# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_Zr4
_database_code_depnum_ccdc_archive 'CCDC 2322411'
loop_
_audit_author_name
_audit_author_address
'wang Fei-Fei'
;Xinzhou Normal University
China
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_audit_creation_date             2024-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C182 H226 O24 Zr4, Cl2, 2CH3OH, 3C3H7NO'
_chemical_formula_sum            'C193 H255 Cl2 O29 Zr4 N3'
_chemical_formula_weight         3516.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   26.4909(13)
_cell_length_b                   22.8712(12)
_cell_length_c                   19.5689(9)
_cell_angle_alpha                90
_cell_angle_beta                 122.050(3)
_cell_angle_gamma                90
_cell_volume                     10049.3(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    296.61
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_shelx_estimated_absorpt_T_max   0.652
_shelx_estimated_absorpt_T_min   0.604
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35632
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        66.848
_diffrn_reflns_theta_max         66.848
_diffrn_reflns_theta_min         2.664
_diffrn_ambient_temperature      296.61
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5° ω and 0.5° φ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5853
_reflns_number_total             8967
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     2041
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.0928
_refine_ls_restrained_S_all      0.986
_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)+(0.0671P)²+136.5390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2447
_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, All O(H) groups
2. Restrained distances
 C55-C33
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C58 \\sim C46 \\sim C54 \\sim C51
\\sim C53 \\sim C55 \\sim C52 \\sim C47 \\sim C56 \\sim C57 \\sim C48 \\sim C49
\\sim C50: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C53)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O1, Zr1, C1, O1, O3, C14, C17, C1, C4, C11, C30, C9, C29, C14, C17, C3, C3,
 C31, C5, C11, C30, C9, C29, C15, C15, C36, C2, C19, C31, C5, C32, C38, C40,
 C41, O8, C8, C16, C36, C2, C19, C37, C13, C21, C35, C38, C40, C41, O8, C8, C16,
  C47, C47, C10, C42, C45, C58, C46, C54, C52, C13, C21, C35, C7, C25, C10, C42,
  C45, C58, C46, C54, C52, O4, C6, C28, C7, C25, Zr2, C23, C24, C33, O4, C6,
 C28, O6, O2, O2, O5, C18, C39, C43, C44, C51, C53, C55, C23, C24, C33, C12,
 C27, C27, C22, C26, C18, C39, C43, C44, C51, C53, C55, O7, C20, C26, C34, C48,
 C47, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C39(0.7) H39A(0.7) H39B(0.7) H39C(0.7) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C43(0.7) H43A(0.7) H43B(0.7) H43C(0.7) C44(0.7) H44A(0.7)
 H44B(0.7) H44C(0.7) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) H58C(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) H54C(0.5) C51(0.3) H51A(0.3) H51B(0.3) H51C(0.3) C53(0.3) H53A(0.3)
 H53B(0.3) H53C(0.3) C55(0.3) H55A(0.3) H55B(0.3) H55C(0.3) C52(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) H57C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C50(0.5) H50A(0.5)
 H50B(0.5) H50C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C21(H21A,H21B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26),
 C29(H29), C30(H30)
6.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C58(H58A,H58B,H58C), C46(H46A,H46B,H46C),
 C54(H54A,H54B,H54C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C52(H52A,H52B,H52C), C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
6.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_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
Zr1 Zr 0.51737(4) 0.500000 0.72194(5) 0.0436(3) Uani 1 2 d S TU P . .
Zr2 Zr 0.32830(4) 0.500000 0.16589(5) 0.0474(3) Uani 1 2 d S TU P . .
O1 O 0.4627(2) 0.4334(2) 0.6720(3) 0.0514(11) Uani 1 1 d . U . . .
O2 O 0.4053(2) 0.55461(19) 0.2081(3) 0.0499(10) Uani 1 1 d . U . . .
O3 O 0.5027(3) 0.500000 0.8157(4) 0.0504(13) Uani 1 2 d S TU P . .
O4 O 0.2770(2) 0.4326(2) 0.1465(3) 0.0539(11) Uani 1 1 d . U . . .
O5 O 0.3568(3) 0.500000 0.2955(4) 0.0522(14) Uani 1 2 d S TU P . .
O6 O 0.3036(3) 0.500000 0.0465(4) 0.0521(14) Uani 1 2 d S TU P . .
O7 O 0.4560(3) 0.500000 0.3674(4) 0.0564(17) Uani 1 2 d S TU P . .
O8 O 0.3224(3) 0.4234(2) 0.4141(3) 0.0628(13) Uani 1 1 d . U . . .
H8 H 0.288721 0.433812 0.379096 0.094 Uiso 1 1 calc GR . . . .
C1 C 0.4361(3) 0.3808(3) 0.6603(4) 0.0492(11) Uani 1 1 d . U . . .
C2 C 0.3381(3) 0.3754(3) 0.3883(4) 0.0523(12) Uani 1 1 d . U . . .
C3 C 0.4169(4) 0.4471(3) 0.7895(4) 0.0551(12) Uani 1 1 d . U . . .
C4 C 0.4450(5) 0.500000 0.7973(6) 0.0517(14) Uani 1 2 d S TU P . .
C5 C 0.3929(3) 0.3499(3) 0.4439(4) 0.0533(12) Uani 1 1 d . U . . .
C6 C 0.2212(3) 0.3623(3) 0.0418(4) 0.0552(12) Uani 1 1 d . U . . .
C7 C 0.2409(3) 0.3861(3) 0.1188(4) 0.0541(11) Uani 1 1 d . U . . .
C8 C 0.3028(3) 0.3527(3) 0.3105(4) 0.0536(12) Uani 1 1 d . U . . .
C9 C 0.4309(3) 0.3740(3) 0.5286(4) 0.0530(12) Uani 1 1 d . U . . .
H9A H 0.472407 0.366769 0.547549 0.064 Uiso 1 1 calc R . . . .
H9B H 0.425415 0.416070 0.526469 0.064 Uiso 1 1 calc R . . . .
C10 C 0.2196(3) 0.3617(3) 0.1646(4) 0.0563(12) Uani 1 1 d . U . . .
C11 C 0.4470(4) 0.3895(3) 0.7972(4) 0.0595(13) Uani 1 1 d . U . . .
H11A H 0.440540 0.364211 0.831663 0.071 Uiso 1 1 calc R . . . .
H11B H 0.489539 0.396369 0.824361 0.071 Uiso 1 1 calc R . . . .
C12 C 0.2443(5) 0.500000 -0.0130(6) 0.0498(16) Uani 1 2 d S TU P . .
C13 C 0.3229(4) 0.3025(3) 0.2921(5) 0.0579(13) Uani 1 1 d . U . . .
H13 H 0.298929 0.286367 0.240970 0.070 Uiso 1 1 calc R . . . .
C14 C 0.4271(4) 0.3570(3) 0.7190(4) 0.0551(11) Uani 1 1 d . U . . .
C15 C 0.3598(4) 0.4478(4) 0.7768(5) 0.0626(14) Uani 1 1 d . U . . .
H15 H 0.340133 0.412648 0.770557 0.075 Uiso 1 1 calc R . . . .
C16 C 0.3756(4) 0.2754(4) 0.3442(5) 0.0638(14) Uani 1 1 d . U . . .
C17 C 0.4183(3) 0.3493(3) 0.5893(4) 0.0523(11) Uani 1 1 d . U . . .
C18 C 0.2147(3) 0.4474(3) -0.0428(4) 0.0535(13) Uani 1 1 d . U . . .
C19 C 0.4104(4) 0.3008(3) 0.4215(5) 0.0599(14) Uani 1 1 d . U . . .
H19 H 0.446637 0.283526 0.458724 0.072 Uiso 1 1 calc R . . . .
C20 C 0.1244(5) 0.500000 -0.1412(7) 0.061(2) Uani 1 2 d S TU P . .
C21 C 0.2455(3) 0.3825(3) 0.2502(4) 0.0574(13) Uani 1 1 d . U . . .
H21A H 0.252517 0.424265 0.252364 0.069 Uiso 1 1 calc R . . . .
H21B H 0.216561 0.375884 0.265349 0.069 Uiso 1 1 calc R . . . .
C22 C 0.4054(4) 0.500000 0.3574(6) 0.0460(18) Uani 1 2 d S TU P . .
H22 H 0.404873 0.500000 0.404539 0.055 Uiso 1 2 calc RS T P . .
C23 C 0.1822(4) 0.3166(4) 0.0136(5) 0.0628(13) Uani 1 1 d . U . . .
H23 H 0.170015 0.301239 -0.036863 0.075 Uiso 1 1 calc R . . . .
C24 C 0.2432(4) 0.3888(3) -0.0078(5) 0.0567(12) Uani 1 1 d . U . . .
H24A H 0.234787 0.362367 -0.051352 0.068 Uiso 1 1 calc R . . . .
H24B H 0.286089 0.393754 0.025644 0.068 Uiso 1 1 calc R . . . .
C25 C 0.1798(4) 0.3153(4) 0.1338(5) 0.0624(13) Uani 1 1 d . U . . .
H25 H 0.166012 0.299391 0.164654 0.075 Uiso 1 1 calc R . . . .
C26 C 0.1557(3) 0.4489(4) -0.1071(5) 0.0604(15) Uani 1 1 d . U . . .
H26 H 0.136352 0.413534 -0.128401 0.073 Uiso 1 1 calc R . . . .
C27 C 0.4057(3) 0.6160(3) 0.2194(6) 0.067(2) Uani 1 1 d . U . . .
H27A H 0.370885 0.627121 0.219682 0.100 Uiso 1 1 calc GR . . . .
H27B H 0.405941 0.635867 0.176343 0.100 Uiso 1 1 calc GR . . . .
H27C H 0.440703 0.626645 0.269949 0.100 Uiso 1 1 calc GR . . . .
C28 C 0.1599(4) 0.2919(4) 0.0577(5) 0.0665(13) Uani 1 1 d . U . . .
C29 C 0.3927(4) 0.2951(3) 0.5797(5) 0.0602(12) Uani 1 1 d . U . . .
H29 H 0.380262 0.274821 0.532193 0.072 Uiso 1 1 calc R . . . .
C30 C 0.4012(4) 0.3025(3) 0.7061(5) 0.0629(13) Uani 1 1 d . U . . .
H30 H 0.394542 0.287367 0.744741 0.076 Uiso 1 1 calc R . . . .
C31 C 0.3844(4) 0.2691(4) 0.6374(5) 0.0663(14) Uani 1 1 d . U . . .
C32 C 0.3318(6) 0.500000 0.7734(8) 0.0699(18) Uani 1 2 d S TU P . .
C33 C 0.1156(4) 0.2412(4) 0.0224(6) 0.0802(16) Uani 1 1 d D U . . .
C34 C 0.0602(6) 0.500000 -0.2131(9) 0.086(3) Uani 1 2 d S TU P . .
C35 C 0.3952(4) 0.2193(4) 0.3223(6) 0.0790(17) Uani 1 1 d . U . . .
C36 C 0.3573(5) 0.2082(4) 0.6286(6) 0.0860(19) Uani 1 1 d . U . . .
C37 C 0.2707(6) 0.500000 0.7653(9) 0.086(2) Uani 1 2 d S TU P . .
C38 C 0.2974(5) 0.2114(5) 0.6202(8) 0.110(3) Uani 1 1 d . U . . .
H38A H 0.301768 0.229403 0.667390 0.165 Uiso 1 1 calc GR . . . .
H38B H 0.281674 0.172653 0.614395 0.165 Uiso 1 1 calc GR . . . .
H38C H 0.270633 0.234193 0.573538 0.165 Uiso 1 1 calc GR . . . .
C39 C 0.0959(7) 0.2180(7) 0.0763(9) 0.089(3) Uani 0.7 1 d . U . A 1
H39A H 0.129365 0.200982 0.123563 0.133 Uiso 0.7 1 calc GR . . A 1
H39B H 0.065782 0.188814 0.048002 0.133 Uiso 0.7 1 calc GR . . A 1
H39C H 0.080080 0.249428 0.091888 0.133 Uiso 0.7 1 calc GR . . A 1
C40 C 0.4095(11) 0.1745(10) 0.7210(13) 0.092(4) Uani 0.5 1 d . U . B 1
H40A H 0.448652 0.177592 0.729584 0.139 Uiso 0.5 1 calc GR . . B 1
H40B H 0.399408 0.134022 0.719350 0.139 Uiso 0.5 1 calc GR . . B 1
H40C H 0.408938 0.193621 0.764224 0.139 Uiso 0.5 1 calc GR . . B 1
C41 C 0.3686(12) 0.1682(10) 0.5723(14) 0.096(4) Uani 0.5 1 d . U . B 1
H41A H 0.345305 0.182301 0.517816 0.143 Uiso 0.5 1 calc GR . . B 1
H41B H 0.357188 0.128748 0.574460 0.143 Uiso 0.5 1 calc GR . . B 1
H41C H 0.410042 0.169292 0.590190 0.143 Uiso 0.5 1 calc GR . . B 1
C42 C 0.4563(9) 0.2282(9) 0.3349(13) 0.086(3) Uani 0.5 1 d . U . C 1
H42A H 0.455163 0.260888 0.303447 0.130 Uiso 0.5 1 calc GR . . C 1
H42B H 0.467663 0.193650 0.318459 0.130 Uiso 0.5 1 calc GR . . C 1
H42C H 0.484696 0.235598 0.390963 0.130 Uiso 0.5 1 calc GR . . C 1
C43 C 0.1434(8) 0.1901(7) 0.0052(11) 0.097(3) Uani 0.7 1 d . U . A 1
H43A H 0.145763 0.198797 -0.041022 0.145 Uiso 0.7 1 calc GR . . A 1
H43B H 0.119379 0.155849 -0.005370 0.145 Uiso 0.7 1 calc GR . . A 1
H43C H 0.182685 0.183212 0.051009 0.145 Uiso 0.7 1 calc GR . . A 1
C44 C 0.0598(6) 0.2609(7) -0.0572(9) 0.099(3) Uani 0.7 1 d . U . A 1
H44A H 0.039689 0.290938 -0.046372 0.148 Uiso 0.7 1 calc GR . . A 1
H44B H 0.033623 0.228220 -0.082290 0.148 Uiso 0.7 1 calc GR . . A 1
H44C H 0.071478 0.275995 -0.092690 0.148 Uiso 0.7 1 calc GR . . A 1
C45 C 0.3505(10) 0.1977(10) 0.2374(12) 0.092(4) Uani 0.5 1 d . U . C 1
H45A H 0.312797 0.190879 0.232161 0.138 Uiso 0.5 1 calc GR . . C 1
H45B H 0.364585 0.161940 0.227618 0.138 Uiso 0.5 1 calc GR . . C 1
H45C H 0.345765 0.226660 0.198942 0.138 Uiso 0.5 1 calc GR . . C 1
Cl1 Cl 0.2085(2) 0.500000 0.3442(3) 0.1152(14) Uani 1 2 d S T P . .
C58 C 0.3926(11) 0.2278(10) 0.2407(13) 0.098(3) Uani 0.5 1 d . U . C 2
H58A H 0.356244 0.247346 0.202579 0.148 Uiso 0.5 1 calc GR . . C 2
H58B H 0.393923 0.190274 0.219681 0.148 Uiso 0.5 1 calc GR . . C 2
H58C H 0.425936 0.250856 0.250094 0.148 Uiso 0.5 1 calc GR . . C 2
C46 C 0.3960(10) 0.1701(8) 0.3777(13) 0.091(3) Uani 0.5 1 d . U . C 1
H46A H 0.429713 0.175376 0.431423 0.136 Uiso 0.5 1 calc GR . . C 1
H46B H 0.398859 0.132707 0.357515 0.136 Uiso 0.5 1 calc GR . . C 1
H46C H 0.360050 0.171687 0.378209 0.136 Uiso 0.5 1 calc GR . . C 1
C54 C 0.4547(10) 0.1969(10) 0.3796(14) 0.096(4) Uani 0.5 1 d . U . C 2
H54A H 0.483919 0.224676 0.385641 0.144 Uiso 0.5 1 calc GR . . C 2
H54B H 0.460465 0.160539 0.360168 0.144 Uiso 0.5 1 calc GR . . C 2
H54C H 0.458761 0.190686 0.430864 0.144 Uiso 0.5 1 calc GR . . C 2
C51 C 0.1059(17) 0.2126(16) -0.050(2) 0.088(4) Uani 0.3 1 d . U . A 2
H51A H 0.080284 0.236440 -0.095882 0.131 Uiso 0.3 1 calc GR . . A 2
H51B H 0.087559 0.175252 -0.055529 0.131 Uiso 0.3 1 calc GR . . A 2
H51C H 0.143360 0.207358 -0.045615 0.131 Uiso 0.3 1 calc GR . . A 2
C53 C 0.1565(15) 0.1839(14) 0.093(2) 0.085(4) Uani 0.3 1 d . U . A 2
H53A H 0.190728 0.174146 0.090456 0.128 Uiso 0.3 1 calc GR . . A 2
H53B H 0.131501 0.150122 0.079709 0.128 Uiso 0.3 1 calc GR . . A 2
H53C H 0.169137 0.196861 0.146354 0.128 Uiso 0.3 1 calc GR . . A 2
C55 C 0.0705(13) 0.2456(17) 0.046(2) 0.086(3) Uani 0.3 1 d D U . A 2
H55A H 0.089589 0.258390 0.100955 0.130 Uiso 0.3 1 calc GR . . A 2
H55B H 0.052494 0.208087 0.040401 0.130 Uiso 0.3 1 calc GR . . A 2
H55C H 0.040323 0.273353 0.011559 0.130 Uiso 0.3 1 calc GR . . A 2
C52 C 0.3516(10) 0.1729(9) 0.3034(16) 0.101(4) Uani 0.5 1 d . U . C 2
H52A H 0.361597 0.139194 0.283733 0.152 Uiso 0.5 1 calc GR . . C 2
H52B H 0.312613 0.186477 0.262861 0.152 Uiso 0.5 1 calc GR . . C 2
H52C H 0.351889 0.162686 0.351189 0.152 Uiso 0.5 1 calc GR . . C 2
C47 C 0.2634(6) 0.4510(7) 0.8084(10) 0.147(4) Uani 1 1 d . U . . .
H47A H 0.258886 0.415145 0.780227 0.221 Uiso 1 1 calc GR . . . .
H47B H 0.228629 0.457524 0.811020 0.221 Uiso 1 1 calc GR . . . .
H47C H 0.297827 0.448474 0.862089 0.221 Uiso 1 1 calc GR . . . .
C56 C 0.3871(12) 0.1709(11) 0.6834(14) 0.104(6) Uani 0.5 1 d . U . B 2
H56A H 0.424589 0.164407 0.688105 0.155 Uiso 0.5 1 calc GR . . B 2
H56B H 0.365295 0.134865 0.669945 0.155 Uiso 0.5 1 calc GR . . B 2
H56C H 0.393883 0.185272 0.733737 0.155 Uiso 0.5 1 calc GR . . B 2
C57 C 0.3337(11) 0.1823(10) 0.5398(14) 0.091(5) Uani 0.5 1 d . U . B 2
H57A H 0.300312 0.204968 0.500381 0.136 Uiso 0.5 1 calc GR . . B 2
H57B H 0.321644 0.142366 0.537276 0.136 Uiso 0.5 1 calc GR . . B 2
H57C H 0.365002 0.184187 0.529007 0.136 Uiso 0.5 1 calc GR . . B 2
C48 C 0.2329(9) 0.4677(10) 0.7118(16) 0.115(4) Uani 0.5 1 d . U . . .
H48A H 0.221235 0.483403 0.659923 0.173 Uiso 0.5 1 calc GR . . . .
H48B H 0.198736 0.465314 0.716591 0.173 Uiso 0.5 1 calc GR . . . .
H48C H 0.249419 0.429364 0.717357 0.173 Uiso 0.5 1 calc GR . . . .
C49 C 0.0263(6) 0.4482(6) -0.2208(9) 0.154(5) Uani 1 1 d . U . . .
H49A H 0.026062 0.442794 -0.172293 0.231 Uiso 1 1 calc GR . . . .
H49B H 0.044149 0.414813 -0.229424 0.231 Uiso 1 1 calc GR . . . .
H49C H -0.013850 0.452688 -0.265670 0.231 Uiso 1 1 calc GR . . . .
C50 C 0.0600(11) 0.4749(10) -0.2874(12) 0.125(5) Uani 0.5 1 d . U . . .
H50A H 0.066607 0.433485 -0.281031 0.187 Uiso 0.5 1 calc GR . . . .
H50B H 0.091000 0.493177 -0.291206 0.187 Uiso 0.5 1 calc GR . . . .
H50C H 0.022149 0.482681 -0.335543 0.187 Uiso 0.5 1 calc GR . . . .


_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 Zr2 3.4653(12) 5_666 ?
Zr1 O1 1.967(4) . ?
