
O19 Li38 O24 99.59(11) . 2_656 ?
O24 Li38 N33 112.90(12) 2_656 . ?
O24 Li38 N30 124.64(12) 2_656 . ?
N8 Li39 N8 115.26(18) . 2_656 ?
N8 Li39 C6 77.97(4) 2_656 2_656 ?
N8 Li39 C6 121.81(5) . 2_656 ?
N8 Li39 C6 77.97(4) . . ?
N8 Li39 C6 121.81(5) 2_656 . ?
N8 Li39 C1 151.53(7) . 2_656 ?
N8 Li39 C1 61.21(4) 2_656 2_656 ?
N8 Li39 C1 151.53(7) 2_656 . ?
N8 Li39 C1 61.21(4) . . ?
N8 Li39 Li37 49.93(8) . 2_656 ?
N8 Li39 Li37 82.19(12) . . ?
N8 Li39 Li37 49.93(8) 2_656 . ?
N8 Li39 Li37 82.19(12) 2_656 2_656 ?
C6 Li39 C6 145.37(16) 2_656 . ?
C1 Li39 C6 31.39(4) 2_656 2_656 ?
C1 Li39 C6 129.25(12) 2_656 . ?
C1 Li39 C6 31.39(4) . . ?
C1 Li39 C6 129.25(12) . 2_656 ?
C1 Li39 C1 136.42(16) 2_656 . ?
C1 Li39 Li37 75.14(6) . 2_656 ?
C1 Li39 Li37 142.84(10) 2_656 2_656 ?
C1 Li39 Li37 75.14(6) 2_656 . ?
C1 Li39 Li37 142.84(10) . . ?
Li37 Li39 C6 150.58(14) . . ?
Li37 Li39 C6 150.58(14) 2_656 2_656 ?
Li37 Li39 C6 64.04(6) 2_656 . ?
Li37 Li39 C6 64.04(6) . 2_656 ?
Li37 Li39 Li37 86.56(15) 2_656 . ?
C14 O19 Li37 116.10(11) . . ?
C14 O19 Li38 150.16(11) . . ?
Li37 O19 Li38 79.34(10) . . ?
C6 O24 Li37 118.60(11) . 2_656 ?
C6 O24 Li38 146.05(11) . 2_656 ?
Li37 O24 Li38 79.14(10) 2_656 2_656 ?
N10 Li1 N10 114.06(18) 2_656 . ?
N10 Li1 C14 119.29(6) 2_656 . ?
N10 Li1 C14 76.81(4) 2_656 2_656 ?
N10 Li1 C14 119.29(6) . 2_656 ?
N10 Li1 C14 76.80(4) . . ?
N10 Li1 C13 149.14(7) 2_656 . ?
N10 Li1 C13 149.14(7) . 2_656 ?
N10 Li1 C13 61.96(4) . . ?
N10 Li1 C13 61.96(4) 2_656 2_656 ?
N10 Li1 Li37 49.36(8) 2_656 2_656 ?
N10 Li1 Li37 49.36(8) . . ?
N10 Li1 Li37 81.22(11) . 2_656 ?
N10 Li1 Li37 81.22(11) 2_656 . ?
C14 Li1 C14 152.26(15) 2_656 . ?
C13 Li1 C14 133.25(11) 2_656 . ?
C13 Li1 C14 31.11(4) . . ?
C13 Li1 C14 133.25(11) . 2_656 ?
C13 Li1 C14 31.11(5) 2_656 2_656 ?
C13 Li1 C13 138.19(16) . 2_656 ?
C13 Li1 Li37 143.02(11) 2_656 . ?
C13 Li1 Li37 74.23(6) . . ?
C13 Li1 Li37 74.23(6) 2_656 2_656 ?
C13 Li1 Li37 143.02(11) . 2_656 ?
Li37 Li1 C14 61.48(6) 2_656 2_656 ?
Li37 Li1 C14 61.48(6) . . ?
Li37 Li1 C14 146.26(14) 2_656 . ?
Li37 Li1 C14 146.26(14) . 2_656 ?
Li37 Li1 Li37 84.78(14) . 2_656 ?

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
N33 C32 C31 N30 54.0(2) . . . . ?
C9 N8 C7 C1 155.89(12) . . . . ?
C9 N10 C11 C13 159.53(12) . . . . ?
C6 C1 C7 N8 61.91(16) . . . . ?
C6 C1 C2 C3 -1.6(2) . . . . ?
C6 C5 C25 C26 66.84(16) . . . . ?
C6 C5 C25 C27 -53.93(17) . . . . ?
C6 C5 C25 C28 -173.29(13) . . . . ?
C6 C5 C4 C3 2.7(2) . . . . ?
C14 C15 C20 C21 63.91(16) . . . . ?
C14 C15 C20 C22 -57.22(17) . . . . ?
C14 C15 C20 C23 -177.06(13) . . . . ?
C14 C15 C16 C17 1.4(2) . . . . ?
C14 C13 C11 N10 64.17(16) . . . . ?
C14 C13 C18 C17 -0.3(2) . . . . ?
C1 C6 C5 C25 173.72(12) . . . . ?
C1 C6 C5 C4 -6.36(19) . . . . ?
C1 C6 O24 Li37 -47.35(16) . . . 2_656 ?
C1 C6 O24 Li38 67.8(2) . . . 2_656 ?
C1 C2 C3 C4 -2.4(3) . . . . ?
C15 C14 C13 C11 -171.29(12) . . . . ?
C15 C14 C13 C18 3.34(19) . . . . ?
C15 C14 C13 Li1 -94.84(13) . . . . ?
C15 C14 O19 Li37 126.85(13) . . . . ?
C15 C14 O19 Li38 -117.0(2) . . . . ?
C15 C16 C17 C18 1.6(3) . . . . ?
C5 C6 C1 C7 -170.21(12) . . . . ?
C5 C6 C1 C2 6.0(2) . . . . ?
C5 C6 C1 Li39 -96.78(13) . . . . ?
C5 C6 O24 Li37 130.37(13) . . . 2_656 ?
C5 C6 O24 Li38 -114.44(19) . . . 2_656 ?
C5 C4 C3 C2 1.8(3) . . . . ?
C13 C14 C15 C20 175.40(12) . . . . ?
C13 C14 C15 C16 -3.80(19) . . . . ?
C13 C14 O19 Li37 -51.08(16) . . . . ?
C13 C14 O19 Li38 65.0(3) . . . . ?
C13 C18 C17 C16 -2.2(3) . . . . ?
C7 N8 C9 N10 170.97(12) . . . . ?
C7 N8 C9 C12 -9.22(19) . . . . ?
C7 C1 C2 C3 174.56(15) . . . . ?
C25 C5 C4 C3 -177.41(16) . . . . ?
C20 C15 C16 C17 -177.79(15) . . . . ?
C11 N10 C9 N8 172.29(12) . . . . ?
C11 N10 C9 C12 -7.52(19) . . . . ?
C11 C13 C18 C17 174.27(15) . . . . ?
C4 C5 C25 C26 -113.08(16) . . . . ?
C4 C5 C25 C27 126.16(15) . . . . ?
C4 C5 C25 C28 6.80(19) . . . . ?
C16 C15 C20 C21 -116.91(15) . . . . ?
C16 C15 C20 C22 121.96(15) . . . . ?
C16 C15 C20 C23 2.13(19) . . . . ?
C2 C1 C7 N8 -114.31(14) . . . . ?
C18 C13 C11 N10 -110.52(15) . . . . ?
C29 N30 C31 C32 69.74(19) . . . . ?
C35 N33 C32 C31 73.4(2) . . . . ?
C34 N33 C32 C31 -167.62(16) . . . . ?
C36 N30 C31 C32 -172.20(16) . . . . ?
Li37 N8 C9 N10 45.73(15) 2_656 . . . ?
Li37 N8 C9 C12 -134.46(13) 2_656 . . . ?
Li37 N8 C7 C1 -73.57(13) 2_656 . . . ?
Li37 N10 C9 N8 47.59(15) . . . . ?
Li37 N10 C9 C12 -132.22(13) . . . . ?
Li37 N10 C11 C13 -70.99(13) . . . . ?
Li37 C14 C15 C20 44.9(2) . . . . ?
Li37 C14 C15 C16 -134.32(15) . . . . ?
Li37 C14 C13 C11 -22.13(13) . . . . ?
Li37 C14 C13 C18 152.49(13) . . . . ?
Li37 C14 C13 Li1 54.31(10) . . . . ?
Li37 C14 O19 Li38 116.1(3) . . . . ?
Li38 N33 C32 C31 -35.94(18) . . . . ?
Li38 N30 C31 C32 -39.22(19) . . . . ?
Li39 N8 C9 N10 -48.42(17) . . . . ?
Li39 N8 C9 C12 131.39(14) . . . . ?
Li39 N8 C7 C1 10.37(13) . . . . ?
Li39 C6 C1 C7 -73.43(13) . . . . ?
Li39 C6 C1 C2 102.74(15) . . . . ?
Li39 C6 C5 C25 96.43(13) . . . . ?
Li39 C6 C5 C4 -83.65(14) . . . . ?
Li39 C6 O24 Li37 23.09(11) . . . 2_656 ?
Li39 C6 O24 Li38 138.28(17) . . . 2_656 ?
Li39 C1 C7 N8 -7.77(10) . . . . ?
Li39 C1 C2 C3 82.68(18) . . . . ?
O19 C14 C15 C20 -2.55(19) . . . . ?
O19 C14 C15 C16 178.24(12) . . . . ?
O19 C14 C13 C11 6.75(18) . . . . ?
O19 C14 C13 C18 -178.63(13) . . . . ?
O19 C14 C13 Li1 83.19(13) . . . . ?
O24 C6 C1 C7 7.63(18) . . . . ?
O24 C6 C1 C2 -176.20(13) . . . . ?
O24 C6 C1 Li39 81.05(13) . . . . ?
O24 C6 C5 C25 -4.04(19) . . . . ?
O24 C6 C5 C4 175.88(13) . . . . ?
Li1 N10 C9 N8 -48.71(17) . . . . ?
Li1 N10 C9 C12 131.48(14) . . . . ?
Li1 N10 C11 C13 14.51(13) . . . . ?
Li1 C14 C15 C20 102.98(13) . . . . ?
Li1 C14 C15 C16 -76.22(14) . . . . ?
Li1 C14 C13 C11 -76.44(13) . . . . ?
Li1 C14 C13 C18 98.18(15) . . . . ?
Li1 C14 O19 Li37 16.57(11) . . . . ?
Li1 C14 O19 Li38 132.7(2) . . . . ?
Li1 C13 C11 N10 -11.06(11) . . . . ?
Li1 C13 C18 C17 85.85(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.455
####################################################################### 
# 
# 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_exp_9747
_database_code_depnum_ccdc_archive 'CCDC 2222931'
loop_
_audit_author_name
_audit_author_address
'Hanhua Xu'
;Peking University
China
;
_audit_update_record             
;
2022-11-29 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_audit_creation_date             2022-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H31 Cl N2 O2 Zr)'
_chemical_formula_sum            'C48 H62 Cl2 N4 O4 Zr2'
_chemical_formula_weight         1012.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zr Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

_cell_length_a                   12.3616(3)
_cell_length_b                   13.1320(3)
_cell_length_c                   16.7306(4)
_cell_angle_alpha                101.875(2)
_cell_angle_beta                 109.119(2)
_cell_angle_gamma                104.700(2)
_cell_volume                     2354.84(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27867
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.0990
_cell_measurement_theta_min      2.6700
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.988
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41430
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.560
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00 -44.00   0.50    0.50    --   -8.20 -38.00-120.00   70
  2  ω    -30.00  98.00   0.50    0.50    --    8.20  77.00  60.00  256
  3  ω    -49.00 -11.00   0.50    0.50    --    8.20 -38.00  60.00   76
  4  ω    -12.00  14.00   0.50    0.50    --    8.20  57.00 -60.00   52
  5  ω     53.00  79.00   0.50    0.50    --    8.20  57.00 -60.00   52
  6  ω    -81.00  37.00   0.50    0.50    --    8.20 -57.00   0.00  236
  7  ω    -26.00  11.00   0.50    0.50    --    8.20 -77.00-120.00   74
  8  ω    -80.00  31.00   0.50    0.50    --    8.20 -77.00 -30.00  222
  9  ω    -18.00  88.00   0.50    0.50    --    8.20  57.00-150.00  212
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0359272000
_diffrn_orient_matrix_UB_12      -0.0340140000
_diffrn_orient_matrix_UB_13      -0.0023228000
_diffrn_orient_matrix_UB_21      -0.0537898000
_diffrn_orient_matrix_UB_22      -0.0476761000
_diffrn_orient_matrix_UB_23      -0.0219463000
_diffrn_orient_matrix_UB_31      -0.0031498000
_diffrn_orient_matrix_UB_32      0.0058656000
_diffrn_orient_matrix_UB_33      -0.0418310000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9822
_reflns_number_total             10762
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         10762
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0240
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²+1.0691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0650
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C11(H11A,H11B), C39(H39A,H39B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C22(H22), C7(H7), C6(H6), C36(H36), C21(H21), C50(H50), C34(H34),
 C20(H20), C35(H35), C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C16(H16A,H16B,H16C), C44(H44A,H44B,H44C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C25(H25A,H25B,H25C), C55(H55A,H55B,H55C),
 C32(H32A,H32B,H32C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.52002(2) 0.12957(2) 0.01380(2) 0.01555(4) Uani 1 1 d . . . . .
Zr2 Zr 0.63781(2) 0.09262(2) 0.50632(2) 0.01584(4) Uani 1 1 d . . . . .
Cl3 Cl 0.52957(4) 0.21539(3) -0.10305(3) 0.02564(8) Uani 1 1 d . . . . .
Cl4 Cl 0.70685(4) 0.00212(3) 0.39864(3) 0.02690(9) Uani 1 1 d . . . . .
O28 O 0.40290(10) 0.19671(8) 0.03619(8) 0.0226(2) Uani 1 1 d . . . . .
O23 O 0.67856(9) 0.23481(8) 0.10537(7) 0.0216(2) Uani 1 1 d . . . . .
O56 O 0.79559(9) 0.15649(9) 0.60848(7) 0.0206(2) Uani 1 1 d . . . . .
O51 O 0.62011(10) 0.21032(9) 0.45287(8) 0.0234(2) Uani 1 1 d . . . . .
N42 N 0.43862(11) 0.08182(10) 0.48443(8) 0.0183(2) Uani 1 1 d . . . . .
N40 N 0.58476(11) 0.14771(10) 0.61963(8) 0.0193(2) Uani 1 1 d . . . . .
N12 N 0.37469(11) -0.01392(10) 0.03102(9) 0.0195(3) Uani 1 1 d . . . . .
N14 N 0.56394(12) 0.03936(10) 0.11944(8) 0.0196(3) Uani 1 1 d . . . . .
C10 C 0.30741(14) 0.18983(13) 0.06094(10) 0.0207(3) Uani 1 1 d . . . . .
C18 C 0.78405(13) 0.24160(12) 0.17048(10) 0.0188(3) Uani 1 1 d . . . . .
C9 C 0.28719(14) 0.28708(13) 0.09738(11) 0.0224(3) Uani 1 1 d . . . . .
C5 C 0.23088(14) 0.08417(13) 0.05047(11) 0.0227(3) Uani 1 1 d . . . . .
C8 C 0.19139(15) 0.27259(14) 0.12545(12) 0.0278(3) Uani 1 1 d . . . . .
H8 H 0.175288 0.336229 0.149913 0.033 Uiso 1 1 calc R U . . .
C13 C 0.45082(14) 0.01746(11) 0.11666(10) 0.0197(3) Uani 1 1 d . . . . .
C45 C 0.42121(14) 0.22065(13) 0.39990(11) 0.0231(3) Uani 1 1 d . . . . .
C17 C 0.78251(14) 0.16103(12) 0.21408(10) 0.0210(3) Uani 1 1 d . . . . .
C15 C 0.66830(15) 0.07438(14) 0.20475(11) 0.0284(4) Uani 1 1 d . . . . .
H15A H 0.688188 0.008168 0.214094 0.034 Uiso 1 1 calc R U . . .
H15B H 0.643770 0.103820 0.252843 0.034 Uiso 1 1 calc R U . . .
C57 C 1.03878(15) 0.14687(14) 0.68514(11) 0.0277(3) Uani 1 1 d . . . . .
C22 C 0.89015(15) 0.16705(14) 0.27983(12) 0.0276(3) Uani 1 1 d . . . . .
H22 H 0.889024 0.112609 0.309467 0.033 Uiso 1 1 calc R U . . .
C41 C 0.48766(13) 0.16033(12) 0.56813(10) 0.0193(3) Uani 1 1 d . . . . .
C37 C 0.96420(14) 0.17318(12) 0.73907(11) 0.0233(3) Uani 1 1 d . . . . .
C7 C 0.11863(15) 0.16909(15) 0.11914(12) 0.0300(4) Uani 1 1 d . . . . .
H7 H 0.055504 0.162811 0.140361 0.036 Uiso 1 1 calc R U . . .
C46 C 0.54701(14) 0.26872(12) 0.42427(10) 0.0208(3) Uani 1 1 d . . . . .
C33 C 0.78078(14) 0.20500(12) 0.74942(10) 0.0208(3) Uani 1 1 d . . . . .
C58 C 0.97392(16) 0.02747(14) 0.62025(12) 0.0318(4) Uani 1 1 d . . . . .
H58A H 0.958112 -0.023986 0.653395 0.048 Uiso 1 1 calc R U . . .
H58B H 1.025973 0.008309 0.590735 0.048 Uiso 1 1 calc R U . . .
H58C H 0.896385 0.022087 0.575323 0.048 Uiso 1 1 calc R U . . .
C38 C 0.84647(13) 0.17839(11) 0.69871(10) 0.0193(3) Uani 1 1 d . . . . .
C6 C 0.13864(15) 0.07505(14) 0.08173(12) 0.0275(3) Uani 1 1 d . . . . .
H6 H 0.089193 0.004021 0.077386 0.033 Uiso 1 1 calc R U . . .
C11 C 0.24663(14) -0.02049(12) 0.00507(11) 0.0239(3) Uani 1 1 d . . . . .
H11A H 0.202246 -0.083447 0.019426 0.029 Uiso 1 1 calc R U . . .
H11B H 0.208781 -0.036281 -0.060297 0.029 Uiso 1 1 calc R U . . .
