# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 1816364'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2015-11-11
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C32 H30 N2 O6 Zr'
_chemical_formula_sum            'C32 H30 N2 O6 Zr'
_chemical_formula_weight         629.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H62 N2 O10 Zr2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.7739(3)
_cell_length_b                   11.5955(4)
_cell_length_c                   12.7567(4)
_cell_angle_alpha                95.728(3)
_cell_angle_beta                 101.347(3)
_cell_angle_gamma                90.395(3)
_cell_volume                     1409.90(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    45964
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.0710
_cell_measurement_theta_min      2.9020
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             648
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0543
0 1 0 0.0543
0 2 -5 0.1429
0 -2 5 0.1429
-1 0 0 0.1125
1 0 0 0.1125

_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.109
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0001 -0.9991 -0.0009 -0.0011 -0.0524 -0.0320
0.0001 0.9991 0.0009 0.0011 0.0524 0.0320
0.0023 2.0020 -4.9975 0.2455 0.0003 0.1695
-0.0023 -2.0020 4.9975 -0.2455 -0.0003 -0.1695
-0.9994 0.0004 -0.0006 0.0495 0.0261 -0.0485
0.9994 -0.0004 0.0006 -0.0495 -0.0261 0.0485

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            83215
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         2.727
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00   8.00   1.00    2.30    --  -17.00 -57.00 -60.00   93
  2  ω    -42.00  51.00   1.00    2.30    --  -17.00  57.00  60.00   93
  3  ω    -91.00 -39.00   1.00    2.30    --  -17.00 154.00 -30.47   52
  4  ω    -88.00   4.00   1.00    2.30    --  -17.00 -38.00  30.00   92
  5  ω    -13.00  89.00   1.00    2.30    --   17.39  77.00-180.00  102
  6  ω    -20.00  56.00   1.00    2.30    --   17.39 -99.00 -30.00   76
  7  ω    -13.00  89.00   1.00    2.30    --   17.39  77.00 -60.00  102
  8  ω    -20.00  56.00   1.00    2.30    --   17.39 -99.00 150.00   76
  9  ω    -54.00  48.00   1.00    2.30    --   17.39 -77.00-150.00  102
 10  ω    -91.00 -39.00   1.00    2.30    --  -17.00 154.00-116.26   52
 11  ω    -89.00 -37.00   1.00    2.30    --  -17.00 152.00 164.37   52
 12  ω    -76.00 -29.00   1.00    2.30    --  -17.00 133.00 121.11   47
 13  ω    -83.00 -34.00   1.00    2.30    --  -17.00 144.00  45.34   49
 14  ω    -88.00   4.00   1.00    2.30    --  -17.00 -38.00-180.00   92
 15  ω    -86.00 -35.00   1.00    2.30    --  -17.00 148.00-128.47   51
 16  ω    -54.00  38.00   1.00    2.30    --   17.39 -38.00 -60.00   92
 17  ω    -88.00 -37.00   1.00    2.30    --  -17.00 151.00 -67.51   51
 18  ω    -47.00  54.00   1.00    2.30    --  -17.00  77.00  90.00  101
 19  ω    -20.00  56.00   1.00    2.30    --   17.39 -99.00-150.00   76
 20  ω    -68.00 103.00   1.00    2.30    --   17.39   0.00-180.00  171
 21  ω    -68.00 103.00   1.00    2.30    --   17.39   0.00-150.00  171
 22  ω    -68.00   5.00   1.00    2.30    --   17.39   0.00-120.00   73
 23  ω     -3.00  68.00   1.00    2.30    --   17.39-119.00 167.38   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0494595000
_diffrn_orient_matrix_UB_12      0.0011878000
_diffrn_orient_matrix_UB_13      -0.0486692000
_diffrn_orient_matrix_UB_21      -0.0261430000
_diffrn_orient_matrix_UB_22      0.0524258000
_diffrn_orient_matrix_UB_23      0.0209228000
_diffrn_orient_matrix_UB_31      0.0485054000
_diffrn_orient_matrix_UB_32      0.0320861000
_diffrn_orient_matrix_UB_33      -0.0210483000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7654
_reflns_number_total             8218
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0245
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+0.7734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0623
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.37025(2) 0.74627(2) 0.73255(2) 0.01283(4) Uani 1 1 d . . . . .
O1 O 0.45126(9) 0.81328(7) 0.88705(7) 0.01667(16) Uani 1 1 d . . . . .
O2 O 0.65785(9) 0.49908(7) 0.92528(7) 0.01621(16) Uani 1 1 d . . . . .
O3 O 0.27443(9) 0.61248(7) 0.62693(7) 0.01611(16) Uani 1 1 d . . . . .
O4 O 0.02301(9) 0.55991(8) 0.85084(7) 0.01755(17) Uani 1 1 d . . . . .
O5 O 0.24796(10) 0.87127(8) 0.69093(8) 0.02102(18) Uani 1 1 d . . . . .
O6 O 0.52433(9) 0.77604(8) 0.66220(7) 0.01751(17) Uani 1 1 d . . . . .
N1 N 0.51164(10) 0.59430(8) 0.80662(8) 0.01382(18) Uani 1 1 d . . . . .
N2 N 0.18900(10) 0.67736(9) 0.81588(8) 0.01498(18) Uani 1 1 d . . . . .
C1 C 0.51173(12) 0.78539(10) 0.98332(10) 0.0153(2) Uani 1 1 d . . . . .
C2 C 0.51688(13) 0.86599(11) 1.07412(10) 0.0192(2) Uani 1 1 d . . . . .
H2 H 0.4769 0.9379 1.0659 0.023 Uiso 1 1 calc R U . . .
C3 C 0.58046(13) 0.83986(12) 1.17530(10) 0.0209(2) Uani 1 1 d . . . . .
H3 H 0.5820 0.8942 1.2343 0.025 Uiso 1 1 calc R U . . .
C4 C 0.64255(13) 0.73278(12) 1.19033(10) 0.0202(2) Uani 1 1 d . . . . .
H4 H 0.6858 0.7161 1.2586 0.024 Uiso 1 1 calc R U . . .
C5 C 0.63873(12) 0.65245(11) 1.10247(10) 0.0171(2) Uani 1 1 d . . . . .
H5 H 0.6797 0.5811 1.1119 0.021 Uiso 1 1 calc R U . . .
C6 C 0.57361(12) 0.67691(10) 0.99849(9) 0.0146(2) Uani 1 1 d . . . . .
C7 C 0.57527(12) 0.59260(10) 0.90734(9) 0.0138(2) Uani 1 1 d . . . . .
C8 C 0.64588(12) 0.43682(10) 0.82563(10) 0.0155(2) Uani 1 1 d . . . . .
C9 C 0.70754(13) 0.33359(11) 0.80099(11) 0.0191(2) Uani 1 1 d . . . . .
H9 H 0.7651 0.2955 0.8529 0.023 Uiso 1 1 calc R U . . .
C10 C 0.67737(13) 0.29063(11) 0.69315(11) 0.0207(2) Uani 1 1 d . . . . .
H10 H 0.7155 0.2210 0.6719 0.025 Uiso 1 1 calc R U . . .
C11 C 0.59118(13) 0.34904(11) 0.61518(11) 0.0198(2) Uani 1 1 d . . . . .
H11 H 0.5746 0.3179 0.5437 0.024 Uiso 1 1 calc R U . . .
C12 C 0.53001(13) 0.45281(11) 0.64296(10) 0.0171(2) Uani 1 1 d . . . . .
H12 H 0.4732 0.4920 0.5915 0.021 Uiso 1 1 calc R U . . .
C13 C 0.55757(12) 0.49541(10) 0.75128(10) 0.0144(2) Uani 1 1 d . . . . .
C14 C 0.19228(12) 0.51912(10) 0.61635(10) 0.0154(2) Uani 1 1 d . . . . .
C15 C 0.17706(13) 0.44076(11) 0.52281(10) 0.0193(2) Uani 1 1 d . . . . .
H15 H 0.2262 0.4544 0.4696 0.023 Uiso 1 1 calc R U . . .
C16 C 0.09013(14) 0.34400(12) 0.50913(11) 0.0221(3) Uani 1 1 d . . . . .
H16 H 0.0812 0.2935 0.4467 0.027 Uiso 1 1 calc R U . . .
C17 C 0.01522(14) 0.32064(11) 0.58757(11) 0.0225(3) Uani 1 1 d . . . . .
H17 H -0.0427 0.2548 0.5776 0.027 Uiso 1 1 calc R U . . .
C18 C 0.02776(13) 0.39594(11) 0.67996(11) 0.0197(2) Uani 1 1 d . . . . .
H18 H -0.0222 0.3809 0.7323 0.024 Uiso 1 1 calc R U . . .
C19 C 0.11590(12) 0.49569(10) 0.69549(10) 0.0156(2) Uani 1 1 d . . . . .
C20 C 0.11671(12) 0.57943(10) 0.78718(9) 0.0151(2) Uani 1 1 d . . . . .
C21 C 0.03408(12) 0.65745(11) 0.92346(10) 0.0170(2) Uani 1 1 d . . . . .
C22 C 0.13527(12) 0.73165(11) 0.90244(10) 0.0159(2) Uani 1 1 d . . . . .
C23 C 0.16061(13) 0.84092(11) 0.95953(10) 0.0186(2) Uani 1 1 d . . . . .
H23 H 0.2273 0.8923 0.9464 0.022 Uiso 1 1 calc R U . . .
C24 C 0.08090(14) 0.86949(12) 1.03737(11) 0.0214(2) Uani 1 1 d . . . . .
H24 H 0.0946 0.9419 1.0769 0.026 Uiso 1 1 calc R U . . .
C25 C -0.01937(14) 0.79201(12) 1.05771(11) 0.0225(3) Uani 1 1 d . . . . .
H25 H -0.0700 0.8143 1.1105 0.027 Uiso 1 1 calc R U . . .
C26 C -0.04487(13) 0.68288(12) 1.00101(10) 0.0207(2) Uani 1 1 d . . . . .
H26 H -0.1105 0.6306 1.0143 0.025 Uiso 1 1 calc R U . . .
C27 C 0.14496(13) 0.93649(10) 0.63274(10) 0.0179(2) Uani 1 1 d . . . . .
H27 H 0.0717 0.8830 0.5908 0.021 Uiso 1 1 calc R U . . .
C28 C 0.20816(15) 1.00126(13) 0.55523(11) 0.0265(3) Uani 1 1 d . . . . .
H28A H 0.2771 1.0569 0.5951 0.040 Uiso 1 1 calc R U . . .
H28B H 0.1361 1.0406 0.5110 0.040 Uiso 1 1 calc R U . . .
H28C H 0.2513 0.9472 0.5106 0.040 Uiso 1 1 calc R U . . .
C29 C 0.08060(14) 1.01665(12) 0.70976(12) 0.0239(3) Uani 1 1 d . . . . .
H29A H 0.0436 0.9718 0.7576 0.036 Uiso 1 1 calc R U . . .
H29B H 0.0068 1.0582 0.6698 0.036 Uiso 1 1 calc R U . . .
H29C H 0.1506 1.0707 0.7506 0.036 Uiso 1 1 calc R U . . .
C30 C 0.65753(12) 0.82238(11) 0.65972(10) 0.0177(2) Uani 1 1 d . . . . .
H30 H 0.6754 0.8061 0.5868 0.021 Uiso 1 1 calc R U . . .
C31 C 0.65921(15) 0.95318(12) 0.68778(13) 0.0278(3) Uani 1 1 d . . . . .
H31A H 0.5898 0.9868 0.6364 0.042 Uiso 1 1 calc R U . . .
H31B H 0.7496 0.9851 0.6863 0.042 Uiso 1 1 calc R U . . .
H31C H 0.6393 0.9702 0.7584 0.042 Uiso 1 1 calc R U . . .
C32 C 0.76892(14) 0.76555(13) 0.73724(12) 0.0256(3) Uani 1 1 d . . . . .
H32A H 0.7528 0.7815 0.8090 0.038 Uiso 1 1 calc R U . . .
H32B H 0.8593 0.7960 0.7338 0.038 Uiso 1 1 calc R U . . .
H32C H 0.7650 0.6833 0.7178 0.038 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.0461(9) . ?
Zr1 O3 2.0410(9) . ?
Zr1 O5 1.9337(9) . ?
Zr1 O6 1.9440(9) . ?
Zr1 N1 2.4000(10) . ?
Zr1 N2 2.4078(10) . ?
O1 C1 1.3261(14) . ?
O2 C7 1.3670(14) . ?
O2 C8 1.3814(14) . ?
O3 C14 1.3233(14) . ?
O4 C20 1.3696(14) . ?
O4 C21 1.3779(15) . ?
O5 C27 1.4017(15) . ?
O6 C30 1.4122(14) . ?
N1 C7 1.3148(15) . ?
N1 C13 1.4089(15) . ?
N2 C20 1.3141(16) . ?
N2 C22 1.4091(15) . ?
C1 C2 1.4064(17) . ?
C1 C6 1.4136(16) . ?
C2 H2 0.9300 . ?
C2 C3 1.3816(18) . ?
C3 H3 0.9300 . ?
C3 C4 1.3996(19) . ?
C4 H4 0.9300 . ?
C4 C5 1.3784(18) . ?
C5 H5 0.9300 . ?
C5 C6 1.4107(16) . ?
C6 C7 1.4453(16) . ?
C8 C9 1.3799(16) . ?
C8 C13 1.3859(16) . ?
C9 H9 0.9300 . ?
C9 C10 1.3889(19) . ?
C10 H10 0.9300 . ?
C10 C11 1.4036(19) . ?
C11 H11 0.9300 . ?
C11 C12 1.3925(17) . ?
C12 H12 0.9300 . ?
C12 C13 1.3933(17) . ?
C14 C15 1.4084(17) . ?
C14 C19 1.4137(17) . ?
C15 H15 0.9300 . ?
C15 C16 1.3786(18) . ?
C16 H16 0.9300 . ?
C16 C17 1.3966(19) . ?
C17 H17 0.9300 . ?
C17 C18 1.3794(18) . ?
C18 H18 0.9300 . ?
C18 C19 1.4116(17) . ?
C19 C20 1.4425(16) . ?
C21 C22 1.3889(17) . ?
C21 C26 1.3807(17) . ?
C22 C23 1.3919(17) . ?
C23 H23 0.9300 . ?
C23 C24 1.3947(17) . ?
C24 H24 0.9300 . ?
C24 C25 1.403(2) . ?
C25 H25 0.9300 . ?
C25 C26 1.3887(19) . ?
C26 H26 0.9300 . ?
C27 H27 0.9800 . ?
C27 C28 1.5183(19) . ?
C27 C29 1.5146(18) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30 0.9800 . ?
C30 C31 1.5224(18) . ?
C30 C32 1.5211(19) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 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 N1 76.10(3) . . ?
O1 Zr1 N2 82.05(3) . . ?
O3 Zr1 O1 149.72(3) . . ?
O3 Zr1 N1 82.73(3) . . ?
O3 Zr1 N2 75.56(3) . . ?
O5 Zr1 O1 98.23(4) . . ?
O5 Zr1 O3 100.50(4) . . ?
O5 Zr1 O6 101.37(4) . . ?
O5 Zr1 N1 172.34(4) . . ?
O5 Zr1 N2 86.62(4) . . ?
O6 Zr1 O1 101.02(4) . . ?
O6 Zr1 O3 98.36(4) . . ?
O6 Zr1 N1 84.91(4) . . ?
O6 Zr1 N2 170.84(4) . . ?
N1 Zr1 N2 87.49(3) . . ?
C1 O1 Zr1 143.59(8) . . ?
C7 O2 C8 104.94(9) . . ?
C14 O3 Zr1 144.31(8) . . ?
C20 O4 C21 104.84(9) . . ?
C27 O5 Zr1 161.98(9) . . ?
C30 O6 Zr1 153.37(8) . . ?
C7 N1 Zr1 126.54(8) . . ?
C7 N1 C13 105.08(10) . . ?
C13 N1 Zr1 128.02(8) . . ?
C20 N2 Zr1 126.09(8) . . ?
C20 N2 C22 105.19(10) . . ?
C22 N2 Zr1 128.71(8) . . ?
O1 C1 C2 119.64(11) . . ?
O1 C1 C6 122.25(11) . . ?
C2 C1 C6 118.11(11) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 120.95(12) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 120.99(12) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.5 . . ?
C5 C4 C3 119.04(12) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.97(12) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 120.25(11) . . ?
C5 C6 C1 119.93(11) . . ?
C5 C6 C7 119.77(11) . . ?
O2 C7 C6 116.87(10) . . ?
N1 C7 O2 113.95(10) . . ?
N1 C7 C6 129.13(11) . . ?
O2 C8 C13 108.03(10) . . ?
C9 C8 O2 127.64(11) . . ?
C9 C8 C13 124.32(12) . . ?
C8 C9 H9 122.4 . . ?
C8 C9 C10 115.18(12) . . ?
C10 C9 H9 122.4 . . ?
C9 C10 H10 119.0 . . ?
C9 C10 C11 122.09(11) . . ?
C11 C10 H10 119.0 . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.22(12) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 121.5 . . ?
C11 C12 C13 117.07(11) . . ?
C13 C12 H12 121.5 . . ?
C8 C13 N1 107.98(10) . . ?
C8 C13 C12 120.08(11) . . ?
C12 C13 N1 131.94(11) . . ?
O3 C14 C15 119.73(11) . . ?
O3 C14 C19 122.14(11) . . ?
C15 C14 C19 118.11(11) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.78(12) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 121.07(12) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 H17 120.3 . . ?
C18 C17 C16 119.48(12) . . ?
C18 C17 H17 120.3 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.39(12) . . ?
C19 C18 H18 119.8 . . ?
C14 C19 C20 120.02(11) . . ?
C18 C19 C14 120.17(11) . . ?
C18 C19 C20 119.51(11) . . ?
O4 C20 C19 116.65(10) . . ?
N2 C20 O4 113.90(10) . . ?
N2 C20 C19 129.29(11) . . ?
O4 C21 C22 108.25(10) . . ?
O4 C21 C26 127.30(12) . . ?
C26 C21 C22 124.36(12) . . ?
C21 C22 N2 107.72(11) . . ?
C21 C22 C23 120.20(11) . . ?
C23 C22 N2 131.95(11) . . ?
C22 C23 H23 121.7 . . ?
C22 C23 C24 116.62(12) . . ?
C24 C23 H23 121.7 . . ?
C23 C24 H24 119.1 . . ?
C23 C24 C25 121.85(12) . . ?
C25 C24 H24 119.1 . . ?
C24 C25 H25 119.1 . . ?
C26 C25 C24 121.72(12) . . ?
C26 C25 H25 119.1 . . ?
C21 C26 C25 115.24(12) . . ?
C21 C26 H26 122.4 . . ?
C25 C26 H26 122.4 . . ?
O5 C27 H27 108.3 . . ?
O5 C27 C28 109.39(10) . . ?
O5 C27 C29 109.65(11) . . ?
C28 C27 H27 108.3 . . ?
C29 C27 H27 108.3 . . ?
C29 C27 C28 112.67(11) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O6 C30 H30 108.8 . . ?
O6 C30 C31 109.15(10) . . ?
O6 C30 C32 109.93(10) . . ?
C31 C30 H30 108.8 . . ?
C32 C30 H30 108.8 . . ?
C32 C30 C31 111.40(12) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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 C2 -163.64(10) . . . . ?
Zr1 O1 C1 C6 17.1(2) . . . . ?
Zr1 O3 C14 C15 -168.15(10) . . . . ?
Zr1 O3 C14 C19 13.1(2) . . . . ?
Zr1 O5 C27 C28 -87.5(3) . . . . ?
Zr1 O5 C27 C29 148.4(2) . . . . ?
Zr1 O6 C30 C31 -59.5(2) . . . . ?
Zr1 O6 C30 C32 63.0(2) . . . . ?
Zr1 N1 C7 O2 -175.06(7) . . . . ?
Zr1 N1 C7 C6 2.31(17) . . . . ?
Zr1 N1 C13 C8 175.14(7) . . . . ?
Zr1 N1 C13 C12 -4.49(18) . . . . ?
Zr1 N2 C20 O4 177.93(7) . . . . ?
Zr1 N2 C20 C19 -6.78(18) . . . . ?
Zr1 N2 C22 C21 -178.73(8) . . . . ?
Zr1 N2 C22 C23 5.51(19) . . . . ?
O1 C1 C2 C3 -179.32(11) . . . . ?
O1 C1 C6 C5 178.89(11) . . . . ?
O1 C1 C6 C7 1.32(17) . . . . ?
O2 C8 C9 C10 -179.72(11) . . . . ?
O2 C8 C13 N1 -1.38(13) . . . . ?
O2 C8 C13 C12 178.30(10) . . . . ?
O3 C14 C15 C16 -178.83(12) . . . . ?
O3 C14 C19 C18 178.96(11) . . . . ?
O3 C14 C19 C20 5.26(18) . . . . ?
O4 C21 C22 N2 -0.92(13) . . . . ?
O4 C21 C22 C23 175.44(11) . . . . ?
O4 C21 C26 C25 -174.86(12) . . . . ?
N2 C22 C23 C24 175.86(12) . . . . ?
C1 C2 C3 C4 0.49(19) . . . . ?
C1 C6 C7 O2 168.59(10) . . . . ?
C1 C6 C7 N1 -8.72(18) . . . . ?
C2 C1 C6 C5 -0.34(17) . . . . ?
C2 C1 C6 C7 -177.91(11) . . . . ?
C2 C3 C4 C5 -0.48(19) . . . . ?
C3 C4 C5 C6 0.07(18) . . . . ?
C4 C5 C6 C1 0.34(18) . . . . ?
C4 C5 C6 C7 177.92(11) . . . . ?
C5 C6 C7 O2 -8.98(16) . . . . ?
C5 C6 C7 N1 173.71(11) . . . . ?
C6 C1 C2 C3 -0.07(18) . . . . ?
C7 O2 C8 C9 -178.80(12) . . . . ?
C7 O2 C8 C13 0.45(12) . . . . ?
C7 N1 C13 C8 1.76(12) . . . . ?
C7 N1 C13 C12 -177.87(13) . . . . ?
C8 O2 C7 N1 0.73(13) . . . . ?
C8 O2 C7 C6 -176.99(10) . . . . ?
C8 C9 C10 C11 0.50(18) . . . . ?
C9 C8 C13 N1 177.91(11) . . . . ?
C9 C8 C13 C12 -2.41(18) . . . . ?
C9 C10 C11 C12 -0.9(2) . . . . ?
C10 C11 C12 C13 -0.35(18) . . . . ?
C11 C12 C13 N1 -178.51(12) . . . . ?
C11 C12 C13 C8 1.90(17) . . . . ?
C13 N1 C7 O2 -1.56(13) . . . . ?
C13 N1 C7 C6 175.82(11) . . . . ?
C13 C8 C9 C10 1.14(18) . . . . ?
C14 C15 C16 C17 -0.3(2) . . . . ?
C14 C19 C20 O4 169.54(10) . . . . ?
C14 C19 C20 N2 -5.64(19) . . . . ?
C15 C14 C19 C18 0.21(18) . . . . ?
C15 C14 C19 C20 -173.50(11) . . . . ?
C15 C16 C17 C18 0.4(2) . . . . ?
C16 C17 C18 C19 -0.2(2) . . . . ?
C17 C18 C19 C14 -0.08(19) . . . . ?
C17 C18 C19 C20 173.66(12) . . . . ?
C18 C19 C20 O4 -4.21(17) . . . . ?
C18 C19 C20 N2 -179.39(12) . . . . ?
C19 C14 C15 C16 -0.04(19) . . . . ?
C20 O4 C21 C22 -0.91(12) . . . . ?
C20 O4 C21 C26 175.92(13) . . . . ?
C20 N2 C22 C21 2.44(13) . . . . ?
C20 N2 C22 C23 -173.32(13) . . . . ?
C21 O4 C20 N2 2.66(13) . . . . ?
C21 O4 C20 C19 -173.27(10) . . . . ?
C21 C22 C23 C24 0.52(18) . . . . ?
C22 N2 C20 O4 -3.20(13) . . . . ?
C22 N2 C20 C19 172.09(12) . . . . ?
C22 C21 C26 C25 1.50(19) . . . . ?
C22 C23 C24 C25 0.31(19) . . . . ?
C23 C24 C25 C26 -0.3(2) . . . . ?
C24 C25 C26 C21 -0.60(19) . . . . ?
C26 C21 C22 N2 -177.87(12) . . . . ?
C26 C21 C22 C23 -1.51(19) . . . . ?