Zr1 O1 1.967(4) 6_565 ?
Zr1 O2 2.157(5) 2_656 ?
Zr1 O2 2.157(5) 5_666 ?
Zr1 O3 2.067(6) . ?
Zr1 O7 2.204(7) 5_666 ?
C39a H39A 0.9600 . ?
C39a H39B 0.9600 . ?
C39a H39C 0.9600 . ?
C40a H40A 0.9600 . ?
C40a H40B 0.9600 . ?
C40a H40C 0.9600 . ?
C41a H41A 0.9600 . ?
C41a H41B 0.9600 . ?
C41a H41C 0.9600 . ?
C42a H42A 0.9600 . ?
C42a H42B 0.9600 . ?
C42a H42C 0.9600 . ?
C43a H43A 0.9600 . ?
C43a H43B 0.9600 . ?
C43a H43C 0.9600 . ?
C44a H44A 0.9600 . ?
C44a H44B 0.9600 . ?
C44a H44C 0.9600 . ?
C45a H45A 0.9600 . ?
C45a H45B 0.9600 . ?
C45a H45C 0.9600 . ?
C58b H58A 0.9600 . ?
C58b H58B 0.9600 . ?
C58b H58C 0.9600 . ?
C46a H46A 0.9600 . ?
C46a H46B 0.9600 . ?
C46a H46C 0.9600 . ?
C54b H54A 0.9600 . ?
C54b H54B 0.9600 . ?
C54b H54C 0.9600 . ?
C51b H51A 0.9600 . ?
C51b H51B 0.9600 . ?
C51b H51C 0.9600 . ?
C53b H53A 0.9600 . ?
C53b H53B 0.9600 . ?
C53b H53C 0.9600 . ?
C55b H55A 0.9600 . ?
C55b H55B 0.9600 . ?
C55b H55C 0.9600 . ?
C52b H52A 0.9600 . ?
C52b H52B 0.9600 . ?
C52b H52C 0.9600 . ?
C56b H56A 0.9600 . ?
C56b H56B 0.9600 . ?
C56b H56C 0.9600 . ?
C57b H57A 0.9600 . ?
C57b H57B 0.9600 . ?
C57b H57C 0.9600 . ?
Zr2 Zr1 3.4653(12) 5_666 ?
Zr2 O2 2.149(5) . ?
Zr2 O2 2.149(5) 6_565 ?
Zr2 O4 1.954(5) 6_565 ?
Zr2 O4 1.954(5) . ?
Zr2 O5 2.230(7) . ?
Zr2 O6 2.065(7) . ?
O1 C1 1.351(8) . ?
O2 Zr1 2.157(5) 5_666 ?
O2 C27 1.422(8) . ?
O3 C4 1.373(12) . ?
O4 C7 1.340(8) . ?
O5 C22 1.211(11) . ?
O6 C12 1.372(12) . ?
O7 Zr1 2.204(7) 5_666 ?
O7 C22 1.249(11) . ?
O8 H8 0.8200 . ?
O8 C2 1.364(8) . ?
C1 C14 1.401(10) . ?
C1 C17 1.407(10) . ?
C2 C5 1.398(10) . ?
C2 C8 1.396(10) . ?
C3 C4 1.385(9) . ?
C3 C11 1.506(11) . ?
C3 C15 1.398(11) . ?
C4 C3 1.385(9) 6_565 ?
C5 C9 1.515(10) . ?
C5 C19 1.373(10) . ?
C6 C7 1.417(10) . ?
C6 C23 1.364(10) . ?
C6 C24 1.499(10) . ?
C7 C10 1.402(10) . ?
C8 C13 1.393(10) . ?
C8 C21 1.502(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C17 1.504(10) . ?
C10 C21 1.511(10) . ?
C10 C25 1.388(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C14 1.522(10) . ?
C12 C18 1.384(9) 6_565 ?
C12 C18 1.384(9) . ?
C13 H13 0.9300 . ?
C13 C16 1.364(11) . ?
C14 C30 1.379(10) . ?
C15 H15 0.9300 . ?
C15 C32 1.387(10) . ?
C16 C19 1.413(11) . ?
C16 C35 1.530(12) . ?
C17 C29 1.377(10) . ?
C18 C24 1.512(10) . ?
C18 C26 1.392(10) . ?
C19 H19 0.9300 . ?
C20 C26 1.383(10) . ?
C20 C26 1.383(10) 6_565 ?
C20 C34 1.528(17) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C23 C28 1.397(11) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25 0.9300 . ?
C25 C28 1.396(11) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C33 1.530(12) . ?
C29 H29 0.9300 . ?
C29 C31 1.392(11) . ?
C30 H30 0.9300 . ?
C30 C31 1.398(11) . ?
C31 C36 1.535(12) . ?
C32 C15 1.387(10) 6_565 ?
C32 C37 1.539(18) . ?
C33 C39 1.499(17) . ?
C33 C43 1.510(18) . ?
C33 C44 1.541(17) . ?
C33 C51 1.45(3) . ?
C33 C53 1.79(3) . ?
C33 C55 1.496(18) . ?
C34 C49 1.445(14) . ?
C34 C49 1.445(14) 6_565 ?
C34 C50 1.56(3) 6_565 ?
C34 C50 1.56(3) . ?
C35 C42 1.51(2) . ?
C35 C45 1.52(2) . ?
C35 C58 1.57(2) . ?
C35 C46 1.56(2) . ?
C35 C54 1.46(2) . ?
C35 C52 1.46(2) . ?
C36 C38 1.509(15) . ?
C36 C40 1.77(2) . ?
C36 C41 1.58(3) . ?
C36 C56 1.26(2) . ?
C36 C57 1.61(2) . ?
C37 C47 1.477(15) 6_565 ?
C37 C47 1.477(15) . ?
C37 C48 1.24(2) . ?
C37 C48 1.24(2) 6_565 ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 Zr2 128.70(15) . 5_666 ?
O1 Zr1 Zr2 128.69(15) 6_565 5_666 ?
O1 Zr1 O1 101.4(3) . 6_565 ?
O1 Zr1 O2 164.68(19) . 2_656 ?
H39Aa C39a H39B 109.5 . . ?
O1 Zr1 O2 93.91(19) 6_565 2_656 ?
H39Ba C39a H39C 109.5 . . ?
O1 Zr1 O2 93.91(19) . 5_666 ?
O1 Zr1 O2 164.68(19) 6_565 5_666 ?
O1 Zr1 O3 90.28(19) . . ?
O1 Zr1 O3 90.28(18) 6_565 . ?
O1 Zr1 O7 93.86(18) 6_565 5_666 ?
O1 Zr1 O7 93.86(18) . 5_666 ?
O2 Zr1 Zr2 36.32(12) 2_656 5_666 ?
H39Aa C39a H39C 109.5 . . ?
H40Aa C40a H40B 109.5 . . ?
H40Aa C40a H40C 109.5 . . ?
H40Ba C40a H40C 109.5 . . ?
H41Aa C41a H41B 109.5 . . ?
H41Aa C41a H41C 109.5 . . ?
H41Ba C41a H41C 109.5 . . ?
H42Aa C42a H42B 109.5 . . ?
H42Aa C42a H42C 109.5 . . ?
H42Ba C42a H42C 109.5 . . ?
H43Aa C43a H43B 109.5 . . ?
H43Ba C43a H43C 109.5 . . ?
H43Aa C43a H43C 109.5 . . ?
H44Aa C44a H44B 109.5 . . ?
H44Aa C44a H44C 109.5 . . ?
O2 Zr1 Zr2 36.32(12) 5_666 5_666 ?
O2 Zr1 O2 70.8(2) 2_656 5_666 ?
O2 Zr1 O7 84.7(2) 5_666 5_666 ?
O2 Zr1 O7 84.7(2) 2_656 5_666 ?
O3 Zr1 Zr2 98.7(2) . 5_666 ?
O3 Zr1 O2 90.0(2) . 5_666 ?
O3 Zr1 O2 90.0(2) . 2_656 ?
O3 Zr1 O7 173.4(3) . 5_666 ?
O7 Zr1 Zr2 74.70(18) 5_666 5_666 ?
O2 Zr2 Zr1 36.48(12) 6_565 5_666 ?
H44Ba C44a H44C 109.5 . . ?
H45Aa C45a H45B 109.5 . . ?
H45Aa C45a H45C 109.5 . . ?
H45Ba C45a H45C 109.5 . . ?
H58Ab C58b H58B 109.5 . . ?
H58Ab C58b H58C 109.5 . . ?
H58Bb C58b H58C 109.5 . . ?
H46Aa C46a H46B 109.5 . . ?
H46Aa C46a H46C 109.5 . . ?
H46Ba C46a H46C 109.5 . . ?
H54Ab C54b H54B 109.5 . . ?
H54Bb C54b H54C 109.5 . . ?
H54Ab C54b H54C 109.5 . . ?
H51Ab C51b H51B 109.5 . . ?
H51Ab C51b H51C 109.5 . . ?
H51Bb C51b H51C 109.5 . . ?
H53Ab C53b H53B 109.5 . . ?
H53Ab C53b H53C 109.5 . . ?
H53Bb C53b H53C 109.5 . . ?
O2 Zr2 Zr1 36.48(12) . 5_666 ?
O2 Zr2 O2 71.1(2) 6_565 . ?
O2 Zr2 O5 83.30(19) 6_565 . ?
O2 Zr2 O5 83.30(19) . . ?
O4 Zr2 Zr1 126.03(15) 6_565 5_666 ?
O4 Zr2 Zr1 126.04(15) . 5_666 ?
O4 Zr2 O2 162.51(19) 6_565 6_565 ?
O4 Zr2 O2 162.51(19) . . ?
O4 Zr2 O2 92.13(19) 6_565 . ?
O4 Zr2 O2 92.13(19) . 6_565 ?
O4 Zr2 O4 104.1(3) 6_565 . ?
O4 Zr2 O5 90.07(18) 6_565 . ?
O4 Zr2 O5 90.06(18) . . ?
O4 Zr2 O6 90.61(18) 6_565 . ?
O4 Zr2 O6 90.61(18) . . ?
H55Ab C55b H55B 109.5 . . ?
H55Bb C55b H55C 109.5 . . ?
H55Ab C55b H55C 109.5 . . ?
H52Ab C52b H52B 109.5 . . ?
H52Ab C52b H52C 109.5 . . ?
O5 Zr2 Zr1 72.91(18) . 5_666 ?
O6 Zr2 Zr1 105.99(19) . 5_666 ?
O6 Zr2 O2 95.8(2) . . ?
O6 Zr2 O2 95.8(2) . 6_565 ?
O6 Zr2 O5 178.9(3) . . ?
C1 O1 Zr1 162.5(5) . . ?
Zr2 O2 Zr1 107.19(19) . 5_666 ?
C27 O2 Zr1 123.2(4) . 5_666 ?
C27 O2 Zr2 124.2(4) . . ?
C4 O3 Zr1 118.4(6) . . ?
C7 O4 Zr2 168.4(5) . . ?
C22 O5 Zr2 132.4(7) . . ?
C12 O6 Zr2 119.5(6) . . ?
C22 O7 Zr1 130.1(6) . 5_666 ?
C2 O8 H8 109.5 . . ?
O1 C1 C14 120.6(6) . . ?
O1 C1 C17 119.6(6) . . ?
C14 C1 C17 119.8(6) . . ?
O8 C2 C5 116.2(6) . . ?
O8 C2 C8 122.9(7) . . ?
C8 C2 C5 120.8(7) . . ?
C4 C3 C11 121.9(7) . . ?
C4 C3 C15 118.5(8) . . ?
C15 C3 C11 119.6(7) . . ?
O3 C4 C3 119.1(5) . 6_565 ?
O3 C4 C3 119.1(5) . . ?
C3 C4 C3 121.7(10) . 6_565 ?
C2 C5 C9 120.8(7) . . ?
C19 C5 C2 118.7(7) . . ?
C19 C5 C9 120.4(7) . . ?
C7 C6 C24 119.0(7) . . ?
C23 C6 C7 119.7(7) . . ?
C23 C6 C24 121.4(7) . . ?
H52Bb C52b H52C 109.5 . . ?
H56Ab C56b H56B 109.5 . . ?
H56Bb C56b H56C 109.5 . . ?
H56Ab C56b H56C 109.5 . . ?
H57Ab C57b H57B 109.5 . . ?
H57Bb C57b H57C 109.5 . . ?
H57Ab C57b H57C 109.5 . . ?
C43a C33 C28 109.8(9) . . ?
C39a C33 C28 114.9(9) . . ?
C51b C33 C28 118.6(16) . . ?
C55b C33 C28 110.9(15) . . ?
C39a C33 C43 106.1(11) . . ?
C39a C33 C44 108.1(11) . . ?
C43a C33 C44 108.7(11) . . ?
C51b C33 C53 98(2) . . ?
C55b C33 C53 94(2) . . ?
C51b C33 C55 125(2) . . ?
C52b C35 C16 109.7(12) . . ?
C42a C35 C16 109.5(10) . . ?
C45a C35 C16 113.2(10) . . ?
C54b C35 C16 117.9(11) . . ?
C42a C35 C45 111.6(14) . . ?
C54b C35 C58 105.9(15) . . ?
C52b C35 C58 103.3(14) . . ?
C42a C35 C46 111.4(13) . . ?
C45a C35 C46 103.9(14) . . ?
C54b C35 C52 109.0(15) . . ?
C56b C36 C31 118.3(14) . . ?
C56b C36 C38 105.7(17) . . ?
C41a C36 C40 97.3(14) . . ?
C56b C36 C57 112.1(17) . . ?
O4 C7 C6 121.1(7) . . ?
O4 C7 C10 120.0(6) . . ?
C10 C7 C6 118.9(7) . . ?
C2 C8 C21 120.1(7) . . ?
C13 C8 C2 117.4(7) . . ?
C13 C8 C21 122.4(7) . . ?
C5 C9 H9A 108.4 . . ?
C5 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C17 C9 C5 115.5(6) . . ?
C17 C9 H9A 108.4 . . ?
C17 C9 H9B 108.4 . . ?
C7 C10 C21 118.9(7) . . ?
C25 C10 C7 119.8(7) . . ?
C25 C10 C21 121.0(7) . . ?
C3 C11 H11A 108.2 . . ?
C3 C11 H11B 108.2 . . ?
C3 C11 C14 116.3(6) . . ?
H11A C11 H11B 107.4 . . ?
C14 C11 H11A 108.2 . . ?
C14 C11 H11B 108.2 . . ?
O6 C12 C18 119.7(5) . . ?
O6 C12 C18 119.7(5) . 6_565 ?
C18 C12 C18 120.6(10) 6_565 . ?
C8 C13 H13 117.9 . . ?
C16 C13 C8 124.2(7) . . ?
C16 C13 H13 117.9 . . ?
C1 C14 C11 121.0(7) . . ?
C30 C14 C1 119.1(7) . . ?
C30 C14 C11 119.9(7) . . ?
C3 C15 H15 119.4 . . ?
C32 C15 C3 121.2(9) . . ?
C32 C15 H15 119.4 . . ?
C13 C16 C19 116.2(8) . . ?
C13 C16 C35 122.5(7) . . ?
C19 C16 C35 121.2(8) . . ?
C1 C17 C9 119.3(6) . . ?
C29 C17 C1 118.5(7) . . ?
C29 C17 C9 122.1(7) . . ?
C12 C18 C24 122.9(7) . . ?
C12 C18 C26 118.2(8) . . ?
C26 C18 C24 118.9(7) . . ?
C5 C19 C16 122.6(8) . . ?
C5 C19 H19 118.7 . . ?
C16 C19 H19 118.7 . . ?
C26 C20 C26 115.4(10) 6_565 . ?
C26 C20 C34 122.3(5) 6_565 . ?
C26 C20 C34 122.3(5) . . ?
C8 C21 C10 113.8(6) . . ?
C8 C21 H21A 108.8 . . ?
C8 C21 H21B 108.8 . . ?
C10 C21 H21A 108.8 . . ?
C10 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
O5 C22 O7 129.8(9) . . ?
O5 C22 H22 115.1 . . ?
O7 C22 H22 115.1 . . ?
C6 C23 H23 118.7 . . ?
C6 C23 C28 122.6(7) . . ?
C28 C23 H23 118.7 . . ?
C6 C24 C18 112.3(6) . . ?
C6 C24 H24A 109.1 . . ?
C6 C24 H24B 109.1 . . ?
C18 C24 H24A 109.1 . . ?
C18 C24 H24B 109.1 . . ?
H24A C24 H24B 107.9 . . ?
C10 C25 H25 119.1 . . ?
C10 C25 C28 121.7(8) . . ?
C28 C25 H25 119.1 . . ?
C18 C26 H26 118.1 . . ?
C20 C26 C18 123.7(8) . . ?
C20 C26 H26 118.1 . . ?
O2 C27 H27A 109.5 . . ?
O2 C27 H27B 109.5 . . ?
O2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C28 C33 120.2(8) . . ?
C25 C28 C23 117.4(7) . . ?
C25 C28 C33 122.4(8) . . ?
C17 C29 H29 118.2 . . ?
C17 C29 C31 123.6(7) . . ?
C31 C29 H29 118.2 . . ?
C14 C30 H30 118.5 . . ?
C14 C30 C31 122.9(7) . . ?
C31 C30 H30 118.5 . . ?
C29 C31 C30 116.1(7) . . ?
C29 C31 C36 124.2(8) . . ?
C30 C31 C36 119.7(8) . . ?
C15 C32 C15 118.7(11) 6_565 . ?
C15 C32 C37 120.7(6) . . ?
C15 C32 C37 120.7(6) 6_565 . ?
C28 C33 C44 109.1(9) . . ?
C28 C33 C53 101.7(12) . . ?
C20 C34 C50 108.1(13) . 6_565 ?
C20 C34 C50 108.1(13) . . ?
C49 C34 C20 115.0(8) . . ?
C33 C39a H39A 109.5 . . ?
C33 C39a H39B 109.5 . . ?
C49 C34 C20 115.0(8) 6_565 . ?
C33 C39a H39C 109.5 . . ?
C33 C43a H43A 109.5 . . ?
C49 C34 C49 110.1(16) . 6_565 ?
C49 C34 C50 120.7(13) 6_565 . ?
C49 C34 C50 120.7(13) . 6_565 ?
C49 C34 C50 84.7(12) 6_565 6_565 ?
C49 C34 C50 84.7(12) . . ?
C50 C34 C50 43.2(18) . 6_565 ?
C16 C35 C58 110.0(10) . . ?
C16 C35 C46 107.0(10) . . ?
C31 C36 C40 102.5(9) . . ?
C31 C36 C41 110.8(11) . . ?
C31 C36 C57 110.2(10) . . ?
C38 C36 C31 111.7(9) . . ?
C38 C36 C40 109.9(12) . . ?
C38 C36 C41 122.0(12) . . ?
C38 C36 C57 96.6(12) . . ?
C47 C37 C32 113.1(9) . . ?
C33 C43a H43B 109.5 . . ?
C33 C43a H43C 109.5 . . ?
C33 C44a H44A 109.5 . . ?
C33 C44a H44B 109.5 . . ?
C33 C44a H44C 109.5 . . ?
C47 C37 C32 113.1(9) 6_565 . ?
C47 C37 C47 98.7(16) 6_565 . ?
C48 C37 C32 114.9(14) . . ?
C48 C37 C32 114.9(14) 6_565 . ?
C48 C37 C47 130.0(16) 6_565 . ?
C48 C37 C47 130.0(16) . 6_565 ?
C48 C37 C47 74.8(14) 6_565 6_565 ?
C33 C51b H51A 109.5 . . ?
C33 C51b H51B 109.5 . . ?
C33 C51b H51C 109.5 . . ?
C33 C53b H53A 109.5 . . ?
C33 C53b H53B 109.5 . . ?
C33 C53b H53C 109.5 . . ?
C33 C55b H55A 109.5 . . ?
C33 C55b H55B 109.5 . . ?
C48 C37 C47 74.8(14) . . ?
C48 C37 C48 73(3) . 6_565 ?
C36 C38 H38A 109.5 . . ?
C33 C55b H55C 109.5 . . ?
C35 C42a H42A 109.5 . . ?
C35 C42a H42B 109.5 . . ?
C35 C42a H42C 109.5 . . ?
C35 C45a H45A 109.5 . . ?
C35 C45a H45B 109.5 . . ?
C35 C45a H45C 109.5 . . ?
C35 C58b H58A 109.5 . . ?
C35 C58b H58B 109.5 . . ?
C35 C58b H58C 109.5 . . ?
C35 C46a H46A 109.5 . . ?
C35 C46a H46B 109.5 . . ?
C35 C46a H46C 109.5 . . ?
C35 C54b H54A 109.5 . . ?
C35 C54b H54B 109.5 . . ?
C35 C54b H54C 109.5 . . ?
C35 C52b H52A 109.5 . . ?