C47 C 0.59856(15) 0.37571(13) 0.42088(10) 0.0234(3) Uani 1 1 d . . . . .
C16 C 0.41740(16) 0.02855(14) 0.19499(11) 0.0282(3) Uani 1 1 d . . . . .
H16A H 0.434174 0.107014 0.224052 0.042 Uiso 1 1 calc R U . . .
H16B H 0.465686 -0.000858 0.237365 0.042 Uiso 1 1 calc R U . . .
H16C H 0.330350 -0.013200 0.175133 0.042 Uiso 1 1 calc R U . . .
C19 C 0.89365(14) 0.33021(12) 0.19422(10) 0.0210(3) Uani 1 1 d . . . . .
C36 C 1.00935(15) 0.19213(14) 0.83094(11) 0.0288(4) Uani 1 1 d . . . . .
H36 H 1.087627 0.188217 0.859957 0.035 Uiso 1 1 calc R U . . .
C39 C 0.66140(14) 0.22383(13) 0.70995(10) 0.0238(3) Uani 1 1 d . . . . .
H39A H 0.616306 0.213953 0.748615 0.029 Uiso 1 1 calc R U . . .
H39B H 0.678737 0.301158 0.708576 0.029 Uiso 1 1 calc R U . . .
C21 C 0.99803(15) 0.25098(15) 0.30228(12) 0.0321(4) Uani 1 1 d . . . . .
H21 H 1.071444 0.254159 0.346607 0.039 Uiso 1 1 calc R U . . .
C29 C 0.36499(16) 0.40214(13) 0.10332(12) 0.0283(4) Uani 1 1 d . . . . .
C50 C 0.34469(16) 0.27875(15) 0.37035(13) 0.0324(4) Uani 1 1 d . . . . .
H50 H 0.259124 0.246078 0.352596 0.039 Uiso 1 1 calc R U . . .
C34 C 0.83065(15) 0.22314(13) 0.84099(11) 0.0261(3) Uani 1 1 d . . . . .
H34 H 0.786329 0.240158 0.875618 0.031 Uiso 1 1 calc R U . . .
C43 C 0.36542(14) 0.10664(13) 0.40576(11) 0.0244(3) Uani 1 1 d . . . . .
H43A H 0.284219 0.099621 0.406685 0.029 Uiso 1 1 calc R U . . .
H43B H 0.352622 0.049913 0.351151 0.029 Uiso 1 1 calc R U . . .
C20 C 0.99856(15) 0.33091(14) 0.25954(12) 0.0280(3) Uani 1 1 d . . . . .
H20 H 1.073585 0.388519 0.275487 0.034 Uiso 1 1 calc R U . . .
C44 C 0.43882(16) 0.24956(14) 0.59348(12) 0.0294(4) Uani 1 1 d . . . . .
H44A H 0.488473 0.319608 0.591700 0.044 Uiso 1 1 calc R U . . .
H44B H 0.441903 0.258416 0.653882 0.044 Uiso 1 1 calc R U . . .
H44C H 0.354102 0.229104 0.551452 0.044 Uiso 1 1 calc R U . . .
C30 C 0.3518(2) 0.40443(16) 0.00937(14) 0.0398(4) Uani 1 1 d . . . . .
H30A H 0.383809 0.350767 -0.015842 0.060 Uiso 1 1 calc R U . . .
H30B H 0.397672 0.478984 0.012543 0.060 Uiso 1 1 calc R U . . .
H30C H 0.265340 0.385000 -0.028613 0.060 Uiso 1 1 calc R U . . .
C52 C 0.73597(16) 0.42775(13) 0.44595(12) 0.0281(3) Uani 1 1 d . . . . .
C35 C 0.94469(16) 0.21643(14) 0.88164(11) 0.0309(4) Uani 1 1 d . . . . .
H35 H 0.978514 0.228436 0.944043 0.037 Uiso 1 1 calc R U . . .
C48 C 0.51766(17) 0.43084(14) 0.39246(13) 0.0325(4) Uani 1 1 d . . . . .
H48 H 0.549449 0.503800 0.390610 0.039 Uiso 1 1 calc R U . . .
C24 C 0.89746(14) 0.42494(12) 0.15335(11) 0.0240(3) Uani 1 1 d . . . . .
C31 C 0.49929(17) 0.43008(15) 0.16361(14) 0.0381(4) Uani 1 1 d . . . . .
H31A H 0.506065 0.427246 0.223076 0.057 Uiso 1 1 calc R U . . .
H31B H 0.546895 0.504763 0.168206 0.057 Uiso 1 1 calc R U . . .
H31C H 0.530777 0.376106 0.138104 0.057 Uiso 1 1 calc R U . . .
C59 C 1.05614(18) 0.22839(16) 0.63254(14) 0.0389(4) Uani 1 1 d . . . . .
H59A H 0.976265 0.221752 0.589921 0.058 Uiso 1 1 calc R U . . .
H59B H 1.105918 0.211058 0.600252 0.058 Uiso 1 1 calc R U . . .
H59C H 1.097302 0.304355 0.673886 0.058 Uiso 1 1 calc R U . . .
C60 C 1.16702(17) 0.15545(19) 0.74701(14) 0.0450(5) Uani 1 1 d . . . . .
H60A H 1.210682 0.230950 0.788925 0.067 Uiso 1 1 calc R U . . .
H60B H 1.212636 0.138219 0.711122 0.067 Uiso 1 1 calc R U . . .
H60C H 1.159143 0.102621 0.780271 0.067 Uiso 1 1 calc R U . . .
C53 C 0.80914(18) 0.43638(16) 0.54252(13) 0.0395(4) Uani 1 1 d . . . . .
H53A H 0.779221 0.475628 0.582223 0.059 Uiso 1 1 calc R U . . .
H53B H 0.895737 0.477299 0.559660 0.059 Uiso 1 1 calc R U . . .
H53C H 0.799181 0.361730 0.547335 0.059 Uiso 1 1 calc R U . . .
C54 C 0.7700(2) 0.54560(16) 0.43856(16) 0.0461(5) Uani 1 1 d . . . . .
H54A H 0.727754 0.542430 0.376772 0.069 Uiso 1 1 calc R U . . .
H54B H 0.858386 0.576885 0.456485 0.069 Uiso 1 1 calc R U . . .
H54C H 0.745346 0.592497 0.477704 0.069 Uiso 1 1 calc R U . . .
C25 C 1.02363(16) 0.51704(14) 0.19759(13) 0.0350(4) Uani 1 1 d . . . . .
H25A H 1.044840 0.546744 0.261614 0.053 Uiso 1 1 calc R U . . .
H25B H 1.021675 0.576631 0.170818 0.053 Uiso 1 1 calc R U . . .
H25C H 1.084836 0.486482 0.188557 0.053 Uiso 1 1 calc R U . . .
C55 C 0.77301(19) 0.35678(16) 0.38183(14) 0.0396(4) Uani 1 1 d . . . . .
H55A H 0.755706 0.281891 0.386966 0.059 Uiso 1 1 calc R U . . .
H55B H 0.860482 0.390525 0.397056 0.059 Uiso 1 1 calc R U . . .
H55C H 0.726483 0.352611 0.320515 0.059 Uiso 1 1 calc R U . . .
C49 C 0.39306(18) 0.38356(16) 0.36687(14) 0.0378(4) Uani 1 1 d . . . . .
H49 H 0.340957 0.423426 0.346908 0.045 Uiso 1 1 calc R U . . .
C32 C 0.3231(2) 0.49400(15) 0.14299(16) 0.0436(5) Uani 1 1 d . . . . .
H32A H 0.236972 0.478323 0.106425 0.065 Uiso 1 1 calc R U . . .
H32B H 0.372569 0.565807 0.143770 0.065 Uiso 1 1 calc R U . . .
H32C H 0.333126 0.496253 0.203978 0.065 Uiso 1 1 calc R U . . .
C26 C 0.86856(19) 0.38062(16) 0.05381(12) 0.0394(4) Uani 1 1 d . . . . .
H26A H 0.929919 0.349393 0.046086 0.059 Uiso 1 1 calc R U . . .
H26B H 0.869754 0.441366 0.028126 0.059 Uiso 1 1 calc R U . . .
H26C H 0.787527 0.322755 0.023524 0.059 Uiso 1 1 calc R U . . .
C27 C 0.80548(17) 0.47857(14) 0.16733(14) 0.0350(4) Uani 1 1 d . . . . .
H27A H 0.722257 0.426994 0.129629 0.052 Uiso 1 1 calc R U . . .
H27B H 0.818451 0.547004 0.151250 0.052 Uiso 1 1 calc R U . . .
H27C H 0.816998 0.495953 0.230051 0.052 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
Zr1 Zr1 3.2231(3) 2_655 ?
Zr1 Cl3 2.4689(4) . ?
Zr1 O28 1.9700(10) . ?
Zr1 O23 1.9711(10) . ?
Zr1 N12 2.3887(12) . ?
Zr1 N12 2.3952(12) 2_655 ?
Zr1 N14 2.4997(13) 2_655 ?
Zr1 N14 2.3200(12) . ?
Zr1 C13 2.6886(14) . ?
Zr1 C13 2.7849(15) 2_655 ?
Zr2 Zr2 3.5609(3) 2_656 ?
Zr2 Cl4 2.4551(4) . ?
Zr2 O56 1.9558(11) . ?
Zr2 O51 1.9618(10) . ?
Zr2 N42 2.3298(12) . ?
Zr2 N42 2.3038(12) 2_656 ?
Zr2 N40 2.2444(12) . ?
Zr2 C41 2.6498(14) . ?
O28 C10 1.3618(18) . ?
O23 C18 1.3658(18) . ?
O56 C38 1.3655(18) . ?
O51 C46 1.3613(18) . ?
N42 C41 1.387(2) . ?
N42 C43 1.4843(19) . ?
N40 C41 1.301(2) . ?
N40 C39 1.463(2) . ?
N12 C13 1.336(2) . ?
N12 C11 1.4720(19) . ?
N14 C13 1.337(2) . ?
N14 C15 1.461(2) . ?
C10 C9 1.417(2) . ?
C10 C5 1.406(2) . ?
C18 C17 1.403(2) . ?
C18 C19 1.416(2) . ?
C9 C8 1.395(2) . ?
C9 C29 1.535(2) . ?
C5 C6 1.391(2) . ?
C5 C11 1.519(2) . ?
C8 H8 0.9500 . ?
C8 C7 1.388(2) . ?
C13 C16 1.489(2) . ?
C45 C46 1.401(2) . ?
C45 C50 1.392(2) . ?
C45 C43 1.519(2) . ?
C17 C15 1.510(2) . ?
C17 C22 1.392(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C57 C37 1.537(2) . ?
C57 C58 1.540(2) . ?
C57 C59 1.537(3) . ?
C57 C60 1.544(2) . ?
C22 H22 0.9500 . ?
C22 C21 1.375(2) . ?
C41 C44 1.497(2) . ?
C37 C38 1.416(2) . ?
C37 C36 1.395(2) . ?
C7 H7 0.9500 . ?
C7 C6 1.384(2) . ?
C46 C47 1.409(2) . ?
C33 C38 1.405(2) . ?
C33 C39 1.513(2) . ?
C33 C34 1.393(2) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C6 H6 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C47 C52 1.534(2) . ?
C47 C48 1.396(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C19 C20 1.392(2) . ?
C19 C24 1.536(2) . ?
C36 H36 0.9500 . ?
C36 C35 1.387(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C21 H21 0.9500 . ?
C21 C20 1.386(3) . ?
C29 C30 1.533(3) . ?
C29 C31 1.533(3) . ?
C29 C32 1.541(2) . ?
C50 H50 0.9500 . ?
C50 C49 1.376(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.385(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C20 H20 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C52 C53 1.535(3) . ?
C52 C54 1.539(2) . ?
C52 C55 1.535(2) . ?
C35 H35 0.9500 . ?
C48 H48 0.9500 . ?
C48 C49 1.384(3) . ?
C24 C25 1.537(2) . ?
C24 C26 1.532(2) . ?
C24 C27 1.535(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C49 H49 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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 . ?

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
Cl3 Zr1 Zr1 122.782(11) . 2_655 ?
Cl3 Zr1 N14 79.31(3) . 2_655 ?
Cl3 Zr1 C13 71.93(3) . 2_655 ?
Cl3 Zr1 C13 166.01(4) . . ?
O28 Zr1 Zr1 122.47(3) . 2_655 ?
O28 Zr1 Cl3 92.31(3) . . ?
O28 Zr1 O23 103.01(5) . . ?
O28 Zr1 N12 75.14(4) . . ?
O28 Zr1 N12 168.02(4) . 2_655 ?
O28 Zr1 N14 105.00(4) . . ?
O28 Zr1 N14 116.87(4) . 2_655 ?
O28 Zr1 C13 142.74(5) . 2_655 ?
O28 Zr1 C13 79.58(4) . . ?
O23 Zr1 Zr1 115.80(3) . 2_655 ?
O23 Zr1 Cl3 94.86(3) . . ?
O23 Zr1 N12 88.52(4) . 2_655 ?
O23 Zr1 N12 127.83(4) . . ?
O23 Zr1 N14 77.40(4) . . ?
O23 Zr1 N14 139.79(4) . 2_655 ?
O23 Zr1 C13 98.06(5) . . ?
O23 Zr1 C13 111.62(5) . 2_655 ?
N12 Zr1 Zr1 47.56(3) 2_655 2_655 ?
N12 Zr1 Zr1 47.73(3) . 2_655 ?
N12 Zr1 Cl3 89.94(3) 2_655 . ?
N12 Zr1 Cl3 137.03(3) . . ?
N12 Zr1 N12 95.29(4) . 2_655 ?
N12 Zr1 N14 70.95(4) . 2_655 ?
N12 Zr1 N14 52.09(4) 2_655 2_655 ?
N12 Zr1 C13 29.77(5) . . ?
N12 Zr1 C13 95.74(4) 2_655 . ?
N12 Zr1 C13 93.41(4) . 2_655 ?
N12 Zr1 C13 28.65(4) 2_655 2_655 ?
N14 Zr1 Zr1 50.45(3) . 2_655 ?
N14 Zr1 Zr1 45.69(3) 2_655 2_655 ?
N14 Zr1 Cl3 162.19(3) . . ?
N14 Zr1 N12 54.34(4) . . ?
N14 Zr1 N12 74.01(4) . 2_655 ?
N14 Zr1 N14 96.15(4) . 2_655 ?
N14 Zr1 C13 29.82(5) . . ?
N14 Zr1 C13 28.67(4) 2_655 2_655 ?
N14 Zr1 C13 95.78(4) . 2_655 ?
N14 Zr1 C13 94.10(4) 2_655 . ?
C13 Zr1 Zr1 55.32(3) . 2_655 ?
C13 Zr1 Zr1 52.55(3) 2_655 2_655 ?
C13 Zr1 C13 107.87(4) . 2_655 ?
Cl4 Zr2 Zr2 110.357(12) . 2_656 ?
Cl4 Zr2 C41 158.62(4) . . ?
O56 Zr2 Zr2 126.92(3) . 2_656 ?
O56 Zr2 Cl4 97.21(3) . . ?
O56 Zr2 O51 106.24(5) . . ?
O56 Zr2 N42 102.24(4) . 2_656 ?
O56 Zr2 N42 135.10(4) . . ?
O56 Zr2 N40 77.85(4) . . ?
O56 Zr2 C41 104.13(5) . . ?
O51 Zr2 Zr2 115.59(3) . 2_656 ?
O51 Zr2 Cl4 94.03(3) . . ?
O51 Zr2 N42 78.03(4) . . ?
O51 Zr2 N42 151.33(5) . 2_656 ?
O51 Zr2 N40 98.65(5) . . ?
O51 Zr2 C41 78.93(4) . . ?
N42 Zr2 Zr2 39.51(3) . 2_656 ?
N42 Zr2 Zr2 40.05(3) 2_656 2_656 ?
N42 Zr2 Cl4 85.57(3) 2_656 . ?
N42 Zr2 Cl4 127.45(3) . . ?
N42 Zr2 N42 79.56(5) 2_656 . ?
N42 Zr2 C41 31.52(5) . . ?
N42 Zr2 C41 91.09(4) 2_656 . ?
N40 Zr2 Zr2 65.26(3) . 2_656 ?
N40 Zr2 Cl4 167.24(3) . . ?
N40 Zr2 N42 57.54(4) . . ?
N40 Zr2 N42 84.03(4) . 2_656 ?
N40 Zr2 C41 29.37(5) . . ?
C41 Zr2 Zr2 56.94(3) . 2_656 ?
C10 O28 Zr1 148.54(9) . . ?
C18 O23 Zr1 143.16(9) . . ?
C38 O56 Zr2 141.63(9) . . ?
C46 O51 Zr2 145.55(10) . . ?
Zr2 N42 Zr2 100.44(5) 2_656 . ?
C41 N42 Zr2 87.07(8) . . ?
C41 N42 Zr2 109.91(9) . 2_656 ?
C41 N42 C43 119.30(12) . . ?
C43 N42 Zr2 116.68(9) . 2_656 ?
C43 N42 Zr2 118.52(9) . . ?
C41 N40 Zr2 92.86(9) . . ?
C41 N40 C39 122.46(13) . . ?
C39 N40 Zr2 129.32(9) . . ?
Zr1 N12 Zr1 84.71(4) . 2_655 ?
C13 N12 Zr1 92.09(9) . 2_655 ?
C13 N12 Zr1 87.64(8) . . ?
C13 N12 C11 121.32(13) . . ?
C11 N12 Zr1 121.09(9) . . ?
C11 N12 Zr1 136.04(9) . 2_655 ?
Zr1 N14 Zr1 83.85(4) . 2_655 ?
C13 N14 Zr1 87.60(9) . 2_655 ?
C13 N14 Zr1 90.54(9) . . ?
C13 N14 C15 120.21(13) . . ?
C15 N14 Zr1 131.15(10) . 2_655 ?
C15 N14 Zr1 130.08(9) . . ?
O28 C10 C9 120.57(13) . . ?
O28 C10 C5 118.31(13) . . ?
C5 C10 C9 121.11(14) . . ?
O23 C18 C17 119.54(13) . . ?
O23 C18 C19 119.98(13) . . ?
C17 C18 C19 120.47(14) . . ?
C10 C9 C29 121.45(14) . . ?
C8 C9 C10 116.65(14) . . ?
C8 C9 C29 121.88(14) . . ?