_olex2_date_sample_data_collection 2015-11-10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.725
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 1816367'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-09-26
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H34 Hf N2 O6'
_chemical_formula_sum            'C34 H34 Hf N2 O6'
_chemical_formula_weight         745.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H34 Hf N2 O6'
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.70835(7)
_cell_length_b                   17.17797(14)
_cell_length_c                   18.59264(14)
_cell_angle_alpha                90
_cell_angle_beta                 95.7585(7)
_cell_angle_gamma                90
_cell_volume                     3085.04(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    83134
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0810
_cell_measurement_theta_min      1.6160
_exptl_absorpt_coefficient_mu    3.429
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       column
_exptl_crystal_F_000             1488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0523
0 1 0 0.0523
0 -1 -1 0.1118
0 1 -1 0.1369
1 1 -1 0.1129
-1 0 0 0.1098
0 1 1 0.0983
0 -1 1 0.0918
1 0 0 0.1213
-1 1 1 0.1299
1 -1 -1 0.1299

_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.105
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0003 -0.9991 -0.0000 -0.0209 0.0144 -0.0325
-0.0003 0.9991 0.0000 0.0209 -0.0144 0.0325
0.0002 -0.9998 -0.9990 -0.0424 0.0359 -0.0092
-0.0004 0.9984 -0.9990 -0.0006 0.0071 0.0558
0.9985 0.9989 -0.9983 0.0513 0.0577 0.0449
-0.9989 -0.0005 -0.0007 -0.0519 -0.0506 0.0110
-0.0002 0.9998 0.9990 0.0424 -0.0359 0.0092
0.0004 -0.9984 0.9990 0.0006 -0.0071 -0.0558
0.9989 0.0005 0.0007 0.0519 0.0506 -0.0110
-0.9991 0.9993 0.9983 -0.0095 -0.0865 0.0201
0.9991 -0.9993 -0.9983 0.0095 0.0865 -0.0201

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            177072
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.9674
_diffrn_reflns_theta_max         30.1135
_diffrn_reflns_theta_min         1.618
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00  83.00   1.00    2.00    --   24.87-131.00 -54.95   77
  2  ω    -46.00  96.00   1.00    2.00    --   24.87   0.00-120.00  142
  3  ω     -4.00  94.00   1.00    2.00    --   24.87  77.00 -30.00   98
  4  ω      6.00  93.00   1.00    2.00    --   24.87  57.00  90.00   87
  5  ω      3.00  95.00   1.00    2.00    --   24.87  38.00 -60.00   92
  6  ω     35.00  99.00   1.00    2.00    --   24.87 178.00 150.00   64
  7  ω     -4.00  94.00   1.00    2.00    --   24.87  77.00-180.00   98
  8  ω    -46.00  47.00   1.00    2.00    --   24.87 -38.00-180.00   93
  9  ω    -20.00  65.00   1.00    2.00    --   24.87 -99.00 150.00   85
 10  ω      7.00  85.00   1.00    2.00    --   24.87-133.00  40.38   78
 11  ω    -85.00  -8.00   1.00    2.00    --  -23.50 135.00  82.14   77
 12  ω    -97.00 -35.00   1.00    2.00    --  -23.50-178.00  90.00   62
 13  ω    -95.00  48.00   1.00    2.00    --  -23.50   0.00-180.00  143
 14  ω     -4.00  94.00   1.00    2.00    --   24.87  77.00-150.00   98
 15  ω      6.00  93.00   1.00    2.00    --   24.87  57.00  30.00   87
 16  ω    -46.00  47.00   1.00    2.00    --   24.87 -38.00 -90.00   93
 17  ω     -4.00  94.00   1.00    2.00    --   24.87  77.00  90.00   98
 18  ω      6.00  93.00   1.00    2.00    --   24.87  57.00 -60.00   87
 19  ω    -95.00  48.00   1.00    2.00    --  -23.50   0.00-120.00  143
 20  ω    -95.00  48.00   1.00    2.00    --  -23.50   0.00 -90.00  143
 21  ω    -95.00  48.00   1.00    2.00    --  -23.50   0.00 -60.00  143
 22  ω    -95.00  48.00   1.00    2.00    --  -23.50   0.00 -30.00  143
 23  ω    -95.00  48.00   1.00    2.00    --  -23.50   0.00-150.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0519449000
_diffrn_orient_matrix_UB_12      0.0209445000
_diffrn_orient_matrix_UB_13      0.0214913000
_diffrn_orient_matrix_UB_21      0.0507184000
_diffrn_orient_matrix_UB_22      -0.0144179000
_diffrn_orient_matrix_UB_23      -0.0215039000
_diffrn_orient_matrix_UB_31      -0.0109824000
_diffrn_orient_matrix_UB_32      0.0325270000
_diffrn_orient_matrix_UB_33      -0.0233771000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8603
_reflns_number_total             9067
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0210
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0074P)²+4.3826P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0434
_refine_special_details          
;
 Disorder of C(32), C(33) and C(34) over two sites(78:22)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.89965(2) 0.44127(2) 0.25866(2) 0.01301(2) Uani 1 1 d . . . . .
O1 O 0.94823(14) 0.55337(8) 0.28527(7) 0.0158(3) Uani 1 1 d . . . . .
O2 O 1.16415(14) 0.46378(8) 0.47448(7) 0.0156(3) Uani 1 1 d . . . . .
O3 O 0.82787(14) 0.33401(9) 0.28265(8) 0.0184(3) Uani 1 1 d . . . . .
O4 O 0.54268(15) 0.44997(10) 0.39995(8) 0.0234(3) Uani 1 1 d . . . . .
O5 O 0.78603(15) 0.46334(9) 0.17053(7) 0.0205(3) Uani 1 1 d . . . . .
O6 O 1.06711(14) 0.40623(9) 0.22074(8) 0.0176(3) Uani 1 1 d . . . . .
N1 N 1.03112(16) 0.43025(10) 0.37346(8) 0.0139(3) Uani 1 1 d . . . . .
N2 N 0.70493(17) 0.46805(10) 0.32353(9) 0.0170(3) Uani 1 1 d . . . . .
C1 C 1.00059(18) 0.59960(12) 0.33805(10) 0.0147(3) Uani 1 1 d . . . . .
C2 C 0.9979(2) 0.68055(12) 0.32791(11) 0.0190(4) Uani 1 1 d . . . . .
H2 H 0.9586 0.7009 0.2842 0.023 Uiso 1 1 calc R U . . .
C3 C 1.0526(2) 0.73068(12) 0.38162(12) 0.0211(4) Uani 1 1 d . . . . .
H3 H 1.0496 0.7841 0.3736 0.025 Uiso 1 1 calc R U . . .
C4 C 1.1123(2) 0.70171(12) 0.44783(12) 0.0198(4) Uani 1 1 d . . . . .
H4 H 1.1483 0.7356 0.4840 0.024 Uiso 1 1 calc R U . . .
C5 C 1.11722(19) 0.62243(12) 0.45887(11) 0.0166(4) Uani 1 1 d . . . . .
H5 H 1.1570 0.6029 0.5028 0.020 Uiso 1 1 calc R U . . .
C6 C 1.06289(18) 0.57037(11) 0.40468(10) 0.0137(3) Uani 1 1 d . . . . .
C7 C 1.07925(18) 0.48742(12) 0.41518(10) 0.0135(3) Uani 1 1 d . . . . .
C8 C 1.1712(2) 0.38369(12) 0.46798(11) 0.0163(4) Uani 1 1 d . . . . .
C9 C 1.2443(2) 0.33242(13) 0.51445(12) 0.0209(4) Uani 1 1 d . . . . .
H9 H 1.2960 0.3487 0.5566 0.025 Uiso 1 1 calc R U . . .
C10 C 1.2351(2) 0.25473(13) 0.49385(13) 0.0247(4) Uani 1 1 d . . . . .
H10 H 1.2819 0.2174 0.5232 0.030 Uiso 1 1 calc R U . . .
C11 C 1.1574(2) 0.23120(13) 0.43019(13) 0.0247(4) Uani 1 1 d . . . . .
H11 H 1.1547 0.1787 0.4181 0.030 Uiso 1 1 calc R U . . .
C12 C 1.0842(2) 0.28394(12) 0.38449(12) 0.0205(4) Uani 1 1 d . . . . .
H12 H 1.0330 0.2681 0.3421 0.025 Uiso 1 1 calc R U . . .
C13 C 1.09129(19) 0.36189(12) 0.40542(10) 0.0154(4) Uani 1 1 d . . . . .
C14 C 0.7496(2) 0.29584(13) 0.32511(11) 0.0188(4) Uani 1 1 d . . . . .
C15 C 0.7518(2) 0.21423(13) 0.32652(12) 0.0238(4) Uani 1 1 d . . . . .
H15 H 0.8086 0.1875 0.2975 0.029 Uiso 1 1 calc R U . . .
C16 C 0.6712(3) 0.17308(15) 0.37021(13) 0.0297(5) Uani 1 1 d . . . . .
H16 H 0.6746 0.1190 0.3706 0.036 Uiso 1 1 calc R U . . .
C17 C 0.5846(3) 0.21176(16) 0.41373(13) 0.0318(5) Uani 1 1 d . . . . .
H17 H 0.5304 0.1835 0.4430 0.038 Uiso 1 1 calc R U . . .
C18 C 0.5793(2) 0.29124(15) 0.41332(12) 0.0272(5) Uani 1 1 d . . . . .
H18 H 0.5214 0.3169 0.4424 0.033 Uiso 1 1 calc R U . . .
C19 C 0.6610(2) 0.33497(13) 0.36910(11) 0.0204(4) Uani 1 1 d . . . . .
C20 C 0.6442(2) 0.41783(13) 0.36348(11) 0.0197(4) Uani 1 1 d . . . . .
C21 C 0.5339(2) 0.52628(14) 0.37733(12) 0.0233(4) Uani 1 1 d . . . . .
C22 C 0.4395(2) 0.58133(16) 0.39468(14) 0.0301(5) Uani 1 1 d . . . . .
H22 H 0.3771 0.5722 0.4285 0.036 Uiso 1 1 calc R U . . .
C23 C 0.4444(2) 0.65097(16) 0.35828(14) 0.0331(6) Uani 1 1 d . . . . .
H23 H 0.3822 0.6901 0.3672 0.040 Uiso 1 1 calc R U . . .
C24 C 0.5405(2) 0.66440(15) 0.30817(13) 0.0290(5) Uani 1 1 d . . . . .
H24 H 0.5389 0.7119 0.2841 0.035 Uiso 1 1 calc R U . . .
C25 C 0.6379(2) 0.60892(14) 0.29332(12) 0.0232(4) Uani 1 1 d . . . . .
H25 H 0.7032 0.6186 0.2611 0.028 Uiso 1 1 calc R U . . .
C26 C 0.6324(2) 0.53837(13) 0.32921(11) 0.0191(4) Uani 1 1 d . . . . .
C27 C 0.6990(2) 0.45838(13) 0.10565(11) 0.0197(4) Uani 1 1 d . . . . .
C28 C 0.6044(3) 0.52931(15) 0.10096(14) 0.0342(6) Uani 1 1 d . . . . .
H28A H 0.5506 0.5297 0.1416 0.051 Uiso 1 1 calc R U . . .
H28B H 0.5436 0.5271 0.0570 0.051 Uiso 1 1 calc R U . . .
H28C H 0.6594 0.5758 0.1014 0.051 Uiso 1 1 calc R U . . .
C29 C 0.7884(3) 0.45661(17) 0.04313(12) 0.0350(6) Uani 1 1 d . . . . .
H29A H 0.8455 0.5023 0.0446 0.052 Uiso 1 1 calc R U . . .
H29B H 0.7302 0.4552 -0.0017 0.052 Uiso 1 1 calc R U . . .
H29C H 0.8461 0.4111 0.0470 0.052 Uiso 1 1 calc R U . . .
C30 C 0.6147(3) 0.38358(15) 0.10748(15) 0.0339(6) Uani 1 1 d . . . . .
H30A H 0.6756 0.3395 0.1077 0.051 Uiso 1 1 calc R U . . .
H30B H 0.5485 0.3813 0.0656 0.051 Uiso 1 1 calc R U . . .
H30C H 0.5671 0.3829 0.1503 0.051 Uiso 1 1 calc R U . . .
C31 C 1.2047(2) 0.41459(13) 0.20269(11) 0.0188(4) Uani 1 1 d . . . . .
C32 C 1.2762(3) 0.4773(2) 0.24860(19) 0.0344(8) Uani 0.785(3) 1 d . . P A 1
H32A H 1.2257 0.5252 0.2412 0.052 Uiso 0.785(3) 1 calc R U P A 1
H32B H 1.3684 0.4843 0.2353 0.052 Uiso 0.785(3) 1 calc R U P A 1
H32C H 1.2802 0.4626 0.2986 0.052 Uiso 0.785(3) 1 calc R U P A 1
C33 C 1.1963(3) 0.4361(2) 0.12208(15) 0.0277(6) Uani 0.785(3) 1 d . . P A 1
H33A H 1.1461 0.3964 0.0940 0.042 Uiso 0.785(3) 1 calc R U P A 1
H33B H 1.2881 0.4402 0.1075 0.042 Uiso 0.785(3) 1 calc R U P A 1
H33C H 1.1494 0.4850 0.1144 0.042 Uiso 0.785(3) 1 calc R U P A 1
C34 C 1.2755(3) 0.3359(2) 0.2138(2) 0.0373(8) Uani 0.785(3) 1 d . . P A 1
H34A H 1.2797 0.3217 0.2639 0.056 Uiso 0.785(3) 1 calc R U P A 1
H34B H 1.3676 0.3390 0.1994 0.056 Uiso 0.785(3) 1 calc R U P A 1
H34C H 1.2237 0.2974 0.1851 0.056 Uiso 0.785(3) 1 calc R U P A 1
C32B C 1.2447(13) 0.5028(9) 0.2122(7) 0.0344(8) Uani 0.215(3) 1 d . . P A 2
H32D H 1.1797 0.5340 0.1824 0.052 Uiso 0.215(3) 1 calc R U P A 2
H32E H 1.3360 0.5109 0.1981 0.052 Uiso 0.215(3) 1 calc R U P A 2
H32F H 1.2428 0.5175 0.2619 0.052 Uiso 0.215(3) 1 calc R U P A 2
C33B C 1.2242(11) 0.3824(8) 0.1335(6) 0.0277(6) Uani 0.215(3) 1 d . . P A 2
H33D H 1.2029 0.3278 0.1333 0.042 Uiso 0.215(3) 1 calc R U P A 2
H33E H 1.3188 0.3895 0.1240 0.042 Uiso 0.215(3) 1 calc R U P A 2
H33F H 1.1642 0.4083 0.0969 0.042 Uiso 0.215(3) 1 calc R U P A 2
C34B C 1.3065(12) 0.3713(8) 0.2622(8) 0.0373(8) Uani 0.215(3) 1 d . . P A 2
H34D H 1.3068 0.3980 0.3076 0.056 Uiso 0.215(3) 1 calc R U P A 2
H34E H 1.3984 0.3710 0.2474 0.056 Uiso 0.215(3) 1 calc R U P A 2
H34F H 1.2757 0.3187 0.2676 0.056 Uiso 0.215(3) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1 2.0319(14) . ?
Hf1 O3 2.0351(14) . ?
Hf1 O5 1.9189(14) . ?
Hf1 O6 1.9319(13) . ?
Hf1 N1 2.3820(16) . ?
Hf1 N2 2.3870(16) . ?
O1 C1 1.324(2) . ?
O2 C7 1.370(2) . ?
O2 C8 1.383(2) . ?
O3 C14 1.323(2) . ?
O4 C20 1.368(2) . ?
O4 C21 1.377(3) . ?
O5 C27 1.404(2) . ?
O6 C31 1.417(2) . ?
N1 C7 1.308(2) . ?
N1 C13 1.415(2) . ?
N2 C20 1.316(3) . ?
N2 C26 1.407(3) . ?
C1 C2 1.403(3) . ?
C1 C6 1.415(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.384(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.398(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.409(3) . ?
C6 C7 1.445(3) . ?
C8 C9 1.379(3) . ?
C8 C13 1.384(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.389(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.398(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.388(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(3) . ?
C14 C15 1.402(3) . ?
C14 C19 1.415(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.379(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.393(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.366(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.414(3) . ?
C19 C20 1.435(3) . ?
C21 C22 1.377(3) . ?
C21 C26 1.390(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.377(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.402(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.390(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.387(3) . ?
C27 C28 1.523(3) . ?
C27 C29 1.520(3) . ?
C27 C30 1.526(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.501(4) . ?
C31 C33 1.538(3) . ?
C31 C34 1.521(4) . ?
C31 C32B 1.571(14) . ?
C31 C33B 1.429(11) . ?
C31 C34B 1.593(13) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C32B H32D 0.9600 . ?
C32B H32E 0.9600 . ?
C32B H32F 0.9600 . ?
C33B H33D 0.9600 . ?
C33B H33E 0.9600 . ?
C33B H33F 0.9600 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 O3 151.75(5) . . ?
O1 Hf1 N1 76.51(5) . . ?
O1 Hf1 N2 82.56(6) . . ?
O3 Hf1 N1 84.04(6) . . ?
O3 Hf1 N2 75.99(6) . . ?
O5 Hf1 O1 96.90(6) . . ?
O5 Hf1 O3 100.71(6) . . ?
O5 Hf1 O6 100.52(6) . . ?
O5 Hf1 N1 172.40(6) . . ?
O5 Hf1 N2 88.67(6) . . ?
O6 Hf1 O1 101.58(6) . . ?
O6 Hf1 O3 96.73(6) . . ?
O6 Hf1 N1 84.68(6) . . ?
O6 Hf1 N2 169.28(6) . . ?
N1 Hf1 N2 86.72(5) . . ?
C1 O1 Hf1 144.26(13) . . ?
C7 O2 C8 104.81(15) . . ?
C14 O3 Hf1 144.01(14) . . ?
C20 O4 C21 104.99(16) . . ?
C27 O5 Hf1 165.09(14) . . ?
C31 O6 Hf1 154.52(13) . . ?
C7 N1 Hf1 126.80(13) . . ?
C7 N1 C13 105.43(16) . . ?
C13 N1 Hf1 127.12(12) . . ?
C20 N2 Hf1 125.53(14) . . ?
C20 N2 C26 105.36(17) . . ?
C26 N2 Hf1 129.10(13) . . ?
O1 C1 C2 119.63(18) . . ?
O1 C1 C6 122.33(18) . . ?
C2 C1 C6 118.03(18) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.27(19) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.21(19) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.06(19) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 119.99(17) . . ?
C5 C6 C1 119.81(18) . . ?
C5 C6 C7 120.06(17) . . ?
O2 C7 C6 116.76(16) . . ?
N1 C7 O2 113.87(17) . . ?
N1 C7 C6 129.22(17) . . ?
O2 C8 C13 108.30(17) . . ?
C9 C8 O2 127.39(19) . . ?
C9 C8 C13 124.3(2) . . ?
C8 C9 H9 122.4 . . ?
C8 C9 C10 115.2(2) . . ?
C10 C9 H9 122.4 . . ?
C9 C10 H10 119.2 . . ?
C9 C10 C11 121.7(2) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 H11 119.0 . . ?
C12 C11 C10 122.0(2) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 H12 121.7 . . ?
C11 C12 C13 116.6(2) . . ?
C13 C12 H12 121.7 . . ?
C8 C13 N1 107.55(17) . . ?
C8 C13 C12 120.15(19) . . ?
C12 C13 N1 132.29(18) . . ?
O3 C14 C15 119.85(19) . . ?
O3 C14 C19 121.9(2) . . ?
C15 C14 C19 118.25(19) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(2) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.6(2) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 120.1 . . ?
C18 C17 C16 119.8(2) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 119.6 . . ?
C17 C18 C19 120.8(2) . . ?
C19 C18 H18 119.6 . . ?
C14 C19 C20 120.02(19) . . ?
C18 C19 C14 119.5(2) . . ?
C18 C19 C20 120.2(2) . . ?
O4 C20 C19 116.53(18) . . ?
N2 C20 O4 113.6(2) . . ?
N2 C20 C19 129.59(19) . . ?
O4 C21 C22 127.2(2) . . ?
O4 C21 C26 108.26(19) . . ?
C22 C21 C26 124.4(2) . . ?
C21 C22 H22 122.4 . . ?
C21 C22 C23 115.1(2) . . ?
C23 C22 H22 122.4 . . ?
C22 C23 H23 119.1 . . ?
C22 C23 C24 121.8(2) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 119.0 . . ?
C25 C24 C23 122.0(2) . . ?
C25 C24 H24 119.0 . . ?
C24 C25 H25 121.8 . . ?
C26 C25 C24 116.3(2) . . ?
C26 C25 H25 121.8 . . ?
C21 C26 N2 107.57(19) . . ?
C25 C26 N2 132.09(19) . . ?
C25 C26 C21 120.2(2) . . ?
O5 C27 C28 107.95(17) . . ?
O5 C27 C29 108.51(17) . . ?
O5 C27 C30 108.04(18) . . ?
C28 C27 C30 110.71(19) . . ?
C29 C27 C28 111.1(2) . . ?
C29 C27 C30 110.4(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O6 C31 C32 109.34(19) . . ?
O6 C31 C33 107.24(18) . . ?
O6 C31 C34 107.55(19) . . ?
O6 C31 C32B 107.4(5) . . ?
O6 C31 C33B 112.8(5) . . ?
O6 C31 C34B 108.8(4) . . ?
C32 C31 C33 111.0(2) . . ?
C32 C31 C34 112.6(3) . . ?
C34 C31 C33 108.9(2) . . ?
C32B C31 C34B 104.1(7) . . ?
C33B C31 C32B 114.9(7) . . ?
C33B C31 C34B 108.4(7) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C32B H32D 109.5 . . ?
C31 C32B H32E 109.5 . . ?
C31 C32B H32F 109.5 . . ?
H32D C32B H32E 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C31 C33B H33D 109.5 . . ?
C31 C33B H33E 109.5 . . ?
C31 C33B H33F 109.5 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C31 C34B H34D 109.5 . . ?
C31 C34B H34E 109.5 . . ?
C31 C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 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
Hf1 O1 C1 C2 -173.47(15) . . . . ?
Hf1 O1 C1 C6 8.0(3) . . . . ?
Hf1 O3 C14 C15 -169.69(16) . . . . ?
Hf1 O3 C14 C19 11.2(3) . . . . ?
Hf1 O5 C27 C28 145.1(5) . . . . ?
Hf1 O5 C27 C29 -94.4(5) . . . . ?
Hf1 O5 C27 C30 25.3(6) . . . . ?
Hf1 O6 C31 C32 23.5(4) . . . . ?
Hf1 O6 C31 C33 -96.9(3) . . . . ?
Hf1 O6 C31 C34 146.1(3) . . . . ?
Hf1 O6 C31 C32B -9.7(7) . . . . ?
Hf1 O6 C31 C33B -137.3(6) . . . . ?
Hf1 O6 C31 C34B 102.4(6) . . . . ?
Hf1 N1 C7 O2 -173.20(11) . . . . ?
Hf1 N1 C7 C6 2.1(3) . . . . ?
Hf1 N1 C13 C8 173.15(12) . . . . ?
Hf1 N1 C13 C12 -5.7(3) . . . . ?
Hf1 N2 C20 O4 174.48(12) . . . . ?
Hf1 N2 C20 C19 -11.4(3) . . . . ?
Hf1 N2 C26 C21 -175.53(13) . . . . ?
Hf1 N2 C26 C25 9.5(3) . . . . ?
O1 C1 C2 C3 -179.50(18) . . . . ?
O1 C1 C6 C5 179.84(17) . . . . ?
O1 C1 C6 C7 4.1(3) . . . . ?
O2 C8 C9 C10 -178.73(19) . . . . ?
O2 C8 C13 N1 -1.3(2) . . . . ?
O2 C8 C13 C12 177.75(17) . . . . ?
O3 C14 C15 C16 -179.9(2) . . . . ?
O3 C14 C19 C18 179.81(19) . . . . ?
O3 C14 C19 C20 5.9(3) . . . . ?
O4 C21 C22 C23 -173.2(2) . . . . ?
O4 C21 C26 N2 -1.2(2) . . . . ?
O4 C21 C26 C25 174.47(18) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C1 C6 C7 O2 167.27(16) . . . . ?
C1 C6 C7 N1 -8.0(3) . . . . ?
C2 C1 C6 C5 1.3(3) . . . . ?
C2 C1 C6 C7 -174.44(17) . . . . ?
C2 C3 C4 C5 0.5(3) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 C1 -0.8(3) . . . . ?
C4 C5 C6 C7 174.93(18) . . . . ?
C5 C6 C7 O2 -8.5(3) . . . . ?
C5 C6 C7 N1 176.32(18) . . . . ?
C6 C1 C2 C3 -0.9(3) . . . . ?
C7 O2 C8 C9 179.97(19) . . . . ?
C7 O2 C8 C13 0.1(2) . . . . ?
C7 N1 C13 C8 1.9(2) . . . . ?
C7 N1 C13 C12 -176.9(2) . . . . ?
C8 O2 C7 N1 1.2(2) . . . . ?
C8 O2 C7 C6 -174.76(16) . . . . ?
C8 C9 C10 C11 0.3(3) . . . . ?
C9 C8 C13 N1 178.88(18) . . . . ?
C9 C8 C13 C12 -2.1(3) . . . . ?
C9 C10 C11 C12 -0.6(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 N1 -179.6(2) . . . . ?
C11 C12 C13 C8 1.6(3) . . . . ?
C13 N1 C7 O2 -2.0(2) . . . . ?
C13 N1 C7 C6 173.37(18) . . . . ?
C13 C8 C9 C10 1.1(3) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C14 C19 C20 O4 171.00(17) . . . . ?
C14 C19 C20 N2 -3.0(3) . . . . ?
C15 C14 C19 C18 0.7(3) . . . . ?
C15 C14 C19 C20 -173.23(19) . . . . ?
C15 C16 C17 C18 -0.1(4) . . . . ?
C16 C17 C18 C19 0.0(4) . . . . ?
C17 C18 C19 C14 -0.3(3) . . . . ?
C17 C18 C19 C20 173.6(2) . . . . ?
C18 C19 C20 O4 -2.9(3) . . . . ?
C18 C19 C20 N2 -176.8(2) . . . . ?
C19 C14 C15 C16 -0.7(3) . . . . ?
C20 O4 C21 C22 174.9(2) . . . . ?
C20 O4 C21 C26 -1.4(2) . . . . ?
C20 N2 C26 C21 3.3(2) . . . . ?
C20 N2 C26 C25 -171.6(2) . . . . ?
C21 O4 C20 N2 3.7(2) . . . . ?
C21 O4 C20 C19 -171.19(17) . . . . ?
C21 C22 C23 C24 -1.0(3) . . . . ?
C22 C21 C26 N2 -177.6(2) . . . . ?
C22 C21 C26 C25 -1.9(3) . . . . ?
C22 C23 C24 C25 -1.2(4) . . . . ?
C23 C24 C25 C26 1.9(3) . . . . ?
C24 C25 C26 N2 174.0(2) . . . . ?
C24 C25 C26 C21 -0.4(3) . . . . ?
C26 N2 C20 O4 -4.4(2) . . . . ?
C26 N2 C20 C19 169.7(2) . . . . ?
C26 C21 C22 C23 2.5(3) . . . . ?