C35 C52b H52B 109.5 . . ?
C35 C52b H52C 109.5 . . ?
C36 C40a H40A 109.5 . . ?
C36 C40a H40B 109.5 . . ?
C36 C40a H40C 109.5 . . ?
C36 C41a H41A 109.5 . . ?
C36 C41a H41B 109.5 . . ?
C36 C41a H41C 109.5 . . ?
C36 C56b H56A 109.5 . . ?
C36 C56b H56B 109.5 . . ?
C36 C56b H56C 109.5 . . ?
C36 C57b H57A 109.5 . . ?
C36 C57b H57B 109.5 . . ?
C36 C57b H57C 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C47 H47A 109.5 . . ?
C37 C47 H47B 109.5 . . ?
C37 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C37 C48 H48A 109.5 . . ?
C37 C48 H48B 109.5 . . ?
C37 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C34 C49 H49A 109.5 . . ?
C34 C49 H49B 109.5 . . ?
C34 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C34 C50 H50A 109.5 . . ?
C34 C50 H50B 109.5 . . ?
C34 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 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 O1 C1 C14 42.8(19) . . . . ?
Zr1 O1 C1 C17 -136.0(13) . . . . ?
Zr1 O3 C4 C3 90.9(8) . . . . ?
Zr1 O3 C4 C3 -90.9(8) . . . 6_565 ?
Zr1 O7 C22 O5 0.000(3) 5_666 . . . ?
Zr2 O4 C7 C6 1(3) . . . . ?
Zr2 O4 C7 C10 -176(2) . . . . ?
Zr2 O5 C22 O7 0.000(3) . . . . ?
Zr2 O6 C12 C18 -90.1(8) . . . . ?
Zr2 O6 C12 C18 90.2(8) . . . 6_565 ?
O1 C1 C14 C11 -0.1(11) . . . . ?
O1 C1 C14 C30 -178.4(7) . . . . ?
O1 C1 C17 C9 1.8(11) . . . . ?
O1 C1 C17 C29 178.3(7) . . . . ?
O4 C7 C10 C21 -9.5(11) . . . . ?
O4 C7 C10 C25 176.7(7) . . . . ?
O6 C12 C18 C24 5.6(13) . . . . ?
O6 C12 C18 C26 -175.4(7) . . . . ?
O8 C2 C5 C9 2.1(10) . . . . ?
O8 C2 C5 C19 178.8(7) . . . . ?
O8 C2 C8 C13 -178.3(7) . . . . ?
O8 C2 C8 C21 1.8(11) . . . . ?
C1 C14 C30 C31 1.4(13) . . . . ?
C1 C17 C29 C31 -1.3(13) . . . . ?
C2 C5 C9 C17 88.1(9) . . . . ?
C2 C5 C19 C16 0.9(12) . . . . ?
C2 C8 C13 C16 -2.3(12) . . . . ?
C2 C8 C21 C10 166.8(7) . . . . ?
C3 C11 C14 C1 63.7(10) . . . . ?
C3 C11 C14 C30 -118.0(9) . . . . ?
C3 C15 C32 C15 4.7(17) . . . 6_565 ?
C3 C15 C32 C37 -175.7(10) . . . . ?
C4 C3 C11 C14 -104.0(9) . . . . ?
C4 C3 C15 C32 -1.0(13) . . . . ?
C5 C2 C8 C13 3.1(11) . . . . ?
C5 C2 C8 C21 -176.7(7) . . . . ?
C5 C9 C17 C1 -159.4(7) . . . . ?
C5 C9 C17 C29 24.2(11) . . . . ?
C6 C7 C10 C21 173.4(7) . . . . ?
C6 C7 C10 C25 -0.4(12) . . . . ?
C6 C23 C28 C25 -1.0(13) . . . . ?
C6 C23 C28 C33 179.2(8) . . . . ?
C7 C6 C23 C28 0.5(13) . . . . ?
C7 C6 C24 C18 -73.6(9) . . . . ?
C7 C10 C21 C8 -83.4(9) . . . . ?
C7 C10 C25 C28 -0.1(13) . . . . ?
C8 C2 C5 C9 -179.2(7) . . . . ?
C8 C2 C5 C19 -2.6(11) . . . . ?
C8 C13 C16 C19 0.7(12) . . . . ?
C8 C13 C16 C35 178.3(8) . . . . ?
C9 C5 C19 C16 177.7(7) . . . . ?
C9 C17 C29 C31 175.1(8) . . . . ?
C10 C25 C28 C23 0.7(13) . . . . ?
C10 C25 C28 C33 -179.5(8) . . . . ?
C11 C3 C4 O3 -2.4(12) . . . . ?
C11 C3 C4 C3 179.4(6) . . . 6_565 ?
C11 C3 C15 C32 176.8(8) . . . . ?
C11 C14 C30 C31 -176.9(8) . . . . ?
C12 C18 C24 C6 105.0(9) . . . . ?
C12 C18 C26 C20 -2.3(13) . . . . ?
C13 C8 C21 C10 -13.1(10) . . . . ?
C13 C16 C19 C5 0.0(12) . . . . ?
C14 C1 C17 C9 -177.0(7) . . . . ?
C14 C1 C17 C29 -0.5(11) . . . . ?
C14 C30 C31 C29 -3.0(13) . . . . ?
C14 C30 C31 C36 178.3(9) . . . . ?
C15 C3 C4 O3 175.2(7) . . . . ?
C15 C3 C4 C3 -2.9(14) . . . 6_565 ?
C15 C3 C11 C14 78.4(9) . . . . ?
C15 C32 C37 C47 34.6(17) . . . . ?
C15 C32 C37 C47 -34.6(17) 6_565 . . 6_565 ?
C15 C32 C37 C47 -145.8(12) 6_565 . . . ?
C15 C32 C37 C47 145.8(12) . . . 6_565 ?
C15 C32 C37 C48 130.9(17) 6_565 . . . ?
C15 C32 C37 C48 -130.9(17) . . . 6_565 ?
C15 C32 C37 C48 49(2) 6_565 . . 6_565 ?
C15 C32 C37 C48 -49(2) . . . . ?
C17 C1 C14 C11 178.7(7) . . . . ?
C17 C1 C14 C30 0.4(12) . . . . ?
C17 C29 C31 C30 2.9(13) . . . . ?
C17 C29 C31 C36 -178.4(9) . . . . ?
C18 C12 C18 C24 -174.7(6) 6_565 . . . ?
C18 C12 C18 C26 4.3(14) 6_565 . . . ?
C19 C5 C9 C17 -88.5(9) . . . . ?
C13 C16 C35 C52b -59.9(16) . . . . ?
C13 C16 C35 C46a -113.6(12) . . . . ?
C13 C16 C35 C45a 0.2(17) . . . . ?
C13 C16 C35 C42a 125.5(12) . . . . ?
C13 C16 C35 C58b 53.1(15) . . . . ?
C13 C16 C35 C54b 174.6(14) . . . . ?
C19 C16 C35 C52b 117.6(14) . . . . ?
C19 C16 C35 C54b -8.0(18) . . . . ?
C19 C16 C35 C46a 63.9(13) . . . . ?
C19 C16 C35 C58b -129.5(13) . . . . ?
C19 C16 C35 C42a -57.0(14) . . . . ?
C19 C16 C35 C45a 177.7(14) . . . . ?
C21 C8 C13 C16 177.6(8) . . . . ?
C21 C10 C25 C28 -173.7(8) . . . . ?
C23 C6 C7 O4 -176.9(7) . . . . ?
C23 C6 C7 C10 0.2(12) . . . . ?
C23 C6 C24 C18 105.4(9) . . . . ?
C24 C6 C7 O4 2.1(11) . . . . ?
C24 C6 C7 C10 179.2(7) . . . . ?
C24 C6 C23 C28 -178.5(8) . . . . ?
C24 C18 C26 C20 176.7(8) . . . . ?
C25 C10 C21 C8 90.4(9) . . . . ?
C26 C18 C24 C6 -74.0(9) . . . . ?
C26 C20 C26 C18 0.3(16) 6_565 . . . ?
C26 C20 C34 C49 -26.3(19) 6_565 . . 6_565 ?
C26 C20 C34 C49 26.3(19) . . . . ?
C26 C20 C34 C49 -155.7(12) 6_565 . . . ?
C26 C20 C34 C49 155.7(12) . . . 6_565 ?
C26 C20 C34 C50 -111.8(13) . . . 6_565 ?
C26 C20 C34 C50 -66.2(15) . . . . ?
C26 C20 C34 C50 66.2(15) 6_565 . . 6_565 ?
C26 C20 C34 C50 111.8(13) 6_565 . . . ?
C23 C28 C33 C39a 179.0(11) . . . . ?
C23 C28 C33 C51b 11(2) . . . . ?
C23 C28 C33 C53b 117.3(15) . . . . ?
C23 C28 C33 C43a 59.6(13) . . . . ?
C23 C28 C33 C44a -59.5(13) . . . . ?
C23 C28 C33 C55b -143.8(18) . . . . ?
C25 C28 C33 C43a -120.2(12) . . . . ?
C25 C28 C33 C55b 36(2) . . . . ?
C25 C28 C33 C51b -169(2) . . . . ?
C25 C28 C33 C53b -62.5(16) . . . . ?
C25 C28 C33 C44a 120.7(11) . . . . ?
C25 C28 C33 C39a -0.8(15) . . . . ?
C29 C31 C36 C41a 27.1(17) . . . . ?
C29 C31 C36 C40a 130.0(13) . . . . ?
C29 C31 C36 C56b 124.6(19) . . . . ?
C29 C31 C36 C57b -6.2(17) . . . . ?
C29 C31 C36 C38 -112.4(11) . . . . ?
C30 C31 C36 C41a -154.3(13) . . . . ?
C30 C31 C36 C40a -51.4(14) . . . . ?
C30 C31 C36 C57b 172.4(13) . . . . ?
C30 C31 C36 C56b -57(2) . . . . ?
C30 C31 C36 C38 66.2(12) . . . . ?
C34 C20 C26 C18 178.4(10) . . . . ?
C35 C16 C19 C5 -177.6(8) . . . . ?

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

data_Hf4
_database_code_depnum_ccdc_archive 'CCDC 2322412'
loop_
_audit_author_name
_audit_author_address
'wang Fei-Fei'
;Xinzhou Normal University
China
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_audit_creation_date             2024-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C182 H226 Hf4 O24, Cl2, 2CH3OH, 3C3H7NO'
_chemical_formula_sum            'C193 H255 Cl2 Hf4 O29 N3'
_chemical_formula_weight         3861.92
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   26.560(8)
_cell_length_b                   22.889(6)
_cell_length_c                   19.280(6)
_cell_angle_alpha                90
_cell_angle_beta                 120.746(10)
_cell_angle_gamma                90
_cell_volume                     10074(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3630
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26987
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.111
_diffrn_reflns_theta_max         25.111
_diffrn_reflns_theta_min         2.470
_diffrn_ambient_temperature      290.56
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5° ω and 0.5° φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5613
_reflns_number_total             9071
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_refine_diff_density_max         1.981
_refine_diff_density_min         -2.142
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         9071
_refine_ls_number_restraints     1066
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0854
_refine_ls_restrained_S_all      1.075
_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)+(0.1393P)²+205.6180P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2798
_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, All O(H) groups
2. Restrained distances
 H40C-H48B
 1.8 with sigma of 0.02
 C50-C42
 2.3 with sigma of 0.02
 C50-C50_$1
 2.45 with sigma of 0.02
 C44-C40 \\sim C48-C40 \\sim C48-C44
 with sigma of 0.02
 C40-C37 \\sim C48-C37 \\sim C44-C37
 with sigma of 0.02
 C50-C36 \\sim C42-C36
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42
\\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim
C50: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
4. Others
 Fixed Sof: C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) H49A(0.5) H49B(0.5)
 H49C(0.5) Cl1(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C16(H16A,H16B), C23(H23A,H23B)
5.b Me refined with riding coordinates:
 C45(H45A,H45B,H45C)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8A), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C28(H28),
  C29(H29)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
5.e Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_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
Hf1 Hf 0.48515(3) 0.500000 0.27207(4) 0.0410(3) Uani 1 2 d S T P . .
Hf2 Hf 0.66572(3) 0.500000 0.83688(4) 0.0452(3) Uani 1 2 d S T P . .
O1 O 0.5043(6) 0.500000 0.1803(7) 0.053(3) Uani 1 2 d S T P . .
O2 O 0.5378(4) 0.5666(3) 0.3240(5) 0.048(2) Uani 1 1 d . . . . .
O3 O 0.4574(6) 0.500000 0.3608(7) 0.051(3) Uani 1 2 d S T P . .
O4 O 0.4093(4) 0.4451(3) 0.2028(5) 0.051(2) Uani 1 1 d . . . . .
O5 O 0.6914(5) 0.500000 0.9549(7) 0.055(3) Uani 1 2 d S T P . .
O6 O 0.7157(4) 0.5674(4) 0.8518(5) 0.056(2) Uani 1 1 d . . . . .
O7 O 0.3607(6) 0.500000 0.2930(8) 0.055(3) Uani 1 2 d S T P . .
O8 O 0.6740(5) 0.5730(4) 0.5846(6) 0.073(3) Uani 1 1 d . . . . .
H8 H 0.709583 0.573041 0.603990 0.110 Uiso 1 1 calc GR . . . .
C1 C 0.7501(10) 0.500000 1.0145(12) 0.058(3) Uani 1 2 d S TU P . .
C2 C 0.5650(7) 0.6193(6) 0.3362(8) 0.057(2) Uani 1 1 d . U . . .
C3 C 0.6582(7) 0.6210(6) 0.6093(9) 0.061(2) Uani 1 1 d . U . . .
C4 C 0.7529(7) 0.6127(6) 0.8795(9) 0.062(2) Uani 1 1 d . U . . .
C5 C 0.6026(7) 0.6484(6) 0.5530(8) 0.059(2) Uani 1 1 d . U . . .
C6 C 0.7717(7) 0.6368(6) 0.9564(9) 0.060(2) Uani 1 1 d . U . . .
C7 C 0.7511(7) 0.6116(6) 1.0081(9) 0.061(2) Uani 1 1 d . U . . .
H7A H 0.708839 0.607425 0.976712 0.073 Uiso 1 1 calc R . . . .
H7B H 0.760501 0.638273 1.052231 0.073 Uiso 1 1 calc R . . . .
C8 C 0.4103(8) 0.500000 0.3562(10) 0.041(4) Uani 1 2 d S TU P . .
H8A H 0.410761 0.500000 0.404819 0.050 Uiso 1 2 calc RS T P . .
C9 C 0.7785(7) 0.5524(6) 1.0425(9) 0.061(2) Uani 1 1 d . U . . .
C10 C 0.6918(7) 0.6439(6) 0.6874(8) 0.059(2) Uani 1 1 d . U . . .
C11 C 0.5666(7) 0.6242(6) 0.4690(8) 0.058(2) Uani 1 1 d . U . . .
H11A H 0.525611 0.631124 0.450302 0.070 Uiso 1 1 calc R . . . .
H11B H 0.572451 0.582277 0.471329 0.070 Uiso 1 1 calc R . . . .
C12 C 0.5799(7) 0.6492(6) 0.4079(8) 0.061(2) Uani 1 1 d . U . . .
C13 C 0.5746(7) 0.6437(6) 0.2784(8) 0.064(2) Uani 1 1 d . U . . .
C14 C 0.5632(10) 0.500000 0.2044(12) 0.061(3) Uani 1 2 d S TU P . .
C15 C 0.7722(7) 0.6364(6) 0.8299(9) 0.063(2) Uani 1 1 d . U . . .
C16 C 0.5583(7) 0.6104(6) 0.2001(8) 0.065(2) Uani 1 1 d . U . . .
H16A H 0.516480 0.602858 0.171208 0.078 Uiso 1 1 calc R . . . .
H16B H 0.566408 0.635398 0.166369 0.078 Uiso 1 1 calc R . . . .
C17 C 0.4104(5) 0.3837(5) 0.2151(8) 0.059(4) Uani 1 1 d . U . . .
H17A H 0.448112 0.368564 0.228786 0.089 Uiso 1 1 calc GR . . . .
H17B H 0.380639 0.365319 0.166617 0.089 Uiso 1 1 calc GR . . . .
H17C H 0.403354 0.375833 0.258326 0.089 Uiso 1 1 calc GR . . . .
C18 C 0.5899(7) 0.5534(6) 0.2122(8) 0.060(2) Uani 1 1 d . U . . .
C19 C 0.8367(7) 0.5520(7) 1.1042(9) 0.067(2) Uani 1 1 d . U . . .
H19 H 0.855151 0.587797 1.124190 0.080 Uiso 1 1 calc R . . . .
C20 C 0.6732(7) 0.6942(6) 0.7067(9) 0.066(2) Uani 1 1 d . U . . .
H20 H 0.697305 0.711211 0.756949 0.079 Uiso 1 1 calc R . . . .
C21 C 0.8119(7) 0.6814(7) 0.9820(10) 0.071(2) Uani 1 1 d . U . . .
H21 H 0.823655 0.697813 1.032169 0.085 Uiso 1 1 calc R . . . .
C22 C 0.6480(7) 0.5525(7) 0.2308(9) 0.067(2) Uani 1 1 d . U . . .
H22 H 0.662220 0.585370 0.217957 0.081 Uiso 1 1 calc R . . . .
C23 C 0.7484(7) 0.6142(6) 0.7461(8) 0.063(2) Uani 1 1 d . U . . .
H23A H 0.741977 0.572453 0.745050 0.075 Uiso 1 1 calc R . . . .
H23B H 0.776922 0.620963 0.729724 0.075 Uiso 1 1 calc R . . . .
C24 C 0.5866(7) 0.6969(6) 0.5785(9) 0.066(2) Uani 1 1 d . U . . .
H24 H 0.551171 0.714508 0.542108 0.079 Uiso 1 1 calc R . . . .
C25 C 0.6065(7) 0.7039(6) 0.4199(9) 0.068(2) Uani 1 1 d . U . . .
H25 H 0.616892 0.724323 0.467073 0.082 Uiso 1 1 calc R . . . .
C26 C 0.6184(7) 0.7215(6) 0.6529(9) 0.066(2) Uani 1 1 d . U . . .
C27 C 0.8701(10) 0.500000 1.1391(13) 0.067(3) Uani 1 2 d S TU P . .
C28 C 0.8154(7) 0.6805(7) 0.8621(9) 0.070(2) Uani 1 1 d . U . . .
H28 H 0.830149 0.694178 0.830624 0.083 Uiso 1 1 calc R . . . .
C29 C 0.6004(7) 0.6970(7) 0.2927(9) 0.068(2) Uani 1 1 d . U . . .
H29 H 0.606747 0.713140 0.253587 0.082 Uiso 1 1 calc R . . . .
C30 C 0.6016(8) 0.7783(7) 0.6789(10) 0.075(3) Uani 1 1 d . U . . .
C31 C 0.8369(8) 0.7043(7) 0.9378(10) 0.074(3) Uani 1 1 d . U . . .
C32 C 0.9327(12) 0.500000 1.2033(15) 0.082(4) Uani 1 2 d S TU P . .
C33 C 0.6180(8) 0.7289(7) 0.3634(9) 0.072(3) Uani 1 1 d . U . . .
C35 C 0.6429(9) 0.7906(8) 0.3722(11) 0.086(3) Uani 1 1 d . U . . .
C36 C 0.7415(12) 0.500000 0.2551(15) 0.088(5) Uani 1 2 d DS TU P . .
C37 C 0.8720(7) 0.7571(8) 0.9570(9) 0.088(3) Uani 1 1 d D U . . .
C38 C 0.6046(10) 0.8286(9) 0.3021(13) 0.117(5) Uani 1 1 d . U . . .
H38A H 0.623725 0.836637 0.272255 0.176 Uiso 1 1 calc GR . . . .
H38B H 0.597400 0.864577 0.321092 0.176 Uiso 1 1 calc GR . . . .
H38C H 0.568141 0.809044 0.267853 0.176 Uiso 1 1 calc GR . . . .
C39 C 0.9638(10) 0.5542(10) 1.2142(15) 0.129(6) Uani 1 1 d . U . . .
H39A H 0.960192 0.565700 1.163938 0.193 Uiso 1 1 calc GR . . . .
H39B H 1.004441 0.548988 1.254033 0.193 Uiso 1 1 calc GR . . . .
H39C H 0.947424 0.584050 1.231811 0.193 Uiso 1 1 calc GR . . . .
C40 C 0.9189(8) 0.7597(10) 0.9424(11) 0.116(5) Uani 1 1 d D U . . .
H40A H 0.942916 0.725455 0.964305 0.173 Uiso 1 1 calc GR . . . .
H40B H 0.942078 0.793859 0.967665 0.173 Uiso 1 1 calc GR . . . .
H40C H 0.903755 0.761373 0.885311 0.173 Uiso 1 1 calc DGR . . . .