C10 C5 C11 121.13(14) . . ?
C6 C5 C10 119.56(14) . . ?
C6 C5 C11 119.31(14) . . ?
C9 C8 H8 118.6 . . ?
C7 C8 C9 122.74(15) . . ?
C7 C8 H8 118.6 . . ?
Zr1 C13 Zr1 72.13(4) . 2_655 ?
N12 C13 Zr1 59.26(8) . 2_655 ?
N12 C13 Zr1 62.59(8) . . ?
N12 C13 N14 107.16(13) . . ?
N12 C13 C16 126.86(14) . . ?
N14 C13 Zr1 63.74(8) . 2_655 ?
N14 C13 Zr1 59.64(7) . . ?
N14 C13 C16 125.97(14) . . ?
C16 C13 Zr1 144.38(10) . 2_655 ?
C16 C13 Zr1 143.49(10) . . ?
C46 C45 C43 121.79(13) . . ?
C50 C45 C46 119.56(15) . . ?
C50 C45 C43 118.65(14) . . ?
C18 C17 C15 124.69(14) . . ?
C22 C17 C18 119.69(14) . . ?
C22 C17 C15 115.07(14) . . ?
N14 C15 C17 115.65(13) . . ?
N14 C15 H15A 108.4 . . ?
N14 C15 H15B 108.4 . . ?
C17 C15 H15A 108.4 . . ?
C17 C15 H15B 108.4 . . ?
H15A C15 H15B 107.4 . . ?
C37 C57 C58 109.79(14) . . ?
C37 C57 C60 111.03(15) . . ?
C58 C57 C60 107.71(14) . . ?
C59 C57 C37 111.25(14) . . ?
C59 C57 C58 109.55(15) . . ?
C59 C57 C60 107.43(16) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 C17 120.66(16) . . ?
C21 C22 H22 119.7 . . ?
N42 C41 Zr2 61.41(7) . . ?
N42 C41 C44 124.60(14) . . ?
N40 C41 Zr2 57.77(8) . . ?
N40 C41 N42 110.03(12) . . ?
N40 C41 C44 125.31(14) . . ?
C44 C41 Zr2 149.71(11) . . ?
C38 C37 C57 122.25(14) . . ?
C36 C37 C57 121.23(14) . . ?
C36 C37 C38 116.52(15) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 C8 119.56(15) . . ?
C6 C7 H7 120.2 . . ?
O51 C46 C45 118.55(13) . . ?
O51 C46 C47 119.94(14) . . ?
C45 C46 C47 121.50(14) . . ?
C38 C33 C39 122.58(14) . . ?
C34 C33 C38 119.41(15) . . ?
C34 C33 C39 117.83(14) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O56 C38 C37 119.17(14) . . ?
O56 C38 C33 119.40(13) . . ?
C33 C38 C37 121.43(14) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.25(15) . . ?
C7 C6 H6 119.9 . . ?
N12 C11 C5 114.02(12) . . ?
N12 C11 H11A 108.7 . . ?
N12 C11 H11B 108.7 . . ?
C5 C11 H11A 108.7 . . ?
C5 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C46 C47 C52 121.62(14) . . ?
C48 C47 C46 116.35(15) . . ?
C48 C47 C52 122.02(14) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C19 C24 122.16(14) . . ?
C20 C19 C18 117.16(14) . . ?
C20 C19 C24 120.62(14) . . ?
C37 C36 H36 118.6 . . ?
C35 C36 C37 122.72(16) . . ?
C35 C36 H36 118.6 . . ?
N40 C39 C33 112.30(12) . . ?
N40 C39 H39A 109.1 . . ?
N40 C39 H39B 109.1 . . ?
C33 C39 H39A 109.1 . . ?
C33 C39 H39B 109.1 . . ?
H39A C39 H39B 107.9 . . ?
C22 C21 H21 120.4 . . ?
C22 C21 C20 119.30(15) . . ?
C20 C21 H21 120.4 . . ?
C9 C29 C32 111.61(14) . . ?
C30 C29 C9 109.25(14) . . ?
C30 C29 C31 110.47(15) . . ?
C30 C29 C32 107.56(15) . . ?
C31 C29 C9 110.71(14) . . ?
C31 C29 C32 107.18(15) . . ?
C45 C50 H50 120.0 . . ?
C49 C50 C45 119.95(17) . . ?
C49 C50 H50 120.0 . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.13(16) . . ?
C35 C34 H34 119.9 . . ?
N42 C43 C45 115.20(13) . . ?
N42 C43 H43A 108.5 . . ?
N42 C43 H43B 108.5 . . ?
C45 C43 H43A 108.5 . . ?
C45 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
C19 C20 H20 118.7 . . ?
C21 C20 C19 122.69(15) . . ?
C21 C20 H20 118.7 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C47 C52 C53 110.52(14) . . ?
C47 C52 C54 111.73(15) . . ?
C53 C52 C54 107.46(16) . . ?
C55 C52 C47 109.30(14) . . ?
C55 C52 C53 110.20(16) . . ?
C55 C52 C54 107.58(15) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 C36 119.75(16) . . ?
C34 C35 H35 120.1 . . ?
C47 C48 H48 118.7 . . ?
C49 C48 C47 122.69(16) . . ?
C49 C48 H48 118.7 . . ?
C19 C24 C25 111.99(14) . . ?
C26 C24 C19 110.09(13) . . ?
C26 C24 C25 107.64(14) . . ?
C26 C24 C27 110.43(16) . . ?
C27 C24 C19 109.68(13) . . ?
C27 C24 C25 106.95(14) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C50 C49 C48 119.93(16) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
Zr1 O28 C10 C9 155.55(15) . . . . ?
Zr1 O28 C10 C5 -23.6(3) . . . . ?
Zr1 O23 C18 C17 -28.1(2) . . . . ?
Zr1 O23 C18 C19 152.65(12) . . . . ?
Zr1 N12 C13 Zr1 -84.62(4) . . . 2_655 ?
Zr1 N12 C13 Zr1 84.62(4) 2_655 . . . ?
Zr1 N12 C13 N14 43.74(11) 2_655 . . . ?
Zr1 N12 C13 N14 -40.88(10) . . . . ?
Zr1 N12 C13 C16 -137.41(14) 2_655 . . . ?
Zr1 N12 C13 C16 137.97(14) . . . . ?
Zr1 N12 C11 C5 -174.42(10) 2_655 . . . ?
Zr1 N12 C11 C5 -56.36(16) . . . . ?
Zr1 N14 C13 Zr1 -83.82(4) 2_655 . . . ?
Zr1 N14 C13 Zr1 83.82(4) . . . 2_655 ?
Zr1 N14 C13 N12 42.32(11) . . . . ?
Zr1 N14 C13 N12 -41.50(10) 2_655 . . . ?
Zr1 N14 C13 C16 139.64(14) 2_655 . . . ?
Zr1 N14 C13 C16 -136.54(14) . . . . ?
Zr1 N14 C15 C17 101.04(15) 2_655 . . . ?
Zr1 N14 C15 C17 -22.3(2) . . . . ?
Zr2 O56 C38 C37 147.28(12) . . . . ?
Zr2 O56 C38 C33 -32.4(2) . . . . ?
Zr2 O51 C46 C45 -23.7(3) . . . . ?
Zr2 O51 C46 C47 155.44(14) . . . . ?
Zr2 N42 C41 Zr2 100.04(6) 2_656 . . . ?
Zr2 N42 C41 N40 67.72(13) 2_656 . . . ?
Zr2 N42 C41 N40 -32.32(11) . . . . ?
Zr2 N42 C41 C44 -115.00(14) 2_656 . . . ?
Zr2 N42 C41 C44 144.96(14) . . . . ?
Zr2 N42 C43 C45 -57.31(16) . . . . ?
Zr2 N42 C43 C45 -177.55(10) 2_656 . . . ?
Zr2 N40 C41 N42 33.70(12) . . . . ?
Zr2 N40 C41 C44 -143.55(14) . . . . ?
Zr2 N40 C39 C33 -42.25(18) . . . . ?
O28 C10 C9 C8 -176.54(14) . . . . ?
O28 C10 C9 C29 5.0(2) . . . . ?
O28 C10 C5 C6 174.87(14) . . . . ?
O28 C10 C5 C11 -5.5(2) . . . . ?
O23 C18 C17 C15 -9.6(2) . . . . ?
O23 C18 C17 C22 179.33(14) . . . . ?
O23 C18 C19 C20 -178.50(13) . . . . ?
O23 C18 C19 C24 4.1(2) . . . . ?
O51 C46 C47 C52 2.0(2) . . . . ?
O51 C46 C47 C48 -178.79(14) . . . . ?
C10 C9 C8 C7 0.3(3) . . . . ?
C10 C9 C29 C30 59.6(2) . . . . ?
C10 C9 C29 C31 -62.2(2) . . . . ?
C10 C9 C29 C32 178.46(16) . . . . ?
C10 C5 C6 C7 3.0(3) . . . . ?
C10 C5 C11 N12 42.2(2) . . . . ?
C18 C17 C15 N14 29.2(2) . . . . ?
C18 C17 C22 C21 -0.2(2) . . . . ?
C18 C19 C20 C21 -1.6(2) . . . . ?
C18 C19 C24 C25 173.58(14) . . . . ?
C18 C19 C24 C26 -66.70(19) . . . . ?
C18 C19 C24 C27 55.01(19) . . . . ?
C9 C10 C5 C6 -4.3(2) . . . . ?
C9 C10 C5 C11 175.35(15) . . . . ?
C9 C8 C7 C6 -1.6(3) . . . . ?
C5 C10 C9 C8 2.6(2) . . . . ?
C5 C10 C9 C29 -175.88(15) . . . . ?
C8 C9 C29 C30 -118.78(18) . . . . ?
C8 C9 C29 C31 119.34(18) . . . . ?
C8 C9 C29 C32 0.0(2) . . . . ?
C8 C7 C6 C5 -0.1(3) . . . . ?
C13 N12 C11 C5 51.74(19) . . . . ?
C13 N14 C15 C17 -142.57(14) . . . . ?
C45 C46 C47 C52 -178.90(15) . . . . ?
C45 C46 C47 C48 0.3(2) . . . . ?
C45 C50 C49 C48 0.2(3) . . . . ?
C17 C18 C19 C20 2.2(2) . . . . ?
C17 C18 C19 C24 -175.22(14) . . . . ?
C17 C22 C21 C20 0.9(3) . . . . ?
C15 N14 C13 Zr1 -137.54(13) . . . 2_655 ?
C15 N14 C13 Zr1 138.64(14) . . . . ?
C15 N14 C13 N12 -179.04(12) . . . . ?
C15 N14 C13 C16 2.1(2) . . . . ?
C15 C17 C22 C21 -172.11(16) . . . . ?
C57 C37 C38 O56 1.8(2) . . . . ?
C57 C37 C38 C33 -178.56(14) . . . . ?
C57 C37 C36 C35 179.77(16) . . . . ?
C22 C17 C15 N14 -159.32(14) . . . . ?
C22 C21 C20 C19 0.1(3) . . . . ?
C41 N42 C43 C45 46.47(19) . . . . ?
C41 N40 C39 C33 -168.94(13) . . . . ?
C37 C36 C35 C34 -0.3(3) . . . . ?
C46 C45 C50 C49 -1.2(3) . . . . ?
C46 C45 C43 N42 38.4(2) . . . . ?
C46 C47 C52 C53 -59.3(2) . . . . ?
C46 C47 C52 C54 -178.91(16) . . . . ?
C46 C47 C52 C55 62.1(2) . . . . ?
C46 C47 C48 C49 -1.4(3) . . . . ?
C33 C34 C35 C36 0.3(2) . . . . ?
C58 C57 C37 C38 -65.34(19) . . . . ?
C58 C57 C37 C36 114.00(17) . . . . ?
C38 C37 C36 C35 -0.9(2) . . . . ?
C38 C33 C39 N40 38.2(2) . . . . ?
C38 C33 C34 C35 0.9(2) . . . . ?
C6 C5 C11 N12 -138.14(15) . . . . ?
C11 N12 C13 Zr1 -125.44(13) . . . . ?
C11 N12 C13 Zr1 149.94(14) . . . 2_655 ?
C11 N12 C13 N14 -166.32(12) . . . . ?
C11 N12 C13 C16 12.5(2) . . . . ?
C11 C5 C6 C7 -176.65(16) . . . . ?
C47 C48 C49 C50 1.1(3) . . . . ?
C19 C18 C17 C15 169.70(15) . . . . ?
C19 C18 C17 C22 -1.4(2) . . . . ?
C36 C37 C38 O56 -177.58(13) . . . . ?
C36 C37 C38 C33 2.1(2) . . . . ?
C39 N40 C41 Zr2 141.60(15) . . . . ?
C39 N40 C41 N42 175.31(13) . . . . ?
C39 N40 C41 C44 -2.0(2) . . . . ?
C39 C33 C38 O56 -7.4(2) . . . . ?
C39 C33 C38 C37 172.96(14) . . . . ?
C39 C33 C34 C35 -174.44(15) . . . . ?
C29 C9 C8 C7 178.80(16) . . . . ?
C50 C45 C46 O51 -179.91(15) . . . . ?
C50 C45 C46 C47 1.0(2) . . . . ?
C50 C45 C43 N42 -140.88(16) . . . . ?
C34 C33 C38 O56 177.54(13) . . . . ?
C34 C33 C38 C37 -2.1(2) . . . . ?
C34 C33 C39 N40 -146.66(14) . . . . ?
C43 N42 C41 Zr2 -121.29(13) . . . . ?
C43 N42 C41 N40 -153.61(13) . . . . ?
C43 N42 C41 C44 23.7(2) . . . . ?
C43 C45 C46 O51 0.8(2) . . . . ?
C43 C45 C46 C47 -178.33(15) . . . . ?
C43 C45 C50 C49 178.07(17) . . . . ?
C20 C19 C24 C25 -3.8(2) . . . . ?
C20 C19 C24 C26 115.95(17) . . . . ?
C20 C19 C24 C27 -122.34(16) . . . . ?
C52 C47 C48 C49 177.84(17) . . . . ?
C48 C47 C52 C53 121.52(18) . . . . ?
C48 C47 C52 C54 1.9(2) . . . . ?
C48 C47 C52 C55 -117.03(18) . . . . ?
C24 C19 C20 C21 175.90(15) . . . . ?
C59 C57 C37 C38 56.1(2) . . . . ?
C59 C57 C37 C36 -124.58(17) . . . . ?
C60 C57 C37 C38 175.67(15) . . . . ?
C60 C57 C37 C36 -5.0(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.363
_oxdiff_exptl_absorpt_empirical_full_min 0.543
####################################################################### 
# 
# 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_exp_10622
_database_code_depnum_ccdc_archive 'CCDC 2222935'
loop_
_audit_author_name
_audit_author_address
'Hanhua Xu'
;Peking University
China
;
_audit_update_record             
;
2022-11-29 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_audit_creation_date             2022-11-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H31 Cl Hf N2 O2)'
_chemical_formula_sum            'C48 H62 Cl2 Hf2 N4 O4'
_chemical_formula_weight         1186.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Hf Cl C H O N'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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'

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

_cell_length_a                   12.2507(2)
_cell_length_b                   13.1833(2)
_cell_length_c                   16.8154(2)
_cell_angle_alpha                100.1710(10)
_cell_angle_beta                 109.6060(10)
_cell_angle_gamma                103.6480(10)
_cell_volume                     2387.07(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    39510
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.7170
_cell_measurement_theta_min      3.0100
_shelx_estimated_absorpt_T_max   0.956
_shelx_estimated_absorpt_T_min   0.915
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.590
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  88.00   0.50    0.50    --   -1.70  38.00-150.00  218
  2  ω    -32.00  84.00   0.50    0.50    --   -1.70  77.00   0.00  232
  3  ω     24.00  72.00   0.50    0.50    --   -1.70  77.00-120.00   96
  4  ω    -25.00  76.00   0.50    0.50    --   -1.70  57.00 -30.00  202
  5  ω    -32.00   2.00   0.50    0.50    --   -1.70  77.00-120.00   68
  6  ω    -25.00  79.00   0.50    0.50    --   -1.70  57.00 120.00  208
  7  ω    -32.00  80.00   0.50    0.50    --   -1.70  77.00  60.00  224
  8  ω     -6.00  26.00   0.50    0.50    --    1.90 -19.00 -60.00   64
  9  ω    -82.00 -23.00   0.50    0.50    --    1.90 -19.00 -60.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120580000
_diffrn_orient_matrix_UB_12      0.0288024000
_diffrn_orient_matrix_UB_13      0.0434580000
_diffrn_orient_matrix_UB_21      -0.0587603000
_diffrn_orient_matrix_UB_22      0.0064013000
_diffrn_orient_matrix_UB_23      -0.0148046000
_diffrn_orient_matrix_UB_31      -0.0246083000
_diffrn_orient_matrix_UB_32      -0.0495422000
_diffrn_orient_matrix_UB_33      0.0081871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9933
_reflns_number_total             10906
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.453
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         10906
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+0.2040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0723
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00I,H00J), C00H(H00D,H00E), C00Z(H00R,H00S), C017(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00V(H00V), C012(H012), C015(H015), C016(H016), C019(H019),
 C01A(H01C), C01C(H01Z), C01E(H01G), C01F(H01H), C01I(H01), C01J(H01O)
2.c Idealised Me refined as rotating group:
 C00E(H00A,H00B,H00C), C00W(H00K,H00L,H00M), C00X(H00O,H00P,H00Q), C00Y(H00F,
 H00G,H00H), C013(H01V,H01W,H01X), C018(H01Y,H,HA), C01B(H01D,H01E,H01F),
 C01G(H01I,H01J,H01K), C01H(H01L,H01M,H01N), C01K(H01P,H01Q,H01R), C01L(H01S,
 H01T,H01U), C01M(H1,HB,HC), C01N(H2,HD,HE), C01O(H3,HF,HG)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf01 Hf 0.54274(2) 0.14046(2) 0.02625(2) 0.01722(5) Uani 1 1 d . . . . .
Hf02 Hf 0.63826(2) 0.09048(2) 0.50757(2) 0.01622(4) Uani 1 1 d . . . . .
Cl03 Cl 0.71153(7) 0.00265(6) 0.40552(5) 0.02608(15) Uani 1 1 d . . . . .
Cl04 Cl 0.53638(8) 0.21024(6) -0.10033(5) 0.02871(17) Uani 1 1 d . . . . .