_olex2_date_sample_data_collection 2016-09-23
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.841
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1816366'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2017-09-27
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H62 N2 O6 Zr'
_chemical_formula_sum            'C48 H62 N2 O6 Zr'
_chemical_formula_weight         854.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H59 N7'
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'

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

_cell_length_a                   10.5451(4)
_cell_length_b                   13.0261(6)
_cell_length_c                   17.4544(8)
_cell_angle_alpha                97.351(4)
_cell_angle_beta                 106.210(4)
_cell_angle_gamma                98.564(4)
_cell_volume                     2240.00(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.6710
_cell_measurement_theta_min      3.4550
_exptl_absorpt_coefficient_mu    2.395
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0049
0 0 1 0.0049
0 -1 1 0.0167
0 1 -1 0.0167
5 -1 -3 0.0805
-5 1 3 0.0805

_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.01
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0024 -0.0026 -1.0012 0.0008 0.0889 0.0287
-0.0024 0.0026 1.0012 -0.0008 -0.0889 -0.0287
-0.0024 -0.9976 1.0026 -0.0139 -0.0314 -0.1350
0.0024 0.9976 -1.0026 0.0139 0.0314 0.1350
5.0088 -1.0037 -2.9968 0.7266 0.0865 -0.0668
-5.0088 1.0037 2.9968 -0.7266 -0.0865 0.0668