C41 C 0.7019(10) 0.7873(9) 0.3782(13) 0.109(5) Uani 1 1 d . U . . .
H41A H 0.727902 0.763375 0.423509 0.163 Uiso 1 1 calc GR . . . .
H41B H 0.718009 0.825870 0.385401 0.163 Uiso 1 1 calc GR . . . .
H41C H 0.697262 0.770531 0.329658 0.163 Uiso 1 1 calc GR . . . .
C42 C 0.7472(17) 0.5325(12) 0.198(2) 0.098(7) Uani 0.5 1 d D U . A -1
H42A H 0.719032 0.519048 0.144477 0.147 Uiso 0.5 1 calc GR . . A -1
H42B H 0.786000 0.527464 0.206637 0.147 Uiso 0.5 1 calc GR . . A -1
H42C H 0.740549 0.573059 0.202653 0.147 Uiso 0.5 1 calc GR . . A -1
C43 C 0.6472(10) 0.8225(9) 0.4451(12) 0.113(5) Uani 1 1 d . U . . .
H43A H 0.612507 0.814957 0.447417 0.169 Uiso 1 1 calc GR . . . .
H43B H 0.650791 0.863719 0.439656 0.169 Uiso 1 1 calc GR . . . .
H43C H 0.680879 0.808717 0.493688 0.169 Uiso 1 1 calc GR . . . .
C44 C 0.8889(9) 0.7855(9) 1.0297(11) 0.126(5) Uani 1 1 d D U . . .
H44A H 0.854901 0.800767 1.028733 0.189 Uiso 1 1 calc GR . . . .
H44B H 0.915048 0.817033 1.036931 0.189 Uiso 1 1 calc GR . . . .
H44C H 0.908488 0.758343 1.073496 0.189 Uiso 1 1 calc GR . . . .
C45 C 0.6376(10) 0.7913(9) 0.7639(13) 0.124(5) Uani 1 1 d . U . . .
H45A H 0.635333 0.759607 0.794756 0.187 Uiso 1 1 calc R . . . .
H45B H 0.677533 0.796370 0.777465 0.187 Uiso 1 1 calc R . . . .
H45C H 0.623948 0.826524 0.775847 0.187 Uiso 1 1 calc R . . . .
C46 C 0.6067(11) 0.8276(9) 0.6351(14) 0.123(5) Uani 1 1 d . U . . .
H46A H 0.632495 0.817438 0.615798 0.184 Uiso 1 1 calc GR . . . .
H46B H 0.622205 0.860698 0.670401 0.184 Uiso 1 1 calc GR . . . .
H46C H 0.568738 0.837093 0.590100 0.184 Uiso 1 1 calc GR . . . .
C47 C 0.5387(10) 0.7721(10) 0.6642(14) 0.127(5) Uani 1 1 d . U . . .
H47A H 0.511035 0.771326 0.607178 0.191 Uiso 1 1 calc GR . . . .
H47B H 0.530303 0.804738 0.687961 0.191 Uiso 1 1 calc GR . . . .
H47C H 0.535815 0.736537 0.688229 0.191 Uiso 1 1 calc GR . . . .
C48 C 0.8384(10) 0.8084(9) 0.9022(12) 0.135(6) Uani 1 1 d D U . . .
H48A H 0.800206 0.795532 0.861113 0.203 Uiso 1 1 calc GR . . . .
H48B H 0.859299 0.823096 0.877324 0.203 Uiso 1 1 calc DGR . . . .
H48C H 0.834617 0.838748 0.933507 0.203 Uiso 1 1 calc GR . . . .
C49 C 0.9339(15) 0.500000 1.2762(19) 0.124(7) Uani 1 2 d S TU P . .
H49A H 0.938533 0.539303 1.295957 0.186 Uiso 0.5 1 calc GR . . B -1
H49B H 0.966113 0.476581 1.314760 0.186 Uiso 0.5 1 calc GR . . B -1
H49C H 0.897867 0.484116 1.268232 0.186 Uiso 0.5 1 calc GR . . B -1
C50 C 0.7706(10) 0.4469(4) 0.2726(16) 0.149(7) Uani 1 1 d D U . . .
H50A H 0.777506 0.432880 0.323653 0.223 Uiso 1 1 calc GR . . . .
H50B H 0.807435 0.452006 0.275160 0.223 Uiso 1 1 calc GR . . . .
H50C H 0.747184 0.419164 0.231182 0.223 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.7867(10) 0.500000 0.6530(12) 0.142(7) Uani 0.5 2 d S T P . .
C0AA C 0.6908(8) 0.500000 0.2716(16) 0.070(5) Uani 1 2 d S TU P A .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 Hf2 3.4444(16) 5_666 ?
Hf1 O1 2.077(12) . ?
Hf1 O2 1.961(8) 6_565 ?
Hf1 O2 1.961(8) . ?
Hf1 O3 2.182(12) . ?
Hf1 O4 2.162(9) . ?
Hf1 O4 2.162(8) 6_565 ?
Hf2 Hf1 3.4445(16) 5_666 ?
Hf2 O4 2.138(8) 5_666 ?
Hf2 O4 2.138(8) 2_656 ?
Hf2 O5 2.014(12) . ?
Hf2 O6 1.958(9) 6_565 ?
Hf2 O6 1.958(9) . ?
Hf2 O7 2.228(13) 5_666 ?
O1 C14 1.38(2) . ?
O2 C2 1.363(15) . ?
O3 C8 1.21(2) . ?
O4 Hf2 2.138(8) 5_666 ?
O4 C17 1.423(14) . ?
O5 C1 1.39(2) . ?
O6 C4 1.340(16) . ?
O7 Hf2 2.228(13) 5_666 ?
O7 C8 1.26(2) . ?
O8 H8 0.8200 . ?
O8 C3 1.348(16) . ?
C1 C9 1.372(18) . ?
C1 C9 1.372(18) 6_565 ?
C2 C12 1.404(18) . ?
C2 C13 1.383(18) . ?
C3 C5 1.45(2) . ?
C3 C10 1.401(19) . ?
C4 C6 1.413(19) . ?
C4 C15 1.405(19) . ?
C5 C11 1.503(18) . ?
C5 C24 1.37(2) . ?
C6 C7 1.478(18) . ?
C6 C21 1.37(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C9 1.52(2) . ?
C8 H8A 0.9300 . ?
C9 C19 1.39(2) . ?
C10 C20 1.378(19) . ?
C10 C23 1.50(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.505(17) . ?
C12 C25 1.399(19) . ?
C13 C16 1.542(19) . ?
C13 C29 1.36(2) . ?
C14 C18 1.382(17) . ?
C14 C18 1.382(17) 6_565 ?
C15 C23 1.491(19) . ?
C15 C28 1.41(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C18 1.50(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C22 1.40(2) . ?
C19 H19 0.9300 . ?
C19 C27 1.43(2) . ?
C20 H20 0.9300 . ?
C20 C26 1.43(2) . ?
C21 H21 0.9300 . ?
C21 C31 1.42(2) . ?
C22 H22 0.9300 . ?
C22 C0AA 1.56(2) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24 0.9300 . ?
C24 C26 1.36(2) . ?
C25 H25 0.9300 . ?
C25 C33 1.394(19) . ?
C26 C30 1.54(2) . ?
C27 C19 1.43(2) 6_565 ?
C27 C32 1.48(3) . ?
C28 H28 0.9300 . ?
C28 C31 1.38(2) . ?
C29 H29 0.9300 . ?
C29 C33 1.40(2) . ?
C30 C45 1.44(2) . ?
C30 C46 1.46(3) . ?
C30 C47 1.55(3) . ?
C31 C37 1.46(2) . ?
C32 C39 1.45(2) 6_565 ?
C32 C39 1.45(2) . ?
C32 C49 1.39(4) . ?
C33 C35 1.53(2) . ?
C35 C38 1.49(3) . ?
C35 C41 1.51(3) . ?
C35 C43 1.53(3) . ?
C36 C42 1.40(2) . ?
C36 C50 1.386(17) 6_565 ?
C36 C50 1.386(17) . ?
C36 C0AA 1.53(3) . ?
C37 C40 1.412(17) . ?
C37 C44 1.395(17) . ?
C37 C48 1.525(18) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C0AA C22 1.56(2) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 Hf2 101.3(4) . 5_666 ?
O1 Hf1 O3 175.2(5) . . ?
O1 Hf1 O4 91.8(4) . . ?
O1 Hf1 O4 91.8(4) . 6_565 ?
O2 Hf1 Hf2 127.9(3) . 5_666 ?
O2 Hf1 Hf2 127.9(3) 6_565 5_666 ?
O2 Hf1 O1 90.8(3) 6_565 . ?
O2 Hf1 O1 90.8(3) . . ?
O2 Hf1 O2 101.9(5) 6_565 . ?
O2 Hf1 O3 92.2(3) . . ?
O2 Hf1 O3 92.2(3) 6_565 . ?
O2 Hf1 O4 164.4(3) 6_565 6_565 ?
O2 Hf1 O4 93.4(3) 6_565 . ?
O2 Hf1 O4 93.5(3) . 6_565 ?
O2 Hf1 O4 164.4(3) . . ?
O3 Hf1 Hf2 74.0(3) . 5_666 ?
O4 Hf1 Hf2 36.5(2) 6_565 5_666 ?
O4 Hf1 Hf2 36.5(2) . 5_666 ?
O4 Hf1 O3 84.4(4) . . ?
O4 Hf1 O3 84.4(4) 6_565 . ?
O4 Hf1 O4 71.1(4) . 6_565 ?
O4 Hf2 Hf1 37.0(2) 5_666 5_666 ?
O4 Hf2 Hf1 37.0(2) 2_656 5_666 ?
O4 Hf2 O4 72.0(5) 2_656 5_666 ?
O4 Hf2 O7 84.1(3) 5_666 5_666 ?
O4 Hf2 O7 84.1(3) 2_656 5_666 ?
O5 Hf2 Hf1 107.8(4) . 5_666 ?
O5 Hf2 O4 96.9(4) . 2_656 ?
O5 Hf2 O4 96.9(4) . 5_666 ?
O5 Hf2 O7 178.8(5) . 5_666 ?
O6 Hf2 Hf1 125.4(3) 6_565 5_666 ?
O6 Hf2 Hf1 125.4(3) . 5_666 ?
O6 Hf2 O4 162.4(3) 6_565 5_666 ?
O6 Hf2 O4 91.5(4) 6_565 2_656 ?
O6 Hf2 O4 162.4(3) . 2_656 ?
O6 Hf2 O4 91.5(4) . 5_666 ?
O6 Hf2 O5 91.2(3) 6_565 . ?
O6 Hf2 O5 91.2(3) . . ?
O6 Hf2 O6 104.0(5) . 6_565 ?
O6 Hf2 O7 88.0(3) 6_565 5_666 ?
O6 Hf2 O7 88.0(3) . 5_666 ?
O7 Hf2 Hf1 73.4(3) 5_666 5_666 ?
C14 O1 Hf1 116.1(11) . . ?
C2 O2 Hf1 162.2(8) . . ?
C8 O3 Hf1 134.1(11) . . ?
Hf2 O4 Hf1 106.4(3) 5_666 . ?
C17 O4 Hf1 122.5(7) . . ?
C17 O4 Hf2 125.3(8) . 5_666 ?
C1 O5 Hf2 121.7(11) . . ?
C4 O6 Hf2 166.9(9) . . ?
C8 O7 Hf2 131.5(11) . 5_666 ?
C3 O8 H8 109.5 . . ?
C9 C1 O5 119.1(11) 6_565 . ?
C9 C1 O5 119.1(11) . . ?
C9 C1 C9 122(2) . 6_565 ?
O2 C2 C12 117.4(11) . . ?
O2 C2 C13 121.3(12) . . ?
C13 C2 C12 121.3(13) . . ?
O8 C3 C5 117.9(12) . . ?
O8 C3 C10 122.8(14) . . ?
C10 C3 C5 119.2(13) . . ?
O6 C4 C6 121.0(13) . . ?
O6 C4 C15 118.6(13) . . ?
C15 C4 C6 120.4(13) . . ?
C3 C5 C11 119.4(12) . . ?
C24 C5 C3 117.7(13) . . ?
C24 C5 C11 122.9(15) . . ?
C4 C6 C7 120.0(13) . . ?
C21 C6 C4 117.5(13) . . ?
C21 C6 C7 122.4(13) . . ?
C6 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C6 C7 C9 112.4(12) . . ?
H7A C7 H7B 107.8 . . ?
C9 C7 H7A 109.1 . . ?
C9 C7 H7B 109.1 . . ?
O3 C8 O7 127.0(16) . . ?
O3 C8 H8A 116.5 . . ?
O7 C8 H8A 116.5 . . ?
C1 C9 C7 124.3(15) . . ?
C1 C9 C19 118.7(15) . . ?
C19 C9 C7 117.0(13) . . ?
C3 C10 C23 118.9(13) . . ?
C20 C10 C3 118.9(15) . . ?
C20 C10 C23 122.2(13) . . ?
C5 C11 H11A 108.4 . . ?
C5 C11 H11B 108.4 . . ?
C5 C11 C12 115.5(11) . . ?
H11A C11 H11B 107.5 . . ?
C12 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
C2 C12 C11 121.6(12) . . ?
C25 C12 C2 117.7(12) . . ?
C25 C12 C11 120.7(12) . . ?
C2 C13 C16 120.9(13) . . ?
C29 C13 C2 118.8(13) . . ?
C29 C13 C16 120.3(12) . . ?
C18 C14 O1 117.7(11) 6_565 . ?
C18 C14 O1 117.7(11) . . ?
C18 C14 C18 124(2) . 6_565 ?
C4 C15 C23 120.5(13) . . ?
C4 C15 C28 118.3(13) . . ?
C28 C15 C23 121.2(13) . . ?
C13 C16 H16A 108.5 . . ?
C13 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C18 C16 C13 115.0(12) . . ?
C18 C16 H16A 108.5 . . ?
C18 C16 H16B 108.5 . . ?
O4 C17 H17A 109.5 . . ?
O4 C17 H17B 109.5 . . ?
O4 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C16 122.4(15) . . ?
C14 C18 C22 117.0(15) . . ?
C22 C18 C16 120.6(13) . . ?
C9 C19 H19 118.0 . . ?
C9 C19 C27 124.0(16) . . ?
C27 C19 H19 118.0 . . ?
C10 C20 H20 118.6 . . ?
C10 C20 C26 122.8(14) . . ?
C26 C20 H20 118.6 . . ?
C6 C21 H21 117.5 . . ?
C6 C21 C31 125.0(15) . . ?
C31 C21 H21 117.5 . . ?
C18 C22 H22 117.8 . . ?
C18 C22 C0AA 124.4(13) . . ?
C0AA C22 H22 117.8 . . ?
C10 C23 H23A 109.3 . . ?
C10 C23 H23B 109.3 . . ?
C15 C23 C10 111.6(12) . . ?
C15 C23 H23A 109.3 . . ?
C15 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C5 C24 H24 117.4 . . ?
C26 C24 C5 125.1(16) . . ?
C26 C24 H24 117.4 . . ?
C12 C25 H25 119.0 . . ?
C33 C25 C12 122.1(14) . . ?
C33 C25 H25 119.0 . . ?
C20 C26 C30 119.3(14) . . ?
C24 C26 C20 116.1(14) . . ?
C24 C26 C30 124.4(15) . . ?
C19 C27 C19 113(2) 6_565 . ?
C19 C27 C32 123.6(10) 6_565 . ?
C19 C27 C32 123.6(10) . . ?
C15 C28 H28 118.3 . . ?
C31 C28 C15 123.5(14) . . ?
C31 C28 H28 118.3 . . ?
C13 C29 H29 118.3 . . ?
C13 C29 C33 123.4(13) . . ?
C33 C29 H29 118.3 . . ?
C26 C30 C47 109.2(14) . . ?
C45 C30 C26 114.1(16) . . ?
C45 C30 C46 107.1(17) . . ?
C45 C30 C47 104.6(18) . . ?
C46 C30 C26 109.7(15) . . ?
C46 C30 C47 112.0(18) . . ?
C21 C31 C37 126.1(15) . . ?
C28 C31 C21 114.9(15) . . ?
C28 C31 C37 117.5(15) . . ?
C39 C32 C27 115.8(14) 6_565 . ?
C39 C32 C27 115.8(14) . . ?
C39 C32 C39 118(3) 6_565 . ?
C49 C32 C27 106(2) . . ?
C49 C32 C39 97.9(18) . 6_565 ?
C49 C32 C39 97.9(18) . . ?
C25 C33 C29 116.7(14) . . ?
C25 C33 C35 123.1(14) . . ?
C29 C33 C35 120.0(14) . . ?
C33 C35 C43 111.5(15) . . ?
C38 C35 C33 112.5(16) . . ?
C38 C35 C41 107.3(16) . . ?
C38 C35 C43 104.5(17) . . ?
C41 C35 C33 109.5(16) . . ?
C41 C35 C43 111.3(17) . . ?
C42 C36 C0AA 129(2) . . ?
C50 C36 C42 57.1(19) 6_565 . ?
C50 C36 C42 113(2) . . ?
C50 C36 C50 122(3) 6_565 . ?
C50 C36 C0AA 112.9(16) . . ?
C50 C36 C0AA 112.9(16) 6_565 . ?
C31 C37 C48 113.0(16) . . ?
C40 C37 C31 120.0(17) . . ?
C40 C37 C48 95.4(13) . . ?
C44 C37 C31 118.5(17) . . ?
C44 C37 C40 108.5(15) . . ?
C44 C37 C48 96.4(13) . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C32 C39 H39A 109.5 . . ?
C32 C39 H39B 109.5 . . ?
C32 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C35 C41 H41A 109.5 . . ?
C35 C41 H41B 109.5 . . ?
C35 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C36 C42 H42A 109.5 . . ?
C36 C42 H42B 109.5 . . ?
C36 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C35 C43 H43A 109.5 . . ?
C35 C43 H43B 109.5 . . ?
C35 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C37 C44 H44A 109.5 . . ?
C37 C44 H44B 109.5 . . ?
C37 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C30 C45 H45A 109.5 . . ?
C30 C45 H45B 109.5 . . ?
C30 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C30 C46 H46A 109.5 . . ?
C30 C46 H46B 109.5 . . ?
C30 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C30 C47 H47A 109.5 . . ?
C30 C47 H47B 109.5 . . ?
C30 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C37 C48 H48A 109.5 . . ?
C37 C48 H48B 109.5 . . ?
C37 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C32 C49 H49A 109.5 . . ?
C32 C49 H49B 109.5 . . ?
C32 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C36 C50 H50A 109.5 . . ?
C36 C50 H50B 109.5 . . ?
C36 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C22 C0AA C22 100.5(16) 6_565 . ?
C36 C0AA C22 112.7(14) . . ?
C36 C0AA C22 112.7(14) . 6_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hf1 O1 C14 C18 92.8(15) . . . 6_565 ?
Hf1 O1 C14 C18 -92.8(15) . . . . ?
Hf1 O2 C2 C12 141(2) . . . . ?
Hf1 O2 C2 C13 -36(4) . . . . ?
Hf1 O3 C8 O7 0.000(5) . . . . ?
Hf2 O5 C1 C9 -89.2(15) . . . 6_565 ?
Hf2 O5 C1 C9 89.2(15) . . . . ?
Hf2 O6 C4 C6 -13(5) . . . . ?
Hf2 O6 C4 C15 168(3) . . . . ?
Hf2 O7 C8 O3 0.000(5) 5_666 . . . ?
O1 C14 C18 C16 4(2) . . . . ?
O1 C14 C18 C22 -175.4(13) . . . . ?
O2 C2 C12 C11 0(2) . . . . ?
O2 C2 C12 C25 -178.5(13) . . . . ?
O2 C2 C13 C16 -4(2) . . . . ?
O2 C2 C13 C29 178.3(14) . . . . ?
O5 C1 C9 C7 -5(2) . . . . ?
O5 C1 C9 C19 177.7(14) . . . . ?
O6 C4 C6 C7 1(2) . . . . ?
O6 C4 C6 C21 177.1(13) . . . . ?
O6 C4 C15 C23 4(2) . . . . ?
O6 C4 C15 C28 -174.3(13) . . . . ?
O8 C3 C5 C11 -2.9(18) . . . . ?
O8 C3 C5 C24 179.7(13) . . . . ?
O8 C3 C10 C20 178.0(13) . . . . ?
O8 C3 C10 C23 1(2) . . . . ?
C1 C9 C19 C27 2(2) . . . . ?
C2 C12 C25 C33 0(2) . . . . ?
C2 C13 C16 C18 -61(2) . . . . ?
C2 C13 C29 C33 0(3) . . . . ?
C3 C5 C11 C12 -88.7(16) . . . . ?
C3 C5 C24 C26 -1(2) . . . . ?