O005 O 0.62205(19) 0.20727(16) 0.45114(14) 0.0235(4) Uani 1 1 d . . . . .
O006 O 0.79471(19) 0.15278(17) 0.60796(12) 0.0215(4) Uani 1 1 d . . . . .
O007 O 0.70004(19) 0.24470(16) 0.10869(12) 0.0224(4) Uani 1 1 d . . . . .
O008 O 0.4219(2) 0.20547(17) 0.04342(14) 0.0248(4) Uani 1 1 d . . . . .
N009 N 0.5870(2) 0.06657(19) 0.13737(15) 0.0207(5) Uani 1 1 d . . . . .
N00A N 0.5808(2) 0.14698(19) 0.61456(15) 0.0189(5) Uani 1 1 d . . . . .
N00B N 0.4370(2) 0.07884(18) 0.48075(15) 0.0172(5) Uani 1 1 d . . . . .
N00C N 0.4006(2) -0.00497(19) 0.03635(15) 0.0212(5) Uani 1 1 d . . . . .
C00D C 0.4733(3) 0.0272(2) 0.12544(18) 0.0203(6) Uani 1 1 d . . . . .
C00E C 0.4259(3) 0.0225(3) 0.19649(19) 0.0287(7) Uani 1 1 d . . . . .
H00A H 0.426864 0.095240 0.223274 0.043 Uiso 1 1 calc R U . . .
H00B H 0.477891 -0.003153 0.241434 0.043 Uiso 1 1 calc R U . . .
H00C H 0.342035 -0.027540 0.171273 0.043 Uiso 1 1 calc R U . . .
C00F C 0.7744(3) 0.2023(2) 0.74495(18) 0.0208(6) Uani 1 1 d . . . . .
C00G C 0.6535(3) 0.2211(2) 0.70287(19) 0.0243(6) Uani 1 1 d . . . . .
H00I H 0.606580 0.211049 0.740255 0.029 Uiso 1 1 calc R U . . .
H00J H 0.669008 0.297066 0.699363 0.029 Uiso 1 1 calc R U . . .
C00H C 0.6848(3) 0.1031(3) 0.22414(19) 0.0292(7) Uani 1 1 d . . . . .
H00D H 0.703349 0.038996 0.241114 0.035 Uiso 1 1 calc R U . . .
H00E H 0.656207 0.138188 0.266846 0.035 Uiso 1 1 calc R U . . .
C00I C 0.4201(3) 0.2168(2) 0.39358(19) 0.0239(6) Uani 1 1 d . . . . .
C00J C 0.5457(3) 0.2652(2) 0.42119(18) 0.0208(6) Uani 1 1 d . . . . .
C00K C 0.8431(3) 0.1750(2) 0.69746(18) 0.0195(6) Uani 1 1 d . . . . .
C00L C 0.9137(3) 0.4297(2) 0.1523(2) 0.0276(7) Uani 1 1 d . . . . .
C00M C 0.8000(3) 0.1816(2) 0.23027(18) 0.0218(6) Uani 1 1 d . . . . .
C00N C 0.8224(3) 0.2199(3) 0.83613(19) 0.0277(7) Uani 1 1 d . . . . .
H00N H 0.776261 0.237445 0.868910 0.033 Uiso 1 1 calc R U . . .
C00O C 0.4813(3) 0.1567(2) 0.56173(18) 0.0184(5) Uani 1 1 d . . . . .
C00P C 0.5968(3) 0.3729(2) 0.42017(19) 0.0240(6) Uani 1 1 d . . . . .
C00Q C 0.8036(3) 0.2548(2) 0.17877(18) 0.0207(6) Uani 1 1 d . . . . .
C00R C 0.2474(3) 0.0890(3) 0.0505(2) 0.0254(6) Uani 1 1 d . . . . .
C00S C 0.9614(3) 0.1692(2) 0.7400(2) 0.0258(6) Uani 1 1 d . . . . .
C00T C 0.7342(3) 0.4266(3) 0.4513(2) 0.0304(7) Uani 1 1 d . . . . .
C00U C 0.3216(3) 0.1942(3) 0.06316(18) 0.0232(6) Uani 1 1 d . . . . .
C00V C 0.9363(3) 0.2119(3) 0.8786(2) 0.0320(7) Uani 1 1 d . . . . .
H00V H 0.967941 0.222949 0.940417 0.038 Uiso 1 1 calc R U . . .
C00W C 0.4263(3) 0.2417(3) 0.5816(2) 0.0284(7) Uani 1 1 d . . . . .
H00K H 0.472457 0.310429 0.576974 0.043 Uiso 1 1 calc R U . . .
H00L H 0.428891 0.251159 0.641439 0.043 Uiso 1 1 calc R U . . .
H00M H 0.341206 0.219639 0.539636 0.043 Uiso 1 1 calc R U . . .
C00X C 0.9777(3) 0.0286(3) 0.6255(2) 0.0360(8) Uani 1 1 d . . . . .
H00O H 0.900708 0.025961 0.580432 0.054 Uiso 1 1 calc R U . . .
H00P H 0.961035 -0.024019 0.657822 0.054 Uiso 1 1 calc R U . . .
H00Q H 1.031606 0.010622 0.597277 0.054 Uiso 1 1 calc R U . . .
C00Y C 0.5041(3) 0.4295(3) 0.1652(3) 0.0423(9) Uani 1 1 d . . . . .
H00F H 0.541657 0.382228 0.139380 0.063 Uiso 1 1 calc R U . . .
H00G H 0.508734 0.418418 0.222162 0.063 Uiso 1 1 calc R U . . .
H00H H 0.547819 0.505572 0.173332 0.063 Uiso 1 1 calc R U . . .
C00Z C 0.3657(3) 0.1040(2) 0.39977(19) 0.0232(6) Uani 1 1 d . . . . .
H00R H 0.282053 0.095838 0.397257 0.028 Uiso 1 1 calc R U . . .
H00S H 0.358591 0.049750 0.347858 0.028 Uiso 1 1 calc R U . . .
C010 C 0.9114(3) 0.3395(2) 0.19887(18) 0.0214(6) Uani 1 1 d . . . . .
C011 C 0.2949(3) 0.2866(3) 0.0969(2) 0.0263(6) Uani 1 1 d . . . . .
C012 C 0.5127(3) 0.4271(3) 0.3891(2) 0.0340(8) Uani 1 1 d . . . . .
H012 H 0.542916 0.500101 0.388399 0.041 Uiso 1 1 calc R U . . .
C013 C 0.7840(4) 0.3642(3) 0.3934(3) 0.0393(9) Uani 1 1 d . . . . .
H01V H 0.770955 0.289930 0.398996 0.059 Uiso 1 1 calc R U . . .
H01W H 0.871673 0.400963 0.412356 0.059 Uiso 1 1 calc R U . . .
H01X H 0.741241 0.361690 0.331981 0.059 Uiso 1 1 calc R U . . .
C014 C 1.0404(3) 0.1438(3) 0.6897(2) 0.0305(7) Uani 1 1 d . . . . .
C015 C 0.1235(3) 0.1650(3) 0.1119(2) 0.0342(8) Uani 1 1 d . . . . .
H015 H 0.057288 0.155801 0.130190 0.041 Uiso 1 1 calc R U . . .
C016 C 0.9071(3) 0.1898(3) 0.2984(2) 0.0295(7) Uani 1 1 d . . . . .
H016 H 0.905399 0.141117 0.333755 0.035 Uiso 1 1 calc R U . . .
C017 C 0.2705(3) -0.0098(3) 0.0069(2) 0.0278(7) Uani 1 1 d . . . . .
H01A H 0.224490 -0.074533 0.017930 0.033 Uiso 1 1 calc R U . . .
H01B H 0.237413 -0.020057 -0.057435 0.033 Uiso 1 1 calc R U . . .
C018 C 0.7998(4) 0.4303(3) 0.5478(2) 0.0394(9) Uani 1 1 d . . . . .
H01Y H 0.759509 0.460812 0.583009 0.059 Uiso 1 1 calc R U . . .
H H 0.885310 0.476035 0.569922 0.059 Uiso 1 1 calc R U . . .
HA H 0.796421 0.356580 0.552133 0.059 Uiso 1 1 calc R U . . .
C019 C 1.0050(3) 0.1877(3) 0.8315(2) 0.0319(7) Uani 1 1 d . . . . .
H019 H 1.083916 0.183523 0.862051 0.038 Uiso 1 1 calc R U . . .
C01A C 0.1493(3) 0.0758(3) 0.0760(2) 0.0289(7) Uani 1 1 d . . . . .
H01C H 0.099720 0.004788 0.068767 0.035 Uiso 1 1 calc R U . . .
C01B C 0.8195(4) 0.4837(3) 0.1636(3) 0.0408(9) Uani 1 1 d . . . . .
H01D H 0.736919 0.432295 0.129857 0.061 Uiso 1 1 calc R U . . .
H01E H 0.828153 0.548422 0.142175 0.061 Uiso 1 1 calc R U . . .
H01F H 0.833385 0.504829 0.225940 0.061 Uiso 1 1 calc R U . . .
C01C C 0.3415(3) 0.2738(3) 0.3613(2) 0.0333(7) Uani 1 1 d . . . . .
H01Z H 0.255610 0.240424 0.340548 0.040 Uiso 1 1 calc R U . . .
C01D C 0.3699(3) 0.4016(3) 0.1035(2) 0.0338(7) Uani 1 1 d . . . . .
C01E C 1.0148(3) 0.2667(3) 0.3155(2) 0.0345(8) Uani 1 1 d . . . . .
H01G H 1.088264 0.269304 0.360432 0.041 Uiso 1 1 calc R U . . .
C01F C 1.0161(3) 0.3410(3) 0.2666(2) 0.0290(7) Uani 1 1 d . . . . .
H01H H 1.091219 0.395162 0.279835 0.035 Uiso 1 1 calc R U . . .
C01G C 0.8863(4) 0.3840(3) 0.0548(2) 0.0450(10) Uani 1 1 d . . . . .
H01I H 0.940915 0.342068 0.049219 0.068 Uiso 1 1 calc R U . . .
H01J H 0.899284 0.444087 0.028447 0.068 Uiso 1 1 calc R U . . .
H01K H 0.801204 0.336669 0.024358 0.068 Uiso 1 1 calc R U . . .
C01H C 1.0379(4) 0.5189(3) 0.1931(3) 0.0420(9) Uani 1 1 d . . . . .
H01L H 1.056049 0.552454 0.254916 0.063 Uiso 1 1 calc R U . . .
H01M H 1.035853 0.574281 0.161169 0.063 Uiso 1 1 calc R U . . .
H01N H 1.101400 0.487194 0.189480 0.063 Uiso 1 1 calc R U . . .
C01I C 0.3879(4) 0.3791(3) 0.3594(3) 0.0406(9) Uani 1 1 d . . . . .
H01 H 0.334094 0.418424 0.337677 0.049 Uiso 1 1 calc R U . . .
C01J C 0.1953(3) 0.2686(3) 0.1210(2) 0.0317(7) Uani 1 1 d . . . . .
H01O H 0.175592 0.329530 0.144530 0.038 Uiso 1 1 calc R U . . .
C01K C 0.3610(4) 0.4073(4) 0.0118(3) 0.0490(10) Uani 1 1 d . . . . .
H01P H 0.274902 0.388677 -0.027435 0.074 Uiso 1 1 calc R U . . .
H01Q H 0.396660 0.355750 -0.011010 0.074 Uiso 1 1 calc R U . . .
H01R H 0.405523 0.481092 0.014799 0.074 Uiso 1 1 calc R U . . .
C01L C 0.3218(4) 0.4888(3) 0.1397(3) 0.0529(11) Uani 1 1 d . . . . .
H01S H 0.369784 0.560399 0.141037 0.079 Uiso 1 1 calc R U . . .
H01T H 0.328924 0.487994 0.199426 0.079 Uiso 1 1 calc R U . . .
H01U H 0.235765 0.473555 0.101857 0.079 Uiso 1 1 calc R U . . .
C01M C 0.7646(4) 0.5451(3) 0.4453(3) 0.0444(9) Uani 1 1 d . . . . .
H1 H 0.729252 0.545164 0.383669 0.067 Uiso 1 1 calc R U . . .
HB H 0.853465 0.578864 0.468957 0.067 Uiso 1 1 calc R U . . .
HC H 0.730221 0.586238 0.479402 0.067 Uiso 1 1 calc R U . . .
C01N C 1.0592(4) 0.2269(3) 0.6374(3) 0.0444(9) Uani 1 1 d . . . . .
H2 H 1.099881 0.300229 0.678059 0.067 Uiso 1 1 calc R U . . .
HD H 0.979746 0.223357 0.594977 0.067 Uiso 1 1 calc R U . . .
HE H 1.110082 0.209898 0.606090 0.067 Uiso 1 1 calc R U . . .
C01O C 1.1668(4) 0.1468(4) 0.7519(3) 0.0537(11) Uani 1 1 d . . . . .
H3 H 1.213153 0.127630 0.717390 0.081 Uiso 1 1 calc R U . . .
HF H 1.156813 0.094694 0.785903 0.081 Uiso 1 1 calc R U . . .
HG H 1.211050 0.220127 0.792091 0.081 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
Hf01 Hf01 3.4620(2) 2_655 ?
Hf01 Cl04 2.4489(7) . ?
Hf01 O007 1.9515(19) . ?
Hf01 O008 1.952(2) . ?
Hf01 N009 2.224(2) . ?
Hf01 N00C 2.279(3) 2_655 ?
Hf01 N00C 2.340(2) . ?
Hf01 C00D 2.639(3) . ?
Hf02 Hf02 3.5532(2) 2_656 ?
Hf02 Cl03 2.4317(7) . ?
Hf02 O005 1.9607(19) . ?
Hf02 O006 1.948(2) . ?
Hf02 N00A 2.216(2) . ?
Hf02 N00B 2.275(2) 2_656 ?
Hf02 N00B 2.315(2) . ?
Hf02 C00O 2.641(3) . ?
O005 C00J 1.366(3) . ?
O006 C00K 1.366(3) . ?
O007 C00Q 1.370(3) . ?
O008 C00U 1.359(4) . ?
N009 C00D 1.298(4) . ?
N009 C00H 1.450(4) . ?
N00A C00G 1.464(4) . ?
N00A C00O 1.296(4) . ?
N00B C00O 1.396(4) . ?
N00B C00Z 1.491(3) . ?
N00C C00D 1.385(4) . ?
N00C C017 1.483(4) . ?
C00D C00E 1.497(4) . ?
C00E H00A 0.9800 . ?
C00E H00B 0.9800 . ?
C00E H00C 0.9800 . ?
C00F C00G 1.512(4) . ?
C00F C00K 1.403(4) . ?
C00F C00N 1.398(4) . ?
C00G H00I 0.9900 . ?
C00G H00J 0.9900 . ?
C00H H00D 0.9900 . ?
C00H H00E 0.9900 . ?
C00H C00M 1.499(4) . ?
C00I C00J 1.394(4) . ?
C00I C00Z 1.517(4) . ?
C00I C01C 1.386(4) . ?
C00J C00P 1.416(4) . ?
C00K C00S 1.412(4) . ?
C00L C010 1.535(4) . ?
C00L C01B 1.536(5) . ?
C00L C01G 1.534(5) . ?
C00L C01H 1.529(4) . ?
C00M C00Q 1.409(4) . ?
C00M C016 1.388(4) . ?
C00N H00N 0.9500 . ?
C00N C00V 1.377(5) . ?
C00O C00W 1.482(4) . ?
C00P C00T 1.524(5) . ?
C00P C012 1.401(5) . ?
C00Q C010 1.405(4) . ?
C00R C00U 1.402(4) . ?
C00R C017 1.514(5) . ?
C00R C01A 1.390(4) . ?
C00S C014 1.538(4) . ?
C00S C019 1.402(4) . ?
C00T C013 1.533(5) . ?
C00T C018 1.536(5) . ?
C00T C01M 1.548(4) . ?
C00U C011 1.407(5) . ?
C00V H00V 0.9500 . ?
C00V C019 1.387(5) . ?
C00W H00K 0.9800 . ?
C00W H00L 0.9800 . ?
C00W H00M 0.9800 . ?
C00X H00O 0.9800 . ?
C00X H00P 0.9800 . ?
C00X H00Q 0.9800 . ?
C00X C014 1.541(5) . ?
C00Y H00F 0.9800 . ?
C00Y H00G 0.9800 . ?
C00Y H00H 0.9800 . ?
C00Y C01D 1.533(5) . ?
C00Z H00R 0.9900 . ?
C00Z H00S 0.9900 . ?
C010 C01F 1.393(4) . ?
C011 C01D 1.540(4) . ?
C011 C01J 1.392(5) . ?
C012 H012 0.9500 . ?
C012 C01I 1.381(5) . ?
C013 H01V 0.9800 . ?
C013 H01W 0.9800 . ?
C013 H01X 0.9800 . ?
C014 C01N 1.543(5) . ?
C014 C01O 1.538(5) . ?
C015 H015 0.9500 . ?
C015 C01A 1.378(5) . ?
C015 C01J 1.389(5) . ?
C016 H016 0.9500 . ?
C016 C01E 1.366(5) . ?
C017 H01A 0.9900 . ?
C017 H01B 0.9900 . ?
C018 H01Y 0.9800 . ?
C018 H 0.9800 . ?
C018 HA 0.9800 . ?
C019 H019 0.9500 . ?
C01A H01C 0.9500 . ?
C01B H01D 0.9800 . ?
C01B H01E 0.9800 . ?
C01B H01F 0.9800 . ?
C01C H01Z 0.9500 . ?
C01C C01I 1.381(5) . ?
C01D C01K 1.526(5) . ?
C01D C01L 1.534(5) . ?
C01E H01G 0.9500 . ?
C01E C01F 1.386(5) . ?
C01F H01H 0.9500 . ?
C01G H01I 0.9800 . ?
C01G H01J 0.9800 . ?
C01G H01K 0.9800 . ?
C01H H01L 0.9800 . ?
C01H H01M 0.9800 . ?
C01H H01N 0.9800 . ?
C01I H01 0.9500 . ?
C01J H01O 0.9500 . ?
C01K H01P 0.9800 . ?
C01K H01Q 0.9800 . ?
C01K H01R 0.9800 . ?
C01L H01S 0.9800 . ?
C01L H01T 0.9800 . ?