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.679
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00  17.00   1.00   20.00    --  -38.50 101.00 -38.00   95
  2  ω      4.00  66.00   1.00   20.00    --   42.95-101.00-142.00   62
  3  ω     76.00 112.00   1.00   49.00    --  111.00-101.00-142.00   36
  4  ω    139.00 178.00   1.00   49.00    --  111.00 101.00 -38.00   39
  5  ω   -109.00 -80.00   1.00   20.00    --  -38.50 -38.00  60.00   29
  6  ω    -51.00 -18.00   1.00   20.00    --  -38.50 -38.00  60.00   33
  7  ω    -57.00  32.00   1.00   20.00    --  -38.50  38.00 120.00   89
  8  ω     77.00 113.00   1.00   20.00    --   42.95  77.00   0.00   36
  9  ω     57.00 117.00   1.00   20.00    --   42.95 178.00-150.00   60
 10  ω     23.00  92.00   1.00   20.00    --   42.95  38.00-150.00   69
 11  ω      1.00  28.00   1.00   20.00    --   42.95 -99.00 -60.00   27
 12  ω     71.00  98.00   1.00   20.00    --   42.95  57.00-150.00   27
 13  ω     13.00 105.00   1.00   20.00    --   42.95  77.00  90.00   92
 14  ω     16.00 114.00   1.00   20.00    --   42.95  77.00 -60.00   98
 15  ω     19.00  52.00   1.00   20.00    --   42.95  57.00  60.00   33
 16  ω     19.00  47.00   1.00   20.00    --   42.95  57.00-150.00   28
 17  ω     17.00  55.00   1.00   20.00    --   42.95  77.00   0.00   38
 18  ω     76.00 110.00   1.00   20.00    --   42.95  57.00   0.00   34
 19  ω     13.00  50.00   1.00   20.00    --   42.95  77.00-180.00   37
 20  ω     59.00 109.00   1.00   20.00    --   42.95  57.00  60.00   50
 21  ω     18.00  46.00   1.00   20.00    --   42.95  57.00   0.00   28
 22  ω     15.00  92.00   1.00   20.00    --   42.95  77.00-120.00   77
 23  ω     45.00 135.00   1.00   49.00    --  111.00 -61.00-150.00   90
 24  ω     86.00 112.00   1.00   49.00    --  111.00  61.00 -30.00   26
 25  ω     85.00 111.00   1.00   49.00    --  111.00  61.00  90.00   26
 26  ω     87.00 127.00   1.00   49.00    --  111.00  61.00-150.00   40
 27  ω     82.00 108.00   1.00   49.00    --  111.00  77.00 120.00   26
 28  ω    116.00 171.00   1.00   49.00    --  111.00  77.00   0.00   55
 29  ω     82.00 109.00   1.00   49.00    --  111.00  72.00 -26.20   27
 30  ω     81.00 107.00   1.00   49.00    --  111.00  77.00  90.00   26
 31  ω    114.00 164.00   1.00   49.00    --  111.00  77.00  90.00   50
 32  ω     82.00 177.00   1.00   49.00    --  111.00  77.00-120.00   95
 33  ω     53.00 122.00   1.00   49.00    --  111.00-125.00  30.00   69
 34  ω     85.00 115.00   1.00   49.00    --  111.00  61.00  30.00   30
 35  ω     81.00 107.00   1.00   49.00    --  111.00  76.00-127.52   26
 36  ω     82.00 107.00   1.00   49.00    --  111.00  77.00   0.00   25
 37  ω     81.00 175.00   1.00   49.00    --  111.00  77.00 150.00   94
 38  ω     85.00 112.00   1.00   49.00    --  111.00  61.00 150.00   27
 39  ω    120.00 176.00   1.00   49.00    --  111.00  77.00-180.00   56
 40  ω    113.00 176.00   1.00   49.00    --  111.00  77.00  30.00   63
 41  ω     81.00 107.00   1.00   49.00    --  111.00  77.00-180.00   26
 42  ω     95.00 122.00   1.00   49.00    --  111.00-125.00-180.00   27
 43  ω     85.00 111.00   1.00   49.00    --  111.00  61.00-180.00   26
 44  ω     81.00 108.00   1.00   49.00    --  111.00  77.00  30.00   27
 45  ω     85.00 112.00   1.00   49.00    --  111.00  61.00-120.00   27
 46  ω     81.00 173.00   1.00   49.00    --  111.00  77.00-150.00   92
 47  ω     89.00 117.00   1.00   49.00    --  111.00  45.00  30.00   28
 48  ω     89.00 115.00   1.00   49.00    --  111.00  45.00 150.00   26
 49  ω     87.00 114.00   1.00   49.00    --  111.00  50.00-158.68   27
 50  ω     85.00 112.00   1.00   49.00    --  111.00  61.00 -90.00   27
 51  ω     81.00 107.00   1.00   49.00    --  111.00  77.00  60.00   26
 52  ω     43.00 141.00   1.00   49.00    --  111.00 -77.00  60.00   98
 53  ω     85.00 171.00   1.00   49.00    --  111.00  61.00 -60.00   86
 54  ω     82.00 178.00   1.00   49.00    --  111.00  72.00 -51.67   96
 55  ω     42.00  76.00   1.00   49.00    --  111.00-125.00-180.00   34
 56  ω     85.00 112.00   1.00   49.00    --  111.00  61.00  60.00   27
 57  ω    113.00 148.00   1.00   49.00    --  111.00  77.00 -90.00   35
 58  ω     81.00 107.00   1.00   49.00    --  111.00  77.00 -90.00   26
 59  ω     85.00 178.00   1.00   49.00    --  111.00  62.00  66.31   93
 60  ω     85.00 121.00   1.00   49.00    --  111.00  61.00   0.00   36
 61  ω     54.00 105.00   1.00   49.00    --  111.00 -94.00  30.00   51
 62  ω     85.00 174.00   1.00   49.00    --  111.00  61.00 120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1473623000
_diffrn_orient_matrix_UB_12      0.0130472000
_diffrn_orient_matrix_UB_13      -0.0005195000
_diffrn_orient_matrix_UB_21      -0.0474024000
_diffrn_orient_matrix_UB_22      -0.0576071000
_diffrn_orient_matrix_UB_23      -0.0887988000
_diffrn_orient_matrix_UB_31      -0.0094008000
_diffrn_orient_matrix_UB_32      0.1062381000
_diffrn_orient_matrix_UB_33      -0.0290044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6451
_reflns_number_total             7924
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7924
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      1.018
_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)+(0.0578P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1155
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.36622(3) 0.39811(2) 0.76186(2) 0.02026(10) Uani 1 1 d . . . . .
O1 O 0.3727(2) 0.55815(18) 0.78962(13) 0.0228(5) Uani 1 1 d . . . . .
O2 O -0.0145(2) 0.49771(18) 0.62789(13) 0.0222(5) Uani 1 1 d . . . . .
O3 O 0.3469(2) 0.25377(18) 0.68950(13) 0.0222(5) Uani 1 1 d . . . . .
O4 O 0.6252(2) 0.41785(18) 0.59714(13) 0.0229(5) Uani 1 1 d . . . . .
O5 O 0.2402(2) 0.35367(19) 0.81872(14) 0.0256(5) Uani 1 1 d . . . . .
O6 O 0.5430(2) 0.39596(19) 0.83151(14) 0.0246(5) Uani 1 1 d . . . . .
N1 N 0.1745(2) 0.4317(2) 0.66434(16) 0.0206(6) Uani 1 1 d . . . . .
N2 N 0.4705(2) 0.4393(2) 0.66139(16) 0.0213(6) Uani 1 1 d . . . . .
C1 C 0.2862(3) 0.6170(2) 0.80125(18) 0.0184(6) Uani 1 1 d . . . . .
C2 C 0.3273(3) 0.7069(3) 0.86408(19) 0.0229(7) Uani 1 1 d . . . . .
C3 C 0.2301(3) 0.7620(3) 0.87550(19) 0.0223(7) Uani 1 1 d . . . . .
H3 H 0.256304 0.819571 0.917686 0.027 Uiso 1 1 calc R . . . .
C4 C 0.0939(3) 0.7372(3) 0.82780(19) 0.0212(7) Uani 1 1 d . . . . .
C5 C 0.0569(3) 0.6520(3) 0.76502(19) 0.0226(7) Uani 1 1 d . . . . .
H5 H -0.031630 0.634309 0.731293 0.027 Uiso 1 1 calc R . . . .
C6 C 0.1504(3) 0.5918(3) 0.75136(19) 0.0208(7) Uani 1 1 d . . . . .
C7 C 0.1092(3) 0.5044(3) 0.68326(19) 0.0206(7) Uani 1 1 d . . . . .
C8 C -0.0243(3) 0.4146(3) 0.56693(19) 0.0234(7) Uani 1 1 d . . . . .
C9 C -0.1265(3) 0.3795(3) 0.4947(2) 0.0261(7) Uani 1 1 d . . . . .
H9 H -0.203763 0.408291 0.481878 0.031 Uiso 1 1 calc R . . . .
C10 C -0.1063(3) 0.2984(3) 0.4425(2) 0.0269(7) Uani 1 1 d . . . . .
H10 H -0.171271 0.272278 0.392682 0.032 Uiso 1 1 calc R . . . .
C11 C 0.0093(3) 0.2550(3) 0.4631(2) 0.0279(8) Uani 1 1 d . . . . .
H11 H 0.019167 0.200629 0.426444 0.033 Uiso 1 1 calc R . . . .
C12 C 0.1102(3) 0.2907(3) 0.53665(19) 0.0242(7) Uani 1 1 d . . . . .
H12 H 0.186392 0.260758 0.550382 0.029 Uiso 1 1 calc R . . . .
C13 C 0.0917(3) 0.3737(3) 0.58885(19) 0.0219(7) Uani 1 1 d . . . . .
C14 C 0.4740(3) 0.7374(3) 0.91970(19) 0.0243(7) Uani 1 1 d . . . . .
C15 C 0.5055(3) 0.6507(3) 0.9705(2) 0.0323(8) Uani 1 1 d . . . . .
H15A H 0.442026 0.640403 1.000298 0.048 Uiso 1 1 calc GR . . . .
H15B H 0.594918 0.671764 1.007653 0.048 Uiso 1 1 calc GR . . . .
H15C H 0.499043 0.586055 0.935164 0.048 Uiso 1 1 calc GR . . . .
C16 C 0.5734(3) 0.7520(3) 0.8704(2) 0.0297(8) Uani 1 1 d . . . . .
H16A H 0.566905 0.686225 0.836316 0.045 Uiso 1 1 calc GR . . . .
H16B H 0.663381 0.774411 0.906729 0.045 Uiso 1 1 calc GR . . . .
H16C H 0.552053 0.804331 0.837419 0.045 Uiso 1 1 calc GR . . . .
C17 C 0.4981(3) 0.8421(3) 0.9780(2) 0.0336(9) Uani 1 1 d . . . . .
H17A H 0.476661 0.896806 0.947444 0.050 Uiso 1 1 calc GR . . . .
H17B H 0.590913 0.860143 1.010540 0.050 Uiso 1 1 calc GR . . . .
H17C H 0.441961 0.834893 1.012616 0.050 Uiso 1 1 calc GR . . . .
C18 C -0.0041(3) 0.8030(3) 0.8493(2) 0.0234(7) Uani 1 1 d . . . . .
C19 C 0.0496(3) 0.9213(3) 0.8549(2) 0.0287(8) Uani 1 1 d . . . . .
H19A H 0.133640 0.943091 0.897535 0.043 Uiso 1 1 calc GR . . . .
H19B H -0.014358 0.961357 0.866423 0.043 Uiso 1 1 calc GR . . . .
H19C H 0.063069 0.933094 0.804345 0.043 Uiso 1 1 calc GR . . . .
C20 C -0.1435(3) 0.7734(3) 0.7854(2) 0.0256(7) Uani 1 1 d . . . . .
H20A H -0.134804 0.782898 0.733356 0.038 Uiso 1 1 calc GR . . . .
H20B H -0.201256 0.817748 0.799838 0.038 Uiso 1 1 calc GR . . . .
H20C H -0.181620 0.700928 0.783108 0.038 Uiso 1 1 calc GR . . . .
C21 C -0.0186(3) 0.7848(3) 0.9323(2) 0.0294(8) Uani 1 1 d . . . . .
H21A H -0.051547 0.711290 0.929695 0.044 Uiso 1 1 calc GR . . . .
H21B H -0.080781 0.825283 0.945924 0.044 Uiso 1 1 calc GR . . . .
H21C H 0.067533 0.806688 0.973032 0.044 Uiso 1 1 calc GR . . . .
C22 C 0.4413(3) 0.2077(3) 0.67117(18) 0.0200(7) Uani 1 1 d . . . . .
C23 C 0.4462(3) 0.1015(3) 0.68016(18) 0.0211(7) Uani 1 1 d . . . . .
C24 C 0.5491(3) 0.0595(3) 0.66156(18) 0.0214(7) Uani 1 1 d . . . . .
H24 H 0.552938 -0.009977 0.667584 0.026 Uiso 1 1 calc R . . . .
C25 C 0.6490(3) 0.1144(3) 0.63408(18) 0.0214(7) Uani 1 1 d . . . . .
C26 C 0.6412(3) 0.2168(3) 0.62451(19) 0.0215(7) Uani 1 1 d . . . . .
H26 H 0.703929 0.254969 0.605367 0.026 Uiso 1 1 calc R . . . .
C27 C 0.5395(3) 0.2646(3) 0.64329(19) 0.0215(7) Uani 1 1 d . . . . .
C28 C 0.5391(3) 0.3736(3) 0.63527(18) 0.0202(7) Uani 1 1 d . . . . .
C29 C 0.6065(3) 0.5203(3) 0.59821(19) 0.0210(7) Uani 1 1 d . . . . .
C30 C 0.6681(3) 0.5971(3) 0.5658(2) 0.0258(7) Uani 1 1 d . . . . .
H30 H 0.732906 0.585141 0.540612 0.031 Uiso 1 1 calc R . . . .
C31 C 0.6272(3) 0.6935(3) 0.5731(2) 0.0270(7) Uani 1 1 d . . . . .
H31 H 0.665150 0.748221 0.552148 0.032 Uiso 1 1 calc R . . . .
C32 C 0.5301(3) 0.7096(3) 0.6112(2) 0.0270(7) Uani 1 1 d . . . . .
H32 H 0.504709 0.775010 0.614612 0.032 Uiso 1 1 calc R . . . .
C33 C 0.4701(3) 0.6319(3) 0.64436(19) 0.0230(7) Uani 1 1 d . . . . .
H33 H 0.406301 0.644015 0.670278 0.028 Uiso 1 1 calc R . . . .
C34 C 0.5102(3) 0.5347(3) 0.63683(18) 0.0206(7) Uani 1 1 d . . . . .
C35 C 0.3456(3) 0.0375(3) 0.71363(19) 0.0229(7) Uani 1 1 d . . . . .
C36 C 0.3701(3) 0.0862(3) 0.8030(2) 0.0284(8) Uani 1 1 d . . . . .
H36A H 0.460047 0.083555 0.834132 0.043 Uiso 1 1 calc GR . . . .
H36B H 0.306835 0.046998 0.823957 0.043 Uiso 1 1 calc GR . . . .
H36C H 0.358818 0.158210 0.806681 0.043 Uiso 1 1 calc GR . . . .
C37 C 0.1994(3) 0.0356(3) 0.6636(2) 0.0275(8) Uani 1 1 d . . . . .
H37A H 0.182833 0.106227 0.666843 0.041 Uiso 1 1 calc GR . . . .
H37B H 0.138831 -0.006269 0.684823 0.041 Uiso 1 1 calc GR . . . .
H37C H 0.185471 0.005475 0.608077 0.041 Uiso 1 1 calc GR . . . .
C38 C 0.3631(3) -0.0769(3) 0.7116(2) 0.0288(8) Uani 1 1 d . . . . .
H38A H 0.351621 -0.109265 0.656929 0.043 Uiso 1 1 calc GR . . . .
H38B H 0.297103 -0.114524 0.731487 0.043 Uiso 1 1 calc GR . . . .
H38C H 0.451667 -0.078825 0.745248 0.043 Uiso 1 1 calc GR . . . .
C39 C 0.7563(3) 0.0587(3) 0.61391(19) 0.0219(7) Uani 1 1 d . . . . .
C40 C 0.6905(3) -0.0200(3) 0.5340(2) 0.0315(8) Uani 1 1 d . . . . .
H40A H 0.616235 -0.068210 0.539027 0.047 Uiso 1 1 calc GR . . . .
H40B H 0.755562 -0.058607 0.522141 0.047 Uiso 1 1 calc GR . . . .
H40C H 0.658669 0.017647 0.490908 0.047 Uiso 1 1 calc GR . . . .
C41 C 0.8153(3) -0.0012(3) 0.6811(2) 0.0301(8) Uani 1 1 d . . . . .
H41A H 0.852040 0.046980 0.731847 0.045 Uiso 1 1 calc GR . . . .
H41B H 0.885124 -0.033243 0.668685 0.045 Uiso 1 1 calc GR . . . .
H41C H 0.745612 -0.054994 0.685059 0.045 Uiso 1 1 calc GR . . . .
C42 C 0.8721(3) 0.1363(3) 0.6037(2) 0.0329(8) Uani 1 1 d . . . . .
H42A H 0.837817 0.172077 0.559773 0.049 Uiso 1 1 calc GR . . . .
H42B H 0.937882 0.098442 0.591973 0.049 Uiso 1 1 calc GR . . . .
H42C H 0.913043 0.186977 0.652796 0.049 Uiso 1 1 calc GR . . . .
C43 C 0.1222(3) 0.3366(3) 0.8420(2) 0.0262(7) Uani 1 1 d . . . . .
H43 H 0.046706 0.345257 0.797141 0.031 Uiso 1 1 calc R . . . .
C44 C 0.1361(3) 0.4192(3) 0.9155(2) 0.0321(8) Uani 1 1 d . . . . .
H44A H 0.213361 0.415022 0.959039 0.048 Uiso 1 1 calc GR . . . .
H44B H 0.056804 0.406496 0.932336 0.048 Uiso 1 1 calc GR . . . .
H44C H 0.147016 0.488234 0.901547 0.048 Uiso 1 1 calc GR . . . .
C45 C 0.0947(4) 0.2248(3) 0.8575(2) 0.0346(9) Uani 1 1 d . . . . .
H45A H 0.091912 0.175993 0.810686 0.052 Uiso 1 1 calc GR . . . .
H45B H 0.009827 0.211520 0.868221 0.052 Uiso 1 1 calc GR . . . .
H45C H 0.164967 0.216178 0.903491 0.052 Uiso 1 1 calc GR . . . .
C46 C 0.6814(3) 0.4066(3) 0.8722(2) 0.0274(8) Uani 1 1 d . . . . .
H46 H 0.697857 0.437596 0.929084 0.033 Uiso 1 1 calc R . . . .
C47 C 0.7642(4) 0.4815(4) 0.8359(3) 0.0438(10) Uani 1 1 d . . . . .
H47A H 0.754396 0.450367 0.781155 0.066 Uiso 1 1 calc GR . . . .
H47B H 0.857280 0.494172 0.867524 0.066 Uiso 1 1 calc GR . . . .
H47C H 0.732943 0.547057 0.836215 0.066 Uiso 1 1 calc GR . . . .
C48 C 0.7207(3) 0.2996(3) 0.8695(2) 0.0337(8) Uani 1 1 d . . . . .
H48A H 0.665012 0.254591 0.891648 0.051 Uiso 1 1 calc GR . . . .
H48B H 0.813352 0.307339 0.900740 0.051 Uiso 1 1 calc GR . . . .
H48C H 0.708715 0.268986 0.814283 0.051 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 O1 2.065(2) . ?
Zr1 O3 2.075(2) . ?
Zr1 O5 1.934(2) . ?
Zr1 O6 1.927(2) . ?
Zr1 N1 2.389(3) . ?
Zr1 N2 2.390(3) . ?
O1 C1 1.317(4) . ?
O2 C7 1.373(4) . ?
O2 C8 1.387(4) . ?
O3 C22 1.326(4) . ?
O4 C28 1.370(4) . ?
O4 C29 1.376(4) . ?
O5 C43 1.409(4) . ?
O6 C46 1.411(4) . ?
N1 C7 1.313(4) . ?
N1 C13 1.405(4) . ?
N2 C28 1.316(4) . ?
N2 C34 1.408(4) . ?
C1 C2 1.420(4) . ?
C1 C6 1.417(4) . ?
C2 C3 1.379(5) . ?
C2 C14 1.540(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.409(4) . ?
C4 C5 1.380(5) . ?
C4 C18 1.531(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.399(5) . ?
C6 C7 1.454(4) . ?
C8 C9 1.382(5) . ?
C8 C13 1.383(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.385(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.395(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.391(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.395(5) . ?
C14 C15 1.541(5) . ?
C14 C16 1.537(5) . ?
C14 C17 1.535(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.542(5) . ?
C18 C20 1.536(4) . ?
C18 C21 1.542(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.419(5) . ?
C22 C27 1.416(4) . ?
C23 C24 1.382(5) . ?
C23 C35 1.540(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.413(4) . ?
C25 C26 1.376(5) . ?
C25 C39 1.528(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.410(4) . ?
C27 C28 1.445(5) . ?
C29 C30 1.379(5) . ?
C29 C34 1.387(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.390(5) . ?
C31 H31 0.9300 . ?
C31 C32 1.394(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.386(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.397(5) . ?
C35 C36 1.541(4) . ?
C35 C37 1.539(4) . ?
C35 C38 1.526(5) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.536(4) . ?
C39 C41 1.531(5) . ?
C39 C42 1.532(4) . ?
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 H43 0.9800 . ?
C43 C44 1.524(5) . ?
C43 C45 1.516(5) . ?
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 H46 0.9800 . ?
C46 C47 1.525(5) . ?
C46 C48 1.510(5) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 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 O3 157.43(9) . . ?
O1 Zr1 N1 74.67(9) . . ?
O1 Zr1 N2 86.33(9) . . ?
O3 Zr1 N1 89.55(9) . . ?
O3 Zr1 N2 75.30(9) . . ?
O5 Zr1 O1 96.70(10) . . ?
O5 Zr1 O3 97.89(9) . . ?
O5 Zr1 N1 84.99(10) . . ?
O5 Zr1 N2 164.95(9) . . ?
O6 Zr1 O1 97.49(9) . . ?
O6 Zr1 O3 94.69(9) . . ?
O6 Zr1 O5 106.70(10) . . ?
O6 Zr1 N1 166.83(10) . . ?
O6 Zr1 N2 87.42(9) . . ?
N1 Zr1 N2 81.60(9) . . ?
C1 O1 Zr1 135.17(19) . . ?
C7 O2 C8 104.7(2) . . ?
C22 O3 Zr1 129.43(18) . . ?
C28 O4 C29 104.9(2) . . ?
C43 O5 Zr1 161.7(2) . . ?
C46 O6 Zr1 168.5(2) . . ?
C7 N1 Zr1 121.1(2) . . ?
C7 N1 C13 105.2(3) . . ?
C13 N1 Zr1 132.3(2) . . ?
C28 N2 Zr1 119.6(2) . . ?
C28 N2 C34 104.9(3) . . ?
C34 N2 Zr1 132.8(2) . . ?
O1 C1 C2 120.6(3) . . ?
O1 C1 C6 120.6(3) . . ?
C6 C1 C2 118.8(3) . . ?
C1 C2 C14 120.6(3) . . ?
C3 C2 C1 117.5(3) . . ?
C3 C2 C14 121.8(3) . . ?
C2 C3 H3 117.7 . . ?
C2 C3 C4 124.7(3) . . ?
C4 C3 H3 117.7 . . ?
C3 C4 C18 119.0(3) . . ?
C5 C4 C3 117.0(3) . . ?
C5 C4 C18 124.0(3) . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 119.3(3) . . ?
C5 C6 C1 120.9(3) . . ?
C5 C6 C7 119.7(3) . . ?
O2 C7 C6 116.3(3) . . ?
N1 C7 O2 113.8(3) . . ?
N1 C7 C6 129.9(3) . . ?
C9 C8 O2 127.8(3) . . ?
C9 C8 C13 124.3(3) . . ?
C13 C8 O2 107.8(3) . . ?
C8 C9 H9 122.3 . . ?
C8 C9 C10 115.5(3) . . ?
C10 C9 H9 122.3 . . ?
C9 C10 H10 119.2 . . ?
C9 C10 C11 121.6(3) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 H11 119.0 . . ?
C12 C11 C10 122.0(3) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 H12 121.6 . . ?
C11 C12 C13 116.8(3) . . ?
C13 C12 H12 121.6 . . ?
C8 C13 N1 108.3(3) . . ?
C8 C13 C12 119.8(3) . . ?
C12 C13 N1 131.8(3) . . ?
C2 C14 C15 109.4(3) . . ?
C16 C14 C2 111.4(3) . . ?
C16 C14 C15 109.4(3) . . ?
C17 C14 C2 111.5(3) . . ?
C17 C14 C15 108.3(3) . . ?
C17 C14 C16 106.8(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 C18 C19 110.4(3) . . ?
C4 C18 C20 111.8(3) . . ?
C4 C18 C21 109.0(3) . . ?
C19 C18 C21 108.7(3) . . ?
C20 C18 C19 107.8(3) . . ?
C20 C18 C21 109.1(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C22 C23 120.6(3) . . ?
O3 C22 C27 120.3(3) . . ?
C27 C22 C23 119.2(3) . . ?
C22 C23 C35 121.3(3) . . ?
C24 C23 C22 117.3(3) . . ?
C24 C23 C35 121.2(3) . . ?
C23 C24 H24 117.6 . . ?
C23 C24 C25 124.8(3) . . ?
C25 C24 H24 117.6 . . ?
C24 C25 C39 119.9(3) . . ?
C26 C25 C24 117.0(3) . . ?
C26 C25 C39 123.1(3) . . ?
C25 C26 H26 119.5 . . ?
C25 C26 C27 121.0(3) . . ?
C27 C26 H26 119.5 . . ?
C22 C27 C28 120.5(3) . . ?
C26 C27 C22 120.7(3) . . ?
C26 C27 C28 118.8(3) . . ?
O4 C28 C27 116.4(3) . . ?
N2 C28 O4 113.9(3) . . ?
N2 C28 C27 129.6(3) . . ?
O4 C29 C30 127.5(3) . . ?
O4 C29 C34 108.2(3) . . ?
C30 C29 C34 124.3(3) . . ?
C29 C30 H30 122.2 . . ?
C29 C30 C31 115.6(3) . . ?
C31 C30 H30 122.2 . . ?
C30 C31 H31 119.4 . . ?
C30 C31 C32 121.1(3) . . ?
C32 C31 H31 119.4 . . ?
C31 C32 H32 118.7 . . ?
C33 C32 C31 122.6(3) . . ?
C33 C32 H32 118.7 . . ?
C32 C33 H33 121.7 . . ?
C32 C33 C34 116.6(3) . . ?
C34 C33 H33 121.7 . . ?
C29 C34 N2 108.0(3) . . ?
C29 C34 C33 119.8(3) . . ?
C33 C34 N2 132.2(3) . . ?
C23 C35 C36 109.2(2) . . ?
C23 C35 C37 111.1(3) . . ?
C37 C35 C36 110.2(3) . . ?
C38 C35 C23 112.0(3) . . ?
C38 C35 C36 107.0(3) . . ?
C38 C35 C37 107.2(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
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 . . ?
C25 C39 C40 108.5(3) . . ?
C25 C39 C41 110.5(3) . . ?
C25 C39 C42 112.0(3) . . ?
C41 C39 C40 109.1(3) . . ?
C41 C39 C42 108.1(3) . . ?
C42 C39 C40 108.5(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C43 H43 108.3 . . ?
O5 C43 C44 109.4(3) . . ?
O5 C43 C45 109.9(3) . . ?
C44 C43 H43 108.3 . . ?
C45 C43 H43 108.3 . . ?
C45 C43 C44 112.6(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O6 C46 H46 108.1 . . ?
O6 C46 C47 110.1(3) . . ?
O6 C46 C48 110.2(3) . . ?
C47 C46 H46 108.1 . . ?
C48 C46 H46 108.1 . . ?
C48 C46 C47 112.2(3) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 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 C2 139.4(3) . . . . ?
Zr1 O1 C1 C6 -40.5(4) . . . . ?
Zr1 O3 C22 C23 129.9(3) . . . . ?
Zr1 O3 C22 C27 -49.4(4) . . . . ?
Zr1 O5 C43 C44 -99.6(7) . . . . ?
Zr1 O5 C43 C45 136.3(6) . . . . ?
Zr1 O6 C46 C47 6.0(13) . . . . ?
Zr1 O6 C46 C48 -118.2(11) . . . . ?
Zr1 N1 C7 O2 -165.67(19) . . . . ?
Zr1 N1 C7 C6 17.0(5) . . . . ?
Zr1 N1 C13 C8 164.7(2) . . . . ?
Zr1 N1 C13 C12 -17.4(5) . . . . ?
Zr1 N2 C28 O4 -161.87(18) . . . . ?
Zr1 N2 C28 C27 16.0(4) . . . . ?
Zr1 N2 C34 C29 158.9(2) . . . . ?
Zr1 N2 C34 C33 -21.7(5) . . . . ?
O1 C1 C2 C3 -176.8(3) . . . . ?
O1 C1 C2 C14 0.1(5) . . . . ?
O1 C1 C6 C5 177.9(3) . . . . ?
O1 C1 C6 C7 -4.4(5) . . . . ?
O2 C8 C9 C10 176.3(3) . . . . ?
O2 C8 C13 N1 0.2(4) . . . . ?
O2 C8 C13 C12 -178.0(3) . . . . ?
O3 C22 C23 C24 -178.6(3) . . . . ?
O3 C22 C23 C35 -1.8(4) . . . . ?
O3 C22 C27 C26 179.3(3) . . . . ?
O3 C22 C27 C28 0.7(4) . . . . ?
O4 C29 C30 C31 177.9(3) . . . . ?
O4 C29 C34 N2 1.0(3) . . . . ?
O4 C29 C34 C33 -178.5(3) . . . . ?
C1 C2 C3 C4 -1.9(5) . . . . ?
C1 C2 C14 C15 -65.2(4) . . . . ?
C1 C2 C14 C16 55.8(4) . . . . ?
C1 C2 C14 C17 175.1(3) . . . . ?
C1 C6 C7 O2 -166.9(3) . . . . ?
C1 C6 C7 N1 10.4(5) . . . . ?
C2 C1 C6 C5 -2.1(5) . . . . ?
C2 C1 C6 C7 175.7(3) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C2 C3 C4 C18 177.9(3) . . . . ?
C3 C2 C14 C15 111.6(4) . . . . ?
C3 C2 C14 C16 -127.3(3) . . . . ?
C3 C2 C14 C17 -8.1(5) . . . . ?
C3 C4 C5 C6 1.7(5) . . . . ?
C3 C4 C18 C19 53.3(4) . . . . ?
C3 C4 C18 C20 173.3(3) . . . . ?
C3 C4 C18 C21 -66.0(4) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C4 C5 C6 C7 -178.2(3) . . . . ?
C5 C4 C18 C19 -128.4(3) . . . . ?
C5 C4 C18 C20 -8.4(5) . . . . ?
C5 C4 C18 C21 112.3(4) . . . . ?
C5 C6 C7 O2 10.9(5) . . . . ?
C5 C6 C7 N1 -171.8(3) . . . . ?
C6 C1 C2 C3 3.2(5) . . . . ?
C6 C1 C2 C14 -179.9(3) . . . . ?
C7 O2 C8 C9 -175.9(3) . . . . ?
C7 O2 C8 C13 1.3(3) . . . . ?
C7 N1 C13 C8 -1.6(4) . . . . ?
C7 N1 C13 C12 176.2(4) . . . . ?
C8 O2 C7 N1 -2.5(4) . . . . ?
C8 O2 C7 C6 175.2(3) . . . . ?
C8 C9 C10 C11 0.9(5) . . . . ?
C9 C8 C13 N1 177.5(3) . . . . ?
C9 C8 C13 C12 -0.6(5) . . . . ?
C9 C10 C11 C12 -0.1(5) . . . . ?
C10 C11 C12 C13 -1.1(5) . . . . ?
C11 C12 C13 N1 -176.2(3) . . . . ?
C11 C12 C13 C8 1.4(5) . . . . ?
C13 N1 C7 O2 2.6(4) . . . . ?
C13 N1 C7 C6 -174.8(3) . . . . ?
C13 C8 C9 C10 -0.5(5) . . . . ?
C14 C2 C3 C4 -178.9(3) . . . . ?
C18 C4 C5 C6 -176.6(3) . . . . ?
C22 C23 C24 C25 -0.3(4) . . . . ?
C22 C23 C35 C36 -66.1(4) . . . . ?
C22 C23 C35 C37 55.7(4) . . . . ?
C22 C23 C35 C38 175.5(3) . . . . ?
C22 C27 C28 O4 -171.0(3) . . . . ?
C22 C27 C28 N2 11.2(5) . . . . ?
C23 C22 C27 C26 0.1(4) . . . . ?
C23 C22 C27 C28 -178.6(3) . . . . ?
C23 C24 C25 C26 -0.8(5) . . . . ?
C23 C24 C25 C39 -178.8(3) . . . . ?
C24 C23 C35 C36 110.6(3) . . . . ?
C24 C23 C35 C37 -127.7(3) . . . . ?
C24 C23 C35 C38 -7.8(4) . . . . ?
C24 C25 C26 C27 1.4(4) . . . . ?
C24 C25 C39 C40 73.0(4) . . . . ?
C24 C25 C39 C41 -46.6(4) . . . . ?
C24 C25 C39 C42 -167.3(3) . . . . ?
C25 C26 C27 C22 -1.1(5) . . . . ?
C25 C26 C27 C28 177.5(3) . . . . ?
C26 C25 C39 C40 -104.9(4) . . . . ?
C26 C25 C39 C41 135.4(3) . . . . ?
C26 C25 C39 C42 14.8(4) . . . . ?
C26 C27 C28 O4 10.4(4) . . . . ?
C26 C27 C28 N2 -167.4(3) . . . . ?
C27 C22 C23 C24 0.6(4) . . . . ?
C27 C22 C23 C35 177.4(3) . . . . ?
C28 O4 C29 C30 -178.6(3) . . . . ?
C28 O4 C29 C34 0.0(3) . . . . ?
C28 N2 C34 C29 -1.7(3) . . . . ?
C28 N2 C34 C33 177.7(3) . . . . ?
C29 O4 C28 N2 -1.2(3) . . . . ?
C29 O4 C28 C27 -179.4(3) . . . . ?
C29 C30 C31 C32 0.2(5) . . . . ?
C30 C29 C34 N2 179.8(3) . . . . ?
C30 C29 C34 C33 0.2(5) . . . . ?
C30 C31 C32 C33 0.5(5) . . . . ?
C31 C32 C33 C34 -0.8(5) . . . . ?
C32 C33 C34 N2 -178.9(3) . . . . ?
C32 C33 C34 C29 0.5(4) . . . . ?
C34 N2 C28 O4 1.9(3) . . . . ?
C34 N2 C28 C27 179.7(3) . . . . ?
C34 C29 C30 C31 -0.6(5) . . . . ?
C35 C23 C24 C25 -177.1(3) . . . . ?
C39 C25 C26 C27 179.4(3) . . . . ?