C3 C10 C20 C26 6(2) . . . . ?
C3 C10 C23 C15 -168.5(12) . . . . ?
C4 C6 C7 C9 71.9(19) . . . . ?
C4 C6 C21 C31 -1(2) . . . . ?
C4 C15 C23 C10 84.8(17) . . . . ?
C4 C15 C28 C31 -5(2) . . . . ?
C5 C3 C10 C20 -4.7(19) . . . . ?
C5 C3 C10 C23 178.3(12) . . . . ?
C5 C11 C12 C2 159.0(15) . . . . ?
C5 C11 C12 C25 -23(2) . . . . ?
C5 C24 C26 C20 1(2) . . . . ?
C5 C24 C26 C30 176.1(14) . . . . ?
C6 C4 C15 C23 -174.8(14) . . . . ?
C6 C4 C15 C28 7(2) . . . . ?
C6 C7 C9 C1 -103.7(18) . . . . ?
C6 C7 C9 C19 74.0(17) . . . . ?
C6 C21 C31 C28 3(3) . . . . ?
C6 C21 C31 C37 169.4(16) . . . . ?
C7 C6 C21 C31 174.7(15) . . . . ?
C7 C9 C19 C27 -175.4(15) . . . . ?
C9 C1 C9 C7 173.7(10) 6_565 . . . ?
C9 C1 C9 C19 -4(3) 6_565 . . . ?
C9 C19 C27 C19 -1(3) . . . 6_565 ?
C9 C19 C27 C32 178.1(19) . . . . ?
C10 C3 C5 C11 179.6(12) . . . . ?
C10 C3 C5 C24 2.2(19) . . . . ?
C10 C20 C26 C24 -4(2) . . . . ?
C10 C20 C26 C30 -179.0(13) . . . . ?
C11 C5 C24 C26 -177.9(14) . . . . ?
C11 C12 C25 C33 -178.2(16) . . . . ?
C12 C2 C13 C16 179.7(14) . . . . ?
C12 C2 C13 C29 2(3) . . . . ?
C12 C25 C33 C29 1(3) . . . . ?
C12 C25 C33 C35 175.4(17) . . . . ?
C13 C2 C12 C11 176.7(15) . . . . ?
C13 C2 C12 C25 -2(2) . . . . ?
C13 C16 C18 C14 104.3(18) . . . . ?
C13 C16 C18 C22 -76.7(17) . . . . ?
C13 C29 C33 C25 -1(3) . . . . ?
C13 C29 C33 C35 -175.7(17) . . . . ?
C14 C18 C22 C0AA -22(2) . . . . ?
C15 C4 C6 C7 179.9(14) . . . . ?
C15 C4 C6 C21 -4(2) . . . . ?
C15 C28 C31 C21 0(2) . . . . ?
C15 C28 C31 C37 -167.7(15) . . . . ?
C16 C13 C29 C33 -178.1(16) . . . . ?
C16 C18 C22 C0AA 158.9(16) . . . . ?
C18 C14 C18 C16 177.6(12) 6_565 . . . ?
C18 C14 C18 C22 -1(3) 6_565 . . . ?
C18 C22 C0AA C22 37(2) . . . 6_565 ?
C18 C22 C0AA C36 157.4(15) . . . . ?
C19 C27 C32 C39 162(2) 6_565 . . . ?
C19 C27 C32 C39 -162(2) . . . 6_565 ?
C19 C27 C32 C39 -17(3) . . . . ?
C19 C27 C32 C39 17(3) 6_565 . . 6_565 ?
C19 C27 C32 C49 90.6(19) . . . . ?
C19 C27 C32 C49 -90.6(19) 6_565 . . . ?
C20 C10 C23 C15 14.6(19) . . . . ?
C20 C26 C30 C45 -14(2) . . . . ?
C20 C26 C30 C46 106.5(18) . . . . ?
C20 C26 C30 C47 -130.4(17) . . . . ?
C21 C6 C7 C9 -104.1(17) . . . . ?
C21 C31 C37 C40 144.5(17) . . . . ?
C21 C31 C37 C44 8(3) . . . . ?
C21 C31 C37 C48 -104.2(19) . . . . ?
C23 C10 C20 C26 -177.4(13) . . . . ?
C23 C15 C28 C31 177.0(16) . . . . ?
C24 C5 C11 C12 88.6(17) . . . . ?
C24 C26 C30 C45 171.7(18) . . . . ?
C24 C26 C30 C46 -68(2) . . . . ?
C24 C26 C30 C47 55(2) . . . . ?
C25 C33 C35 C38 -123(2) . . . . ?
C25 C33 C35 C41 117.8(19) . . . . ?
C25 C33 C35 C43 -6(3) . . . . ?
C28 C15 C23 C10 -96.8(17) . . . . ?
C28 C31 C37 C40 -50(2) . . . . ?
C28 C31 C37 C44 173.2(16) . . . . ?
C28 C31 C37 C48 62(2) . . . . ?
C29 C13 C16 C18 116.8(17) . . . . ?
C29 C33 C35 C38 51(3) . . . . ?
C29 C33 C35 C41 -68(2) . . . . ?
C29 C33 C35 C43 168.0(17) . . . . ?
C42 C36 C0AA C22 -14(3) . . . . ?
C42 C36 C0AA C22 99(2) . . . 6_565 ?
C50 C36 C0AA C22 -51(3) . . . 6_565 ?
C50 C36 C0AA C22 164.4(17) 6_565 . . 6_565 ?
C50 C36 C0AA C22 51(3) 6_565 . . . ?
C50 C36 C0AA C22 -164.4(17) . . . . ?

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

data_Zr8
_database_code_depnum_ccdc_archive 'CCDC 2322413'
loop_
_audit_author_name
_audit_author_address
'wang Fei-Fei'
;Xinzhou Normal University
China
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_audit_creation_date             2024-02-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         "C188 H236 N4 O32 Zr8, 8CH3OH, 7C3H7NO'"
_chemical_formula_sum            'C217 H317 N11 O47 Zr8'
_chemical_formula_weight         4561.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   20.8087(15)
_cell_length_b                   30.081(2)
_cell_length_c                   18.0516(14)
_cell_angle_alpha                90
_cell_angle_beta                 106.317(4)
_cell_angle_gamma                90
_cell_volume                     10844.3(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_shelx_estimated_absorpt_T_max   0.652
_shelx_estimated_absorpt_T_min   0.604
_exptl_absorpt_coefficient_mu    3.502
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46213
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.184
_diffrn_reflns_theta_max         67.184
_diffrn_reflns_theta_min         4.092
_diffrn_ambient_temperature      296.31
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7295
_reflns_number_total             9798
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.231
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9798
_refine_ls_number_restraints     1110
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0766
_refine_ls_restrained_S_all      1.073
_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)+(0.0876P)²+136.3443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2161
_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. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C14(H14A,H14B), C23(H23A,H23B), C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C13(H13), C17(H17), C18(H18), C20(H20), C24(H24), C25(H25),
 C29(H29)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_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 0.48428(2) 0.55689(2) 0.58848(3) 0.03513(17) Uani 1 1 d . . . . .
Zr2 Zr 0.62351(4) 0.500000 0.57416(4) 0.0378(2) Uani 1 2 d S T P . .
Zr3 Zr 0.33416(4) 0.500000 0.60628(5) 0.0408(2) Uani 1 2 d S T P . .
O1 O 0.4199(3) 0.500000 0.5618(4) 0.0401(13) Uani 1 2 d S T P . .
O2 O 0.5435(3) 0.500000 0.6250(3) 0.0412(13) Uani 1 2 d S T P . .
O3 O 0.5627(2) 0.56005(14) 0.5325(2) 0.0412(10) Uani 1 1 d . . . . .
O4 O 0.3914(2) 0.56772(13) 0.6234(3) 0.0427(10) Uani 1 1 d . . . . .
O5 O 0.4790(2) 0.63122(14) 0.5780(3) 0.0508(11) Uani 1 1 d . . . . .
O6 O 0.6811(2) 0.54648(15) 0.6434(3) 0.0479(11) Uani 1 1 d . . . . .
O7 O 0.3564(4) 0.500000 0.7374(5) 0.0643(19) Uani 1 2 d S T P . .
O8 O 0.3001(3) 0.500000 0.4851(4) 0.0514(16) Uani 1 2 d S T P . .
O9 O 0.5370(2) 0.57851(15) 0.6968(3) 0.0468(10) Uani 1 1 d . . . . .
O10 O 0.2590(2) 0.54504(15) 0.5967(3) 0.0508(11) Uani 1 1 d . . . . .
N1 N 0.4389(4) 0.7005(2) 0.5536(4) 0.0705(18) Uani 1 1 d . . . . .
C1 C 0.8060(5) 0.500000 0.7030(7) 0.058(2) Uani 1 2 d S TU P . .
H1A H 0.784632 0.500000 0.647830 0.070 Uiso 1 2 calc RS T P . .
H1B H 0.854062 0.500000 0.710597 0.070 Uiso 1 2 calc RS T P . .
C2 C 0.7871(4) 0.5418(2) 0.7368(5) 0.0571(15) Uani 1 1 d . U . . .
C3 C 0.6063(4) 0.6411(2) 0.7474(4) 0.0527(13) Uani 1 1 d . U . . .
C4 C 0.7261(4) 0.5636(2) 0.7045(4) 0.0529(14) Uani 1 1 d . U . . .
C5 C 0.6523(3) 0.6314(2) 0.6973(4) 0.0519(14) Uani 1 1 d . U . . .
H5A H 0.626807 0.615985 0.651182 0.062 Uiso 1 1 calc R . . . .
H5B H 0.667313 0.659358 0.681300 0.062 Uiso 1 1 calc R . . . .
C6 C 0.3874(4) 0.6228(2) 0.7189(4) 0.0531(13) Uani 1 1 d . U . . .
C7 C 0.6182(4) 0.6773(3) 0.7967(5) 0.0608(14) Uani 1 1 d . U . . .
H7 H 0.654817 0.695350 0.798066 0.073 Uiso 1 1 calc R . . . .
C8 C 0.1638(4) 0.6111(3) 0.4351(5) 0.0616(14) Uani 1 1 d . U . . .
H8 H 0.171365 0.634339 0.404529 0.074 Uiso 1 1 calc R . . . .
C9 C 0.2166(4) 0.5951(2) 0.4933(5) 0.0545(13) Uani 1 1 d . U . . .
C10 C 0.5494(3) 0.6145(2) 0.7432(4) 0.0480(12) Uani 1 1 d . U . . .
C11 C 0.3169(3) 0.6292(2) 0.5903(4) 0.0502(12) Uani 1 1 d . U . . .
C12 C 0.7130(4) 0.6036(2) 0.7364(4) 0.0553(14) Uani 1 1 d . U . . .
C13 C 0.4428(4) 0.6576(2) 0.5357(5) 0.0571(16) Uani 1 1 d . U . . .
H13 H 0.416178 0.647621 0.488229 0.069 Uiso 1 1 calc R . . . .
C14 C 0.2870(3) 0.6144(2) 0.5068(4) 0.0532(13) Uani 1 1 d . U . . .
H14A H 0.315844 0.592096 0.493978 0.064 Uiso 1 1 calc R . . . .
H14B H 0.285058 0.639590 0.472788 0.064 Uiso 1 1 calc R . . . .
C15 C 0.2065(4) 0.5600(2) 0.5405(5) 0.0542(13) Uani 1 1 d . U . . .
C16 C 0.5076(4) 0.6249(2) 0.7892(4) 0.0541(13) Uani 1 1 d . U . . .
C17 C 0.2895(4) 0.6687(2) 0.6120(5) 0.0615(14) Uani 1 1 d . U . . .
H17 H 0.256651 0.683787 0.574827 0.074 Uiso 1 1 calc R . . . .
C18 C 0.3587(4) 0.6614(3) 0.7377(5) 0.0651(14) Uani 1 1 d . U . . .
H18 H 0.373415 0.671583 0.788254 0.078 Uiso 1 1 calc R . . . .
C19 C 0.1429(4) 0.5412(2) 0.5262(5) 0.0573(15) Uani 1 1 d . U . . .
C20 C 0.0911(4) 0.5588(3) 0.4680(5) 0.0652(16) Uani 1 1 d . U . . .
H20 H 0.048541 0.546664 0.459970 0.078 Uiso 1 1 calc R . . . .
C21 C 0.3655(3) 0.6067(2) 0.6432(4) 0.0509(12) Uani 1 1 d . U . . .
C22 C 0.3093(4) 0.6856(3) 0.6855(5) 0.0673(16) Uani 1 1 d . U . . .
C23 C 0.4427(4) 0.5998(2) 0.7790(4) 0.0552(14) Uani 1 1 d . U . . .
H23A H 0.447649 0.569513 0.762795 0.066 Uiso 1 1 calc R . . . .
H23B H 0.431604 0.598646 0.827672 0.066 Uiso 1 1 calc R . . . .
C24 C 0.5229(4) 0.6610(3) 0.8396(5) 0.0646(14) Uani 1 1 d . U . . .
H24 H 0.495416 0.667212 0.871004 0.077 Uiso 1 1 calc R . . . .
C25 C 0.8300(4) 0.5591(3) 0.8045(5) 0.0715(17) Uani 1 1 d . U . . .
H25 H 0.869816 0.544140 0.826753 0.086 Uiso 1 1 calc R . . . .
C26 C 0.0992(4) 0.5936(3) 0.4207(5) 0.0676(16) Uani 1 1 d . U . . .
C27 C 0.1326(5) 0.500000 0.5694(7) 0.058(2) Uani 1 2 d S TU P . .
H27A H 0.087592 0.500000 0.575052 0.069 Uiso 1 2 calc RS T P . .
H27B H 0.163976 0.500000 0.620564 0.069 Uiso 1 2 calc RS T P . .
C28 C 0.5784(4) 0.6883(3) 0.8440(5) 0.0667(16) Uani 1 1 d . U . . .
C29 C 0.7582(4) 0.6197(3) 0.8039(5) 0.0679(16) Uani 1 1 d . U . . .
H29 H 0.748797 0.646349 0.824957 0.081 Uiso 1 1 calc R . . . .
C30 C 0.8168(4) 0.5971(3) 0.8404(5) 0.0728(17) Uani 1 1 d . U . . .
C31 C 0.2769(5) 0.7276(3) 0.7074(6) 0.084(2) Uani 1 1 d . U . . .
C32 C 0.5935(5) 0.7294(3) 0.8975(6) 0.084(2) Uani 1 1 d . U . . .
C33 C 0.2849(7) 0.7655(4) 0.6545(8) 0.119(4) Uani 1 1 d . U . . .
H33A H 0.331599 0.770213 0.659728 0.178 Uiso 1 1 calc GR . . . .
H33B H 0.265853 0.792190 0.668606 0.178 Uiso 1 1 calc GR . . . .
H33C H 0.262267 0.758051 0.601948 0.178 Uiso 1 1 calc GR . . . .
C34 C 0.3010(7) 0.7382(4) 0.7902(8) 0.129(4) Uani 1 1 d . U . . .
H34A H 0.308423 0.711156 0.819647 0.194 Uiso 1 1 calc GR . . . .
H34B H 0.267996 0.755816 0.804833 0.194 Uiso 1 1 calc GR . . . .
H34C H 0.342105 0.754580 0.800272 0.194 Uiso 1 1 calc GR . . . .
C35 C 0.0409(4) 0.6108(3) 0.3554(6) 0.080(2) Uani 1 1 d . U . . .
C36 C 0.4739(6) 0.7178(4) 0.6277(7) 0.107(4) Uani 1 1 d . U . . .
H36A H 0.450204 0.743013 0.639239 0.161 Uiso 1 1 calc GR . . . .
H36B H 0.518165 0.726639 0.627420 0.161 Uiso 1 1 calc GR . . . .
H36C H 0.476879 0.695248 0.666196 0.161 Uiso 1 1 calc GR . . . .
C37 C 0.3935(6) 0.7299(4) 0.5004(7) 0.110(4) Uani 1 1 d . U . . .
H37A H 0.418366 0.753555 0.485770 0.165 Uiso 1 1 calc GR . . . .
H37B H 0.361946 0.742098 0.524781 0.165 Uiso 1 1 calc GR . . . .
H37C H 0.369901 0.713535 0.455254 0.165 Uiso 1 1 calc GR . . . .
C38 C 0.8642(6) 0.6136(4) 0.9160(6) 0.095(2) Uani 1 1 d . U . . .
C39 C 0.2011(5) 0.7201(4) 0.6901(7) 0.105(3) Uani 1 1 d . U . . .
H39A H 0.182230 0.714954 0.635842 0.157 Uiso 1 1 calc GR . . . .
H39B H 0.180763 0.745906 0.705217 0.157 Uiso 1 1 calc GR . . . .
H39C H 0.192957 0.694727 0.718468 0.157 Uiso 1 1 calc GR . . . .
C40 C 0.6618(7) 0.7436(5) 0.9169(9) 0.146(4) Uani 1 1 d . U . . .
H40A H 0.690505 0.718177 0.921109 0.220 Uiso 1 1 calc GR . . . .
H40B H 0.672747 0.759189 0.965210 0.220 Uiso 1 1 calc GR . . . .
H40C H 0.668051 0.763025 0.877236 0.220 Uiso 1 1 calc GR . . . .
C41 C 0.0085(7) 0.5741(5) 0.3011(9) 0.146(5) Uani 1 1 d . U . . .
H41A H 0.042406 0.554721 0.292671 0.219 Uiso 1 1 calc GR . . . .
H41B H -0.016759 0.586634 0.252786 0.219 Uiso 1 1 calc GR . . . .
H41C H -0.020939 0.557459 0.323243 0.219 Uiso 1 1 calc GR . . . .
C42 C -0.0105(7) 0.6303(5) 0.3862(9) 0.146(5) Uani 1 1 d . U . . .
H42A H -0.033771 0.607001 0.404419 0.219 Uiso 1 1 calc GR . . . .
H42B H -0.041655 0.646704 0.346290 0.219 Uiso 1 1 calc GR . . . .
H42C H 0.010112 0.649835 0.428131 0.219 Uiso 1 1 calc GR . . . .
C43 C 0.8915(8) 0.5770(5) 0.9705(8) 0.143(5) Uani 1 1 d . U . . .
H43A H 0.855571 0.558055 0.974841 0.215 Uiso 1 1 calc GR . . . .
H43B H 0.913846 0.589122 1.020272 0.215 Uiso 1 1 calc GR . . . .
H43C H 0.922746 0.560025 0.951782 0.215 Uiso 1 1 calc GR . . . .
C44 C 0.0601(7) 0.6450(5) 0.3077(9) 0.145(5) Uani 1 1 d . U . . .
H44A H 0.083868 0.668436 0.340219 0.218 Uiso 1 1 calc GR . . . .
H44B H 0.020634 0.656962 0.271965 0.218 Uiso 1 1 calc GR . . . .
H44C H 0.088404 0.632095 0.279646 0.218 Uiso 1 1 calc GR . . . .
C45 C 0.9188(8) 0.6393(6) 0.8995(9) 0.157(5) Uani 1 1 d . U . . .
H45A H 0.944545 0.620134 0.876146 0.236 Uiso 1 1 calc GR . . . .
H45B H 0.947215 0.651166 0.946717 0.236 Uiso 1 1 calc GR . . . .
H45C H 0.900328 0.663158 0.864809 0.236 Uiso 1 1 calc GR . . . .
C46 C 0.5360(8) 0.7551(5) 0.8927(10) 0.165(5) Uani 1 1 d . U . . .
H46A H 0.520867 0.768286 0.842281 0.247 Uiso 1 1 calc GR . . . .
H46B H 0.546639 0.778177 0.930985 0.247 Uiso 1 1 calc GR . . . .
H46C H 0.501365 0.736556 0.901392 0.247 Uiso 1 1 calc GR . . . .
C47 C 0.5973(9) 0.7139(6) 0.9783(9) 0.159(5) Uani 1 1 d . U . . .
H47A H 0.591697 0.738850 1.008940 0.239 Uiso 1 1 calc GR . . . .
H47B H 0.640117 0.700362 1.000980 0.239 Uiso 1 1 calc GR . . . .
H47C H 0.562506 0.692546 0.976136 0.239 Uiso 1 1 calc GR . . . .
C48 C 0.8346(8) 0.6461(6) 0.9557(9) 0.165(5) Uani 1 1 d . U . . .
H48A H 0.815282 0.669760 0.920800 0.247 Uiso 1 1 calc GR . . . .
H48B H 0.868499 0.657953 0.998768 0.247 Uiso 1 1 calc GR . . . .
H48C H 0.800328 0.632173 0.973792 0.247 Uiso 1 1 calc GR . . . .


_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 3.4227(9) 6_565 ?
Zr1 Zr1 3.4359(10) 2_656 ?
Zr1 Zr2 3.4366(8) . ?
Zr1 Zr2 3.5887(8) 5_666 ?