C01L H01U 0.9800 . ?
C01M H1 0.9800 . ?
C01M HB 0.9800 . ?
C01M HC 0.9800 . ?
C01N H2 0.9800 . ?
C01N HD 0.9800 . ?
C01N HE 0.9800 . ?
C01O H3 0.9800 . ?
C01O HF 0.9800 . ?
C01O HG 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
Cl04 Hf01 Hf01 112.954(19) . 2_655 ?
Cl04 Hf01 C00D 160.58(7) . . ?
O007 Hf01 Hf01 127.67(6) . 2_655 ?
O007 Hf01 Cl04 96.31(6) . . ?
O007 Hf01 O008 104.64(9) . . ?
O007 Hf01 N009 78.20(8) . . ?
O007 Hf01 N00C 134.32(8) . . ?
O007 Hf01 N00C 102.19(9) . 2_655 ?
O007 Hf01 C00D 102.86(8) . . ?
O008 Hf01 Hf01 116.12(6) . 2_655 ?
O008 Hf01 Cl04 91.78(6) . . ?
O008 Hf01 N009 102.03(9) . . ?
O008 Hf01 N00C 153.14(9) . 2_655 ?
O008 Hf01 N00C 77.46(9) . . ?
O008 Hf01 C00D 80.53(9) . . ?
N009 Hf01 Hf01 62.88(6) . 2_655 ?
N009 Hf01 Cl04 166.02(7) . . ?
N009 Hf01 N00C 82.05(9) . 2_655 ?
N009 Hf01 N00C 57.33(8) . . ?
N009 Hf01 C00D 29.39(9) . . ?
N00C Hf01 Hf01 42.12(6) 2_655 2_655 ?
N00C Hf01 Hf01 40.77(6) . 2_655 ?
N00C Hf01 Cl04 129.36(6) . . ?
N00C Hf01 Cl04 86.63(6) 2_655 . ?
N00C Hf01 N00C 82.89(10) 2_655 . ?
N00C Hf01 C00D 31.58(8) . . ?
N00C Hf01 C00D 92.24(9) 2_655 . ?
C00D Hf01 Hf01 56.63(6) . 2_655 ?
Cl03 Hf02 Hf02 109.689(19) . 2_656 ?
Cl03 Hf02 C00O 157.66(7) . . ?
O005 Hf02 Hf02 116.11(6) . 2_656 ?
O005 Hf02 Cl03 93.24(7) . . ?
O005 Hf02 N00A 97.92(9) . . ?
O005 Hf02 N00B 151.44(9) . 2_656 ?
O005 Hf02 N00B 79.18(8) . . ?
O005 Hf02 C00O 79.45(9) . . ?
O006 Hf02 Hf02 128.58(6) . 2_656 ?
O006 Hf02 Cl03 97.14(6) . . ?
O006 Hf02 O005 104.78(9) . . ?
O006 Hf02 N00A 78.52(9) . . ?
O006 Hf02 N00B 103.67(8) . 2_656 ?
O006 Hf02 N00B 136.45(8) . . ?
O006 Hf02 C00O 105.12(9) . . ?
N00A Hf02 Hf02 66.62(6) . 2_656 ?
N00A Hf02 Cl03 168.73(6) . . ?
N00A Hf02 N00B 85.26(8) . 2_656 ?
N00A Hf02 N00B 58.14(8) . . ?
N00A Hf02 C00O 29.31(9) . . ?
N00B Hf02 Hf02 38.87(6) . 2_656 ?
N00B Hf02 Hf02 39.69(6) 2_656 2_656 ?
N00B Hf02 Cl03 126.22(6) . . ?
N00B Hf02 Cl03 85.69(6) 2_656 . ?
N00B Hf02 N00B 78.56(9) 2_656 . ?
N00B Hf02 C00O 90.79(8) 2_656 . ?
N00B Hf02 C00O 31.86(8) . . ?
C00O Hf02 Hf02 57.00(6) . 2_656 ?
C00J O005 Hf02 143.30(19) . . ?
C00K O006 Hf02 140.76(18) . . ?
C00Q O007 Hf01 142.42(18) . . ?
C00U O008 Hf01 147.06(19) . . ?
C00D N009 Hf01 93.35(18) . . ?
C00D N009 C00H 121.9(2) . . ?
C00H N009 Hf01 132.90(18) . . ?
C00G N00A Hf02 130.01(19) . . ?
C00O N00A Hf02 93.85(17) . . ?
C00O N00A C00G 123.0(2) . . ?
Hf02 N00B Hf02 101.44(9) 2_656 . ?
C00O N00B Hf02 87.05(16) . . ?
C00O N00B Hf02 110.79(16) . 2_656 ?
C00O N00B C00Z 118.9(2) . . ?
C00Z N00B Hf02 116.28(17) . 2_656 ?
C00Z N00B Hf02 117.76(17) . . ?
Hf01 N00C Hf01 97.10(10) 2_655 . ?
C00D N00C Hf01 86.22(15) . . ?
C00D N00C Hf01 106.47(19) . 2_655 ?
C00D N00C C017 119.5(2) . . ?
C017 N00C Hf01 121.12(18) . 2_655 ?
C017 N00C Hf01 119.35(18) . . ?
N009 C00D Hf01 57.26(14) . . ?
N009 C00D N00C 109.5(2) . . ?
N009 C00D C00E 125.8(3) . . ?
N00C C00D Hf01 62.20(13) . . ?
N00C C00D C00E 124.7(3) . . ?
C00E C00D Hf01 148.3(2) . . ?
C00D C00E H00A 109.5 . . ?
C00D C00E H00B 109.5 . . ?
C00D C00E H00C 109.5 . . ?
H00A C00E H00B 109.5 . . ?
H00A C00E H00C 109.5 . . ?
H00B C00E H00C 109.5 . . ?
C00K C00F C00G 122.9(3) . . ?
C00N C00F C00G 117.9(3) . . ?
C00N C00F C00K 119.1(3) . . ?
N00A C00G C00F 112.0(2) . . ?
N00A C00G H00I 109.2 . . ?
N00A C00G H00J 109.2 . . ?
C00F C00G H00I 109.2 . . ?
C00F C00G H00J 109.2 . . ?
H00I C00G H00J 107.9 . . ?
N009 C00H H00D 108.8 . . ?
N009 C00H H00E 108.8 . . ?
N009 C00H C00M 113.9(2) . . ?
H00D C00H H00E 107.7 . . ?
C00M C00H H00D 108.8 . . ?
C00M C00H H00E 108.8 . . ?
C00J C00I C00Z 122.1(3) . . ?
C01C C00I C00J 119.6(3) . . ?
C01C C00I C00Z 118.3(3) . . ?
O005 C00J C00I 119.0(3) . . ?
O005 C00J C00P 119.0(3) . . ?
C00I C00J C00P 122.0(3) . . ?
O006 C00K C00F 119.6(3) . . ?
O006 C00K C00S 118.9(3) . . ?
C00F C00K C00S 121.5(3) . . ?
C010 C00L C01B 108.3(3) . . ?
C01G C00L C010 111.0(3) . . ?
C01G C00L C01B 111.1(3) . . ?
C01H C00L C010 112.1(3) . . ?
C01H C00L C01B 106.8(3) . . ?
C01H C00L C01G 107.5(3) . . ?
C00Q C00M C00H 124.2(3) . . ?
C016 C00M C00H 116.4(3) . . ?
C016 C00M C00Q 118.9(3) . . ?
C00F C00N H00N 119.9 . . ?
C00V C00N C00F 120.2(3) . . ?
C00V C00N H00N 119.9 . . ?
N00A C00O Hf02 56.84(15) . . ?
N00A C00O N00B 109.8(2) . . ?
N00A C00O C00W 125.5(3) . . ?
N00B C00O Hf02 61.09(14) . . ?
N00B C00O C00W 124.6(3) . . ?
C00W C00O Hf02 150.7(2) . . ?
C00J C00P C00T 122.2(3) . . ?
C012 C00P C00J 115.6(3) . . ?
C012 C00P C00T 122.2(3) . . ?
O007 C00Q C00M 119.7(2) . . ?
O007 C00Q C010 119.3(3) . . ?
C010 C00Q C00M 121.1(3) . . ?
C00U C00R C017 120.8(3) . . ?
C01A C00R C00U 119.3(3) . . ?
C01A C00R C017 119.8(3) . . ?
C00K C00S C014 122.5(3) . . ?
C019 C00S C00K 116.9(3) . . ?
C019 C00S C014 120.6(3) . . ?
C00P C00T C013 110.0(3) . . ?
C00P C00T C018 110.5(3) . . ?
C00P C00T C01M 111.3(3) . . ?
C013 C00T C018 110.0(3) . . ?
C013 C00T C01M 107.6(3) . . ?
C018 C00T C01M 107.4(3) . . ?
O008 C00U C00R 118.4(3) . . ?
O008 C00U C011 120.3(3) . . ?
C00R C00U C011 121.2(3) . . ?
C00N C00V H00V 119.8 . . ?
C00N C00V C019 120.3(3) . . ?
C019 C00V H00V 119.8 . . ?
C00O C00W H00K 109.5 . . ?
C00O C00W H00L 109.5 . . ?
C00O C00W H00M 109.5 . . ?
H00K C00W H00L 109.5 . . ?
H00K C00W H00M 109.5 . . ?
H00L C00W H00M 109.5 . . ?
H00O C00X H00P 109.5 . . ?
H00O C00X H00Q 109.5 . . ?
H00P C00X H00Q 109.5 . . ?
C014 C00X H00O 109.5 . . ?
C014 C00X H00P 109.5 . . ?
C014 C00X H00Q 109.5 . . ?
H00F C00Y H00G 109.5 . . ?
H00F C00Y H00H 109.5 . . ?
H00G C00Y H00H 109.5 . . ?
C01D C00Y H00F 109.5 . . ?
C01D C00Y H00G 109.5 . . ?
C01D C00Y H00H 109.5 . . ?
N00B C00Z C00I 114.7(2) . . ?
N00B C00Z H00R 108.6 . . ?
N00B C00Z H00S 108.6 . . ?
C00I C00Z H00R 108.6 . . ?
C00I C00Z H00S 108.6 . . ?
H00R C00Z H00S 107.6 . . ?
C00Q C010 C00L 122.2(3) . . ?
C01F C010 C00L 121.0(3) . . ?
C01F C010 C00Q 116.8(3) . . ?
C00U C011 C01D 121.2(3) . . ?
C01J C011 C00U 116.9(3) . . ?
C01J C011 C01D 121.9(3) . . ?
C00P C012 H012 118.5 . . ?
C01I C012 C00P 123.0(3) . . ?
C01I C012 H012 118.5 . . ?
C00T C013 H01V 109.5 . . ?
C00T C013 H01W 109.5 . . ?
C00T C013 H01X 109.5 . . ?
H01V C013 H01W 109.5 . . ?
H01V C013 H01X 109.5 . . ?
H01W C013 H01X 109.5 . . ?
C00S C014 C00X 109.9(3) . . ?
C00S C014 C01N 110.5(3) . . ?
C00X C014 C01N 109.2(3) . . ?
C01O C014 C00S 111.9(3) . . ?
C01O C014 C00X 107.1(3) . . ?
C01O C014 C01N 108.2(3) . . ?
C01A C015 H015 120.3 . . ?
C01A C015 C01J 119.4(3) . . ?
C01J C015 H015 120.3 . . ?
C00M C016 H016 119.5 . . ?
C01E C016 C00M 121.1(3) . . ?
C01E C016 H016 119.5 . . ?
N00C C017 C00R 115.3(2) . . ?
N00C C017 H01A 108.5 . . ?
N00C C017 H01B 108.5 . . ?
C00R C017 H01A 108.5 . . ?
C00R C017 H01B 108.5 . . ?
H01A C017 H01B 107.5 . . ?
C00T C018 H01Y 109.5 . . ?
C00T C018 H 109.5 . . ?
C00T C018 HA 109.5 . . ?
H01Y C018 H 109.5 . . ?
H01Y C018 HA 109.5 . . ?
H C018 HA 109.5 . . ?
C00S C019 H019 119.1 . . ?
C00V C019 C00S 121.8(3) . . ?
C00V C019 H019 119.1 . . ?
C00R C01A H01C 119.8 . . ?
C015 C01A C00R 120.5(3) . . ?
C015 C01A H01C 119.8 . . ?
C00L C01B H01D 109.5 . . ?
C00L C01B H01E 109.5 . . ?
C00L C01B H01F 109.5 . . ?
H01D C01B H01E 109.5 . . ?
H01D C01B H01F 109.5 . . ?
H01E C01B H01F 109.5 . . ?
C00I C01C H01Z 120.0 . . ?
C01I C01C C00I 120.0(3) . . ?
C01I C01C H01Z 120.0 . . ?
C00Y C01D C011 111.1(3) . . ?
C00Y C01D C01L 107.1(3) . . ?
C01K C01D C00Y 109.9(3) . . ?
C01K C01D C011 108.8(3) . . ?
C01K C01D C01L 108.1(3) . . ?
C01L C01D C011 111.8(3) . . ?
C016 C01E H01G 120.3 . . ?
C016 C01E C01F 119.4(3) . . ?
C01F C01E H01G 120.3 . . ?
C010 C01F H01H 118.7 . . ?
C01E C01F C010 122.5(3) . . ?
C01E C01F H01H 118.7 . . ?
C00L C01G H01I 109.5 . . ?
C00L C01G H01J 109.5 . . ?
C00L C01G H01K 109.5 . . ?
H01I C01G H01J 109.5 . . ?
H01I C01G H01K 109.5 . . ?
H01J C01G H01K 109.5 . . ?
C00L C01H H01L 109.5 . . ?
C00L C01H H01M 109.5 . . ?
C00L C01H H01N 109.5 . . ?
H01L C01H H01M 109.5 . . ?
H01L C01H H01N 109.5 . . ?
H01M C01H H01N 109.5 . . ?
C012 C01I H01 120.1 . . ?
C01C C01I C012 119.8(3) . . ?
C01C C01I H01 120.1 . . ?
C011 C01J H01O 118.7 . . ?
C015 C01J C011 122.5(3) . . ?
C015 C01J H01O 118.7 . . ?
C01D C01K H01P 109.5 . . ?
C01D C01K H01Q 109.5 . . ?
C01D C01K H01R 109.5 . . ?
H01P C01K H01Q 109.5 . . ?
H01P C01K H01R 109.5 . . ?
H01Q C01K H01R 109.5 . . ?
C01D C01L H01S 109.5 . . ?
C01D C01L H01T 109.5 . . ?
C01D C01L H01U 109.5 . . ?
H01S C01L H01T 109.5 . . ?
H01S C01L H01U 109.5 . . ?
H01T C01L H01U 109.5 . . ?
C00T C01M H1 109.5 . . ?
C00T C01M HB 109.5 . . ?
C00T C01M HC 109.5 . . ?
H1 C01M HB 109.5 . . ?
H1 C01M HC 109.5 . . ?
HB C01M HC 109.5 . . ?
C014 C01N H2 109.5 . . ?
C014 C01N HD 109.5 . . ?
C014 C01N HE 109.5 . . ?
H2 C01N HD 109.5 . . ?
H2 C01N HE 109.5 . . ?
HD C01N HE 109.5 . . ?
C014 C01O H3 109.5 . . ?
C014 C01O HF 109.5 . . ?
C014 C01O HG 109.5 . . ?
H3 C01O HF 109.5 . . ?
H3 C01O HG 109.5 . . ?
HF C01O HG 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
Hf01 O007 C00Q C00M -22.1(5) . . . . ?
Hf01 O007 C00Q C010 158.9(2) . . . . ?
Hf01 O008 C00U C00R -22.0(5) . . . . ?
Hf01 O008 C00U C011 156.9(3) . . . . ?
Hf01 N009 C00D N00C 35.3(2) . . . . ?
Hf01 N009 C00D C00E -141.5(3) . . . . ?
Hf01 N009 C00H C00M -26.2(4) . . . . ?
Hf01 N00C C00D Hf01 96.30(12) 2_655 . . . ?
Hf01 N00C C00D N009 -33.4(2) . . . . ?
Hf01 N00C C00D N009 62.9(2) 2_655 . . . ?
Hf01 N00C C00D C00E 143.5(3) . . . . ?
Hf01 N00C C00D C00E -120.2(3) 2_655 . . . ?
Hf01 N00C C017 C00R -56.1(3) . . . . ?
Hf01 N00C C017 C00R -176.40(19) 2_655 . . . ?
Hf02 O005 C00J C00I -27.4(5) . . . . ?
Hf02 O005 C00J C00P 151.9(2) . . . . ?
Hf02 O006 C00K C00F -32.0(4) . . . . ?
Hf02 O006 C00K C00S 147.5(2) . . . . ?
Hf02 N00A C00G C00F -40.7(3) . . . . ?
Hf02 N00A C00O N00B 31.9(2) . . . . ?
Hf02 N00A C00O C00W -144.5(3) . . . . ?
Hf02 N00B C00O Hf02 101.12(13) 2_656 . . . ?
Hf02 N00B C00O N00A 70.8(2) 2_656 . . . ?
Hf02 N00B C00O N00A -30.3(2) . . . . ?
Hf02 N00B C00O C00W -112.8(3) 2_656 . . . ?
Hf02 N00B C00O C00W 146.1(3) . . . . ?
Hf02 N00B C00Z C00I -58.2(3) . . . . ?
Hf02 N00B C00Z C00I -178.8(2) 2_656 . . . ?
O005 C00J C00P C00T 0.0(4) . . . . ?
O005 C00J C00P C012 -179.6(3) . . . . ?
O006 C00K C00S C014 2.9(4) . . . . ?
O006 C00K C00S C019 -177.1(3) . . . . ?
O007 C00Q C010 C00L 7.8(4) . . . . ?
O007 C00Q C010 C01F -175.3(3) . . . . ?
O008 C00U C011 C01D 6.4(4) . . . . ?
O008 C00U C011 C01J -175.9(3) . . . . ?
N009 C00H C00M C00Q 30.1(4) . . . . ?
N009 C00H C00M C016 -157.8(3) . . . . ?
C00D N009 C00H C00M -158.4(3) . . . . ?
C00D N00C C017 C00R 47.3(4) . . . . ?
C00F C00K C00S C014 -177.6(3) . . . . ?
C00F C00K C00S C019 2.4(4) . . . . ?
C00F C00N C00V C019 0.9(5) . . . . ?