_olex2_date_sample_data_collection 2017-02-07
_olex2_date_sample_submission    1486335600
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C43(H43), C46(H46)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.512
_oxdiff_exptl_absorpt_empirical_full_min 0.684
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
####################################################################### 
# 
# 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_compound10
_database_code_depnum_ccdc_archive 'CCDC 1816373'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-07-20
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C68 H40 Hf N4 O8, 2(C H2 Cl2)'
_chemical_formula_sum            'C70 H44 Cl4 Hf N4 O8'
_chemical_formula_weight         1389.38
_chemical_absolute_configuration unk
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C70 H42 Cl4 Hf N4 O8 '
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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
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'

_cell_length_a                   12.08302(9)
_cell_length_b                   18.98014(13)
_cell_length_c                   27.6971(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6351.99(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    94740
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.2510
_cell_measurement_theta_min      2.7730
_exptl_absorpt_coefficient_mu    5.063
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2784
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 3 -5 0.0653
-1 -2 -5 0.0838
5 -9 -5 0.0463
4 5 5 0.0788
-4 -5 -5 0.0748
1 0 -5 0.0829
1 2 5 0.0938
0 -1 0 0.0307
0 1 0 0.0257
-5 9 5 0.0463
4 -9 6 0.0620
-4 9 -6 0.0620
-1 0 5 0.0829
-4 -3 5 0.0653

_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.056
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.9988 2.9981 -4.9907 -0.1813 0.5153 -0.3133
-0.9979 -1.9993 -4.9970 0.1148 -0.1783 -0.2732
5.0035 -8.9808 -5.0005 0.7951 0.4769 -0.3951
3.9960 4.9977 5.0008 -0.2924 0.5945 0.2492
-3.9960 -4.9977 -5.0008 0.2924 -0.5945 -0.2492
1.0008 -0.0003 -4.9945 -0.0037 0.0991 -0.2892
0.9979 1.9993 4.9970 -0.1148 0.1783 0.2732
0.0004 -0.9983 -0.0008 0.0797 -0.0136 -0.0057
-0.0004 0.9983 0.0008 -0.0797 0.0136 0.0057
-5.0035 8.9808 5.0005 -0.7951 -0.4769 0.3951
4.0015 -8.9787 5.9878 0.8277 0.4089 0.2248
-4.0015 8.9787 -5.9878 -0.8277 -0.4089 -0.2248
-1.0008 0.0003 4.9945 0.0037 -0.0991 0.2892
-3.9988 -2.9981 4.9907 0.1813 -0.5153 0.3133

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            184852
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.73
_diffrn_reflns_theta_min         2.82
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  33.00   1.00    2.04    --  -38.50  38.00 120.00   92
  2  ω   -116.00  -5.00   1.00    2.04    --  -38.50 -19.00 -30.00  111
  3  ω     57.00 127.00   1.00    2.04    --   43.20 178.00 -30.00   70
  4  ω     13.00 115.00   1.00    2.04    --   43.20  77.00   0.00  102
  5  ω     57.00 127.00   1.00    2.04    --   43.20 178.00  90.00   70
  6  ω     13.00 115.00   1.00    2.04    --   43.20  77.00-180.00  102
  7  ω     13.00 115.00   1.00    2.04    --   43.20  77.00 120.00  102
  8  ω     13.00 115.00   1.00    2.04    --   43.20  77.00 -60.00  102
  9  ω    -25.00  68.00   1.00    2.04    --   43.20 -57.00 -90.00   93
 10  ω     11.00  40.00   1.00    2.04    --   43.20  83.00  56.18   29
 11  ω     23.00 114.00   1.00    2.04    --   43.20  38.00 120.00   91
 12  ω     13.00 115.00   1.00    2.04    --   43.20  77.00-120.00  102
 13  ω      1.00  82.00   1.00    2.04    --   43.20 -99.00-180.00   81
 14  ω     23.00 114.00   1.00    2.04    --   43.20  38.00-150.00   91
 15  ω     82.00 178.00   1.00    8.18    --  111.00  72.00-151.42   96
 16  ω     81.00 178.00   1.00    8.18    --  111.00  76.00-104.60   97
 17  ω     84.00 178.00   1.00    8.18    --  111.00  65.00-111.47   94
 18  ω     84.00 178.00   1.00    8.18    --  111.00  63.00 124.17   94
 19  ω     81.00 178.00   1.00    8.18    --  111.00  77.00-180.00   97
 20  ω     40.00 141.00   1.00    8.18    --  111.00 -77.00  30.00  101
 21  ω     81.00 178.00   1.00    8.18    --  111.00  76.00 -68.10   97
 22  ω     81.00 178.00   1.00    8.18    --  111.00  77.00 -60.00   97
 23  ω     81.00 178.00   1.00    8.18    --  111.00  77.00  90.00   97
 24  ω     81.00 178.00   1.00    8.18    --  111.00  77.00 -90.00   97
 25  ω     41.00 122.00   1.00    8.18    --  111.00-125.00  30.00   81
 26  ω     81.00 178.00   1.00    8.18    --  111.00  77.00 150.00   97
 27  ω     81.00 178.00   1.00    8.18    --  111.00  76.00 -38.09   97
 28  ω     85.00 178.00   1.00    8.18    --  111.00  61.00-168.13   93
 29  ω     85.00 178.00   1.00    8.18    --  111.00  61.00 -60.00   93
 30  ω     82.00 178.00   1.00    8.18    --  111.00  73.00   5.27   96
 31  ω     85.00 178.00   1.00    8.18    --  111.00  61.00 -30.00   93
 32  ω     85.00 178.00   1.00    8.18    --  111.00  61.00 120.00   93
 33  ω     85.00 178.00   1.00    8.18    --  111.00  60.00 -93.38   93
 34  ω     85.00 178.00   1.00    8.18    --  111.00  62.00  35.35   93
 35  ω     81.00 178.00   1.00    8.18    --  111.00  77.00  30.00   97
 36  ω     81.00 178.00   1.00    8.18    --  111.00  77.00-150.00   97
 37  ω     81.00 178.00   1.00    8.18    --  111.00  77.00 120.00   97
 38  ω     85.00 178.00   1.00    8.18    --  111.00  61.00 150.00   93
 39  ω     81.00 178.00   1.00    8.18    --  111.00  77.00 -30.00   97
 40  ω     85.00 178.00   1.00    8.18    --  111.00  61.00  30.00   93
 41  ω     85.00 178.00   1.00    8.18    --  111.00  61.00   0.00   93
 42  ω     81.00 174.00   1.00    8.18    --  111.00  77.00  60.00   93
 43  ω     85.00 111.00   1.00    8.18    --  111.00  61.00-180.00   26
 44  ω     85.00 115.00   1.00    8.18    --  111.00  61.00  60.00   30
 45  ω     85.00 111.00   1.00    8.18    --  111.00  59.00  14.43   26
 46  ω     41.00 101.00   1.00    8.18    --  111.00-125.00-150.00   60
 47  ω     82.00 140.00   1.00    8.18    --  111.00 -77.00 -30.00   58
 48  ω     85.00 152.00   1.00    8.18    --  111.00  61.00-150.00   67
 49  ω     85.00 111.00   1.00    8.18    --  111.00  61.00-120.00   26
 50  ω     43.00 109.00   1.00    8.18    --  111.00 -94.00-120.00   66
 51  ω     41.00 121.00   1.00    8.18    --  111.00-125.00 150.00   80
 52  ω     85.00 111.00   1.00    8.18    --  111.00  61.00  90.00   26
 53  ω     51.00 137.00   1.00    8.18    --  111.00 -61.00-120.00   86
 54  ω     65.00 122.00   1.00    8.18    --  111.00-125.00-120.00   57
 55  ω     83.00 108.00   1.00    8.18    --  111.00  72.00  54.15   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0205329000
_diffrn_orient_matrix_UB_12      -0.0797918000
_diffrn_orient_matrix_UB_13      0.0048556000
_diffrn_orient_matrix_UB_21      0.1251043000
_diffrn_orient_matrix_UB_22      0.0136917000
_diffrn_orient_matrix_UB_23      0.0052222000
_diffrn_orient_matrix_UB_31      -0.0137192000
_diffrn_orient_matrix_UB_32      0.0056382000
_diffrn_orient_matrix_UB_33      0.0551636000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12231
_reflns_number_total             12561
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.965
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
 
 Highly disordered solvent in four voids were squeezed
 with the SQUEEZE procedure of Olex2 program 
 (Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; 
 Puschmann, H., J. Appl. Cryst. (2009). 42, 339-341.)
 The sum formular and further calculations disregard this 
 electron density.

Miller array info: D:\Data\lisa37\struct\olex2_lisa37\lisa37.hkl:Iobs,SigIobs
Observation type: xray.intensity
Type of data: double, size=184852
Type of sigmas: double, size=184852
Number of Miller indices: 184852
Anomalous flag: True
Unit cell: (12.083, 18.9801, 27.6971, 90, 90, 90)
Space group: P 21 21 2 (No. 18)
Systematic absences: 148
Systematic absences not included in following:
Centric reflections: 18083
Resolution range: 15.6567 0.807313

use_set_completion: False
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
    C    Cl     H    Hf     N     O
 1.70  1.75  1.09  2.00  1.55  1.52

Total solvent accessible volume / cell = 949.8 Ang^3 [15.0%]
Total electron count / cell = 264.4

gridding: (60,96,144)
Void #Grid points Vol/A^3 Vol/%  Centre of mass (frac)   Eigenvectors (frac)
   1        26653   204.1   3.2  (-0.000,-0.000, 0.453)  1  ( 0.980, 0.199, 0.000)
                                                         2  (-0.199, 0.980, 0.000)
                                                         3  ( 0.000, 0.000, 1.000)
   2        35362   270.8   4.3  (-0.000, 0.500, 0.104)  1  ( 0.966, 0.260, 0.000)
                                                         2  (-0.260, 0.966, 0.000)
                                                         3  ( 0.000, 0.000, 1.000)
   3        35362   270.8   4.3  ( 0.500,-0.000, 0.896)  1  ( 0.966,-0.260, 0.000)
                                                         2  ( 0.260, 0.966, 0.000)
                                                         3  ( 0.000, 0.000, 1.000)
   4        26653   204.1   3.2  ( 0.500, 0.500, 0.547)  1  ( 0.980,-0.199, 0.000)
                                                         2  ( 0.199, 0.980, 0.000)
                                                         3  ( 0.000, 0.000, 1.000)

Void  Vol/Ang^3  #Electrons
   1      204.1         58.5
   2      270.8         96.9
   3      270.8         97.7
   4      204.1         57.8