Zr1 Zr3 3.6544(8) . ?
Zr1 O1 2.143(4) . ?
Zr1 O2 2.104(4) . ?
Zr1 O3 2.149(4) . ?
Zr1 O3 2.130(4) 2_656 ?
Zr1 O4 2.220(4) . ?
Zr1 O5 2.244(4) . ?
Zr1 O9 2.061(4) . ?
Zr2 Zr1 3.5888(8) 2_656 ?
Zr2 Zr1 3.4365(8) 6_565 ?
Zr2 Zr1 3.5888(8) 5_666 ?
Zr2 Zr3 3.6050(11) 5_666 ?
Zr2 O1 2.365(6) 5_666 ?
Zr2 O2 2.114(6) . ?
Zr2 O3 2.212(4) 6_565 ?
Zr2 O3 2.212(4) . ?
Zr2 O6 2.027(4) . ?
Zr2 O6 2.027(4) 6_565 ?
Zr2 O8 2.151(6) 5_666 ?
Zr3 Zr1 3.6545(8) 6_565 ?
Zr3 Zr2 3.6050(11) 5_666 ?
Zr3 O1 2.153(6) . ?
Zr3 O4 2.336(4) . ?
Zr3 O4 2.335(4) 6_565 ?
Zr3 O7 2.281(8) . ?
Zr3 O8 2.101(7) . ?
Zr3 O10 2.039(5) 6_565 ?
Zr3 O10 2.039(5) . ?
O1 Zr1 2.143(4) 6_565 ?
O1 Zr2 2.365(6) 5_666 ?
O2 Zr1 2.104(4) 6_565 ?
O3 Zr1 2.130(4) 2_656 ?
O4 C21 1.378(8) . ?
O5 C13 1.208(9) . ?
O6 C4 1.334(8) . ?
O8 Zr2 2.151(6) 5_666 ?
O9 C10 1.348(8) . ?
O10 C15 1.343(9) . ?
N1 C13 1.337(10) . ?
N1 C36 1.429(13) . ?
N1 C37 1.445(12) . ?
C1 C2 1.497(10) . ?
C1 C2 1.497(10) 6_565 ?
C2 C4 1.402(10) . ?
C2 C25 1.396(11) . ?
C3 C5 1.518(10) . ?
C3 C7 1.384(10) . ?
C3 C10 1.413(9) . ?
C4 C12 1.394(10) . ?
C5 C12 1.514(10) . ?
C6 C18 1.388(10) . ?
C6 C21 1.400(10) . ?
C6 C23 1.511(11) . ?
C7 C28 1.385(11) . ?
C8 C9 1.377(11) . ?
C8 C26 1.399(11) . ?
C9 C14 1.529(9) . ?
C9 C15 1.409(10) . ?
C10 C16 1.396(9) . ?
C11 C14 1.527(10) . ?
C11 C17 1.421(10) . ?
C11 C21 1.360(11) . ?
C12 C29 1.401(10) . ?
C15 C19 1.394(10) . ?
C16 C23 1.513(10) . ?
C16 C24 1.396(10) . ?
C17 C22 1.370(11) . ?
C18 C22 1.389(12) . ?
C19 C20 1.382(11) . ?
C19 C27 1.512(10) . ?
C20 C26 1.392(12) . ?
C22 C31 1.536(11) . ?
C24 C28 1.401(11) . ?
C25 C30 1.378(12) . ?
C26 C35 1.525(12) . ?
C27 C19 1.512(10) 6_565 ?
C28 C32 1.545(11) . ?
C29 C30 1.390(12) . ?
C30 C38 1.525(12) . ?
C31 C33 1.527(16) . ?
C31 C34 1.473(15) . ?
C31 C39 1.536(14) . ?
C32 C40 1.431(16) . ?
C32 C46 1.408(17) . ?
C32 C47 1.511(19) . ?
C35 C41 1.505(16) . ?
C35 C42 1.459(17) . ?
C35 C44 1.467(16) . ?
C38 C43 1.481(17) . ?
C38 C45 1.472(19) . ?
C38 C48 1.447(18) . ?

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
Zr1 Zr1 Zr1 90.000(1) 6_565 2_656 ?
Zr1 Zr1 Zr2 61.520(10) 6_565 5_666 ?
Zr1 Zr1 Zr2 58.529(17) 2_656 5_666 ?
Zr1 Zr1 Zr2 60.133(10) 6_565 . ?
Zr1 Zr1 Zr2 62.959(18) 2_656 . ?
Zr1 Zr1 Zr3 118.19(2) 2_656 . ?
Zr1 Zr1 Zr3 62.078(9) 6_565 . ?
Zr2 Zr1 Zr2 92.72(2) . 5_666 ?
Zr2 Zr1 Zr3 59.690(19) 5_666 . ?
Zr2 Zr1 Zr3 122.208(16) . . ?
O1 Zr1 Zr1 37.00(12) . 6_565 ?
O1 Zr1 Zr1 93.49(16) . 2_656 ?
O1 Zr1 Zr2 39.43(16) . 5_666 ?
O1 Zr1 Zr2 94.13(13) . . ?
O1 Zr1 Zr3 31.81(14) . . ?
O1 Zr1 O3 116.01(19) . . ?
O1 Zr1 O4 69.02(17) . . ?
O1 Zr1 O5 139.83(17) . . ?
O2 Zr1 Zr1 92.48(16) . 2_656 ?
O2 Zr1 Zr1 35.56(14) . 6_565 ?
O2 Zr1 Zr2 35.54(15) . . ?
O2 Zr1 Zr2 92.57(14) . 5_666 ?
O2 Zr1 Zr3 91.82(14) . . ?
O2 Zr1 O1 72.24(19) . . ?
O2 Zr1 O3 114.67(19) . 2_656 ?
O2 Zr1 O3 74.20(19) . . ?
O2 Zr1 O4 120.73(19) . . ?
O2 Zr1 O5 147.93(18) . . ?
O3 Zr1 Zr1 92.53(11) . 6_565 ?
O3 Zr1 Zr1 92.56(11) 2_656 6_565 ?
O3 Zr1 Zr1 36.78(11) 2_656 2_656 ?
O3 Zr1 Zr1 36.39(12) . 2_656 ?
O3 Zr1 Zr2 35.01(11) 2_656 5_666 ?
O3 Zr1 Zr2 38.66(11) . . ?
O3 Zr1 Zr2 91.10(12) . 5_666 ?
O3 Zr1 Zr2 95.68(11) 2_656 . ?
O3 Zr1 Zr3 147.43(12) . . ?
O3 Zr1 Zr3 87.33(11) 2_656 . ?
O3 Zr1 O1 74.2(2) 2_656 . ?
O3 Zr1 O3 72.93(18) 2_656 . ?
O3 Zr1 O4 164.58(16) . . ?
O3 Zr1 O4 95.67(16) 2_656 . ?
O3 Zr1 O5 86.68(16) . . ?
O3 Zr1 O5 82.64(17) 2_656 . ?
O4 Zr1 Zr1 98.44(11) . 6_565 ?
O4 Zr1 Zr1 132.25(12) . 2_656 ?
O4 Zr1 Zr2 156.14(11) . . ?
O4 Zr1 Zr2 84.72(11) . 5_666 ?
O4 Zr1 Zr3 37.75(10) . . ?
O4 Zr1 O5 81.47(16) . . ?
O5 Zr1 Zr1 86.53(12) . 2_656 ?
O5 Zr1 Zr1 175.16(13) . 6_565 ?
O5 Zr1 Zr2 113.70(13) . 5_666 ?
O5 Zr1 Zr2 120.81(12) . . ?
O5 Zr1 Zr3 116.82(12) . . ?
O9 Zr1 Zr1 133.87(13) . 2_656 ?
O9 Zr1 Zr1 108.40(13) . 6_565 ?
O9 Zr1 Zr2 89.63(12) . . ?
O9 Zr1 Zr2 166.08(13) . 5_666 ?
O9 Zr1 Zr3 107.72(13) . . ?
O9 Zr1 O1 126.7(2) . . ?
O9 Zr1 O2 81.42(19) . . ?
O9 Zr1 O3 99.24(17) . . ?
O9 Zr1 O3 158.12(17) . 2_656 ?
O9 Zr1 O4 87.59(17) . . ?
O9 Zr1 O5 76.44(18) . . ?
Zr1 Zr2 Zr1 87.28(2) 6_565 2_656 ?
Zr1 Zr2 Zr1 87.28(2) . 5_666 ?
Zr1 Zr2 Zr1 58.511(18) . 2_656 ?
Zr1 Zr2 Zr1 56.961(19) 5_666 2_656 ?
Zr1 Zr2 Zr1 58.510(18) 6_565 5_666 ?
Zr1 Zr2 Zr1 59.73(2) 6_565 . ?
Zr1 Zr2 Zr3 61.061(18) 5_666 5_666 ?
Zr1 Zr2 Zr3 119.54(2) 6_565 5_666 ?
Zr1 Zr2 Zr3 119.54(2) . 5_666 ?
Zr1 Zr2 Zr3 61.061(18) 2_656 5_666 ?
O1 Zr2 Zr1 35.14(8) 5_666 2_656 ?
O1 Zr2 Zr1 35.14(8) 5_666 5_666 ?
O1 Zr2 Zr1 89.62(12) 5_666 . ?
O1 Zr2 Zr1 89.62(12) 5_666 6_565 ?
O1 Zr2 Zr3 35.09(14) 5_666 5_666 ?
O2 Zr2 Zr1 35.34(8) . . ?
O2 Zr2 Zr1 88.14(15) . 5_666 ?
O2 Zr2 Zr1 88.14(15) . 2_656 ?
O2 Zr2 Zr1 35.34(9) . 6_565 ?
O2 Zr2 Zr3 144.48(17) . 5_666 ?
O2 Zr2 O1 109.4(2) . 5_666 ?
O2 Zr2 O3 72.70(14) . 6_565 ?
O2 Zr2 O3 72.70(14) . . ?
O2 Zr2 O8 176.1(2) . 5_666 ?
O3 Zr2 Zr1 37.37(11) . . ?
O3 Zr2 Zr1 91.06(11) 6_565 . ?
O3 Zr2 Zr1 33.52(11) 6_565 5_666 ?
O3 Zr2 Zr1 86.85(12) . 5_666 ?
O3 Zr2 Zr1 86.85(12) 6_565 2_656 ?
O3 Zr2 Zr1 33.52(11) . 2_656 ?
O3 Zr2 Zr1 37.37(11) 6_565 6_565 ?
O3 Zr2 Zr1 91.06(11) . 6_565 ?
O3 Zr2 Zr3 87.39(11) . 5_666 ?
O3 Zr2 Zr3 87.39(11) 6_565 5_666 ?
O3 Zr2 O1 68.40(13) . 5_666 ?
O3 Zr2 O1 68.40(13) 6_565 5_666 ?
O3 Zr2 O3 109.5(2) 6_565 . ?
O6 Zr2 Zr1 107.51(13) 6_565 5_666 ?
O6 Zr2 Zr1 131.41(13) 6_565 . ?
O6 Zr2 Zr1 107.51(13) . 2_656 ?
O6 Zr2 Zr1 88.55(13) 6_565 6_565 ?
O6 Zr2 Zr1 163.43(14) . 5_666 ?
O6 Zr2 Zr1 88.55(12) . . ?
O6 Zr2 Zr1 163.43(14) 6_565 2_656 ?
O6 Zr2 Zr1 131.41(13) . 6_565 ?
O6 Zr2 Zr3 107.77(14) 6_565 5_666 ?
O6 Zr2 Zr3 107.77(14) . 5_666 ?
O6 Zr2 O1 128.85(15) 6_565 5_666 ?
O6 Zr2 O1 128.85(15) . 5_666 ?
O6 Zr2 O2 97.65(17) . . ?
O6 Zr2 O2 97.65(17) 6_565 . ?
O6 Zr2 O3 80.15(17) . . ?
O6 Zr2 O3 80.15(17) 6_565 6_565 ?
O6 Zr2 O3 162.73(18) 6_565 . ?
O6 Zr2 O3 162.73(18) . 6_565 ?
O6 Zr2 O6 87.2(3) 6_565 . ?
O6 Zr2 O8 85.17(19) 6_565 5_666 ?
O6 Zr2 O8 85.17(19) . 5_666 ?
O8 Zr2 Zr1 142.54(11) 5_666 . ?
O8 Zr2 Zr1 88.42(16) 5_666 5_666 ?
O8 Zr2 Zr1 88.42(16) 5_666 2_656 ?
O8 Zr2 Zr1 142.54(11) 5_666 6_565 ?
O8 Zr2 Zr3 31.60(18) 5_666 5_666 ?
O8 Zr2 O1 66.7(2) 5_666 5_666 ?
O8 Zr2 O3 105.24(15) 5_666 6_565 ?
O8 Zr2 O3 105.24(15) 5_666 . ?
Zr1 Zr3 Zr1 55.846(19) . 6_565 ?
Zr2 Zr3 Zr1 59.250(17) 5_666 . ?
Zr2 Zr3 Zr1 59.249(17) 5_666 6_565 ?
O1 Zr3 Zr1 31.63(8) . . ?
O1 Zr3 Zr1 31.63(8) . 6_565 ?
O1 Zr3 Zr2 39.14(17) . 5_666 ?
O1 Zr3 O4 66.69(11) . . ?
O1 Zr3 O4 66.69(11) . 6_565 ?
O1 Zr3 O7 116.1(3) . . ?
O4 Zr3 Zr1 35.58(10) 6_565 6_565 ?
O4 Zr3 Zr1 35.58(10) . . ?
O4 Zr3 Zr1 90.21(10) 6_565 . ?
O4 Zr3 Zr1 90.21(10) . 6_565 ?
O4 Zr3 Zr2 82.80(11) . 5_666 ?
O4 Zr3 Zr2 82.80(11) 6_565 5_666 ?
O4 Zr3 O4 121.4(2) 6_565 . ?
O7 Zr3 Zr1 99.33(17) . . ?
O7 Zr3 Zr1 99.33(17) . 6_565 ?
O7 Zr3 Zr2 155.2(2) . 5_666 ?
O7 Zr3 O4 85.16(15) . . ?
O7 Zr3 O4 85.16(14) . 6_565 ?
O8 Zr3 Zr1 87.43(15) . 6_565 ?
O8 Zr3 Zr1 87.43(15) . . ?
O8 Zr3 Zr2 32.44(17) . 5_666 ?
O8 Zr3 O1 71.6(2) . . ?
O8 Zr3 O4 98.50(14) . . ?
O8 Zr3 O4 98.50(14) . 6_565 ?
O8 Zr3 O7 172.3(3) . . ?
O10 Zr3 Zr1 163.29(13) . 6_565 ?
O10 Zr3 Zr1 109.61(13) . . ?
O10 Zr3 Zr1 109.61(13) 6_565 6_565 ?
O10 Zr3 Zr1 163.29(13) 6_565 . ?
O10 Zr3 Zr2 107.44(14) 6_565 5_666 ?
O10 Zr3 Zr2 107.44(14) . 5_666 ?
O10 Zr3 O1 131.66(15) . . ?
O10 Zr3 O1 131.66(15) 6_565 . ?
O10 Zr3 O4 77.41(17) . . ?
O10 Zr3 O4 160.18(16) 6_565 . ?
O10 Zr3 O4 77.40(17) 6_565 6_565 ?
O10 Zr3 O4 160.17(16) . 6_565 ?
O10 Zr3 O7 90.9(2) . . ?
O10 Zr3 O7 90.9(2) 6_565 . ?
O10 Zr3 O8 83.43(19) . . ?
O10 Zr3 O8 83.43(19) 6_565 . ?
O10 Zr3 O10 83.3(3) . 6_565 ?
Zr1 O1 Zr1 106.0(2) . 6_565 ?
Zr1 O1 Zr2 105.43(19) 6_565 5_666 ?
Zr1 O1 Zr2 105.43(19) . 5_666 ?
Zr1 O1 Zr3 116.56(18) . . ?
Zr1 O1 Zr3 116.56(18) 6_565 . ?
Zr3 O1 Zr2 105.8(2) . 5_666 ?
Zr1 O2 Zr1 108.9(3) . 6_565 ?
Zr1 O2 Zr2 109.12(19) 6_565 . ?
Zr1 O2 Zr2 109.12(19) . . ?
Zr1 O3 Zr1 106.83(18) 2_656 . ?
Zr1 O3 Zr2 103.97(17) . . ?
Zr1 O3 Zr2 111.47(18) 2_656 . ?
Zr1 O4 Zr3 106.66(16) . . ?
C21 O4 Zr1 129.3(4) . . ?
C21 O4 Zr3 123.7(4) . . ?
C13 O5 Zr1 135.7(5) . . ?
C4 O6 Zr2 158.8(5) . . ?
Zr3 O8 Zr2 116.0(3) . 5_666 ?
C10 O9 Zr1 143.2(4) . . ?
C15 O10 Zr3 136.7(4) . . ?
C13 N1 C36 121.8(8) . . ?
C13 N1 C37 120.1(8) . . ?
C36 N1 C37 117.7(8) . . ?
C2 C1 C2 114.3(10) 6_565 . ?
C4 C2 C1 122.3(7) . . ?
C25 C2 C1 119.6(8) . . ?
C25 C2 C4 118.1(7) . . ?
C7 C3 C5 120.4(6) . . ?
C7 C3 C10 118.5(7) . . ?
C10 C3 C5 121.1(6) . . ?
O6 C4 C2 120.4(6) . . ?
O6 C4 C12 120.1(6) . . ?
C12 C4 C2 119.4(7) . . ?
C12 C5 C3 114.4(6) . . ?
C18 C6 C21 118.9(7) . . ?
C18 C6 C23 120.1(7) . . ?
C21 C6 C23 120.9(6) . . ?
C3 C7 C28 123.6(7) . . ?
C9 C8 C26 121.9(8) . . ?
C8 C9 C14 120.7(7) . . ?
C8 C9 C15 120.1(7) . . ?
C15 C9 C14 119.2(7) . . ?
O9 C10 C3 120.0(6) . . ?
O9 C10 C16 120.4(6) . . ?
C16 C10 C3 119.6(6) . . ?
C17 C11 C14 115.6(7) . . ?
C21 C11 C14 124.3(6) . . ?
C21 C11 C17 120.0(7) . . ?
C4 C12 C5 121.2(6) . . ?
C4 C12 C29 119.8(7) . . ?
C29 C12 C5 118.9(7) . . ?
O5 C13 N1 123.4(8) . . ?
C11 C14 C9 112.0(6) . . ?
O10 C15 C9 118.6(6) . . ?
O10 C15 C19 122.2(7) . . ?
C19 C15 C9 119.2(7) . . ?
C10 C16 C23 120.0(6) . . ?
C24 C16 C10 119.7(7) . . ?
C24 C16 C23 120.0(6) . . ?
C22 C17 C11 122.7(8) . . ?
C6 C18 C22 124.0(8) . . ?
C15 C19 C27 120.1(7) . . ?
C20 C19 C15 118.9(7) . . ?
C20 C19 C27 120.8(7) . . ?
C19 C20 C26 123.4(7) . . ?
O4 C21 C6 120.3(7) . . ?
C11 C21 O4 120.6(6) . . ?
C11 C21 C6 119.1(6) . . ?
C17 C22 C18 115.3(7) . . ?
C17 C22 C31 121.2(8) . . ?
C18 C22 C31 123.5(8) . . ?
C6 C23 C16 109.4(6) . . ?
C16 C24 C28 121.8(7) . . ?
C30 C25 C2 123.9(8) . . ?
C8 C26 C35 122.1(8) . . ?
C20 C26 C8 116.5(8) . . ?
C20 C26 C35 121.5(8) . . ?
C19 C27 C19 110.2(9) . 6_565 ?
C7 C28 C24 116.9(7) . . ?
C7 C28 C32 121.6(7) . . ?
C24 C28 C32 121.6(7) . . ?
C30 C29 C12 121.8(8) . . ?
C25 C30 C29 116.6(8) . . ?
C25 C30 C38 121.8(8) . . ?
C29 C30 C38 121.6(8) . . ?
C22 C31 C39 109.1(8) . . ?
C33 C31 C22 108.7(8) . . ?
C33 C31 C39 105.6(10) . . ?
C34 C31 C22 113.1(9) . . ?
C34 C31 C33 114.0(10) . . ?
C34 C31 C39 105.9(10) . . ?
C40 C32 C28 113.9(9) . . ?
C40 C32 C47 94.5(12) . . ?
C46 C32 C28 112.4(9) . . ?
C46 C32 C40 128.2(12) . . ?
C46 C32 C47 92.5(12) . . ?
C47 C32 C28 107.6(10) . . ?
C41 C35 C26 111.6(9) . . ?
C42 C35 C26 110.5(10) . . ?
C42 C35 C41 107.4(11) . . ?
C42 C35 C44 107.0(11) . . ?