C00G N00A C00O Hf02 144.3(3) . . . . ?
C00G N00A C00O N00B 176.2(2) . . . . ?
C00G N00A C00O C00W -0.2(4) . . . . ?
C00G C00F C00K O006 -7.3(4) . . . . ?
C00G C00F C00K C00S 173.2(3) . . . . ?
C00G C00F C00N C00V -175.1(3) . . . . ?
C00H N009 C00D Hf01 147.1(3) . . . . ?
C00H N009 C00D N00C -177.6(3) . . . . ?
C00H N009 C00D C00E 5.5(5) . . . . ?
C00H C00M C00Q O007 -11.1(4) . . . . ?
C00H C00M C00Q C010 168.0(3) . . . . ?
C00H C00M C016 C01E -173.1(3) . . . . ?
C00I C00J C00P C00T 179.2(3) . . . . ?
C00I C00J C00P C012 -0.4(4) . . . . ?
C00I C01C C01I C012 0.4(6) . . . . ?
C00J C00I C00Z N00B 38.6(4) . . . . ?
C00J C00I C01C C01I -2.1(5) . . . . ?
C00J C00P C00T C013 62.4(4) . . . . ?
C00J C00P C00T C018 -59.3(4) . . . . ?
C00J C00P C00T C01M -178.5(3) . . . . ?
C00J C00P C012 C01I -1.3(5) . . . . ?
C00K C00F C00G N00A 37.2(4) . . . . ?
C00K C00F C00N C00V 0.8(4) . . . . ?
C00K C00S C014 C00X -63.4(4) . . . . ?
C00K C00S C014 C01N 57.1(4) . . . . ?
C00K C00S C014 C01O 177.7(3) . . . . ?
C00K C00S C019 C00V -0.7(5) . . . . ?
C00L C010 C01F C01E 173.9(3) . . . . ?
C00M C00Q C010 C00L -171.2(3) . . . . ?
C00M C00Q C010 C01F 5.6(4) . . . . ?
C00M C016 C01E C01F 3.1(5) . . . . ?
C00N C00F C00G N00A -147.0(3) . . . . ?
C00N C00F C00K O006 177.0(2) . . . . ?
C00N C00F C00K C00S -2.5(4) . . . . ?
C00N C00V C019 C00S -0.9(5) . . . . ?
C00O N00A C00G C00F -171.2(3) . . . . ?
C00O N00B C00Z C00I 44.7(4) . . . . ?
C00P C012 C01I C01C 1.4(6) . . . . ?
C00Q C00M C016 C01E -0.5(5) . . . . ?
C00Q C010 C01F C01E -3.0(5) . . . . ?
C00R C00U C011 C01D -174.7(3) . . . . ?
C00R C00U C011 C01J 3.0(4) . . . . ?
C00T C00P C012 C01I 179.0(3) . . . . ?
C00U C00R C017 N00C 43.4(4) . . . . ?
C00U C00R C01A C015 1.3(5) . . . . ?
C00U C011 C01D C00Y -62.1(4) . . . . ?
C00U C011 C01D C01K 59.1(4) . . . . ?
C00U C011 C01D C01L 178.3(3) . . . . ?
C00U C011 C01J C015 -0.6(5) . . . . ?
C00Z N00B C00O Hf02 -120.3(2) . . . . ?
C00Z N00B C00O N00A -150.6(2) . . . . ?
C00Z N00B C00O C00W 25.8(4) . . . . ?
C00Z C00I C00J O005 3.0(4) . . . . ?
C00Z C00I C00J C00P -176.2(3) . . . . ?
C00Z C00I C01C C01I 176.3(3) . . . . ?
C012 C00P C00T C013 -118.0(3) . . . . ?
C012 C00P C00T C018 120.3(3) . . . . ?
C012 C00P C00T C01M 1.1(4) . . . . ?
C014 C00S C019 C00V 179.3(3) . . . . ?
C016 C00M C00Q O007 176.9(3) . . . . ?
C016 C00M C00Q C010 -4.0(4) . . . . ?
C016 C01E C01F C010 -1.3(5) . . . . ?
C017 N00C C00D Hf01 -121.8(2) . . . . ?
C017 N00C C00D N009 -155.2(3) . . . . ?
C017 N00C C00D C00E 21.7(4) . . . . ?
C017 C00R C00U O008 -6.4(4) . . . . ?
C017 C00R C00U C011 174.7(3) . . . . ?
C017 C00R C01A C015 -176.8(3) . . . . ?
C019 C00S C014 C00X 116.6(3) . . . . ?
C019 C00S C014 C01N -122.9(3) . . . . ?
C019 C00S C014 C01O -2.3(5) . . . . ?
C01A C00R C00U O008 175.5(3) . . . . ?
C01A C00R C00U C011 -3.4(5) . . . . ?
C01A C00R C017 N00C -138.4(3) . . . . ?
C01A C015 C01J C011 -1.4(5) . . . . ?
C01B C00L C010 C00Q 55.7(4) . . . . ?
C01B C00L C010 C01F -121.0(3) . . . . ?
C01C C00I C00J O005 -178.7(3) . . . . ?
C01C C00I C00J C00P 2.1(4) . . . . ?
C01C C00I C00Z N00B -139.8(3) . . . . ?
C01D C011 C01J C015 177.1(3) . . . . ?
C01G C00L C010 C00Q -66.4(4) . . . . ?
C01G C00L C010 C01F 116.8(3) . . . . ?
C01H C00L C010 C00Q 173.3(3) . . . . ?
C01H C00L C010 C01F -3.4(4) . . . . ?
C01J C011 C01D C00Y 120.3(4) . . . . ?
C01J C011 C01D C01K -118.6(4) . . . . ?
C01J C011 C01D C01L 0.7(5) . . . . ?
C01J C015 C01A C00R 1.0(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.965
_oxdiff_exptl_absorpt_empirical_full_min 0.455
####################################################################### 
# 
# 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_exp_11297
_database_code_depnum_ccdc_archive 'CCDC 2249134'
loop_
_audit_author_name
_audit_author_address
'Hanhua Xu'
;Peking University
China
;
_audit_update_record             
;
2023-03-16 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_audit_creation_date             2023-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H31 Cl4 Hf2 N8 O2, C16 H32 Li O4'
_chemical_formula_sum            'C40 H63 Cl4 Hf2 Li N8 O6'
_chemical_formula_weight         1256.709
_chemical_oxdiff_formula         'Hf C H O N  K Li'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Li -0.00003 0.00005 1.12820 0.75080 0.61750 0.46530 3.95460 1.05240 85.39050
168.26100 0.0377000011504
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Hf -0.36352 6.43351 29.14400 15.17260 14.75860 4.30013 1.83262 9.59990 0.27512
72.02900 8.58154010773
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   12.5852(2)
_cell_length_b                   12.8869(2)
_cell_length_c                   17.0743(2)
_cell_angle_alpha                89.129(1)
_cell_angle_beta                 71.984(1)
_cell_angle_gamma                72.209(1)
_cell_volume                     2497.84(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    25481
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.7120
_cell_measurement_theta_min      2.5830
_exptl_absorpt_coefficient_mu    4.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             1243.080
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60063
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9989
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.52
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  15.00   0.50    0.62    --   -1.70 -38.00 -30.00   50
  2  ω    -90.00 -26.00   0.50    0.62    --   -1.70 -38.00 -30.00  128
  3  ω    -91.00 -23.00   0.50    0.62    --   -1.70 -57.00 120.00  136
  4  ω    -44.00  31.00   0.50    0.62    --   -1.70 -82.00 150.00  150
  5  ω    -35.00 -10.00   0.50    0.62    --   -1.70 -38.00-150.00   50
  6  ω    -21.00  40.00   0.50    0.62    --   -1.70  38.00 -60.00  122
  7  ω     50.00  86.00   0.50    0.62    --   -1.70  38.00 -60.00   72
  8  ω    -87.00 -50.00   0.50    0.62    --   -1.70 -38.00 -60.00   74
  9  ω    -59.00 -27.00   0.50    0.62    --    1.70 -57.00  30.00   64
 10  ω    -88.00   0.00   0.50    0.62    --    1.70 -57.00  60.00  176
 11  ω     43.00  68.00   0.50    0.62    --    1.70  38.00  30.00   50
 12  ω     57.00  82.00   0.50    0.62    --    1.70  38.00-180.00   50
 13  ω     16.00  41.00   0.50    0.62    --    1.70  38.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0330824000
_diffrn_orient_matrix_UB_12      0.0519668000
_diffrn_orient_matrix_UB_13      0.0219601000
_diffrn_orient_matrix_UB_21      -0.0223611000
_diffrn_orient_matrix_UB_22      0.0167088000
_diffrn_orient_matrix_UB_23      -0.0331223000
_diffrn_orient_matrix_UB_31      -0.0480481000
_diffrn_orient_matrix_UB_32      -0.0196849000
_diffrn_orient_matrix_UB_33      0.0185386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8772
_reflns_number_total             9843
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.7688
_refine_diff_density_min         -0.9497
_refine_diff_density_rms         0.1097
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             8.0874
_refine_ls_goodness_of_fit_ref   1.0515
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    107
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9843
_refine_ls_number_restraints     142
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0231
_refine_ls_restrained_S_all      1.0435
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0120P)²+3.6203P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0568
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H3ab of C3a, H15 of C15, H29 of C29, H30 of C30, H16 of
  C16, H14 of C14, H28 of C28
 At 1.5 times of:
  All C(H,H,H) groups, H3aa of C3a
2. Restrained distances
 O1a-C3a = O1a-C2a
 1.43 with sigma of 0.01
 C5a-C3a = C5a-C4a = C4a-C2a = C4-C2 = C5-C4 = C5-C3
 1.54 with sigma of 0.01
 O1-C3 = O1-C2
 1.43 with sigma of 0.01
 C3a-C2a
 2.336 with sigma of 0.01
 C2a-C5a = C4a-C3a
 2.515 with sigma of 0.02
 C2-C3
 2.336 with sigma of 0.02
 C2-C5 = C4-C3
 2.515 with sigma of 0.02
 O1a-C4a
 2.426 with sigma of 0.02
 O1a-C5a
 2.426 with sigma of 0.02
 O1-C4
 2.426 with sigma of 0.02
 O1-C5
 2.426 with sigma of 0.02
 O1a-Li61 \\sim O1-Li61
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O1a \\sim C2a \\sim C4a \\sim C5a \\sim C3a: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O1 \\sim C2 \\sim C4 \\sim C5 \\sim C3: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O1a, C3a, C5a, C4a, C2a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C2, C4, C5, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(O1a)=Sof(C2a)=Sof(H2aa)=Sof(H2ab)=Sof(C4a)=Sof(H4aa)=Sof(H4ab)=Sof(C5a)=
 Sof(H5aa)=Sof(H5ab)=Sof(C3a)=Sof(H3aa)=Sof(H3ab)=1-FVAR(1)
 Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(C3)=Sof(H3a)=Sof(H3b)=Sof(O1)=Sof(C4)=Sof(H4a)=
 Sof(H4b)=Sof(C5)=Sof(H5a)=Sof(H5b)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C23(H23a,H23b), C41(H41a,H41b), C42(H42a,H42b), C43(H43a,
 H43b), C52(H52a,H52b), C55(H55a,H55b), C45(H45a,H45b), C57(H57a,H57b),
 C58(H58a,H58b), C60(H60a,H60b), C53(H53a,H53b), C54(H54a,H54b), C59(H59a,H59b),
  C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C2a(H2aa,H2ab), C4a(H4aa,
 H4ab), C5a(H5aa,H5ab), C3a(H3aa,H3ab)
6.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C15(H15), C30(H30), C28(H28), C29(H29)
6.c Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C33(H33a,H33b,
 H33c), C40(H40a,H40b,H40c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_group
Hf1 Hf 0.204434(11) 0.611894(10) 0.197991(8) 0.02495(4) Uani 1.000000 . . .
Hf2 Hf 0.372457(11) 0.791700(10) 0.196450(8) 0.02733(4) Uani 1.000000 . . .
Cl3 Cl 0.12288(7) 0.59675(7) 0.08884(5) 0.03663(18) Uani 1.000000 . . .
Cl4 Cl 0.02381(7) 0.71360(7) 0.30310(6) 0.0410(2) Uani 1.000000 . . .
Cl5 Cl 0.22407(8) 0.93251(7) 0.29921(6) 0.0435(2) Uani 1.000000 . . .
Cl6 Cl 0.41593(9) 0.90534(8) 0.08595(6) 0.0444(2) Uani 1.000000 . . .
N7 N 0.2948(2) 0.6731(2) 0.27236(16) 0.0282(6) Uani 1.000000 . . .
N8 N 0.2699(3) 0.6709(2) 0.34726(18) 0.0367(7) Uani 1.000000 . . .
N11 N 0.2289(3) 0.7936(2) 0.07469(18) 0.0350(6) Uani 1.000000 . . .
C13 C 0.3727(3) 0.3312(3) 0.1631(2) 0.0280(7) Uani 1.000000 . . .
C18 C 0.2768(3) 0.3659(3) 0.2359(2) 0.0279(7) Uani 1.000000 . . .
C19 C 0.3898(3) 0.4109(3) 0.09850(19) 0.0290(7) Uani 1.000000 . . .
H19a H 0.4655(3) 0.3762(3) 0.05448(19) 0.0348(8) Uiso 1.000000 R . .
H19b H 0.3265(3) 0.4234(3) 0.07319(19) 0.0348(8) Uiso 1.000000 R . .
C17 C 0.2484(3) 0.2949(3) 0.2960(2) 0.0311(7) Uani 1.000000 . . .
C21 C 0.4939(3) 0.5351(3) 0.11575(18) 0.0256(6) Uani 1.000000 . . .
N10 N 0.2110(4) 0.8273(3) 0.0169(2) 0.0571(10) Uani 1.000000 . . .
C23 C 0.6185(3) 0.6507(3) 0.1018(2) 0.0312(7) Uani 1.000000 . . .
H23a H 0.6121(3) 0.7213(3) 0.0769(2) 0.0375(8) Uiso 1.000000 R . .
H23b H 0.6731(3) 0.5921(3) 0.0582(2) 0.0375(8) Uiso 1.000000 R . .
C16 C 0.3204(3) 0.1855(3) 0.2784(2) 0.0382(8) Uani 1.000000 . . .
H16 H 0.3045(3) 0.1345(3) 0.3175(2) 0.0458(10) Uiso 1.000000 R . .
C25 C 0.6716(3) 0.6498(3) 0.1697(2) 0.0316(7) Uani 1.000000 . . .
C24 C 0.6052(3) 0.4375(3) 0.0894(2) 0.0337(7) Uani 1.000000 . . .
H24a H 0.5872(5) 0.3719(5) 0.1111(13) 0.0505(11) Uiso 1.000000 GR . .
H24b H 0.6364(12) 0.4270(13) 0.0289(2) 0.0505(11) Uiso 1.000000 GR . .
H24c H 0.6640(8) 0.4505(9) 0.1110(13) 0.0505(11) Uiso 1.000000 GR . .
C26 C 0.6053(3) 0.7192(3) 0.2420(2) 0.0313(7) Uani 1.000000 . . .
C14 C 0.4409(3) 0.2211(3) 0.1483(2) 0.0337(7) Uani 1.000000 . . .
H14 H 0.5054(3) 0.1960(3) 0.0987(2) 0.0405(9) Uiso 1.000000 R . .
N9 N 0.2460(4) 0.6682(4) 0.4164(2) 0.0647(11) Uani 1.000000 . . .
C27 C 0.6502(3) 0.7266(3) 0.3067(2) 0.0343(7) Uani 1.000000 . . .
C38 C 0.1608(4) 0.4208(3) 0.4263(2) 0.0431(9) Uani 1.000000 . . .
H38a H 0.158(2) 0.4867(9) 0.3965(8) 0.0646(13) Uiso 1.000000 GR . .
H38b H 0.0983(14) 0.4393(17) 0.4799(7) 0.0646(13) Uiso 1.000000 GR . .
H38c H 0.2375(11) 0.3915(9) 0.4349(15) 0.0646(13) Uiso 1.000000 GR . .
C15 C 0.4142(3) 0.1492(3) 0.2056(2) 0.0407(8) Uani 1.000000 . . .
H15 H 0.4603(3) 0.0741(3) 0.1954(2) 0.0489(10) Uiso 1.000000 R . .
C37 C 0.1425(3) 0.3347(3) 0.3753(2) 0.0357(8) Uani 1.000000 . . .
C30 C 0.7870(3) 0.5869(3) 0.1600(2) 0.0372(8) Uani 1.000000 . . .
H30 H 0.8338(3) 0.5411(3) 0.1106(2) 0.0446(9) Uiso 1.000000 R . .
C28 C 0.7662(3) 0.6587(3) 0.2948(2) 0.0421(9) Uani 1.000000 . . .
H28 H 0.7994(3) 0.6592(3) 0.3378(2) 0.0506(10) Uiso 1.000000 R . .
C39 C 0.0277(3) 0.3835(3) 0.3541(2) 0.0436(9) Uani 1.000000 . . .
H39a H -0.0397(4) 0.401(2) 0.4050(3) 0.0654(13) Uiso 1.000000 GR . .
H39b H 0.0298(11) 0.4502(13) 0.3261(16) 0.0654(13) Uiso 1.000000 GR . .
H39c H 0.0201(13) 0.3302(9) 0.3176(14) 0.0654(13) Uiso 1.000000 GR . .
C33 C 0.4635(4) 0.7814(4) 0.4292(2) 0.0549(11) Uani 1.000000 . . .
H33a H 0.4809(4) 0.7040(7) 0.4397(18) 0.0824(17) Uiso 1.000000 GR . .
H33b H 0.4235(14) 0.827(2) 0.4818(10) 0.0824(17) Uiso 1.000000 GR . .
H33c H 0.4125(12) 0.798(3) 0.3943(9) 0.0824(17) Uiso 1.000000 GR . .
C29 C 0.8334(3) 0.5918(3) 0.2235(3) 0.0444(9) Uani 1.000000 . . .
H29 H 0.9120(3) 0.5485(3) 0.2176(3) 0.0533(11) Uiso 1.000000 R . .
C40 C 0.1291(4) 0.2405(3) 0.4292(3) 0.0496(10) Uani 1.000000 . . .
H40a H 0.2009(11) 0.2087(16) 0.4441(16) 0.0744(15) Uiso 1.000000 GR . .