;
_refine_ls_abs_structure_Flack   0.481(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         12561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.028
_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)+(0.0565P)²+8.9315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0902
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 1.0000 1.0000 0.03280(2) 0.01732(8) Uani 1 2 d S T P . .
O1 O 0.8505(3) 0.96094(17) 0.05747(13) 0.0209(7) Uani 1 1 d . . . . .
O2 O 1.0212(3) 0.88139(18) 0.17523(12) 0.0249(8) Uani 1 1 d . . . . .
O3 O 1.0598(3) 0.90351(17) 0.00797(12) 0.0210(7) Uani 1 1 d . . . . .
O4 O 1.2151(3) 1.00987(19) -0.10249(12) 0.0235(7) Uani 1 1 d . . . . .
N1 N 1.0378(3) 0.9288(2) 0.10135(14) 0.0175(8) Uani 1 1 d . . . . .
N2 N 1.1148(3) 1.0242(2) -0.03516(14) 0.0172(8) Uani 1 1 d . . . . .
C1 C 0.8000(4) 0.9476(3) 0.09854(18) 0.0200(9) Uani 1 1 d . . . . .
C2 C 0.6812(4) 0.9473(3) 0.09793(19) 0.0235(10) Uani 1 1 d . . . . .
H2 H 0.6440 0.9540 0.0689 0.028 Uiso 1 1 calc R U . . .
C3 C 0.6230(4) 0.9374(3) 0.1388(2) 0.0244(10) Uani 1 1 d . . . . .
H3 H 0.5462 0.9356 0.1372 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6755(4) 0.9297(3) 0.1842(2) 0.0248(10) Uani 1 1 d . . . . .
C5 C 0.6128(5) 0.9224(3) 0.2267(2) 0.0307(12) Uani 1 1 d . . . . .
H5 H 0.5360 0.9220 0.2246 0.037 Uiso 1 1 calc R U . . .
C6 C 0.6624(5) 0.9157(3) 0.2713(2) 0.0364(13) Uani 1 1 d . . . . .
H6 H 0.6202 0.9096 0.2990 0.044 Uiso 1 1 calc R U . . .
C7 C 0.7784(6) 0.9184(4) 0.2736(2) 0.0402(14) Uani 1 1 d . . . . .
H7 H 0.8128 0.9162 0.3036 0.048 Uiso 1 1 calc R U . . .
C8 C 0.8425(5) 0.9242(3) 0.2328(2) 0.0338(12) Uani 1 1 d . . . . .
H8 H 0.9191 0.9256 0.2357 0.041 Uiso 1 1 calc R U . . .
C9 C 0.7936(4) 0.9280(3) 0.18671(19) 0.0242(10) Uani 1 1 d . . . . .
C10 C 0.8553(4) 0.9336(3) 0.14203(18) 0.0211(10) Uani 1 1 d . . . . .
C11 C 0.9722(4) 0.9177(2) 0.13821(18) 0.0203(10) Uani 1 1 d . . . . .
C12 C 1.1276(4) 0.8671(3) 0.15932(18) 0.0224(10) Uani 1 1 d . . . . .
C13 C 1.2095(5) 0.8319(3) 0.1833(2) 0.0306(11) Uani 1 1 d . . . . .
H13 H 1.1994 0.8144 0.2143 0.037 Uiso 1 1 calc R U . . .
C14 C 1.3094(5) 0.8238(3) 0.1584(2) 0.0307(12) Uani 1 1 d . . . . .
H14 H 1.3679 0.7999 0.1728 0.037 Uiso 1 1 calc R U . . .
C15 C 1.3222(5) 0.8515(3) 0.1115(2) 0.0275(11) Uani 1 1 d . . . . .
H15 H 1.3896 0.8459 0.0958 0.033 Uiso 1 1 calc R U . . .
C16 C 1.2373(4) 0.8870(3) 0.08799(19) 0.0222(10) Uani 1 1 d . . . . .
H16 H 1.2466 0.9048 0.0570 0.027 Uiso 1 1 calc R U . . .
C17 C 1.1376(4) 0.8949(2) 0.11277(18) 0.0203(10) Uani 1 1 d . . . . .
C18 C 1.0781(4) 0.8723(2) -0.03368(17) 0.0174(9) Uani 1 1 d . . . . .
C19 C 1.0686(4) 0.7971(3) -0.03509(19) 0.0240(10) Uani 1 1 d . . . . .
H19 H 1.0517 0.7729 -0.0068 0.029 Uiso 1 1 calc R U . . .
C20 C 1.0835(4) 0.7606(3) -0.0763(2) 0.0254(10) Uani 1 1 d . . . . .
H20 H 1.0781 0.7117 -0.0759 0.030 Uiso 1 1 calc R U . . .
C21 C 1.1076(4) 0.7959(3) -0.12052(19) 0.0247(10) Uani 1 1 d . . . . .
C22 C 1.1202(5) 0.7562(3) -0.1635(2) 0.0313(12) Uani 1 1 d . . . . .
H22 H 1.1111 0.7075 -0.1626 0.038 Uiso 1 1 calc R U . . .
C23 C 1.1457(5) 0.7883(3) -0.2063(2) 0.0355(13) Uani 1 1 d . . . . .
H23 H 1.1556 0.7617 -0.2342 0.043 Uiso 1 1 calc R U . . .
C24 C 1.1566(5) 0.8617(3) -0.2075(2) 0.0334(13) Uani 1 1 d . . . . .
H24 H 1.1732 0.8836 -0.2367 0.040 Uiso 1 1 calc R U . . .
C25 C 1.1433(4) 0.9025(3) -0.16633(19) 0.0261(11) Uani 1 1 d . . . . .
H25 H 1.1484 0.9513 -0.1685 0.031 Uiso 1 1 calc R U . . .
C26 C 1.1218(4) 0.8703(3) -0.12061(18) 0.0224(10) Uani 1 1 d . . . . .
C27 C 1.1104(4) 0.9078(3) -0.07617(18) 0.0202(9) Uani 1 1 d . . . . .
C28 C 1.1413(4) 0.9817(2) -0.07007(18) 0.0219(11) Uani 1 1 d . . . . .
C29 C 1.2357(4) 1.0767(3) -0.0855(2) 0.0257(11) Uani 1 1 d . . . . .
C30 C 1.3050(5) 1.1268(3) -0.1053(2) 0.0339(13) Uani 1 1 d . . . . .
H30 H 1.3462 1.1185 -0.1330 0.041 Uiso 1 1 calc R U . . .
C31 C 1.3087(5) 1.1907(3) -0.0806(2) 0.0334(13) Uani 1 1 d . . . . .
H31 H 1.3528 1.2268 -0.0927 0.040 Uiso 1 1 calc R U . . .
C32 C 1.2482(5) 1.2025(3) -0.0381(2) 0.0311(12) Uani 1 1 d . . . . .
H32 H 1.2529 1.2459 -0.0226 0.037 Uiso 1 1 calc R U . . .
C33 C 1.1812(4) 1.1496(3) -0.0188(2) 0.0255(10) Uani 1 1 d . . . . .
H33 H 1.1419 1.1566 0.0097 0.031 Uiso 1 1 calc R U . . .
C34 C 1.1754(4) 1.0863(3) -0.04349(19) 0.0218(10) Uani 1 1 d . . . . .
Hf2 Hf 1.0000 0.5000 0.45820(2) 0.01920(8) Uani 1 2 d S T P . .
O5 O 0.9355(3) 0.59452(18) 0.48524(13) 0.0217(7) Uani 1 1 d . . . . .
O6 O 0.7879(4) 0.4780(2) 0.59325(14) 0.0333(9) Uani 1 1 d . . . . .
O7 O 1.1526(3) 0.53380(19) 0.43281(13) 0.0235(7) Uani 1 1 d . . . . .
O8 O 0.9937(4) 0.64517(19) 0.32538(11) 0.0266(7) Uani 1 1 d . . . . .
N3 N 0.8857(3) 0.4708(2) 0.52513(15) 0.0198(8) Uani 1 1 d . . . . .
N4 N 0.9687(3) 0.5768(2) 0.39098(15) 0.0206(8) Uani 1 1 d . . . . .
C35 C 0.9219(4) 0.6220(3) 0.52870(18) 0.0199(9) Uani 1 1 d . . . . .
C36 C 0.9366(4) 0.6964(3) 0.53328(19) 0.0231(10) Uani 1 1 d . . . . .
H36 H 0.9503 0.7231 0.5058 0.028 Uiso 1 1 calc R U . . .
C37 C 0.9311(4) 0.7289(3) 0.5766(2) 0.0260(11) Uani 1 1 d . . . . .
H37 H 0.9409 0.7774 0.5784 0.031 Uiso 1 1 calc R U . . .
C38 C 0.9103(4) 0.6895(3) 0.61992(19) 0.0245(10) Uani 1 1 d . . . . .
C39 C 0.9115(4) 0.7228(3) 0.6658(2) 0.0269(11) Uani 1 1 d . . . . .
H39 H 0.9264 0.7708 0.6676 0.032 Uiso 1 1 calc R U . . .
C40 C 0.8915(5) 0.6863(3) 0.7070(2) 0.0308(12) Uani 1 1 d . . . . .
H40 H 0.8923 0.7091 0.7367 0.037 Uiso 1 1 calc R U . . .
C41 C 0.8692(4) 0.6129(3) 0.7043(2) 0.0283(11) Uani 1 1 d . . . . .
H41 H 0.8548 0.5876 0.7324 0.034 Uiso 1 1 calc R U . . .
C42 C 0.8689(4) 0.5792(3) 0.66064(19) 0.0268(11) Uani 1 1 d . . . . .
H42 H 0.8555 0.5309 0.6596 0.032 Uiso 1 1 calc R U . . .
C43 C 0.8886(4) 0.6161(3) 0.61654(18) 0.0223(10) Uani 1 1 d . . . . .
C44 C 0.8904(4) 0.5822(3) 0.56957(19) 0.0227(10) Uani 1 1 d . . . . .
C45 C 0.8607(4) 0.5111(2) 0.56197(17) 0.0195(10) Uani 1 1 d . . . . .
C46 C 0.7693(5) 0.4125(3) 0.5738(2) 0.0293(12) Uani 1 1 d . . . . .
C47 C 0.7026(6) 0.3592(3) 0.5916(2) 0.0395(15) Uani 1 1 d . . . . .
H47 H 0.6616 0.3641 0.6198 0.047 Uiso 1 1 calc R U . . .
C48 C 0.7010(5) 0.2973(3) 0.5641(2) 0.0321(12) Uani 1 1 d . . . . .
H48 H 0.6595 0.2592 0.5749 0.039 Uiso 1 1 calc R U . . .
C49 C 0.7595(4) 0.2912(3) 0.5212(2) 0.0269(11) Uani 1 1 d . . . . .
H49 H 0.7565 0.2490 0.5041 0.032 Uiso 1 1 calc R U . . .
C50 C 0.8228(4) 0.3467(3) 0.50314(19) 0.0234(10) Uani 1 1 d . . . . .
H50 H 0.8600 0.3431 0.4738 0.028 Uiso 1 1 calc R U . . .
C51 C 0.8277(4) 0.4079(3) 0.53109(19) 0.0219(10) Uani 1 1 d . . . . .
C52 C 1.2071(4) 0.5550(3) 0.39501(18) 0.0212(10) Uani 1 1 d . . . . .
C53 C 1.3248(4) 0.5491(3) 0.3976(2) 0.0280(11) Uani 1 1 d . . . . .
H53 H 1.3581 0.5336 0.4259 0.034 Uiso 1 1 calc R U . . .
C54 C 1.3882(4) 0.5657(3) 0.3590(2) 0.0263(11) Uani 1 1 d . . . . .
H54 H 1.4645 0.5602 0.3611 0.032 Uiso 1 1 calc R U . . .
C55 C 1.3412(4) 0.5913(3) 0.3158(2) 0.0258(10) Uani 1 1 d . . . . .
C56 C 1.4096(5) 0.6060(3) 0.2751(2) 0.0310(12) Uani 1 1 d . . . . .
H56 H 1.4847 0.5957 0.2767 0.037 Uiso 1 1 calc R U . . .
C57 C 1.3675(5) 0.6349(3) 0.2337(2) 0.0382(14) Uani 1 1 d . . . . .
H57 H 1.4133 0.6436 0.2074 0.046 Uiso 1 1 calc R U . . .
C58 C 1.2557(5) 0.6510(4) 0.2314(2) 0.0385(14) Uani 1 1 d . . . . .
H58 H 1.2273 0.6717 0.2037 0.046 Uiso 1 1 calc R U . . .
C59 C 1.1866(5) 0.6368(3) 0.2694(2) 0.0349(13) Uani 1 1 d . . . . .
H59 H 1.1120 0.6484 0.2667 0.042 Uiso 1 1 calc R U . . .
C60 C 1.2247(4) 0.6051(3) 0.31263(19) 0.0241(10) Uani 1 1 d . . . . .
C61 C 1.1575(4) 0.5854(3) 0.35397(18) 0.0207(10) Uani 1 1 d . . . . .
C62 C 1.0401(4) 0.5996(3) 0.35810(18) 0.0232(10) Uani 1 1 d . . . . .
C63 C 0.8849(4) 0.6531(3) 0.33916(18) 0.0249(10) Uani 1 1 d . . . . .
C64 C 0.8058(5) 0.6953(3) 0.3176(2) 0.0319(12) Uani 1 1 d . . . . .
H64 H 0.8203 0.7225 0.2904 0.038 Uiso 1 1 calc R U . . .
C65 C 0.7029(5) 0.6937(3) 0.3399(2) 0.0364(13) Uani 1 1 d . . . . .
H65 H 0.6449 0.7196 0.3267 0.044 Uiso 1 1 calc R U . . .
C66 C 0.6844(4) 0.6541(3) 0.3814(2) 0.0312(12) Uani 1 1 d . . . . .
H66 H 0.6148 0.6553 0.3957 0.037 Uiso 1 1 calc R U . . .
C67 C 0.7663(4) 0.6128(3) 0.4022(2) 0.0260(11) Uani 1 1 d . . . . .
H67 H 0.7531 0.5868 0.4301 0.031 Uiso 1 1 calc R U . . .
C68 C 0.8679(4) 0.6121(3) 0.37982(19) 0.0234(10) Uani 1 1 d . . . . .
Cl1 Cl 0.89918(14) 0.75814(9) 0.09375(6) 0.0455(4) Uani 1 1 d . . . . .
Cl2 Cl 0.97179(13) 0.70642(8) 0.18757(6) 0.0423(3) Uani 1 1 d . . . . .
C69 C 0.9041(6) 0.6857(3) 0.1329(3) 0.0434(15) Uani 1 1 d . . . . .
H69A H 0.9426 0.6472 0.1172 0.052 Uiso 1 1 calc R U . . .
H69B H 0.8292 0.6702 0.1399 0.052 Uiso 1 1 calc R U . . .
Cl3 Cl 1.03233(13) 0.82469(10) 0.30602(6) 0.0506(4) Uani 1 1 d . . . . .
Cl4 Cl 1.08377(17) 0.77523(12) 0.40341(6) 0.0580(5) Uani 1 1 d . . . . .
C70 C 1.1352(6) 0.7959(4) 0.3453(3) 0.0467(16) Uani 1 1 d . . . . .
H70A H 1.1911 0.8323 0.3482 0.056 Uiso 1 1 calc R U . . .
H70B H 1.1703 0.7544 0.3317 0.056 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1 2.069(3) 2_775 ?
Hf1 O1 2.069(3) . ?
Hf1 O3 2.085(3) . ?
Hf1 O3 2.085(3) 2_775 ?
Hf1 N1 2.375(4) . ?
Hf1 N1 2.375(4) 2_775 ?
Hf1 N2 2.383(4) . ?
Hf1 N2 2.382(4) 2_775 ?
O1 C1 1.315(6) . ?
O2 C11 1.370(6) . ?
O2 C12 1.385(6) . ?
O3 C18 1.315(6) . ?
O4 C28 1.373(6) . ?
O4 C29 1.376(7) . ?
N1 C11 1.309(6) . ?
N1 C17 1.403(6) . ?
N2 C28 1.299(6) . ?
N2 C34 1.407(6) . ?
C1 C2 1.436(7) . ?
C1 C10 1.403(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.345(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.417(8) . ?
C4 C5 1.407(7) . ?
C4 C9 1.429(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.378(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.404(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.374(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.409(8) . ?
C9 C10 1.448(7) . ?
C10 C11 1.449(7) . ?
C12 C13 1.366(7) . ?
C12 C17 1.398(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.400(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.408(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.395(7) . ?
C18 C19 1.433(7) . ?
C18 C27 1.411(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.347(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.427(8) . ?
C21 C22 1.417(7) . ?
C21 C26 1.422(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.368(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.400(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.389(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.430(7) . ?
C26 C27 1.429(7) . ?
C27 C28 1.462(7) . ?
C29 C30 1.380(8) . ?
C29 C34 1.385(8) . ?
C30 H30 0.9300 . ?
C30 C31 1.392(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.403(9) . ?
C32 H32 0.9300 . ?
C32 C33 1.396(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.384(7) . ?
Hf2 O5 2.094(3) 2_765 ?
Hf2 O5 2.094(3) . ?
Hf2 O7 2.075(3) 2_765 ?
Hf2 O7 2.075(3) . ?
Hf2 N3 2.377(4) 2_765 ?
Hf2 N3 2.377(4) . ?
Hf2 N4 2.395(4) 2_765 ?
Hf2 N4 2.395(4) . ?
O5 C35 1.322(6) . ?
O6 C45 1.385(6) . ?
O6 C46 1.374(7) . ?
O7 C52 1.301(6) . ?
O8 C62 1.372(6) . ?
O8 C63 1.377(7) . ?
N3 C45 1.310(7) . ?
N3 C51 1.395(7) . ?
N4 C62 1.327(7) . ?
N4 C68 1.424(6) . ?
C35 C36 1.430(7) . ?
C35 C44 1.412(7) . ?
C36 H36 0.9300 . ?
C36 C37 1.351(8) . ?
C37 H37 0.9300 . ?
C37 C38 1.435(7) . ?
C38 C39 1.418(7) . ?
C38 C43 1.421(7) . ?
C39 H39 0.9300 . ?
C39 C40 1.357(8) . ?
C40 H40 0.9300 . ?
C40 C41 1.421(8) . ?
C41 H41 0.9300 . ?
C41 C42 1.368(8) . ?
C42 H42 0.9300 . ?
C42 C43 1.428(7) . ?
C43 C44 1.451(7) . ?
C44 C45 1.413(7) . ?
C46 C47 1.384(8) . ?
C46 C51 1.381(7) . ?
C47 H47 0.9300 . ?
C47 C48 1.400(8) . ?
C48 H48 0.9300 . ?
C48 C49 1.386(8) . ?
C49 H49 0.9300 . ?
C49 C50 1.395(7) . ?
C50 H50 0.9300 . ?
C50 C51 1.398(7) . ?
C52 C53 1.429(7) . ?
C52 C61 1.408(7) . ?
C53 H53 0.9300 . ?
C53 C54 1.351(8) . ?
C54 H54 0.9300 . ?
C54 C55 1.413(8) . ?
C55 C56 1.425(7) . ?
C55 C60 1.434(7) . ?
C56 H56 0.9300 . ?
C56 C57 1.367(9) . ?
C57 H57 0.9300 . ?
C57 C58 1.386(9) . ?
C58 H58 0.9300 . ?
C58 C59 1.370(8) . ?
C59 H59 0.9300 . ?
C59 C60 1.418(8) . ?
C60 C61 1.453(7) . ?
C61 C62 1.449(7) . ?
C63 C64 1.383(7) . ?
C63 C68 1.385(7) . ?
C64 H64 0.9300 . ?
C64 C65 1.389(9) . ?
C65 H65 0.9300 . ?
C65 C66 1.393(9) . ?
C66 H66 0.9300 . ?
C66 C67 1.387(8) . ?
C67 H67 0.9300 . ?
C67 C68 1.375(7) . ?
Cl1 C69 1.752(6) . ?
Cl2 C69 1.764(7) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
Cl3 C70 1.739(7) . ?
Cl4 C70 1.769(7) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?

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 O1 141.43(19) . 2_775 ?
O1 Hf1 O3 95.55(13) . . ?
O1 Hf1 O3 96.95(13) 2_775 . ?
O1 Hf1 O3 96.95(13) . 2_775 ?
O1 Hf1 O3 95.55(13) 2_775 2_775 ?
O1 Hf1 N1 72.53(14) . . ?
O1 Hf1 N1 76.83(14) 2_775 . ?
O1 Hf1 N1 72.53(14) 2_775 2_775 ?
O1 Hf1 N1 76.83(14) . 2_775 ?
O1 Hf1 N2 71.56(14) 2_775 . ?
O1 Hf1 N2 71.55(14) . 2_775 ?
O1 Hf1 N2 146.96(13) 2_775 2_775 ?
O1 Hf1 N2 146.95(13) . . ?
O3 Hf1 O3 141.50(18) 2_775 . ?
O3 Hf1 N1 146.11(13) . 2_775 ?
O3 Hf1 N1 72.36(13) 2_775 2_775 ?
O3 Hf1 N1 72.36(13) . . ?
O3 Hf1 N1 146.11(13) 2_775 . ?
O3 Hf1 N2 76.84(14) 2_775 . ?
O3 Hf1 N2 72.95(13) . . ?
O3 Hf1 N2 76.84(14) . 2_775 ?
O3 Hf1 N2 72.95(13) 2_775 2_775 ?
N1 Hf1 N1 73.87(19) 2_775 . ?
N1 Hf1 N2 128.99(14) . . ?
N1 Hf1 N2 129.33(14) 2_775 . ?
N1 Hf1 N2 129.33(14) . 2_775 ?
N1 Hf1 N2 128.98(14) 2_775 2_775 ?
N2 Hf1 N2 75.63(19) 2_775 . ?
C1 O1 Hf1 139.4(3) . . ?
C11 O2 C12 105.1(4) . . ?
C18 O3 Hf1 137.9(3) . . ?
C28 O4 C29 104.6(4) . . ?
C11 N1 Hf1 126.7(3) . . ?
C11 N1 C17 105.7(4) . . ?
C17 N1 Hf1 127.3(3) . . ?
C28 N2 Hf1 127.8(3) . . ?
C28 N2 C34 105.6(4) . . ?
C34 N2 Hf1 126.4(3) . . ?
O1 C1 C2 117.0(5) . . ?
O1 C1 C10 123.9(5) . . ?
C10 C1 C2 119.0(5) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.9(5) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.8(5) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C9 119.5(5) . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 C9 119.7(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.6(5) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 120.9 . . ?
C5 C6 C7 118.1(5) . . ?
C7 C6 H6 120.9 . . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.9(6) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.9(6) . . ?
C9 C8 H8 119.6 . . ?
C4 C9 C10 118.1(5) . . ?
C8 C9 C4 117.6(5) . . ?
C8 C9 C10 124.3(5) . . ?
C1 C10 C9 120.2(5) . . ?
C1 C10 C11 116.2(4) . . ?
C9 C10 C11 123.3(5) . . ?
O2 C11 C10 118.1(4) . . ?
N1 C11 O2 113.7(4) . . ?
N1 C11 C10 127.9(5) . . ?
O2 C12 C17 107.4(4) . . ?
C13 C12 O2 127.8(5) . . ?
C13 C12 C17 124.7(5) . . ?
C12 C13 H13 122.0 . . ?
C12 C13 C14 116.1(5) . . ?
C14 C13 H13 122.0 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.5(5) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 118.9 . . ?
C16 C15 C14 122.2(5) . . ?
C16 C15 H15 118.9 . . ?
C15 C16 H16 121.4 . . ?
C15 C16 C17 117.3(5) . . ?
C17 C16 H16 121.4 . . ?
C12 C17 N1 107.8(4) . . ?
C16 C17 N1 132.9(5) . . ?
C16 C17 C12 119.2(5) . . ?
O3 C18 C19 117.3(4) . . ?
O3 C18 C27 124.3(4) . . ?
C27 C18 C19 118.3(4) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 C18 121.7(5) . . ?
C20 C19 H19 119.2 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.9(5) . . ?
C21 C20 H20 119.6 . . ?
C22 C21 C20 119.5(5) . . ?
C22 C21 C26 120.9(5) . . ?
C26 C21 C20 119.5(5) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 121.0(5) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 H23 120.5 . . ?
C22 C23 C24 119.1(5) . . ?
C24 C23 H23 120.5 . . ?
C23 C24 H24 119.2 . . ?
C25 C24 C23 121.6(6) . . ?
C25 C24 H24 119.2 . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.7(5) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 116.6(5) . . ?
C21 C26 C27 118.8(5) . . ?
C27 C26 C25 124.5(5) . . ?
C18 C27 C26 120.5(4) . . ?
C18 C27 C28 115.6(4) . . ?
C26 C27 C28 123.6(5) . . ?
O4 C28 C27 117.6(4) . . ?
N2 C28 O4 114.0(4) . . ?
N2 C28 C27 128.2(5) . . ?
O4 C29 C30 127.5(5) . . ?
O4 C29 C34 108.3(4) . . ?
C30 C29 C34 124.2(5) . . ?
C29 C30 H30 122.4 . . ?
C29 C30 C31 115.2(6) . . ?
C31 C30 H30 122.4 . . ?
C30 C31 H31 118.9 . . ?
C30 C31 C32 122.2(5) . . ?
C32 C31 H31 118.9 . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(5) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 121.2 . . ?
C34 C33 C32 117.7(5) . . ?
C34 C33 H33 121.2 . . ?
C29 C34 N2 107.5(5) . . ?
C33 C34 N2 132.3(5) . . ?
C33 C34 C29 120.2(5) . . ?
O5 Hf2 O5 138.10(19) 2_765 . ?
O5 Hf2 N3 72.81(14) . . ?
O5 Hf2 N3 74.80(14) 2_765 . ?
O5 Hf2 N3 74.80(14) . 2_765 ?
O5 Hf2 N3 72.82(14) 2_765 2_765 ?
O5 Hf2 N4 149.11(13) . 2_765 ?
O5 Hf2 N4 149.11(13) 2_765 . ?
O5 Hf2 N4 72.41(14) 2_765 2_765 ?
O5 Hf2 N4 72.41(14) . . ?
O7 Hf2 O5 100.77(14) 2_765 2_765 ?
O7 Hf2 O5 93.19(13) . 2_765 ?
O7 Hf2 O5 93.19(13) 2_765 . ?
O7 Hf2 O5 100.77(14) . . ?
O7 Hf2 O7 140.4(2) 2_765 . ?
O7 Hf2 N3 71.11(14) 2_765 . ?
O7 Hf2 N3 148.49(14) . . ?
O7 Hf2 N3 71.11(14) . 2_765 ?
O7 Hf2 N3 148.49(14) 2_765 2_765 ?
O7 Hf2 N4 71.85(13) 2_765 2_765 ?
O7 Hf2 N4 77.54(14) . 2_765 ?
O7 Hf2 N4 77.54(14) 2_765 . ?
O7 Hf2 N4 71.85(13) . . ?
N3 Hf2 N3 77.5(2) . 2_765 ?
N3 Hf2 N4 123.81(14) . 2_765 ?
N3 Hf2 N4 131.03(14) 2_765 2_765 ?
N3 Hf2 N4 131.03(14) . . ?
N3 Hf2 N4 123.81(14) 2_765 . ?
N4 Hf2 N4 77.92(19) . 2_765 ?
C35 O5 Hf2 135.2(3) . . ?
C46 O6 C45 105.6(4) . . ?
C52 O7 Hf2 144.9(3) . . ?
C62 O8 C63 106.0(4) . . ?
C45 N3 Hf2 127.3(3) . . ?
C45 N3 C51 106.9(4) . . ?
C51 N3 Hf2 125.7(3) . . ?
C62 N4 Hf2 129.0(3) . . ?
C62 N4 C68 104.7(4) . . ?
C68 N4 Hf2 126.1(3) . . ?
O5 C35 C36 117.1(5) . . ?
O5 C35 C44 123.6(4) . . ?
C44 C35 C36 119.3(5) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.6(5) . . ?
C37 C36 H36 119.2 . . ?
C36 C37 H37 119.5 . . ?
C36 C37 C38 120.9(5) . . ?
C38 C37 H37 119.5 . . ?
C39 C38 C37 121.0(5) . . ?
C39 C38 C43 119.8(5) . . ?
C43 C38 C37 119.2(5) . . ?
C38 C39 H39 119.2 . . ?
C40 C39 C38 121.6(5) . . ?
C40 C39 H39 119.2 . . ?
C39 C40 H40 120.3 . . ?
C39 C40 C41 119.3(5) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 119.8 . . ?
C42 C41 C40 120.4(5) . . ?
C42 C41 H41 119.8 . . ?
C41 C42 H42 119.1 . . ?
C41 C42 C43 121.7(5) . . ?
C43 C42 H42 119.1 . . ?
C38 C43 C42 117.1(5) . . ?
C38 C43 C44 119.4(5) . . ?
C42 C43 C44 123.5(5) . . ?
C35 C44 C43 119.1(5) . . ?
C35 C44 C45 117.3(5) . . ?
C45 C44 C43 123.6(5) . . ?
O6 C45 C44 120.1(4) . . ?
N3 C45 O6 111.7(4) . . ?
N3 C45 C44 127.9(5) . . ?
O6 C46 C47 128.2(5) . . ?
O6 C46 C51 108.0(5) . . ?
C51 C46 C47 123.8(5) . . ?
C46 C47 H47 122.4 . . ?
C46 C47 C48 115.3(5) . . ?
C48 C47 H47 122.4 . . ?
C47 C48 H48 119.0 . . ?
C49 C48 C47 122.0(5) . . ?
C49 C48 H48 119.0 . . ?
C48 C49 H49 119.2 . . ?
C48 C49 C50 121.6(5) . . ?
C50 C49 H49 119.2 . . ?
C49 C50 H50 121.5 . . ?
C49 C50 C51 116.9(5) . . ?
C51 C50 H50 121.5 . . ?
N3 C51 C50 131.9(5) . . ?
C46 C51 N3 107.7(4) . . ?
C46 C51 C50 120.4(5) . . ?
O7 C52 C53 116.1(5) . . ?
O7 C52 C61 124.1(5) . . ?
C61 C52 C53 119.7(5) . . ?
C52 C53 H53 119.8 . . ?
C54 C53 C52 120.4(5) . . ?
C54 C53 H53 119.8 . . ?
C53 C54 H54 119.2 . . ?
C53 C54 C55 121.6(5) . . ?
C55 C54 H54 119.2 . . ?
C54 C55 C56 120.4(5) . . ?
C54 C55 C60 120.6(5) . . ?
C56 C55 C60 119.0(5) . . ?
C55 C56 H56 119.2 . . ?
C57 C56 C55 121.7(5) . . ?
C57 C56 H56 119.2 . . ?
C56 C57 H57 120.4 . . ?
C56 C57 C58 119.3(6) . . ?
C58 C57 H57 120.4 . . ?
C57 C58 H58 119.4 . . ?
C59 C58 C57 121.1(6) . . ?
C59 C58 H58 119.4 . . ?
C58 C59 H59 118.9 . . ?
C58 C59 C60 122.2(6) . . ?
C60 C59 H59 118.9 . . ?
C55 C60 C61 117.0(5) . . ?
C59 C60 C55 116.6(5) . . ?
C59 C60 C61 126.4(5) . . ?
C52 C61 C60 120.2(4) . . ?
C52 C61 C62 115.4(5) . . ?
C62 C61 C60 124.2(5) . . ?
O8 C62 C61 117.7(5) . . ?
N4 C62 O8 113.2(4) . . ?
N4 C62 C61 129.0(5) . . ?
O8 C63 C64 127.1(5) . . ?
O8 C63 C68 107.8(4) . . ?
C64 C63 C68 125.1(5) . . ?
C63 C64 H64 122.8 . . ?
C63 C64 C65 114.4(5) . . ?
C65 C64 H64 122.8 . . ?
C64 C65 H65 119.2 . . ?
C64 C65 C66 121.5(5) . . ?
C66 C65 H65 119.2 . . ?
C65 C66 H66 118.9 . . ?
C67 C66 C65 122.3(5) . . ?
C67 C66 H66 118.9 . . ?
C66 C67 H67 121.5 . . ?
C68 C67 C66 117.0(5) . . ?
C68 C67 H67 121.5 . . ?
C63 C68 N4 108.3(4) . . ?
C67 C68 N4 132.1(5) . . ?
C67 C68 C63 119.6(5) . . ?
Cl1 C69 Cl2 111.9(4) . . ?
Cl1 C69 H69A 109.2 . . ?
Cl1 C69 H69B 109.2 . . ?
Cl2 C69 H69A 109.2 . . ?
Cl2 C69 H69B 109.2 . . ?
H69A C69 H69B 107.9 . . ?
Cl3 C70 Cl4 112.8(4) . . ?
Cl3 C70 H70A 109.0 . . ?
Cl3 C70 H70B 109.0 . . ?
Cl4 C70 H70A 109.0 . . ?
Cl4 C70 H70B 109.0 . . ?
H70A C70 H70B 107.8 . . ?