C44 C35 C26 113.8(8) . . ?
C44 C35 C41 106.2(12) . . ?
C43 C38 C30 112.5(9) . . ?
C45 C38 C30 109.3(10) . . ?
C45 C38 C43 110.5(12) . . ?
C48 C38 C30 113.9(10) . . ?
C48 C38 C43 108.1(12) . . ?
C48 C38 C45 102.0(12) . . ?

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

data_Hf8
_database_code_depnum_ccdc_archive 'CCDC 2322414'
loop_
_audit_author_name
_audit_author_address
'wang Fei-Fei'
;Xinzhou Normal University
China
;
_audit_update_record             
;
2024-03-02 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_audit_creation_date             2024-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C184 H226 Hf8 N2 O35, 8CH3OH, 7C3H7NO'
_chemical_formula_sum            'C213 H307 Hf8 N9 O50'
_chemical_formula_weight         5221.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.070(4)
_cell_length_b                   30.684(5)
_cell_length_c                   17.217(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.524(7)
_cell_angle_gamma                90
_cell_volume                     10672(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9335
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      63.858
_cell_measurement_theta_min      3.933
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.415
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55861
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        64.436
_diffrn_reflns_theta_max         64.436
_diffrn_reflns_theta_min         2.677
_diffrn_ambient_temperature      290.56
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6868
_reflns_number_total             8967
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.329
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.216
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     1229
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.1020
_refine_ls_restrained_S_all      1.051
_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)+(0.1331P)²+347.7014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2682
_refine_ls_wR_factor_ref         0.2960
_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
 H42B-H43B
 1.8 with sigma of 0.02
 H13-H47A
 1.8 with sigma of 0.02
 H44B-H45B
 1.8 with sigma of 0.02
 C42-C36 = C43-C36 = C46-C36 = C44-C26 = C47-C26 = C45-C26
 1.5 with sigma of 0.02
 O10-O2
 2.47 with sigma of 0.02
 C47-C44 \\sim C45-C44 \\sim C47-C45
 with sigma of 0.02
 C44-C26 \\sim C47-C26 \\sim C45-C26
 with sigma of 0.02
 C35-C27 \\sim C39-C35 \\sim C39-C27
 with sigma of 0.02
 C39-C28 \\sim C35-C28 \\sim C28-C27
 with sigma of 0.02
 C44-C12 \\sim C47-C12 \\sim C45-C12
 with sigma of 0.02
 C40-C38 \\sim C41-C38 \\sim C41-C40
 with sigma of 0.02
 C41-C37 \\sim C40-C37 \\sim C38-C37
 with sigma of 0.02
 C46-C43 \\sim C42-C43 \\sim C42-C46
 with sigma of 0.02
 C42-C36 \\sim C36-C43 \\sim C46-C36
 with sigma of 0.02
 C46-C6 \\sim C43-C6 \\sim C42-C6
 with sigma of 0.02
3. Rigid bond restraints
 Hf1, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
O10: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Hf2(0.8) Hf3(0.3) Hf4(0.2) Hf5(0.2) O8(0.3) O10(0.25) O11(0.2)
 O13(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B)
6.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C11(H11), C13(H13), C18(H18), C20(H20), C31(H31), C33(H33)
6.d Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C9(C10,C11,C12,C13,C14), C16(C17,C18,C19,C20,C21),
 C29(C30,C31,C32,C33,C34)
6.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C)
;
_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
Hf1 Hf 0.37528(4) 0.500000 0.41426(5) 0.0498(3) Uani 1 2 d S TU P A .
Hf2 Hf 0.51715(6) 0.44423(5) 0.40718(10) 0.0527(4) Uani 0.8 1 d . . . A 1
Hf3 Hf 0.66048(7) 0.500000 0.38503(9) 0.0545(4) Uani 0.6 2 d S T P A 1
Hf4 Hf 0.44619(15) 0.500000 0.23572(18) 0.0719(7) Uani 0.4 2 d S T P A 2
Hf5 Hf 0.5436(2) 0.4447(2) 0.4259(5) 0.0576(16) Uani 0.2 1 d . . . A 2
O1 O 0.5151(5) 0.3762(3) 0.4409(7) 0.071(3) Uani 1 1 d . . . . .
O2 O 0.4603(8) 0.500000 0.3673(10) 0.081(4) Uani 1 2 d DS T P A .
O3 O 0.4365(6) 0.4446(4) 0.4613(8) 0.095(4) Uani 1 1 d . . . . .
O4 O 0.6099(6) 0.4276(4) 0.3823(9) 0.103(4) Uani 1 1 d . . . . .
O5 O 0.3151(6) 0.4536(4) 0.3577(9) 0.106(4) Uani 1 1 d . U . . .
O6 O 0.7369(7) 0.4561(5) 0.3996(10) 0.117(5) Uani 1 1 d . . . . .
O7 O 0.4687(7) 0.4230(4) 0.2948(7) 0.102(4) Uani 1 1 d . . . . .
O8 O 0.6420(14) 0.500000 0.2607(15) 0.086(7) Uani 0.6 2 d S T P . .
O9 O 0.3060(12) 0.500000 0.4854(13) 0.113(6) Uani 1 2 d S T P A .
O10 O 0.3499(12) 0.500000 0.2754(17) 0.102(3) Uani 0.5 2 d DS TU P A .
O11 O 0.513(2) 0.500000 0.170(4) 0.105(15) Uani 0.4 2 d S T P . .
O12 O 0.5846(10) 0.500000 0.4486(13) 0.103(5) Uani 1 2 d S TU P . .
O13 O 0.3898(14) 0.5450(10) 0.1594(19) 0.109(8) Uani 0.5 1 d . . . . .
N1 N 0.500000 0.3133(6) 0.500000 0.110(8) Uani 1 2 d S T P . .
C1 C 0.500000 0.3578(6) 0.500000 0.083(6) Uani 1 2 d S TU P A .
C2 C 0.1939(18) 0.500000 0.2803(19) 0.112(4) Uani 1 2 d S TU P . .
H2A H 0.214897 0.500000 0.338331 0.134 Uiso 1 2 calc RS T P . .
H2B H 0.146340 0.499999 0.271232 0.134 Uiso 1 2 calc RS T P . .
C3 C 0.4548(8) 0.3847(4) 0.2516(9) 0.115(2) Uani 1 1 d . U . . .
C4 C 0.3985(7) 0.3602(5) 0.2475(9) 0.121(2) Uani 1 1 d G U . . .
C5 C 0.3870(6) 0.3217(4) 0.2030(10) 0.123(2) Uani 1 1 d G U . . .
H5 H 0.349330 0.305311 0.200249 0.147 Uiso 1 1 calc R . . . .
C6 C 0.4319(7) 0.3078(4) 0.1627(9) 0.124(3) Uani 1 1 d DG U . . .
C7 C 0.4882(7) 0.3323(4) 0.1668(9) 0.124(2) Uani 1 1 d G U . . .
H7 H 0.518235 0.322980 0.139838 0.149 Uiso 1 1 calc R . . . .
C8 C 0.4997(7) 0.3708(4) 0.2113(10) 0.119(2) Uani 1 1 d G U . . .
C9 C 0.7885(8) 0.4405(5) 0.4617(9) 0.127(3) Uani 1 1 d . U . . .
C10 C 0.7765(7) 0.4077(5) 0.5113(11) 0.127(3) Uani 1 1 d G U . . .
C11 C 0.8275(9) 0.3925(4) 0.5760(10) 0.131(3) Uani 1 1 d G U . . .
H11 H 0.819458 0.370525 0.609121 0.157 Uiso 1 1 calc R . . . .
C12 C 0.8906(8) 0.4102(5) 0.5911(9) 0.136(3) Uani 1 1 d DG U . . .
C13 C 0.9026(7) 0.4431(5) 0.5415(11) 0.136(3) Uani 1 1 d G U . . .
H13 H 0.944798 0.454923 0.551645 0.163 Uiso 1 1 calc DR . . . .
C14 C 0.8516(10) 0.4582(4) 0.4768(10) 0.132(3) Uani 1 1 d G U . . .
C15 C 0.3482(13) 0.3725(7) 0.2953(14) 0.122(3) Uani 1 1 d . U . . .
H15A H 0.334356 0.345876 0.316036 0.146 Uiso 1 1 calc R . . . .
H15B H 0.371383 0.389994 0.341659 0.146 Uiso 1 1 calc R . . . .
C16 C 0.2705(8) 0.4351(5) 0.2832(7) 0.120(3) Uani 1 1 d . U . . .
C17 C 0.2870(7) 0.3970(5) 0.2498(9) 0.121(2) Uani 1 1 d G U . . .
C18 C 0.2479(8) 0.3826(4) 0.1749(9) 0.125(3) Uani 1 1 d G U . . .
H18 H 0.258926 0.357071 0.152542 0.150 Uiso 1 1 calc R . . . .
C19 C 0.1924(8) 0.4063(5) 0.1334(8) 0.129(3) Uani 1 1 d G U . . .
C20 C 0.1759(7) 0.4444(5) 0.1668(9) 0.127(3) Uani 1 1 d G U . . .
H20 H 0.138787 0.460231 0.139051 0.153 Uiso 1 1 calc R . . . .
C21 C 0.2150(8) 0.4588(4) 0.2417(9) 0.121(3) Uani 1 1 d G U . . .
C22 C 0.7095(13) 0.3854(8) 0.5089(15) 0.125(3) Uani 1 1 d . U . . .
H22A H 0.716142 0.362635 0.549565 0.149 Uiso 1 1 calc R . . . .
H22B H 0.678458 0.406553 0.518865 0.149 Uiso 1 1 calc R . . . .
C23 C 0.856(2) 0.500000 0.423(2) 0.131(4) Uani 1 2 d S TU P . .
H23A H 0.819609 0.500000 0.373659 0.158 Uiso 1 2 calc RS T P . .
H23B H 0.897273 0.499999 0.409065 0.158 Uiso 1 2 calc RS T P . .
C24 C 0.5196(13) 0.2895(6) 0.4366(14) 0.119(6) Uani 1 1 d . U . . .
H24A H 0.493395 0.299259 0.384352 0.179 Uiso 1 1 calc GR . . . .
H24B H 0.512614 0.258862 0.442018 0.179 Uiso 1 1 calc GR . . . .
H24C H 0.565549 0.294765 0.442024 0.179 Uiso 1 1 calc GR . . . .
C25 C 0.5621(12) 0.3937(7) 0.2200(14) 0.120(3) Uani 1 1 d . U . . .
H25A H 0.557092 0.424049 0.232662 0.144 Uiso 1 1 calc R . . . .
H25B H 0.573327 0.392471 0.169141 0.144 Uiso 1 1 calc R . . . .
C26 C 0.9511(12) 0.3902(6) 0.6438(13) 0.138(3) Uani 1 1 d D U . . .
C27 C 0.7941(13) 0.2676(8) 0.3465(14) 0.150(5) Uani 1 1 d D U . . .
H27A H 0.812984 0.295728 0.342630 0.225 Uiso 1 1 calc GR . . . .
H27B H 0.813265 0.246425 0.318857 0.225 Uiso 1 1 calc GR . . . .
H27C H 0.803176 0.259582 0.402526 0.225 Uiso 1 1 calc GR . . . .
C28 C 0.7243(11) 0.2693(7) 0.3103(12) 0.133(3) Uani 1 1 d D U . . .
C29 C 0.6373(8) 0.3889(4) 0.3669(9) 0.117(2) Uani 1 1 d . U . . .
C30 C 0.6846(8) 0.3669(5) 0.4271(7) 0.121(3) Uani 1 1 d G U . . .
C31 C 0.7133(7) 0.3290(5) 0.4084(8) 0.125(2) Uani 1 1 d G U . . .
H31 H 0.744931 0.314330 0.448645 0.150 Uiso 1 1 calc R . . . .
C32 C 0.6948(8) 0.3131(4) 0.3296(9) 0.125(3) Uani 1 1 d G U . . .
C33 C 0.6475(8) 0.3350(5) 0.2694(7) 0.126(2) Uani 1 1 d G U . . .
H33 H 0.635085 0.324385 0.216658 0.151 Uiso 1 1 calc R . . . .
C34 C 0.6188(7) 0.3729(5) 0.2881(8) 0.119(2) Uani 1 1 d G U . . .
C35 C 0.7150(13) 0.2616(8) 0.2257(14) 0.153(5) Uani 1 1 d D U . . .
H35A H 0.717085 0.288755 0.198917 0.230 Uiso 1 1 calc GR . . . .
H35B H 0.672633 0.248267 0.202522 0.230 Uiso 1 1 calc GR . . . .
H35C H 0.749255 0.242527 0.218974 0.230 Uiso 1 1 calc GR . . . .
C36 C 0.4207(8) 0.2668(7) 0.1170(11) 0.129(3) Uani 1 1 d D U . . .
C37 C 0.1447(12) 0.3877(7) 0.0605(15) 0.130(3) Uani 1 1 d D U . . .
C38 C 0.1074(13) 0.3534(8) 0.0729(17) 0.153(5) Uani 1 1 d D U . . .
H38A H 0.132841 0.327089 0.078333 0.230 Uiso 1 1 calc GR . . . .
H38B H 0.068498 0.350844 0.027666 0.230 Uiso 1 1 calc GR . . . .
H38C H 0.094584 0.358274 0.121471 0.230 Uiso 1 1 calc GR . . . .
C39 C 0.6980(13) 0.2319(8) 0.3389(15) 0.155(5) Uani 1 1 d D U . . .
H39A H 0.728689 0.221917 0.388296 0.232 Uiso 1 1 calc GR . . . .
H39B H 0.690872 0.209202 0.298920 0.232 Uiso 1 1 calc GR . . . .
H39C H 0.656721 0.239241 0.348832 0.232 Uiso 1 1 calc GR . . . .
C40 C 0.1020(13) 0.4161(8) 0.0124(17) 0.157(5) Uani 1 1 d D U . . .
H40A H 0.075659 0.429709 0.042796 0.235 Uiso 1 1 calc R . . . .
H40B H 0.126338 0.437906 -0.006957 0.235 Uiso 1 1 calc R . . . .
H40C H 0.073586 0.400669 -0.032799 0.235 Uiso 1 1 calc R . . . .
C41 C 0.1785(13) 0.3709(8) 0.0105(17) 0.157(5) Uani 1 1 d D U . . .
H41A H 0.198573 0.394139 -0.011387 0.236 Uiso 1 1 calc GR . . . .
H41B H 0.148434 0.355209 -0.032884 0.236 Uiso 1 1 calc GR . . . .
H41C H 0.212262 0.351427 0.040686 0.236 Uiso 1 1 calc GR . . . .
C42 C 0.4800(11) 0.2402(7) 0.1245(15) 0.153(5) Uani 1 1 d D U . . .
H42A H 0.517546 0.258891 0.129855 0.230 Uiso 1 1 calc GR . . . .
H42B H 0.473724 0.222354 0.077089 0.230 Uiso 1 1 calc DGR . . . .
H42C H 0.487642 0.221886 0.171505 0.230 Uiso 1 1 calc GR . . . .
C43 C 0.3937(12) 0.2727(8) 0.0294(10) 0.156(5) Uani 1 1 d D U . . .
H43A H 0.349078 0.261927 0.012365 0.234 Uiso 1 1 calc GR . . . .
H43B H 0.420271 0.256924 0.002014 0.234 Uiso 1 1 calc DGR . . . .
H43C H 0.393950 0.303113 0.016532 0.234 Uiso 1 1 calc GR . . . .
C44 C 0.9695(12) 0.3514(7) 0.6059(15) 0.162(5) Uani 1 1 d D U . . .
H44A H 0.932919 0.342565 0.561233 0.243 Uiso 1 1 calc GR . . . .
H44B H 0.980678 0.328253 0.644939 0.243 Uiso 1 1 calc DGR . . . .
H44C H 1.006947 0.357898 0.586635 0.243 Uiso 1 1 calc GR . . . .
C45 C 0.9429(14) 0.3768(8) 0.7216(12) 0.166(5) Uani 1 1 d D U . . .
H45A H 0.969971 0.394841 0.763785 0.249 Uiso 1 1 calc GR . . . .
H45B H 0.956054 0.346938 0.731817 0.249 Uiso 1 1 calc DGR . . . .
H45C H 0.897334 0.379947 0.720522 0.249 Uiso 1 1 calc GR . . . .
C46 C 0.3738(12) 0.2370(6) 0.1373(15) 0.157(5) Uani 1 1 d D U . . .
H46A H 0.387637 0.231170 0.194456 0.235 Uiso 1 1 calc R . . . .
H46B H 0.330608 0.250152 0.122941 0.235 Uiso 1 1 calc R . . . .
H46C H 0.372137 0.210270 0.107991 0.235 Uiso 1 1 calc R . . . .
C47 C 1.0068(10) 0.4204(8) 0.6596(16) 0.170(5) Uani 1 1 d D U . . .
H47A H 1.017266 0.426452 0.610003 0.255 Uiso 1 1 calc DGR . . . .
H47B H 1.044516 0.407560 0.697812 0.255 Uiso 1 1 calc GR . . . .
H47C H 0.995199 0.447004 0.681559 0.255 Uiso 1 1 calc GR . . . .
C48 C 0.331(2) 0.5565(12) 0.138(2) 0.096(8) Uani 0.5 1 d . U . A .
H48A H 0.324793 0.579743 0.099583 0.144 Uiso 0.5 1 calc R . . . .
H48B H 0.303351 0.532207 0.114043 0.144 Uiso 0.5 1 calc R . . . .
H48C H 0.318168 0.566287 0.184770 0.144 Uiso 0.5 1 calc R . . . .


_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
HF5b Hf1 3.271(6) 5_666 ?
Hf1 Hf2 3.4764(16) . ?
HF2a Hf2 3.472(3) 2_656 ?
Hf1 Hf2 3.4764(16) 6_565 ?
HF2a Hf2 3.422(3) 6_565 ?
HF3a Hf2 3.5847(19) 6_565 ?
HF2a Hf3 3.5847(19) . ?
Hf1 Hf5 3.271(6) 5_666 ?
HF5b Hf5 3.543(16) 2_656 ?
Hf1 Hf5 3.271(6) 2_656 ?
HF5b Hf5 3.394(12) 6_565 ?
HF5b O1 2.220(11) . ?
HF2a O1 2.169(9) . ?
HF5b O2 2.443(12) . ?
HF2a O2 2.089(9) . ?
HF4b O2 2.200(17) . ?
Hf1 O2 2.165(17) . ?
HF2a O3 2.197(13) 2_656 ?
HF5b O3 1.867(15) 2_656 ?
HF2a O3 2.158(13) . ?
Hf1 O3 2.148(10) . ?
Hf1 O3 2.148(10) 6_565 ?
HF5b O3 2.499(14) . ?
HF3a O4 2.459(11) . ?
HF2a O4 2.177(11) . ?
HF3a O4 2.459(11) 6_565 ?
HF5b O4 1.840(12) . ?
Hf1 O5 1.969(11) 6_565 ?
Hf1 O5 1.969(11) . ?
HF3a O6 2.059(16) . ?
HF3a O6 2.059(16) 6_565 ?
HF4b O7 2.563(12) 6_565 ?
HF4b O7 2.563(12) . ?
HF2a O7 2.022(11) . ?
HF5b O7 2.450(13) . ?
HF3a O8 2.06(2) . ?
Hf1 O9 2.155(19) . ?
HF3a O9 2.14(2) 5_666 ?
HF4b O10 2.32(3) . ?
Hf1 O10 2.30(3) . ?
HF4b O11 2.04(5) . ?
HF5b O12 1.894(10) . ?
Hf1 O12 2.27(2) 5_666 ?
HF3a O12 2.18(2) . ?
HF2a O12 2.209(13) . ?
HF4b O13 2.04(3) 6_565 ?
HF4b O13 2.04(3) . ?
O1 C1 1.281(13) . ?
O2 Hf2 2.089(9) 6_565 ?
O2 Hf5 2.443(12) 6_565 ?
O3 Hf2 2.197(13) 2_656 ?
O3 Hf5 1.867(15) 2_656 ?
O4 C29 1.379(14) . ?
O5 C16 1.472(16) . ?
O6 C9 1.375(19) . ?
O7 C3 1.376(14) . ?
O9 Hf3 2.14(2) 5_666 ?
O12 Hf1 2.27(2) 5_666 ?
O12 Hf2 2.210(13) 6_565 ?
O12 Hf5 1.894(10) 6_565 ?
O13 C48 1.25(5) . ?
N1 C1 1.37(3) . ?
N1 C24 1.47(2) . ?
N1 C24 1.47(2) 2_656 ?
C1 O1 1.281(13) 2_656 ?
C2 C21 1.55(2) . ?
C2 C21 1.55(3) 6_565 ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 C5 1.3900 . ?
C4 C15 1.56(2) . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C36 1.47(2) . ?
C7 C8 1.3900 . ?