H40b H 0.0617(17) 0.2682(6) 0.4796(9) 0.0744(15) Uiso 1.000000 GR . .
H40c H 0.116(3) 0.1844(12) 0.3985(7) 0.0744(15) Uiso 1.000000 GR . .
C41 C -0.1359(5) 0.9843(4) 0.4391(3) 0.0671(13) Uani 1.000000 . . .
H41a H -0.0793(5) 0.9157(4) 0.4472(3) 0.0805(16) Uiso 1.000000 R . .
H41b H -0.2166(5) 0.9882(4) 0.4735(3) 0.0805(16) Uiso 1.000000 R . .
C32 C 0.5786(4) 0.8049(3) 0.3850(2) 0.0422(9) Uani 1.000000 . . .
C42 C -0.1053(5) 1.0832(4) 0.4588(3) 0.0622(12) Uani 1.000000 . . .
H42a H -0.1436(5) 1.1100(4) 0.5179(3) 0.0746(15) Uiso 1.000000 R . .
H42b H -0.0190(5) 1.0663(4) 0.4450(3) 0.0746(15) Uiso 1.000000 R . .
C34 C 0.6476(4) 0.7952(4) 0.4462(3) 0.0566(12) Uani 1.000000 . . .
H34a H 0.7221(14) 0.809(3) 0.4189(7) 0.0848(17) Uiso 1.000000 GR . .
H34b H 0.6010(13) 0.8489(19) 0.4939(10) 0.0848(17) Uiso 1.000000 GR . .
H34c H 0.664(3) 0.7214(9) 0.4647(16) 0.0848(17) Uiso 1.000000 GR . .
C35 C 0.5499(5) 0.9236(4) 0.3606(3) 0.0578(12) Uani 1.000000 . . .
H35a H 0.504(3) 0.9740(4) 0.4103(4) 0.0868(17) Uiso 1.000000 GR . .
H35b H 0.6233(5) 0.9397(9) 0.3338(19) 0.0868(17) Uiso 1.000000 GR . .
H35c H 0.504(3) 0.9324(8) 0.3223(16) 0.0868(17) Uiso 1.000000 GR . .
C43 C -0.1518(5) 1.1647(4) 0.4053(3) 0.0647(13) Uani 1.000000 . . .
H43a H -0.1019(5) 1.2126(4) 0.3874(3) 0.0776(15) Uiso 1.000000 R . .
H43b H -0.2333(5) 1.2109(4) 0.4355(3) 0.0776(15) Uiso 1.000000 R . .
C52 C -0.2819(4) 1.0400(4) 0.1617(3) 0.0568(11) Uani 1.000000 . . .
H52a H -0.3109(4) 1.0974(4) 0.1273(3) 0.0681(13) Uiso 1.000000 R . .
H52b H -0.3434(4) 1.0505(4) 0.2163(3) 0.0681(13) Uiso 1.000000 R . .
C55 C -0.0829(5) 0.9488(5) 0.1330(4) 0.0836(18) Uani 1.000000 . . .
H55a H -0.0280(5) 0.9256(5) 0.1654(4) 0.100(2) Uiso 1.000000 R . .
H55b H -0.0382(5) 0.9595(5) 0.0762(4) 0.100(2) Uiso 1.000000 R . .
C45 C -0.1267(7) 0.9928(4) 0.3500(4) 0.096(2) Uani 1.000000 . . .
H45a H -0.1844(7) 0.9639(4) 0.3373(4) 0.115(3) Uiso 1.000000 R . .
H45b H -0.0467(7) 0.9498(4) 0.3145(4) 0.115(3) Uiso 1.000000 R . .
C57 C 0.0885(5) 1.1439(5) 0.1657(5) 0.092(2) Uani 1.000000 . . .
H57a H 0.1083(5) 1.0695(5) 0.1394(5) 0.110(2) Uiso 1.000000 R . .
H57b H 0.1020(5) 1.1373(5) 0.2199(5) 0.110(2) Uiso 1.000000 R . .
C58 C 0.1606(6) 1.2037(8) 0.1130(4) 0.102(2) Uani 1.000000 . . .
H58a H 0.2032(6) 1.2303(8) 0.1440(4) 0.122(3) Uiso 1.000000 R . .
H58b H 0.2191(6) 1.1553(8) 0.0643(4) 0.122(3) Uiso 1.000000 R . .
C60 C -0.0329(5) 1.2742(5) 0.1115(4) 0.088(2) Uani 1.000000 . . .
H60a H -0.0418(5) 1.2380(5) 0.0643(4) 0.106(2) Uiso 1.000000 R . .
H60b H -0.0991(5) 1.3432(5) 0.1306(4) 0.106(2) Uiso 1.000000 R . .
C53 C -0.2550(6) 0.9292(5) 0.1207(4) 0.0909(19) Uani 1.000000 . . .
H53a H -0.3173(6) 0.8963(5) 0.1476(4) 0.109(2) Uiso 1.000000 R . .
H53b H -0.2474(6) 0.9330(5) 0.0614(4) 0.109(2) Uiso 1.000000 R . .
C54 C -0.1435(7) 0.8666(5) 0.1314(5) 0.107(2) Uani 1.000000 . . .
H54a H -0.0966(7) 0.8096(5) 0.0849(5) 0.128(3) Uiso 1.000000 R . .
H54b H -0.1566(7) 0.8310(5) 0.1838(5) 0.128(3) Uiso 1.000000 R . .
Li61 Li -0.1675(6) 1.1628(6) 0.2364(4) 0.0505(16) Uani 1.000000 D . .
O36 O 0.20926(19) 0.47295(17) 0.24440(13) 0.0279(5) Uani 1.000000 . . .
O31 O 0.4953(2) 0.78307(19) 0.24526(14) 0.0323(5) Uani 1.000000 . . .
N20 N 0.3900(2) 0.5198(2) 0.12755(15) 0.0253(5) Uani 1.000000 . . .
N22 N 0.4999(2) 0.6352(2) 0.12798(16) 0.0267(5) Uani 1.000000 . . .
N12 N 0.2469(2) 0.7577(2) 0.13782(17) 0.0304(6) Uani 1.000000 . . .
O51 O -0.1761(3) 1.0470(3) 0.1714(2) 0.0594(8) Uani 1.000000 . . .
O56 O -0.0319(3) 1.2053(3) 0.1760(2) 0.0581(8) Uani 1.000000 . . .
O44 O -0.1496(3) 1.1028(2) 0.33549(19) 0.0571(8) Uani 1.000000 . . .
C59 C 0.0814(7) 1.2968(6) 0.0864(5) 0.105(2) Uani 1.000000 . . .
H59a H 0.0736(7) 1.3668(6) 0.1144(5) 0.126(3) Uiso 1.000000 R . .
H59b H 0.1109(7) 1.3001(6) 0.0258(5) 0.126(3) Uiso 1.000000 R . .
C2 C -0.4271(9) 1.2876(7) 0.3097(9) 0.071(3) Uani 0.749(16) D U 1
H2a H -0.4601(9) 1.2750(7) 0.2664(9) 0.085(3) Uiso 0.749(16) R . 1
H2b H -0.4287(9) 1.2284(7) 0.3473(9) 0.085(3) Uiso 0.749(16) R . 1
C3 C -0.2968(8) 1.3889(9) 0.3010(9) 0.084(3) Uani 0.749(16) D U 1
H3a H -0.2259(8) 1.3722(9) 0.3186(9) 0.101(3) Uiso 0.749(16) R . 1
H3b H -0.2892(8) 1.4383(9) 0.2560(9) 0.101(3) Uiso 0.749(16) R . 1
O1 O -0.3093(7) 1.2905(7) 0.2733(7) 0.061(2) Uani 0.749(16) D U 1
C4 C -0.4976(7) 1.3990(7) 0.3578(7) 0.088(3) Uani 0.749(16) D U 1
H4a H -0.5408(7) 1.4483(7) 0.3250(7) 0.105(3) Uiso 0.749(16) R . 1
H4b H -0.5549(7) 1.3913(7) 0.4106(7) 0.105(3) Uiso 0.749(16) R . 1
C5 C -0.4069(7) 1.4424(7) 0.3733(7) 0.091(3) Uani 0.749(16) D U 1
H5a H -0.3945(7) 1.4209(7) 0.4266(7) 0.109(4) Uiso 0.749(16) R . 1
H5b H -0.4307(7) 1.5231(7) 0.3739(7) 0.109(4) Uiso 0.749(16) R . 1
O1a O -0.3107(18) 1.2911(15) 0.2731(13) 0.040(6) Uani 0.251(16) D U 2
C2a C -0.424(2) 1.2792(13) 0.316(2) 0.053(6) Uani 0.251(16) D U 2
H2aa H -0.444(2) 1.2326(13) 0.281(2) 0.063(7) Uiso 0.251(16) R . 2
H2ab H -0.423(2) 1.2453(13) 0.368(2) 0.063(7) Uiso 0.251(16) R . 2
C4a C -0.5134(15) 1.3960(15) 0.3333(17) 0.067(5) Uani 0.251(16) D U 2
H4aa H -0.5547(15) 1.4111(15) 0.2915(17) 0.080(6) Uiso 0.251(16) R . 2
H4ab H -0.5725(15) 1.4054(15) 0.3889(17) 0.080(6) Uiso 0.251(16) R . 2
C5a C -0.4384(14) 1.4716(12) 0.3282(15) 0.060(5) Uani 0.251(16) D U 2
H5aa H -0.4511(14) 1.5259(12) 0.2876(15) 0.071(6) Uiso 0.251(16) R . 2
H5ab H -0.4588(14) 1.5111(12) 0.3828(15) 0.071(6) Uiso 0.251(16) R . 2
C3a C -0.3099(13) 1.3958(18) 0.3005(17) 0.048(5) Uani 0.251(16) D U 2
H3aa H -0.2777(13) 1.3886(18) 0.3471(17) 0.072(8) Uiso 0.251(16) R . 2
H3ab H -0.2605(13) 1.4258(18) 0.2549(17) 0.057(7) Uiso 0.251(16) R . 2


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 Hf2 3.57762(19) . ?
Hf1 Cl3 2.4251(8) . ?
Hf1 Cl4 2.4153(8) . ?
Hf1 N7 2.236(3) . ?
Hf1 O36 1.939(2) . ?
Hf1 N20 2.219(3) . ?
Hf1 N12 2.255(3) . ?
Hf2 Cl5 2.4203(9) . ?
Hf2 Cl6 2.4022(9) . ?
Hf2 N7 2.245(3) . ?
Hf2 O31 1.945(2) . ?
Hf2 N22 2.223(3) . ?
Hf2 N12 2.259(3) . ?
N7 N8 1.221(4) . ?
N8 N9 1.127(4) . ?
N11 N10 1.130(4) . ?
N11 N12 1.225(4) . ?
C13 C18 1.400(4) . ?
C13 C19 1.507(5) . ?
C13 C14 1.395(5) . ?
C18 C17 1.401(5) . ?
C18 O36 1.364(4) . ?
C19 H19a 0.9900 . ?
C19 H19b 0.9900 . ?
C19 N20 1.498(4) . ?
C17 C16 1.401(5) . ?
C17 C37 1.537(5) . ?
C21 C24 1.516(4) . ?
C21 N20 1.335(4) . ?
C21 N22 1.337(4) . ?
C23 H23a 0.9900 . ?
C23 H23b 0.9900 . ?
C23 C25 1.504(5) . ?
C23 N22 1.496(4) . ?
C16 H16 0.9500 . ?
C16 C15 1.389(5) . ?
C25 C26 1.400(5) . ?
C25 C30 1.390(5) . ?
C24 H24a 0.9800 . ?
C24 H24b 0.9800 . ?
C24 H24c 0.9800 . ?
C26 C27 1.404(5) . ?
C26 O31 1.362(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.375(5) . ?
C27 C28 1.407(5) . ?
C27 C32 1.535(5) . ?
C38 H38a 0.9800 . ?
C38 H38b 0.9800 . ?
C38 H38c 0.9800 . ?
C38 C37 1.534(5) . ?
C15 H15 0.9500 . ?
C37 C39 1.541(5) . ?
C37 C40 1.530(5) . ?
C30 H30 0.9500 . ?
C30 C29 1.392(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.375(6) . ?
C39 H39a 0.9800 . ?
C39 H39b 0.9800 . ?
C39 H39c 0.9800 . ?
C33 H33a 0.9800 . ?
C33 H33b 0.9800 . ?
C33 H33c 0.9800 . ?
C33 C32 1.531(5) . ?
C29 H29 0.9500 . ?
C40 H40a 0.9800 . ?
C40 H40b 0.9800 . ?
C40 H40c 0.9800 . ?
C41 H41a 0.9900 . ?
C41 H41b 0.9900 . ?
C41 C42 1.509(7) . ?
C41 C45 1.494(7) . ?
C32 C34 1.534(5) . ?
C32 C35 1.542(6) . ?
C42 H42a 0.9900 . ?
C42 H42b 0.9900 . ?
C42 C43 1.485(6) . ?
C34 H34a 0.9800 . ?
C34 H34b 0.9800 . ?
C34 H34c 0.9800 . ?
C35 H35a 0.9800 . ?
C35 H35b 0.9800 . ?
C35 H35c 0.9800 . ?
C43 H43a 0.9900 . ?
C43 H43b 0.9900 . ?
C43 O44 1.433(5) . ?
C52 H52a 0.9900 . ?
C52 H52b 0.9900 . ?
C52 C53 1.494(7) . ?
C52 O51 1.421(5) . ?
C55 H55a 0.9900 . ?
C55 H55b 0.9900 . ?
C55 C54 1.487(9) . ?
C55 O51 1.432(5) . ?
C45 H45a 0.9900 . ?
C45 H45b 0.9900 . ?
C45 O44 1.392(5) . ?
C57 H57a 0.9900 . ?
C57 H57b 0.9900 . ?
C57 C58 1.458(9) . ?
C57 O56 1.435(6) . ?
C58 H58a 0.9900 . ?
C58 H58b 0.9900 . ?
C58 C59 1.474(10) . ?
C60 H60a 0.9900 . ?
C60 H60b 0.9900 . ?
C60 O56 1.404(6) . ?
C60 C59 1.486(8) . ?
C53 H53a 0.9900 . ?
C53 H53b 0.9900 . ?
C53 C54 1.455(9) . ?
C54 H54a 0.9900 . ?
C54 H54b 0.9900 . ?
Li61 O51 1.921(8) . ?
Li61 O56 1.934(8) . ?
Li61 O44 1.898(8) . ?
Li61 O1 1.957(9) . ?
Li61 O1a 1.971(13) . ?
C59 H59a 0.9900 . ?
C59 H59b 0.9900 . ?
C2 H2a 0.9900 . ?
C2 H2b 0.9900 . ?
C2 O1 1.431(6) . ?
C2 C4 1.525(7) . ?
C3 H3a 0.9900 . ?
C3 H3b 0.9900 . ?
C3 O1 1.430(6) . ?
C3 C5 1.518(8) . ?
C4 H4a 0.9900 . ?
C4 H4b 0.9900 . ?
C4 C5 1.506(7) . ?
C5 H5a 0.9900 . ?
C5 H5b 0.9900 . ?
O1a C2a 1.440(9) . ?
O1a C3a 1.438(9) . ?
C2a H2aa 0.9900 . ?
C2a H2ab 0.9900 . ?
C2a C4a 1.547(9) . ?
C4a H4aa 0.9900 . ?
C4a H4ab 0.9900 . ?
C4a C5a 1.536(9) . ?
C5a H5aa 0.9900 . ?
C5a H5ab 0.9900 . ?
C5a C3a 1.540(9) . ?
C3a H3aa 0.9900 . ?
C3a H3ab 0.9900 . ?

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
Cl3 Hf1 Hf2 122.82(2) . . ?
Cl4 Hf1 Hf2 98.82(2) . . ?
Cl4 Hf1 Cl3 98.29(3) . . ?
N7 Hf1 Hf2 37.11(7) . . ?
N7 Hf1 Cl3 159.75(7) . . ?
N7 Hf1 Cl4 85.54(7) . . ?
O36 Hf1 Hf2 131.65(7) . . ?
O36 Hf1 Cl3 100.66(7) . . ?
O36 Hf1 Cl4 94.30(7) . . ?
O36 Hf1 N7 98.85(9) . . ?
N20 Hf1 Hf2 73.45(7) . . ?
N20 Hf1 Cl3 96.60(7) . . ?
N20 Hf1 Cl4 165.09(7) . . ?
N20 Hf1 N7 80.71(9) . . ?
N20 Hf1 O36 82.23(9) . . ?
N12 Hf1 Hf2 37.62(7) . . ?
N12 Hf1 Cl3 86.38(7) . . ?
N12 Hf1 Cl4 96.73(7) . . ?
N12 Hf1 N7 73.41(10) . . ?
N12 Hf1 O36 165.93(9) . . ?
N12 Hf1 N20 84.89(10) . . ?
Cl5 Hf2 Hf1 98.53(2) . . ?
Cl6 Hf2 Hf1 122.58(2) . . ?
Cl6 Hf2 Cl5 98.24(3) . . ?
N7 Hf2 Hf1 36.94(7) . . ?
N7 Hf2 Cl5 86.07(7) . . ?
N7 Hf2 Cl6 159.42(7) . . ?
O31 Hf2 Hf1 131.07(7) . . ?
O31 Hf2 Cl5 94.00(7) . . ?
O31 Hf2 Cl6 101.80(7) . . ?
O31 Hf2 N7 97.93(10) . . ?
N22 Hf2 Hf1 73.66(7) . . ?
N22 Hf2 Cl5 165.39(7) . . ?
N22 Hf2 Cl6 96.37(7) . . ?
N22 Hf2 N7 80.34(9) . . ?
N22 Hf2 O31 82.66(9) . . ?
N12 Hf2 Hf1 37.55(7) . . ?
N12 Hf2 Cl5 95.73(7) . . ?
N12 Hf2 Cl6 86.36(7) . . ?
N12 Hf2 N7 73.17(10) . . ?
N12 Hf2 O31 166.29(10) . . ?
N12 Hf2 N22 85.51(10) . . ?
Hf2 N7 Hf1 105.95(11) . . ?
N8 N7 Hf1 123.3(2) . . ?
N8 N7 Hf2 126.2(2) . . ?
N9 N8 N7 179.2(4) . . ?
N12 N11 N10 179.2(4) . . ?
C19 C13 C18 118.8(3) . . ?
C14 C13 C18 119.0(3) . . ?