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 C1 C2 155.1(4) . . . . ?
Hf1 O1 C1 C10 -25.3(8) . . . . ?
Hf1 O3 C18 C19 -150.1(4) . . . . ?
Hf1 O3 C18 C27 32.6(8) . . . . ?
Hf1 N1 C11 O2 -172.3(3) . . . . ?
Hf1 N1 C11 C10 13.6(7) . . . . ?
Hf1 N1 C17 C12 171.9(3) . . . . ?
Hf1 N1 C17 C16 -6.0(8) . . . . ?
Hf1 N2 C28 O4 -175.9(3) . . . . ?
Hf1 N2 C28 C27 -1.8(8) . . . . ?
Hf1 N2 C34 C29 176.4(3) . . . . ?
Hf1 N2 C34 C33 -4.8(8) . . . . ?
O1 C1 C2 C3 -176.9(5) . . . . ?
O1 C1 C10 C9 172.5(4) . . . . ?
O1 C1 C10 C11 -14.2(7) . . . . ?
O2 C12 C13 C14 179.0(5) . . . . ?
O2 C12 C17 N1 2.4(5) . . . . ?
O2 C12 C17 C16 -179.4(4) . . . . ?
O3 C18 C19 C20 178.6(5) . . . . ?
O3 C18 C27 C26 -176.1(4) . . . . ?
O3 C18 C27 C28 9.9(7) . . . . ?
O4 C29 C30 C31 179.1(5) . . . . ?
O4 C29 C34 N2 -1.0(6) . . . . ?
O4 C29 C34 C33 180.0(4) . . . . ?
C1 C2 C3 C4 2.5(8) . . . . ?
C1 C10 C11 O2 -158.4(4) . . . . ?
C1 C10 C11 N1 15.5(8) . . . . ?
C2 C1 C10 C9 -7.9(7) . . . . ?
C2 C1 C10 C11 165.4(4) . . . . ?
C2 C3 C4 C5 177.3(5) . . . . ?
C2 C3 C4 C9 -3.9(8) . . . . ?
C3 C4 C5 C6 -179.2(5) . . . . ?
C3 C4 C9 C8 176.6(5) . . . . ?
C3 C4 C9 C10 -0.6(7) . . . . ?
C4 C5 C6 C7 1.8(9) . . . . ?
C4 C9 C10 C1 6.5(7) . . . . ?
C4 C9 C10 C11 -166.4(5) . . . . ?
C5 C4 C9 C8 -4.6(8) . . . . ?
C5 C4 C9 C10 178.2(5) . . . . ?
C5 C6 C7 C8 -3.0(10) . . . . ?
C6 C7 C8 C9 0.3(10) . . . . ?
C7 C8 C9 C4 3.5(9) . . . . ?
C7 C8 C9 C10 -179.5(6) . . . . ?
C8 C9 C10 C1 -170.5(5) . . . . ?
C8 C9 C10 C11 16.6(8) . . . . ?
C9 C4 C5 C6 2.1(8) . . . . ?
C9 C10 C11 O2 14.8(7) . . . . ?
C9 C10 C11 N1 -171.4(5) . . . . ?
C10 C1 C2 C3 3.4(8) . . . . ?
C11 O2 C12 C13 179.9(5) . . . . ?
C11 O2 C12 C17 -0.8(5) . . . . ?
C11 N1 C17 C12 -3.1(5) . . . . ?
C11 N1 C17 C16 179.0(5) . . . . ?
C12 O2 C11 N1 -1.3(5) . . . . ?
C12 O2 C11 C10 173.4(4) . . . . ?
C12 C13 C14 C15 0.6(8) . . . . ?
C13 C12 C17 N1 -178.2(5) . . . . ?
C13 C12 C17 C16 0.0(8) . . . . ?
C13 C14 C15 C16 -0.7(9) . . . . ?
C14 C15 C16 C17 0.4(8) . . . . ?
C15 C16 C17 N1 177.6(5) . . . . ?
C15 C16 C17 C12 -0.1(7) . . . . ?
C17 N1 C11 O2 2.8(5) . . . . ?
C17 N1 C11 C10 -171.3(5) . . . . ?
C17 C12 C13 C14 -0.3(8) . . . . ?
C18 C19 C20 C21 -1.1(8) . . . . ?
C18 C27 C28 O4 152.7(4) . . . . ?
C18 C27 C28 N2 -21.2(8) . . . . ?
C19 C18 C27 C26 6.6(7) . . . . ?
C19 C18 C27 C28 -167.5(4) . . . . ?
C19 C20 C21 C22 -178.5(5) . . . . ?
C19 C20 C21 C26 3.4(8) . . . . ?
C20 C21 C22 C23 -178.6(6) . . . . ?
C20 C21 C26 C25 -178.7(5) . . . . ?
C20 C21 C26 C27 -0.6(7) . . . . ?
C21 C22 C23 C24 -1.5(9) . . . . ?
C21 C26 C27 C18 -4.4(7) . . . . ?
C21 C26 C27 C28 169.2(5) . . . . ?
C22 C21 C26 C25 3.3(8) . . . . ?
C22 C21 C26 C27 -178.7(5) . . . . ?
C22 C23 C24 C25 0.6(10) . . . . ?
C23 C24 C25 C26 2.3(9) . . . . ?
C24 C25 C26 C21 -4.2(8) . . . . ?
C24 C25 C26 C27 177.9(5) . . . . ?
C25 C26 C27 C18 173.5(5) . . . . ?
C25 C26 C27 C28 -13.0(8) . . . . ?
C26 C21 C22 C23 -0.5(9) . . . . ?
C26 C27 C28 O4 -21.1(7) . . . . ?
C26 C27 C28 N2 165.0(5) . . . . ?
C27 C18 C19 C20 -3.9(8) . . . . ?
C28 O4 C29 C30 179.9(5) . . . . ?
C28 O4 C29 C34 0.7(5) . . . . ?
C28 N2 C34 C29 1.0(5) . . . . ?
C28 N2 C34 C33 179.8(6) . . . . ?
C29 O4 C28 N2 0.0(5) . . . . ?
C29 O4 C28 C27 -174.8(4) . . . . ?
C29 C30 C31 C32 1.4(9) . . . . ?
C30 C29 C34 N2 179.7(5) . . . . ?
C30 C29 C34 C33 0.7(8) . . . . ?
C30 C31 C32 C33 0.0(9) . . . . ?
C31 C32 C33 C34 -1.1(8) . . . . ?
C32 C33 C34 N2 -177.9(5) . . . . ?
C32 C33 C34 C29 0.8(8) . . . . ?
C34 N2 C28 O4 -0.7(6) . . . . ?
C34 N2 C28 C27 173.5(5) . . . . ?
C34 C29 C30 C31 -1.8(9) . . . . ?
Hf2 O5 C35 C36 144.3(4) . . . . ?
Hf2 O5 C35 C44 -38.0(7) . . . . ?
Hf2 O7 C52 C53 -159.5(4) . . . . ?
Hf2 O7 C52 C61 23.3(9) . . . . ?
Hf2 N3 C45 O6 177.3(3) . . . . ?
Hf2 N3 C45 C44 3.6(7) . . . . ?
Hf2 N3 C51 C46 -178.4(4) . . . . ?
Hf2 N3 C51 C50 2.9(8) . . . . ?
Hf2 N4 C62 O8 -178.0(3) . . . . ?
Hf2 N4 C62 C61 -1.0(8) . . . . ?
Hf2 N4 C68 C63 178.0(3) . . . . ?
Hf2 N4 C68 C67 0.0(8) . . . . ?
O5 C35 C36 C37 -176.0(5) . . . . ?
O5 C35 C44 C43 173.8(4) . . . . ?
O5 C35 C44 C45 -7.0(7) . . . . ?
O6 C46 C47 C48 -179.2(6) . . . . ?
O6 C46 C51 N3 2.0(6) . . . . ?
O6 C46 C51 C50 -179.2(5) . . . . ?
O7 C52 C53 C54 176.0(5) . . . . ?
O7 C52 C61 C60 -177.6(5) . . . . ?
O7 C52 C61 C62 6.8(7) . . . . ?
O8 C63 C64 C65 -179.0(5) . . . . ?
O8 C63 C68 N4 -1.0(6) . . . . ?
O8 C63 C68 C67 177.3(5) . . . . ?
C35 C36 C37 C38 0.1(8) . . . . ?
C35 C44 C45 O6 -152.9(5) . . . . ?
C35 C44 C45 N3 20.3(8) . . . . ?
C36 C35 C44 C43 -8.5(7) . . . . ?
C36 C35 C44 C45 170.7(5) . . . . ?
C36 C37 C38 C39 175.9(5) . . . . ?
C36 C37 C38 C43 -3.8(8) . . . . ?
C37 C38 C39 C40 179.7(5) . . . . ?
C37 C38 C43 C42 179.7(5) . . . . ?
C37 C38 C43 C44 1.3(7) . . . . ?
C38 C39 C40 C41 0.3(8) . . . . ?
C38 C43 C44 C35 4.8(7) . . . . ?
C38 C43 C44 C45 -174.3(5) . . . . ?
C39 C38 C43 C42 0.0(7) . . . . ?
C39 C38 C43 C44 -178.4(5) . . . . ?
C39 C40 C41 C42 0.6(8) . . . . ?
C40 C41 C42 C43 -1.2(8) . . . . ?
C41 C42 C43 C38 0.9(8) . . . . ?
C41 C42 C43 C44 179.2(5) . . . . ?
C42 C43 C44 C35 -173.5(5) . . . . ?
C42 C43 C44 C45 7.4(8) . . . . ?
C43 C38 C39 C40 -0.6(8) . . . . ?
C43 C44 C45 O6 26.2(7) . . . . ?
C43 C44 C45 N3 -160.6(5) . . . . ?
C44 C35 C36 C37 6.2(8) . . . . ?
C45 O6 C46 C47 179.9(6) . . . . ?
C45 O6 C46 C51 -1.7(6) . . . . ?
C45 N3 C51 C46 -1.4(6) . . . . ?
C45 N3 C51 C50 180.0(6) . . . . ?
C46 O6 C45 N3 0.9(6) . . . . ?
C46 O6 C45 C44 175.1(5) . . . . ?
C46 C47 C48 C49 -2.1(10) . . . . ?
C47 C46 C51 N3 -179.6(6) . . . . ?
C47 C46 C51 C50 -0.8(9) . . . . ?
C47 C48 C49 C50 -0.3(10) . . . . ?
C48 C49 C50 C51 2.3(8) . . . . ?
C49 C50 C51 N3 176.8(5) . . . . ?
C49 C50 C51 C46 -1.7(8) . . . . ?
C51 N3 C45 O6 0.3(6) . . . . ?
C51 N3 C45 C44 -173.3(5) . . . . ?
C51 C46 C47 C48 2.7(10) . . . . ?
C52 C53 C54 C55 1.8(8) . . . . ?
C52 C61 C62 O8 163.1(4) . . . . ?
C52 C61 C62 N4 -13.8(8) . . . . ?
C53 C52 C61 C60 5.3(7) . . . . ?
C53 C52 C61 C62 -170.3(5) . . . . ?
C53 C54 C55 C56 -177.7(5) . . . . ?
C53 C54 C55 C60 4.4(8) . . . . ?
C54 C55 C56 C57 -175.9(6) . . . . ?
C54 C55 C60 C59 174.3(5) . . . . ?
C54 C55 C60 C61 -5.6(8) . . . . ?
C55 C56 C57 C58 0.7(10) . . . . ?
C55 C60 C61 C52 0.7(7) . . . . ?
C55 C60 C61 C62 175.9(5) . . . . ?
C56 C55 C60 C59 -3.7(8) . . . . ?
C56 C55 C60 C61 176.5(5) . . . . ?
C56 C57 C58 C59 -1.7(10) . . . . ?
C57 C58 C59 C60 -0.2(11) . . . . ?
C58 C59 C60 C55 2.8(9) . . . . ?
C58 C59 C60 C61 -177.3(6) . . . . ?
C59 C60 C61 C52 -179.1(5) . . . . ?
C59 C60 C61 C62 -3.9(9) . . . . ?
C60 C55 C56 C57 2.0(9) . . . . ?
C60 C61 C62 O8 -12.2(7) . . . . ?
C60 C61 C62 N4 170.8(5) . . . . ?
C61 C52 C53 C54 -6.7(8) . . . . ?
C62 O8 C63 C64 178.5(6) . . . . ?
C62 O8 C63 C68 -0.1(6) . . . . ?
C62 N4 C68 C63 1.8(6) . . . . ?
C62 N4 C68 C67 -176.2(6) . . . . ?
C63 O8 C62 N4 1.4(6) . . . . ?
C63 O8 C62 C61 -176.0(4) . . . . ?
C63 C64 C65 C66 2.0(9) . . . . ?
C64 C63 C68 N4 -179.7(5) . . . . ?
C64 C63 C68 C67 -1.4(9) . . . . ?
C64 C65 C66 C67 -1.6(10) . . . . ?
C65 C66 C67 C68 -0.4(9) . . . . ?
C66 C67 C68 N4 179.7(5) . . . . ?
C66 C67 C68 C63 1.9(8) . . . . ?
C68 N4 C62 O8 -2.0(6) . . . . ?
C68 N4 C62 C61 175.1(5) . . . . ?
C68 C63 C64 C65 -0.5(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.453 204.1 58.5 ?
2 0.000 0.500 0.104 270.8 96.9 ?
3 0.500 0.000 0.896 270.8 97.7 ?
4 0.500 0.500 0.547 204.1 57.8 ?

_olex2_date_sample_data_collection 2016-07-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.735
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound8
_database_code_depnum_ccdc_archive 'CCDC 1816371'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2015-12-10
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C34 H20 N2 O4 Zr0.5)'
_chemical_formula_sum            'C68 H40 N4 O8 Zr'
_chemical_formula_weight         1132.26
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H44 Cl8 N4 O8 Zr'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
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'

_cell_length_a                   12.0743(2)
_cell_length_b                   18.9545(4)
_cell_length_c                   27.7599(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6353.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31447
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0140
_cell_measurement_theta_min      2.4720
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2320
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 2 0.1224
-5 5 -2 0.1033
0 1 0 0.1056
1 0 0 0.0869
0 0 -1 0.0529
0 0 1 0.0529
-5 -4 1 0.1664

_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.106
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0032 -4.9940 1.9901 0.0041 -0.0946 -0.1689
-4.9932 4.9981 -2.0075 -0.0268 0.3497 0.0254
0.0004 0.9981 0.0016 -0.0106 0.0168 0.0316
0.9993 -0.0008 0.0035 0.0045 -0.0510 0.0287
0.0006 0.0018 -0.9990 0.0244 0.0052 0.0054
-0.0006 -0.0018 0.9990 -0.0244 -0.0052 -0.0054
-4.9987 -3.9901 0.9753 -0.0048 0.1825 -0.2754

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            110062
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.13
_diffrn_reflns_theta_min         2.60
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9960
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  60.00   1.00   22.00    --  -17.00  19.00-180.00  110
  2  ω    -47.00  54.00   1.00   22.00    --  -17.00  77.00   0.00  101
  3  ω    -76.00 -29.00   1.00   22.00    --  -17.00 133.00-113.31   47
  4  ω    -72.00 -24.00   1.00   22.00    --  -17.00 126.00 155.27   48
  5  ω    -42.00  51.00   1.00   22.00    --  -17.00  57.00 -90.00   93
  6  ω    -11.00  62.00   1.00   22.00    --   17.39-110.00 144.00   73
  7  ω    -13.00  85.00   1.00   22.00    --   17.39  77.00 -90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0046244000
_diffrn_orient_matrix_UB_12      -0.0105540000
_diffrn_orient_matrix_UB_13      -0.0244295000
_diffrn_orient_matrix_UB_21      -0.0510194000
_diffrn_orient_matrix_UB_22      0.0168972000
_diffrn_orient_matrix_UB_23      -0.0052381000
_diffrn_orient_matrix_UB_31      0.0287624000
_diffrn_orient_matrix_UB_32      0.0316764000
_diffrn_orient_matrix_UB_33      -0.0053373000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                16523
_reflns_number_total             18701
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         18701
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0534
_refine_ls_restrained_S_all      1.074
_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)+(0.0787P)²+8.5670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1584
_refine_special_details          
;Refined as a 2-component inversion twin.
 
Disordered solvent was treated with the SQUEEZE procedure of Olex2 
program (Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; 
Puschmann, H., J. Appl. Cryst. (2009). 42, 339-341.)
The sum formular and further calculations disregard this electron density.
 