C8 C25 1.46(3) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 C22 1.56(3) . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C26 1.47(3) . ?
C13 C14 1.3900 . ?
C14 C23 1.60(2) . ?
C15 C17 1.51(3) . ?
C16 C17 1.3900 . ?
C16 C21 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C19 C37 1.48(3) . ?
C20 C21 1.3900 . ?
C22 C30 1.47(3) . ?
C23 C14 1.60(3) 6_565 ?
C25 C34 1.55(3) . ?
C26 C44 1.462(13) . ?
C26 C45 1.458(13) . ?
C26 C47 1.458(14) . ?
C27 C28 1.43(2) . ?
C28 C32 1.56(2) . ?
C28 C35 1.43(2) . ?
C28 C39 1.42(2) . ?
C29 C30 1.3900 . ?
C29 C34 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C36 C42 1.467(13) . ?
C36 C43 1.463(13) . ?
C36 C46 1.460(13) . ?
C37 C38 1.37(2) . ?
C37 C40 1.35(2) . ?
C37 C41 1.37(2) . ?

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
HF2a HF2a Hf1 63.99(4) 2_656 . ?
HF2a HF2a Hf1 60.51(3) 6_565 . ?
HF2a HF3a Hf2 57.03(5) . 6_565 ?
O2 Hf1 Hf2 34.5(2) . 6_565 ?
HF2a HF2a Hf2 90.0 6_565 2_656 ?
O2 Hf1 Hf2 34.5(2) . . ?
O2 Hf1 Hf5 91.4(4) . 2_656 ?
O2 Hf1 Hf5 91.4(4) . 5_666 ?
O2 Hf1 O10 65.4(7) . . ?
O2 Hf1 O12 106.6(7) . 5_666 ?
O3 Hf1 Hf2 88.4(4) . 6_565 ?
O3 Hf1 Hf2 88.4(4) 6_565 . ?
O3 Hf1 Hf2 36.2(3) . . ?
HF2a Hf1 Hf2 58.98(5) . 6_565 ?
HF2a HF2a Hf3 61.49(3) 6_565 . ?
HF2a HF2a Hf3 120.02(6) 2_656 . ?
Hf1 HF2a Hf3 121.84(4) . . ?
Hf1 HF5b Hf5 58.75(11) 5_666 6_565 ?
HF5b HF5b Hf5 89.999(1) 6_565 2_656 ?
Hf1 HF5b Hf5 69.4(2) 5_666 2_656 ?
HF5b Hf1 Hf5 62.5(2) 5_666 2_656 ?
HF2a O2 Hf1 109.6(5) . . ?
HF2a O2 Hf1 109.6(5) 6_565 . ?
HF2a O2 Hf2 110.0(7) . 6_565 ?
HF4b O2 Hf5 107.2(6) . 6_565 ?
HF5b O2 Hf5 88.0(6) 6_565 . ?
O3 Hf1 Hf2 36.2(3) 6_565 6_565 ?
O3 Hf1 Hf5 32.7(4) 6_565 5_666 ?
O3 Hf1 Hf5 88.8(4) . 5_666 ?
O3 Hf1 Hf5 32.7(4) . 2_656 ?
O3 Hf1 Hf5 88.8(4) 6_565 2_656 ?
O3 Hf1 O2 70.6(4) . . ?
O3 Hf1 O2 70.6(4) 6_565 . ?
O3 Hf1 O3 104.6(8) . 6_565 ?
O3 Hf1 O9 102.5(5) . . ?
O3 Hf1 O9 102.5(5) 6_565 . ?
O3 Hf1 O10 109.2(5) 6_565 . ?
O3 Hf1 O10 109.2(5) . . ?
O3 Hf1 O12 66.6(4) 6_565 5_666 ?
O3 Hf1 O12 66.6(4) . 5_666 ?
O5 Hf1 Hf2 141.0(5) . 6_565 ?
O5 Hf1 Hf2 93.8(4) . . ?
O5 Hf1 Hf2 93.8(4) 6_565 6_565 ?
O5 Hf1 Hf2 141.0(5) 6_565 . ?
O5 Hf1 Hf5 98.6(4) . 2_656 ?
O5 Hf1 Hf5 98.6(4) 6_565 5_666 ?
O5 Hf1 Hf5 154.1(5) . 5_666 ?
O5 Hf1 Hf5 154.1(5) 6_565 2_656 ?
O5 Hf1 O2 107.5(5) . . ?
O5 Hf1 O2 107.5(5) 6_565 . ?
O5 Hf1 O3 81.2(5) . . ?
O5 Hf1 O3 172.4(6) . 6_565 ?
O5 Hf1 O3 81.2(5) 6_565 6_565 ?
O5 Hf1 O3 172.4(5) 6_565 . ?
O5 Hf1 O5 92.5(7) . 6_565 ?
O5 Hf1 O9 80.6(6) . . ?
O5 Hf1 O9 80.6(6) 6_565 . ?
O5 Hf1 O10 63.8(6) 6_565 . ?
O5 Hf1 O10 63.8(6) . . ?
O5 Hf1 O12 120.7(5) . 5_666 ?
O5 Hf1 O12 120.7(5) 6_565 5_666 ?
O9 Hf1 Hf2 138.4(4) . 6_565 ?
O9 Hf1 Hf2 138.4(4) . . ?
O9 Hf1 Hf5 78.4(5) . 5_666 ?
O9 Hf1 Hf5 78.4(5) . 2_656 ?
O9 Hf1 O2 168.0(8) . . ?
O9 Hf1 O10 126.6(9) . . ?
O9 Hf1 O12 61.4(8) . 5_666 ?
O10 Hf1 Hf2 84.9(6) . . ?
O10 Hf1 Hf2 84.9(6) . 6_565 ?
O10 Hf1 Hf5 141.9(4) . 2_656 ?
O10 Hf1 Hf5 141.9(4) . 5_666 ?
O12 Hf1 Hf2 88.1(4) 5_666 . ?
O12 Hf1 Hf2 88.1(4) 5_666 6_565 ?
O12 Hf1 Hf5 34.3(2) 5_666 2_656 ?
O12 Hf1 Hf5 34.3(2) 5_666 5_666 ?
O12 Hf1 O10 172.0(9) 5_666 . ?
C1 O1 Hf2 131.7(10) . . ?
C1 O1 Hf5 130.2(10) . . ?
Hf1 O2 Hf4 120.0(7) . . ?
Hf1 O2 Hf5 114.8(6) . 6_565 ?
Hf1 O2 Hf5 114.8(6) . . ?
HF4b O2 Hf5 107.2(6) . . ?
HF5b O3 Hf1 108.9(6) 2_656 . ?
HF2a O3 Hf2 105.7(5) . 2_656 ?
Hf1 O3 Hf2 107.7(5) . . ?
Hf1 O3 Hf2 115.9(6) . 2_656 ?
Hf1 O3 Hf5 113.2(5) . . ?
HF5b O3 Hf5 107.6(6) 2_656 . ?
C29 O4 Hf2 133.5(10) . . ?
C29 O4 Hf3 125.4(9) . . ?
C29 O4 Hf5 137.1(11) . . ?
HF2a O4 Hf3 101.1(4) . . ?
C16 O5 Hf1 150.6(12) . . ?
C9 O6 Hf3 137.7(13) . . ?
C3 O7 Hf2 139.8(10) . . ?
HF5b O7 Hf4 96.5(4) . . ?
HF3a O9 Hf1 121.1(11) 5_666 . ?
HF5b O12 Hf1 103.2(7) 6_565 5_666 ?
HF5b O12 Hf1 103.2(7) . 5_666 ?
HF2a O12 Hf1 110.5(6) 6_565 5_666 ?
HF3a O12 Hf1 114.4(9) . 5_666 ?
HF2a O12 Hf1 110.5(6) . 5_666 ?
HF3a O12 Hf2 109.5(7) . . ?
HF2a O12 Hf2 101.5(8) . 6_565 ?
HF3a O12 Hf2 109.5(7) . 6_565 ?
HF5b O12 Hf5 127.3(11) 6_565 . ?
O1 HF5b Hf1 119.2(4) . 5_666 ?
O1 HF2a Hf1 112.4(3) . . ?
O1 HF2a Hf2 74.2(3) . 2_656 ?
O1 HF2a Hf2 164.1(3) . 6_565 ?
O1 HF2a Hf3 124.7(3) . . ?
O1 HF5b Hf5 161.1(3) . 6_565 ?
O1 HF5b Hf5 72.7(3) . 2_656 ?
O1 HF5b O2 121.2(4) . . ?
O1 HF5b O3 71.2(4) . . ?
C3 O7 Hf4 125.8(10) . . ?
C3 O7 Hf5 135.4(10) . . ?
Hf1 O10 Hf4 110.0(9) . . ?
C48 O13 Hf4 137(3) . . ?
C1 N1 C24 119.9(10) . 2_656 ?
C1 N1 C24 119.9(10) . . ?
C24 N1 C24 120(2) 2_656 . ?
O1 HF2a O3 76.5(4) . 2_656 ?
O1 HF2a O4 85.1(5) . . ?
O1 HF5b O7 74.0(4) . . ?
O1 HF2a O12 135.9(5) . . ?
O1 C1 O1 127.7(17) 2_656 . ?
O1 C1 N1 116.1(8) . . ?
O1 C1 N1 116.1(8) 2_656 . ?
O2 HF2a Hf1 35.9(5) . . ?
C21 C2 C21 109(3) . 6_565 ?
O7 C3 C4 122.5(11) . . ?
O7 C3 C8 117.5(11) . . ?
O2 HF5b Hf1 97.4(4) . 5_666 ?
O2 HF2a Hf2 35.0(4) . 6_565 ?
C4 C3 C8 120.0 . . ?
C3 C4 C15 122.6(13) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C15 117.3(13) . . ?
C4 C5 C6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C36 120.2(10) . . ?
C7 C6 C36 119.7(10) . . ?
C8 C7 C6 120.0 . . ?
C3 C8 C25 121.4(12) . . ?
C7 C8 C3 120.0 . . ?
C7 C8 C25 118.4(12) . . ?
O6 C9 C10 119.2(15) . . ?
O6 C9 C14 120.8(15) . . ?
C10 C9 C14 120.0 . . ?
C9 C10 C22 128.6(16) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 C22 111.3(16) . . ?
C10 C11 C12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C26 124.5(12) . . ?
C13 C12 C26 113.8(12) . . ?
C14 C13 C12 120.0 . . ?
C9 C14 C23 114(2) . . ?
C13 C14 C9 120.0 . . ?
C13 C14 C23 125(2) . . ?
C17 C15 C4 117.1(18) . . ?
C17 C16 O5 120.9(11) . . ?
C17 C16 C21 120.0 . . ?
C21 C16 O5 118.8(11) . . ?
C16 C17 C15 118.8(13) . . ?
O2 HF2a Hf2 93.0(5) . 2_656 ?
O2 HF2a Hf3 89.7(4) . . ?
O2 HF5b Hf5 46.0(3) . 6_565 ?
O2 HF5b Hf5 80.7(4) . 2_656 ?
O2 HF2a O1 145.3(5) . . ?
O2 HF5b O3 60.6(5) . . ?
O2 HF2a O3 112.3(6) . 2_656 ?
O2 HF2a O3 71.9(5) . . ?
O2 HF2a O4 126.2(6) . . ?
O2 HF4b O7 68.6(3) . . ?
O2 HF4b O7 68.6(3) . 6_565 ?
O2 HF5b O7 67.0(4) . . ?
O2 HF4b O10 64.5(6) . . ?
O2 HF2a O12 74.2(6) . . ?
O3 HF5b Hf1 38.4(3) 2_656 5_666 ?
O3 HF2a Hf1 95.5(4) 2_656 . ?
O3 HF2a Hf1 36.1(3) . . ?
O3 HF5b Hf1 95.0(4) . 5_666 ?
O3 HF2a Hf2 89.7(3) . 6_565 ?
O3 HF2a Hf2 89.7(3) 2_656 6_565 ?
O3 HF2a Hf2 36.7(3) 2_656 2_656 ?
O3 HF2a Hf2 37.5(3) . 2_656 ?
O3 HF2a Hf3 146.5(4) . . ?
O3 HF2a Hf3 88.1(3) 2_656 . ?
O3 HF5b Hf5 30.1(3) . 2_656 ?
O3 HF5b Hf5 90.1(3) . 6_565 ?
O3 HF5b Hf5 42.2(4) 2_656 2_656 ?
O3 HF5b Hf5 90.1(4) 2_656 6_565 ?
O3 HF5b O1 82.3(5) 2_656 . ?
O3 HF2a O1 79.1(4) . . ?
O3 HF5b O2 110.7(7) 2_656 . ?
O3 HF2a O3 74.3(5) . 2_656 ?
O3 HF5b O3 72.4(6) 2_656 . ?
O3 HF2a O4 161.4(5) . . ?
O3 HF5b O7 148.6(6) 2_656 . ?
O3 HF5b O12 80.3(8) 2_656 . ?
O3 HF2a O12 66.8(6) 2_656 . ?
O3 HF2a O12 111.7(6) . . ?
O4 HF2a Hf1 162.0(4) . . ?
O4 HF5b Hf1 102.5(4) . 5_666 ?
O4 HF3a Hf2 36.6(2) 6_565 6_565 ?
O4 HF3a Hf2 93.4(3) . 6_565 ?
O4 HF2a Hf2 127.9(4) . 2_656 ?
O4 HF2a Hf2 103.6(3) . 6_565 ?
O4 HF3a Hf2 36.6(2) . . ?
O4 HF3a Hf2 93.4(3) 6_565 . ?
O4 HF2a Hf3 42.3(3) . . ?
O4 HF5b Hf5 154.6(6) . 2_656 ?
O4 HF5b Hf5 106.6(4) . 6_565 ?
O4 HF5b O1 92.3(5) . . ?
O4 HF5b O2 124.7(8) . . ?
O4 HF5b O3 116.9(7) . 2_656 ?
O4 HF5b O3 160.4(5) . . ?
O4 HF2a O3 92.5(5) . 2_656 ?
O4 HF3a O4 129.2(5) . 6_565 ?
O4 HF5b O7 84.9(6) . . ?
O4 HF2a O12 73.4(5) . . ?
O4 HF5b O12 89.2(7) . . ?
O6 HF3a Hf2 109.2(4) . . ?
O6 HF3a Hf2 109.2(4) 6_565 6_565 ?
O6 HF3a Hf2 162.3(4) . 6_565 ?
O6 HF3a Hf2 162.3(4) 6_565 . ?
O6 HF3a O4 74.4(5) 6_565 6_565 ?
O6 HF3a O4 155.9(5) . 6_565 ?
O6 HF3a O4 155.9(5) 6_565 . ?
O6 HF3a O4 74.4(5) . . ?
O6 HF3a O6 81.7(8) 6_565 . ?
O6 HF3a O8 92.1(8) 6_565 . ?
O6 HF3a O8 92.1(8) . . ?
O6 HF3a O9 81.9(6) 6_565 5_666 ?
O6 HF3a O9 81.9(6) . 5_666 ?
O6 HF3a O12 126.8(5) . . ?
O6 HF3a O12 126.8(5) 6_565 . ?
O7 HF5b Hf1 164.1(3) . 5_666 ?
O7 HF2a Hf1 89.3(3) . . ?
O7 HF2a Hf2 134.5(5) . 2_656 ?
O7 HF2a Hf2 108.8(3) . 6_565 ?
O7 HF2a Hf3 105.3(5) . . ?
O7 HF5b Hf5 109.5(4) . 2_656 ?
O7 HF5b Hf5 105.8(3) . 6_565 ?
O7 HF2a O1 84.4(5) . . ?
O7 HF2a O2 82.2(5) . . ?
O7 HF2a O3 99.8(6) . . ?
O7 HF2a O3 160.7(5) . 2_656 ?
O7 HF5b O3 80.5(5) . . ?
O7 HF2a O4 88.5(5) . . ?
O7 HF4b O7 134.4(5) . 6_565 ?
O7 HF2a O12 131.5(7) . . ?
O8 HF3a Hf2 101.2(7) . . ?
O8 HF3a Hf2 101.2(7) . 6_565 ?
O8 HF3a O4 91.5(5) . . ?
O8 HF3a O4 91.5(5) . 6_565 ?
O8 HF3a O9 172.0(10) . 5_666 ?
O8 HF3a O12 124.9(10) . . ?
O9 HF3a Hf2 85.8(5) 5_666 6_565 ?
O9 HF3a Hf2 85.8(5) 5_666 . ?
O9 HF3a O4 91.9(4) 5_666 6_565 ?
O9 HF3a O4 91.9(4) 5_666 . ?
O9 HF3a O12 63.1(8) 5_666 . ?
O10 HF4b O7 87.8(4) . 6_565 ?
O10 HF4b O7 87.8(4) . . ?
O11 HF4b O2 131.2(17) . . ?
O11 HF4b O7 98.1(7) . 6_565 ?
O11 HF4b O7 98.1(7) . . ?
O11 HF4b O10 164.3(17) . . ?
O12 HF5b Hf1 42.5(6) . 5_666 ?
C16 C17 C18 120.0 . . ?
C18 C17 C15 121.2(13) . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C37 120.3(13) . . ?
C20 C19 C37 119.0(13) . . ?
C19 C20 C21 120.0 . . ?
C16 C21 C2 120.5(17) . . ?
C20 C21 C2 119.4(17) . . ?
C20 C21 C16 120.0 . . ?
C30 C22 C10 105.5(17) . . ?
C14 C23 C14 107(3) . 6_565 ?
C8 C25 C34 110.9(18) . . ?
C44 C26 C12 111.0(15) . . ?
C45 C26 C12 112.1(15) . . ?
C45 C26 C44 107.3(15) . . ?
C45 C26 C47 107.8(16) . . ?
C47 C26 C12 111.1(15) . . ?
C47 C26 C44 107.4(16) . . ?
C27 C28 C32 111.2(19) . . ?
C27 C28 C35 105.3(15) . . ?
C35 C28 C32 114(2) . . ?
C39 C28 C27 106.0(16) . . ?
C39 C28 C32 113.9(19) . . ?
C39 C28 C35 105.4(15) . . ?
O4 C29 C30 121.7(12) . . ?
O4 C29 C34 118.3(12) . . ?
C30 C29 C34 120.0 . . ?
C29 C30 C22 120.8(14) . . ?
C29 C30 C31 120.0 . . ?
C31 C30 C22 119.0(14) . . ?
C32 C31 C30 120.0 . . ?
C31 C32 C28 119.6(12) . . ?
C33 C32 C28 120.3(12) . . ?
C33 C32 C31 120.0 . . ?
C32 C33 C34 120.0 . . ?
C29 C34 C25 122.4(12) . . ?
C33 C34 C25 117.4(12) . . ?
C33 C34 C29 120.0 . . ?
C42 C36 C6 115.3(14) . . ?
C43 C36 C6 113.7(14) . . ?
C43 C36 C42 103.4(14) . . ?
C46 C36 C6 115.0(13) . . ?
C46 C36 C42 104.5(15) . . ?
C46 C36 C43 103.5(15) . . ?
C38 C37 C19 116(2) . . ?
C40 C37 C19 116(2) . . ?
C40 C37 C38 106.2(18) . . ?
C40 C37 C41 103.4(18) . . ?
C41 C37 C19 109(2) . . ?
C41 C37 C38 103.5(17) . . ?
O12 HF2a Hf1 95.1(4) . . ?
O12 HF2a Hf2 89.2(5) . 2_656 ?
O12 HF3a Hf2 35.5(3) . . ?
O12 HF2a Hf2 39.2(4) . 6_565 ?
O12 HF3a Hf2 35.5(3) . 6_565 ?
O12 HF2a Hf3 35.0(5) . . ?
O12 HF5b Hf5 98.7(7) . 2_656 ?
O12 HF5b Hf5 26.4(6) . 6_565 ?
O12 HF5b O1 161.2(8) . . ?
O12 HF5b O2 72.2(7) . . ?
O12 HF5b O3 110.0(7) . . ?
O12 HF3a O4 68.5(3) . 6_565 ?
O12 HF3a O4 68.5(3) . . ?
O12 HF5b O7 124.8(8) . . ?
O13 HF4b O2 123.2(8) 6_565 . ?
O13 HF4b O2 123.2(8) . . ?
O13 HF4b O7 68.9(9) . 6_565 ?
O13 HF4b O7 68.9(9) 6_565 . ?
O13 HF4b O7 152.6(8) 6_565 6_565 ?
O13 HF4b O7 152.6(8) . . ?
O13 HF4b O10 78.0(9) 6_565 . ?
O13 HF4b O10 78.0(9) . . ?
O13 HF4b O11 90.6(14) 6_565 . ?
O13 HF4b O11 90.6(14) . . ?
O13 HF4b O13 85.2(16) . 6_565 ?

_olex2_submission_special_instructions 'No special instructions were received'