C14 C13 C19 121.7(3) . . ?
C17 C18 C13 122.6(3) . . ?
O36 C18 C13 116.2(3) . . ?
O36 C18 C17 121.2(3) . . ?
H19a C19 C13 108.19(17) . . ?
H19b C19 C13 108.19(17) . . ?
H19b C19 H19a 107.3 . . ?
N20 C19 C13 116.4(2) . . ?
N20 C19 H19a 108.19(16) . . ?
N20 C19 H19b 108.19(16) . . ?
C16 C17 C18 116.0(3) . . ?
C37 C17 C18 121.6(3) . . ?
C37 C17 C16 122.3(3) . . ?
N20 C21 C24 119.2(3) . . ?
N22 C21 C24 120.2(3) . . ?
N22 C21 N20 120.5(3) . . ?
H23b C23 H23a 107.5 . . ?
C25 C23 H23a 108.47(19) . . ?
C25 C23 H23b 108.47(18) . . ?
N22 C23 H23a 108.47(17) . . ?
N22 C23 H23b 108.47(16) . . ?
N22 C23 C25 115.2(3) . . ?
H16 C16 C17 118.9(2) . . ?
C15 C16 C17 122.2(3) . . ?
C15 C16 H16 118.9(2) . . ?
C26 C25 C23 119.0(3) . . ?
C30 C25 C23 121.4(3) . . ?
C30 C25 C26 119.5(3) . . ?
H24a C24 C21 109.5 . . ?
H24b C24 C21 109.5 . . ?
H24b C24 H24a 109.5 . . ?
H24c C24 C21 109.5 . . ?
H24c C24 H24a 109.5 . . ?
H24c C24 H24b 109.5 . . ?
C27 C26 C25 122.5(3) . . ?
O31 C26 C25 116.3(3) . . ?
O31 C26 C27 121.2(3) . . ?
H14 C14 C13 120.1(2) . . ?
C15 C14 C13 119.7(3) . . ?
C15 C14 H14 120.1(2) . . ?
C28 C27 C26 115.7(3) . . ?
C32 C27 C26 122.4(3) . . ?
C32 C27 C28 121.8(3) . . ?
H38b C38 H38a 109.5 . . ?
H38c C38 H38a 109.5 . . ?
H38c C38 H38b 109.5 . . ?
C37 C38 H38a 109.5 . . ?
C37 C38 H38b 109.5 . . ?
C37 C38 H38c 109.5 . . ?
C14 C15 C16 120.5(3) . . ?
H15 C15 C16 119.8(2) . . ?
H15 C15 C14 119.8(2) . . ?
C38 C37 C17 109.7(3) . . ?
C39 C37 C17 110.4(3) . . ?
C39 C37 C38 110.0(3) . . ?
C40 C37 C17 111.1(3) . . ?
C40 C37 C38 107.5(3) . . ?
C40 C37 C39 108.0(3) . . ?
H30 C30 C25 120.4(2) . . ?
C29 C30 C25 119.2(3) . . ?
C29 C30 H30 120.4(2) . . ?
H28 C28 C27 118.7(2) . . ?
C29 C28 C27 122.6(3) . . ?
C29 C28 H28 118.7(2) . . ?
H39a C39 C37 109.5 . . ?
H39b C39 C37 109.5 . . ?
H39b C39 H39a 109.5 . . ?
H39c C39 C37 109.5 . . ?
H39c C39 H39a 109.5 . . ?
H39c C39 H39b 109.5 . . ?
H33b C33 H33a 109.5 . . ?
H33c C33 H33a 109.5 . . ?
H33c C33 H33b 109.5 . . ?
C32 C33 H33a 109.5 . . ?
C32 C33 H33b 109.5 . . ?
C32 C33 H33c 109.5 . . ?
C28 C29 C30 120.5(3) . . ?
H29 C29 C30 119.8(2) . . ?
H29 C29 C28 119.8(2) . . ?
H40a C40 C37 109.5 . . ?
H40b C40 C37 109.5 . . ?
H40b C40 H40a 109.5 . . ?
H40c C40 C37 109.5 . . ?
H40c C40 H40a 109.5 . . ?
H40c C40 H40b 109.5 . . ?
H41b C41 H41a 109.2 . . ?
C42 C41 H41a 111.4(3) . . ?
C42 C41 H41b 111.4(3) . . ?
C45 C41 H41a 111.4(3) . . ?
C45 C41 H41b 111.4(4) . . ?
C45 C41 C42 101.9(4) . . ?
C33 C32 C27 111.0(3) . . ?
C34 C32 C27 111.7(3) . . ?
C34 C32 C33 108.1(3) . . ?
C35 C32 C27 109.0(3) . . ?
C35 C32 C33 109.2(4) . . ?
C35 C32 C34 107.8(3) . . ?
H42a C42 C41 111.1(3) . . ?
H42b C42 C41 111.1(3) . . ?
H42b C42 H42a 109.0 . . ?
C43 C42 C41 103.4(4) . . ?
C43 C42 H42a 111.1(3) . . ?
C43 C42 H42b 111.1(3) . . ?
H34a C34 C32 109.5 . . ?
H34b C34 C32 109.5 . . ?
H34b C34 H34a 109.5 . . ?
H34c C34 C32 109.5 . . ?
H34c C34 H34a 109.5 . . ?
H34c C34 H34b 109.5 . . ?
H35a C35 C32 109.5 . . ?
H35b C35 C32 109.5 . . ?
H35b C35 H35a 109.5 . . ?
H35c C35 C32 109.5 . . ?
H35c C35 H35a 109.5 . . ?
H35c C35 H35b 109.5 . . ?
H43a C43 C42 110.5(3) . . ?
H43b C43 C42 110.5(3) . . ?
H43b C43 H43a 108.7 . . ?
O44 C43 C42 106.0(4) . . ?
O44 C43 H43a 110.5(2) . . ?
O44 C43 H43b 110.5(3) . . ?
H52b C52 H52a 108.5 . . ?
C53 C52 H52a 110.2(3) . . ?
C53 C52 H52b 110.2(3) . . ?
O51 C52 H52a 110.2(2) . . ?
O51 C52 H52b 110.2(2) . . ?
O51 C52 C53 107.5(4) . . ?
H55b C55 H55a 108.9 . . ?
C54 C55 H55a 110.8(4) . . ?
C54 C55 H55b 110.8(4) . . ?
O51 C55 H55a 110.8(3) . . ?
O51 C55 H55b 110.8(3) . . ?
O51 C55 C54 104.6(5) . . ?
H45a C45 C41 110.2(3) . . ?
H45b C45 C41 110.2(4) . . ?
H45b C45 H45a 108.5 . . ?
O44 C45 C41 107.7(4) . . ?
O44 C45 H45a 110.2(3) . . ?
O44 C45 H45b 110.2(4) . . ?
H57b C57 H57a 108.6 . . ?
C58 C57 H57a 110.4(4) . . ?
C58 C57 H57b 110.4(4) . . ?
O56 C57 H57a 110.4(3) . . ?
O56 C57 H57b 110.4(3) . . ?
O56 C57 C58 106.6(5) . . ?
H58a C58 C57 110.2(4) . . ?
H58b C58 C57 110.2(4) . . ?
H58b C58 H58a 108.5 . . ?
C59 C58 C57 107.8(5) . . ?
C59 C58 H58a 110.2(4) . . ?
C59 C58 H58b 110.2(4) . . ?
H60b C60 H60a 108.6 . . ?
O56 C60 H60a 110.4(3) . . ?
O56 C60 H60b 110.4(3) . . ?
C59 C60 H60a 110.4(4) . . ?
C59 C60 H60b 110.4(4) . . ?
C59 C60 O56 106.8(5) . . ?
H53a C53 C52 111.0(3) . . ?
H53b C53 C52 111.0(3) . . ?
H53b C53 H53a 109.0 . . ?
C54 C53 C52 104.0(5) . . ?
C54 C53 H53a 111.0(4) . . ?
C54 C53 H53b 111.0(4) . . ?
C53 C54 C55 104.5(5) . . ?
H54a C54 C55 110.8(4) . . ?
H54a C54 C53 110.8(4) . . ?
H54b C54 C55 110.8(4) . . ?
H54b C54 C53 110.8(5) . . ?
H54b C54 H54a 108.9 . . ?
O56 Li61 O51 108.7(4) . . ?
O44 Li61 O51 105.7(4) . . ?
O44 Li61 O56 110.8(4) . . ?
O1 Li61 O51 116.1(5) . . ?
O1 Li61 O56 111.0(5) . . ?
O1 Li61 O44 104.4(5) . . ?
O1a Li61 O51 115.8(9) . . ?
O1a Li61 O56 111.1(8) . . ?
O1a Li61 O44 104.7(7) . . ?
O1a Li61 O1 0.3(11) . . ?
C18 O36 Hf1 142.9(2) . . ?
C26 O31 Hf2 141.3(2) . . ?
C19 N20 Hf1 106.29(18) . . ?
C21 N20 Hf1 135.1(2) . . ?
C21 N20 C19 118.0(3) . . ?
C21 N22 Hf2 134.7(2) . . ?
C23 N22 Hf2 106.43(19) . . ?
C23 N22 C21 118.3(3) . . ?
Hf2 N12 Hf1 104.83(10) . . ?
N11 N12 Hf1 126.8(2) . . ?
N11 N12 Hf2 126.3(2) . . ?
C55 O51 C52 108.4(4) . . ?
Li61 O51 C52 124.3(3) . . ?
Li61 O51 C55 126.9(4) . . ?
C60 O56 C57 107.8(4) . . ?
Li61 O56 C57 125.4(4) . . ?
Li61 O56 C60 122.6(4) . . ?
C45 O44 C43 109.9(4) . . ?
Li61 O44 C43 124.3(3) . . ?
Li61 O44 C45 125.7(4) . . ?
C60 C59 C58 104.0(5) . . ?
H59a C59 C58 111.0(4) . . ?
H59a C59 C60 111.0(4) . . ?
H59b C59 C58 111.0(4) . . ?
H59b C59 C60 111.0(4) . . ?
H59b C59 H59a 109.0 . . ?
H2b C2 H2a 108.7 . . ?
O1 C2 H2a 110.5(7) . . ?
O1 C2 H2b 110.5(7) . . ?
C4 C2 H2a 110.5(7) . . ?
C4 C2 H2b 110.5(8) . . ?
C4 C2 O1 105.9(5) . . ?
H3b C3 H3a 108.609209426(18) . . ?
O1 C3 H3a 110.4(6) . . ?
O1 C3 H3b 110.4(8) . . ?
C5 C3 H3a 110.4(7) . . ?
C5 C3 H3b 110.4(7) . . ?
C5 C3 O1 106.7(6) . . ?
C2 O1 Li61 125.7(7) . . ?
C3 O1 Li61 117.4(7) . . ?
C3 O1 C2 111.1(5) . . ?
H4a C4 C2 110.8(8) . . ?
H4b C4 C2 110.8(6) . . ?
H4b C4 H4a 108.9 . . ?
C5 C4 C2 104.8(5) . . ?
C5 C4 H4a 110.8(6) . . ?
C5 C4 H4b 110.8(5) . . ?
C4 C5 C3 103.4(6) . . ?
H5a C5 C3 111.1(8) . . ?
H5a C5 C4 111.1(6) . . ?
H5b C5 C3 111.1(6) . . ?
H5b C5 C4 111.1(5) . . ?
H5b C5 H5a 109.1 . . ?
C2a O1a Li61 121.2(15) . . ?
C3a O1a Li61 122.8(15) . . ?
C3a O1a C2a 108.5(8) . . ?
H2aa C2a O1a 110.5(13) . . ?
H2ab C2a O1a 110.5(15) . . ?
H2ab C2a H2aa 108.7 . . ?
C4a C2a O1a 106.2(9) . . ?
C4a C2a H2aa 110.5(13) . . ?
C4a C2a H2ab 110.5(16) . . ?
H4aa C4a C2a 110.8(16) . . ?
H4ab C4a C2a 110.8(14) . . ?
H4ab C4a H4aa 108.89272557(2) . . ?
C5a C4a C2a 104.5(8) . . ?
C5a C4a H4aa 110.8(12) . . ?
C5a C4a H4ab 110.8(12) . . ?
H5aa C5a C4a 110.7(12) . . ?
H5ab C5a C4a 110.7(12) . . ?
H5ab C5a H5aa 108.8 . . ?
C3a C5a C4a 105.4(7) . . ?
C3a C5a H5aa 110.7(13) . . ?
C3a C5a H5ab 110.7(13) . . ?
C5a C3a O1a 106.9(8) . . ?
H3aa C3a O1a 110.3(13) . . ?
H3aa C3a C5a 110.3(14) . . ?
H3ab C3a O1a 110.3(12) . . ?
H3ab C3a C5a 110.3(11) . . ?
H3ab C3a H3aa 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
C13 C18 C17 C16 -1.4(4) . . . . ?
C13 C18 C17 C37 -179.9(3) . . . . ?
C13 C19 N20 C21 98.8(3) . . . . ?
C13 C14 C15 C16 -0.3(4) . . . . ?
C18 C17 C16 C15 -0.2(4) . . . . ?
C18 C17 C37 C38 -62.7(4) . . . . ?
C18 C17 C37 C39 58.6(4) . . . . ?
C18 C17 C37 C40 178.5(3) . . . . ?
C19 N20 C21 C24 -11.7(3) . . . . ?
C19 N20 C21 N22 169.1(3) . . . . ?
C17 C16 C15 C14 1.0(4) . . . . ?
C21 N22 C23 C25 -98.1(3) . . . . ?
C23 C25 C26 C27 -177.3(3) . . . . ?
C23 C25 C26 O31 0.4(3) . . . . ?
C23 C25 C30 C29 177.7(3) . . . . ?
C25 C26 C27 C28 -0.6(4) . . . . ?
C25 C26 C27 C32 178.4(3) . . . . ?
C25 C30 C29 C28 -0.6(4) . . . . ?
C26 C27 C28 C29 2.0(4) . . . . ?
C26 C27 C32 C33 58.4(4) . . . . ?
C26 C27 C32 C34 179.1(4) . . . . ?
C26 C27 C32 C35 -61.9(4) . . . . ?
C27 C28 C29 C30 -1.5(5) . . . . ?
C41 C42 C43 O44 -27.6(4) . . . . ?
C41 C45 O44 C43 10.7(7) . . . . ?
C41 C45 O44 Li61 -172.3(4) . . . . ?
C42 C43 O44 C45 11.0(6) . . . . ?
C42 C43 O44 Li61 -166.1(4) . . . . ?
C52 C53 C54 C55 -30.1(5) . . . . ?
C52 O51 C55 C54 -22.9(5) . . . . ?
C57 C58 C59 C60 -11.2(6) . . . . ?
C57 O56 C60 C59 -27.4(5) . . . . ?
C58 C59 C60 O56 23.5(6) . . . . ?
Li61 O1 C2 C4 158.1(12) . . . . ?
Li61 O1 C3 C5 -142.5(10) . . . . ?
Li61 O1a C2a C4a -179(2) . . . . ?
Li61 O1a C3a C5a -177(2) . . . . ?
C2 O1 C3 C5 12.2(11) . . . . ?
C2 C4 C5 C3 28.3(12) . . . . ?
O1a C2a C4a C5a -21(2) . . . . ?
O1a C3a C5a C4a 13(2) . . . . ?
C2a C4a C5a C3a 5(2) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.703
_oxdiff_exptl_absorpt_empirical_full_min 0.515
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
C2 C3 1 2.3360 0.0200 -0.0229
C2 C5 1 2.5150 0.0200 0.1137
O1 C2 1 1.4300 0.0100 -0.0009
O1 C3 1 1.4300 0.0100 0.0004
O1 C4 1 2.4260 0.0200 0.0653
O1 C5 1 2.4260 0.0200 0.0614
C4 C2 1 1.5400 0.0100 0.0147
C4 C3 1 2.5150 0.0200 0.1422
C5 C3 1 1.5400 0.0100 0.0222
C5 C4 1 1.5400 0.0100 0.0338
O1a C2a 1 1.4300 0.0100 -0.0097
O1a C4a 1 2.4260 0.0200 0.0375
O1a C5a 1 2.4260 0.0200 0.0328
O1a C3a 1 1.4300 0.0100 -0.0080
C2a C5a 1 2.5150 0.0200 0.0772
C4a C2a 1 1.5400 0.0100 -0.0066
C4a C3a 1 2.5150 0.0200 0.0690
C5a C4a 1 1.5400 0.0100 0.0045
C5a C3a 1 1.5400 0.0100 0.0002
C3a C2a 1 2.3360 0.0100 0.0000

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
O1 Li61 1 1
O1a Li61 1 1

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0100 1.9644 0.0070 0.0070

loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
C2 C3 0.010000 -0.025844 0.001652 -0.006153
C2 O1 0.010000 -0.002680 0.007647 -0.000386
C2 C4 0.010000 -0.004171 -0.012433 -0.000133
C2 C5 0.010000 -0.025756 0.000376 -0.002145
C3 O1 0.010000 -0.006870 -0.011848 -0.000612
C3 C4 0.010000 -0.020222 0.009862 0.014775
C3 C5 0.010000 0.005968 0.009485 0.007512
O1 C4 0.010000 -0.000673 -0.003083 -0.005065
O1 C5 0.010000 -0.002711 0.009786 -0.008785
C4 C5 0.010000 -0.027826 0.001854 -0.012870
O1a C2a 0.010000 -0.001391 -0.006086 -0.007352
O1a C4a 0.010000 0.001006 -0.003194 -0.023152
O1a C5a 0.010000 0.002279 -0.002193 -0.010335
O1a C3a 0.010000 -0.003117 0.009685 0.001551
C2a C4a 0.010000 0.001272 -0.004542 -0.009103
C2a C5a 0.010000 -0.007294 -0.002091 0.001701
C2a C3a 0.010000 -0.010072 0.009155 0.009691
C4a C5a 0.010000 -0.005919 0.008248 0.006185
C4a C3a 0.010000 -0.005335 0.011597 0.017067
C5a C3a 0.010000 0.001519 0.000190 0.008609

loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
C2 O1 0.0100
C2 C4 0.0100
C3 O1 0.0100
C3 C5 0.0100
C4 C5 0.0100
O1a C2a 0.0100
O1a C3a 0.0100
C2a C4a 0.0100
C4a C5a 0.0100
C5a C3a 0.0100