Miller array info: D:\Data\Lisa25\struct\olex2_Lisa25\Lisa25.hkl:Iobs,SigIobs
Observation type: xray.intensity
Type of data: double, size=110062
Type of sigmas: double, size=110062
Number of Miller indices: 110062
Anomalous flag: True
Unit cell: (12.0743, 18.9545, 27.7599, 90, 90, 90)
Space group: P 21 21 2 (No. 18)
Systematic absences: 80
Systematic absences not included in following:
Centric reflections: 10294
Resolution range: 7.82679 0.708037

use_set_completion: False
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
    C     H     N     O    Zr
 1.70  1.09  1.55  1.52  2.00

Total solvent accessible volume / cell = 1782.0 Ang^3 [28.0%]
Total electron count / cell = 88.8

gridding: (72,108,160)
Void #Grid points Vol/A^3 Vol/%  Centre of mass (frac)   Eigenvectors (frac)
 1       174485   891.0  14.0  (-0.000,-0.547, 0.751)  1  ( 1.000, 0.012, 0.002)
                                                       2  (-0.002, 0.018, 1.000)
                                                       3  (-0.012, 1.000,-0.018)
 2       174485   891.0  14.0  ( 0.500,-0.668, 0.249)  1  ( 0.998, 0.053,-0.027)
                                                       2  ( 0.053,-0.583, 0.811)
                                                       3  (-0.028, 0.811, 0.585)

Void  Vol/Ang^3  #Electrons
   1      891.0         61.7
   2      891.0         61.7,Twin,SQUEEZE
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.5000 0.5000 0.04239(2) 0.01715(11) Uani 1 2 d S T P . .
Zr2 Zr 0.0000 0.5000 0.53322(2) 0.01367(11) Uani 1 2 d S T P . .
O1 O 0.4339(2) 0.59436(17) 0.01487(11) 0.0184(6) Uani 1 1 d . . . . .
O2 O 0.2903(3) 0.47723(18) -0.09406(12) 0.0266(7) Uani 1 1 d . . . . .
O3 O 0.3492(3) 0.46611(17) 0.06836(11) 0.0200(6) Uani 1 1 d . . . . .
O4 O 0.5069(3) 0.35324(18) 0.17550(10) 0.0253(6) Uani 1 1 d . . . . .
O5 O 0.0605(3) 0.59572(17) 0.50734(10) 0.0188(6) Uani 1 1 d . . . . .
O6 O 0.2154(3) 0.48981(18) 0.39757(10) 0.0231(7) Uani 1 1 d . . . . .
O7 O 0.1503(2) 0.46027(15) 0.55854(10) 0.0165(6) Uani 1 1 d . . . . .
O8 O -0.0224(2) 0.38132(17) 0.67587(10) 0.0204(6) Uani 1 1 d . . . . .
N1 N 0.3857(3) 0.4709(2) -0.02453(13) 0.0189(7) Uani 1 1 d . . . . .
N2 N 0.5326(3) 0.4204(2) 0.10959(14) 0.0199(7) Uani 1 1 d . . . . .
N3 N 0.1153(3) 0.47468(19) 0.46489(12) 0.0159(6) Uani 1 1 d . . . . .
N4 N -0.0386(3) 0.42964(18) 0.60202(13) 0.0165(6) Uani 1 1 d . . . . .
C1 C 0.4202(4) 0.6217(3) -0.02842(16) 0.0210(8) Uani 1 1 d . . . . .
C2 C 0.4367(4) 0.6946(3) -0.03344(17) 0.0237(9) Uani 1 1 d . . . . .
H2 H 0.4525 0.7215 -0.0054 0.028 Uiso 1 1 calc R U . . .
C3 C 0.4311(4) 0.7293(2) -0.07711(17) 0.0224(9) Uani 1 1 d . . . . .
H3 H 0.4416 0.7789 -0.0788 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4096(4) 0.6901(3) -0.11925(16) 0.0214(8) Uani 1 1 d . . . . .
C5 C 0.4099(4) 0.7243(3) -0.16523(18) 0.0266(10) Uani 1 1 d . . . . .
H5 H 0.4232 0.7736 -0.1672 0.032 Uiso 1 1 calc R U . . .
C6 C 0.3915(4) 0.6868(3) -0.20565(17) 0.0265(9) Uani 1 1 d . . . . .
H6 H 0.3933 0.7097 -0.2361 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3693(4) 0.6134(3) -0.20310(17) 0.0281(10) Uani 1 1 d . . . . .
H7 H 0.3546 0.5879 -0.2318 0.034 Uiso 1 1 calc R U . . .
C8 C 0.3688(4) 0.5790(2) -0.16002(16) 0.0221(8) Uani 1 1 d . . . . .
H8 H 0.3558 0.5296 -0.1594 0.027 Uiso 1 1 calc R U . . .
C9 C 0.3873(3) 0.6154(2) -0.11627(16) 0.0196(8) Uani 1 1 d . . . . .
C10 C 0.3907(4) 0.5825(2) -0.06960(15) 0.0180(8) Uani 1 1 d . . . . .
C11 C 0.3594(3) 0.5092(2) -0.06173(15) 0.0192(8) Uani 1 1 d . . . . .
C12 C 0.2709(4) 0.4113(2) -0.07400(17) 0.0243(9) Uani 1 1 d . . . . .
C13 C 0.2085(5) 0.3559(3) -0.09264(18) 0.0349(12) Uani 1 1 d . . . . .
H13 H 0.1720 0.3589 -0.1229 0.042 Uiso 1 1 calc R U . . .
C14 C 0.2034(5) 0.2968(3) -0.06445(19) 0.0300(10) Uani 1 1 d . . . . .
H14 H 0.1586 0.2585 -0.0749 0.036 Uiso 1 1 calc R U . . .
C15 C 0.2596(4) 0.2902(3) -0.02196(18) 0.0260(9) Uani 1 1 d . . . . .
H15 H 0.2565 0.2469 -0.0048 0.031 Uiso 1 1 calc R U . . .
C16 C 0.3219(4) 0.3466(2) -0.00324(16) 0.0203(8) Uani 1 1 d . . . . .
H16 H 0.3580 0.3434 0.0271 0.024 Uiso 1 1 calc R U . . .
C17 C 0.3283(3) 0.4070(2) -0.03110(16) 0.0202(8) Uani 1 1 d . . . . .
C18 C 0.2924(4) 0.4444(2) 0.10546(16) 0.0209(8) Uani 1 1 d . . . . .
C19 C 0.1765(4) 0.4495(3) 0.10341(18) 0.0251(9) Uani 1 1 d . . . . .
H19 H 0.1419 0.4639 0.0743 0.030 Uiso 1 1 calc R U . . .
C20 C 0.1123(4) 0.4340(3) 0.14298(18) 0.0246(9) Uani 1 1 d . . . . .
H20 H 0.0345 0.4411 0.1414 0.030 Uiso 1 1 calc R U . . .
C21 C 0.1589(4) 0.4079(3) 0.18536(17) 0.0240(9) Uani 1 1 d . . . . .
C22 C 0.0899(4) 0.3925(3) 0.22572(19) 0.0295(10) Uani 1 1 d . . . . .
H22 H 0.0131 0.4033 0.2241 0.035 Uiso 1 1 calc R U . . .
C23 C 0.1323(5) 0.3623(3) 0.2671(2) 0.0368(12) Uani 1 1 d . . . . .
H23 H 0.0855 0.3523 0.2938 0.044 Uiso 1 1 calc R U . . .
C24 C 0.2431(4) 0.3471(3) 0.26888(19) 0.0352(12) Uani 1 1 d . . . . .
H24 H 0.2720 0.3252 0.2970 0.042 Uiso 1 1 calc R U . . .
C25 C 0.3152(5) 0.3626(3) 0.23105(18) 0.0361(12) Uani 1 1 d . . . . .
H25 H 0.3919 0.3525 0.2343 0.043 Uiso 1 1 calc R U . . .
C26 C 0.2752(4) 0.3931(2) 0.18782(16) 0.0218(8) Uani 1 1 d . . . . .
C27 C 0.3433(3) 0.4133(2) 0.14601(15) 0.0170(7) Uani 1 1 d . . . . .
C28 C 0.4617(4) 0.4004(2) 0.14244(15) 0.0187(8) Uani 1 1 d . . . . .
C29 C 0.6153(4) 0.3460(3) 0.16139(17) 0.0254(9) Uani 1 1 d . . . . .
C30 C 0.6965(4) 0.3053(3) 0.18219(19) 0.0338(12) Uani 1 1 d . . . . .
H30 H 0.6822 0.2782 0.2103 0.041 Uiso 1 1 calc R U . . .
C31 C 0.7987(5) 0.3054(3) 0.1609(2) 0.0368(13) Uani 1 1 d . . . . .
H31 H 0.8569 0.2774 0.1737 0.044 Uiso 1 1 calc R U . . .
C32 C 0.8168(4) 0.3476(3) 0.11968(19) 0.0290(10) Uani 1 1 d . . . . .
H32 H 0.8889 0.3480 0.1059 0.035 Uiso 1 1 calc R U . . .
C33 C 0.7359(4) 0.3880(2) 0.09830(18) 0.0236(9) Uani 1 1 d . . . . .
H33 H 0.7500 0.4142 0.0698 0.028 Uiso 1 1 calc R U . . .
C34 C 0.6320(4) 0.3885(2) 0.12052(15) 0.0192(8) Uani 1 1 d . . . . .
C35 C 0.0785(3) 0.6270(2) 0.46664(14) 0.0146(7) Uani 1 1 d . . . . .
C36 C 0.0677(4) 0.7029(2) 0.46495(17) 0.0193(8) Uani 1 1 d . . . . .
H36 H 0.0476 0.7275 0.4935 0.023 Uiso 1 1 calc R U . . .
C37 C 0.0851(4) 0.7396(3) 0.42464(16) 0.0231(9) Uani 1 1 d . . . . .
H37 H 0.0818 0.7897 0.4255 0.028 Uiso 1 1 calc R U . . .
C38 C 0.1090(4) 0.7045(3) 0.37966(17) 0.0233(9) Uani 1 1 d . . . . .
C39 C 0.1204(4) 0.7437(3) 0.33655(19) 0.0308(11) Uani 1 1 d . . . . .
H39 H 0.1110 0.7934 0.3373 0.037 Uiso 1 1 calc R U . . .
C40 C 0.1448(4) 0.7113(3) 0.29399(18) 0.0307(10) Uani 1 1 d . . . . .
H40 H 0.1539 0.7383 0.2655 0.037 Uiso 1 1 calc R U . . .
C41 C 0.1562(4) 0.6380(3) 0.29268(17) 0.0283(10) Uani 1 1 d . . . . .
H41 H 0.1726 0.6152 0.2630 0.034 Uiso 1 1 calc R U . . .
C42 C 0.1438(4) 0.5980(3) 0.33439(16) 0.0219(8) Uani 1 1 d . . . . .
H42 H 0.1499 0.5481 0.3326 0.026 Uiso 1 1 calc R U . . .
C43 C 0.1220(3) 0.6306(2) 0.37997(15) 0.0177(8) Uani 1 1 d . . . . .
C44 C 0.1113(3) 0.5916(2) 0.42444(14) 0.0165(7) Uani 1 1 d . . . . .
C45 C 0.1414(3) 0.5186(2) 0.42996(14) 0.0173(8) Uani 1 1 d . . . . .
C46 C 0.2340(4) 0.4225(3) 0.41444(17) 0.0236(9) Uani 1 1 d . . . . .
C47 C 0.3043(4) 0.3726(3) 0.3942(2) 0.0284(10) Uani 1 1 d . . . . .
H47 H 0.3471 0.3816 0.3661 0.034 Uiso 1 1 calc R U . . .
C48 C 0.3069(4) 0.3074(3) 0.4188(2) 0.0339(12) Uani 1 1 d . . . . .
H48 H 0.3497 0.2697 0.4060 0.041 Uiso 1 1 calc R U . . .
C49 C 0.2486(4) 0.2973(3) 0.4609(2) 0.0282(10) Uani 1 1 d . . . . .
H49 H 0.2538 0.2530 0.4768 0.034 Uiso 1 1 calc R U . . .
C50 C 0.1816(4) 0.3503(2) 0.48115(17) 0.0249(9) Uani 1 1 d . . . . .
H50 H 0.1420 0.3431 0.5103 0.030 Uiso 1 1 calc R U . . .
C51 C 0.1764(4) 0.4134(2) 0.45628(15) 0.0195(8) Uani 1 1 d . . . . .
C52 C 0.1993(3) 0.4467(2) 0.59948(15) 0.0161(7) Uani 1 1 d . . . . .
C53 C 0.3196(4) 0.4468(2) 0.59857(16) 0.0201(8) Uani 1 1 d . . . . .
H53 H 0.3577 0.4536 0.5690 0.024 Uiso 1 1 calc R U . . .
C54 C 0.3771(4) 0.4372(3) 0.63948(19) 0.0259(9) Uani 1 1 d . . . . .
H54 H 0.4557 0.4359 0.6381 0.031 Uiso 1 1 calc R U . . .
C55 C 0.3234(4) 0.4291(2) 0.68512(17) 0.0233(9) Uani 1 1 d . . . . .
C56 C 0.3867(4) 0.4223(3) 0.72718(19) 0.0273(10) Uani 1 1 d . . . . .
H56 H 0.4652 0.4225 0.7249 0.033 Uiso 1 1 calc R U . . .
C57 C 0.3377(5) 0.4154(3) 0.7715(2) 0.0344(12) Uani 1 1 d . . . . .
H57 H 0.3811 0.4090 0.7997 0.041 Uiso 1 1 calc R U . . .
C58 C 0.2221(5) 0.4179(4) 0.7742(2) 0.0418(14) Uani 1 1 d . . . . .
H58 H 0.1867 0.4145 0.8047 0.050 Uiso 1 1 calc R U . . .
C59 C 0.1582(4) 0.4254(3) 0.73291(17) 0.0294(10) Uani 1 1 d . . . . .
H59 H 0.0801 0.4292 0.7358 0.035 Uiso 1 1 calc R U . . .
C60 C 0.2064(4) 0.4273(2) 0.68712(15) 0.0212(8) Uani 1 1 d . . . . .
C61 C 0.1448(3) 0.4339(2) 0.64263(14) 0.0155(7) Uani 1 1 d . . . . .
C62 C 0.0277(4) 0.4187(2) 0.63856(14) 0.0203(9) Uani 1 1 d . . . . .
C63 C -0.1275(4) 0.3671(2) 0.65929(15) 0.0195(8) Uani 1 1 d . . . . .
C64 C -0.2118(4) 0.3327(3) 0.68399(17) 0.0287(10) Uani 1 1 d . . . . .
H64 H -0.2027 0.3161 0.7161 0.034 Uiso 1 1 calc R U . . .
C65 C -0.3091(4) 0.3241(3) 0.65900(18) 0.0254(9) Uani 1 1 d . . . . .
H65 H -0.3683 0.2990 0.6737 0.030 Uiso 1 1 calc R U . . .
C66 C -0.3235(4) 0.3517(3) 0.61199(17) 0.0239(9) Uani 1 1 d . . . . .
H66 H -0.3927 0.3463 0.5961 0.029 Uiso 1 1 calc R U . . .
C67 C -0.2375(3) 0.3865(2) 0.58904(15) 0.0191(8) Uani 1 1 d . . . . .
H67 H -0.2460 0.4046 0.5573 0.023 Uiso 1 1 calc R U . . .
C68 C -0.1392(4) 0.3940(2) 0.61374(15) 0.0202(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.102(3) . ?
Zr1 O1 2.102(3) 2_665 ?
Zr1 O3 2.061(3) . ?
Zr1 O3 2.061(3) 2_665 ?
Zr1 N1 2.379(4) 2_665 ?
Zr1 N1 2.379(4) . ?
Zr1 N2 2.432(4) . ?
Zr1 N2 2.432(4) 2_665 ?
Zr2 O5 2.084(3) 2_565 ?
Zr2 O5 2.084(3) . ?
Zr2 O7 2.087(3) . ?
Zr2 O7 2.087(3) 2_565 ?
Zr2 N3 2.402(3) 2_565 ?
Zr2 N3 2.402(3) . ?
Zr2 N4 2.375(3) 2_565 ?
Zr2 N4 2.375(3) . ?
O1 C1 1.319(5) . ?
O2 C11 1.367(5) . ?
O2 C12 1.389(6) . ?
O3 C18 1.304(5) . ?
O4 C28 1.392(5) . ?
O4 C29 1.373(6) . ?
O5 C35 1.294(5) . ?
O6 C45 1.380(5) . ?
O6 C46 1.378(6) . ?
O7 C52 1.307(5) . ?
O8 C62 1.393(5) . ?
O8 C63 1.377(5) . ?
N1 C11 1.301(6) . ?
N1 C17 1.408(6) . ?
N2 C28 1.307(6) . ?
N2 C34 1.377(6) . ?
N3 C45 1.317(5) . ?
N3 C51 1.397(6) . ?
N4 C62 1.308(5) . ?
N4 C68 1.428(5) . ?
C1 C2 1.404(7) . ?
C1 C10 1.409(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.381(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.411(7) . ?
C4 C5 1.432(6) . ?
C4 C9 1.443(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.347(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.418(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.362(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.415(6) . ?
C9 C10 1.438(6) . ?
C10 C11 1.457(6) . ?
C12 C13 1.392(7) . ?
C12 C17 1.380(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.368(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.367(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.407(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(6) . ?
C18 C19 1.403(6) . ?
C18 C27 1.412(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.377(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.394(6) . ?
C21 C22 1.427(6) . ?
C21 C26 1.434(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.370(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.395(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.417(7) . ?
C26 C27 1.473(6) . ?
C27 C28 1.454(6) . ?
C29 C30 1.374(7) . ?
C29 C34 1.407(7) . ?
C30 H30 0.9500 . ?
C30 C31 1.369(8) . ?
C31 H31 0.9500 . ?
C31 C32 1.412(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.376(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.398(6) . ?
C35 C36 1.445(6) . ?
C35 C44 1.407(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.334(7) . ?
C37 H37 0.9500 . ?
C37 C38 1.444(6) . ?
C38 C39 1.415(6) . ?
C38 C43 1.410(6) . ?
C39 H39 0.9500 . ?
C39 C40 1.364(7) . ?
C40 H40 0.9500 . ?
C40 C41 1.396(8) . ?
C41 H41 0.9500 . ?
C41 C42 1.392(6) . ?
C42 H42 0.9500 . ?
C42 C43 1.432(6) . ?
C43 C44 1.444(5) . ?
C44 C45 1.439(6) . ?
C46 C47 1.390(6) . ?
C46 C51 1.365(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.413(8) . ?
C48 H48 0.9500 . ?
C48 C49 1.379(8) . ?
C49 H49 0.9500 . ?
C49 C50 1.407(7) . ?
C50 H50 0.9500 . ?
C50 C51 1.382(6) . ?
C52 C53 1.453(6) . ?
C52 C61 1.388(6) . ?
C53 H53 0.9500 . ?
C53 C54 1.343(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.432(7) . ?
C55 C56 1.401(6) . ?
C55 C60 1.415(7) . ?
C56 H56 0.9500 . ?
C56 C57 1.372(8) . ?
C57 H57 0.9500 . ?
C57 C58 1.399(9) . ?
C58 H58 0.9500 . ?
C58 C59 1.388(7) . ?
C59 H59 0.9500 . ?
C59 C60 1.398(6) . ?
C60 C61 1.447(5) . ?
C61 C62 1.448(6) . ?
C63 C64 1.389(6) . ?
C63 C68 1.371(6) . ?
C64 H64 0.9500 . ?
C64 C65 1.374(7) . ?
C65 H65 0.9500 . ?
C65 C66 1.417(7) . ?
C66 H66 0.9500 . ?
C66 C67 1.385(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.378(6) . ?

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 O1 137.38(16) . 2_665 ?
O1 Zr1 N1 74.88(13) . 2_665 ?
O1 Zr1 N1 74.88(13) 2_665 . ?
O1 Zr1 N1 72.14(12) . . ?
O1 Zr1 N1 72.14(12) 2_665 2_665 ?
O1 Zr1 N2 71.89(12) 2_665 . ?
O1 Zr1 N2 150.27(12) . . ?
O1 Zr1 N2 150.27(12) 2_665 2_665 ?
O1 Zr1 N2 71.89(12) . 2_665 ?
O3 Zr1 O1 93.28(12) . . ?
O3 Zr1 O1 101.37(12) 2_665 . ?
O3 Zr1 O1 93.28(12) 2_665 2_665 ?
O3 Zr1 O1 101.37(12) . 2_665 ?
O3 Zr1 O3 139.04(17) 2_665 . ?
O3 Zr1 N1 71.85(12) 2_665 2_665 ?
O3 Zr1 N1 149.08(12) . 2_665 ?
O3 Zr1 N1 71.85(12) . . ?
O3 Zr1 N1 149.08(12) 2_665 . ?
O3 Zr1 N2 71.40(12) . . ?
O3 Zr1 N2 77.42(12) 2_665 . ?
O3 Zr1 N2 77.42(12) . 2_665 ?
O3 Zr1 N2 71.40(12) 2_665 2_665 ?
N1 Zr1 N1 77.31(17) 2_665 . ?
N1 Zr1 N2 130.47(13) 2_665 . ?
N1 Zr1 N2 123.30(12) . . ?
N1 Zr1 N2 130.47(13) . 2_665 ?
N1 Zr1 N2 123.30(12) 2_665 2_665 ?
N2 Zr1 N2 79.81(18) . 2_665 ?
O5 Zr2 O5 139.66(16) 2_565 . ?
O5 Zr2 O7 96.13(12) 2_565 . ?
O5 Zr2 O7 97.21(12) . . ?
O5 Zr2 O7 97.21(12) 2_565 2_565 ?
O5 Zr2 O7 96.13(12) . 2_565 ?
O5 Zr2 N3 75.93(12) . 2_565 ?
O5 Zr2 N3 72.45(12) 2_565 2_565 ?
O5 Zr2 N3 72.45(12) . . ?
O5 Zr2 N3 75.93(12) 2_565 . ?
O5 Zr2 N4 146.60(12) . . ?
O5 Zr2 N4 73.71(12) 2_565 . ?
O5 Zr2 N4 146.59(12) 2_565 2_565 ?
O5 Zr2 N4 73.72(12) . 2_565 ?
O7 Zr2 O7 140.62(16) . 2_565 ?
O7 Zr2 N3 71.92(12) . . ?
O7 Zr2 N3 147.40(12) . 2_565 ?
O7 Zr2 N3 71.92(12) 2_565 2_565 ?
O7 Zr2 N3 147.40(12) 2_565 . ?
O7 Zr2 N4 76.19(12) 2_565 . ?
O7 Zr2 N4 72.36(12) . . ?
O7 Zr2 N4 76.19(12) . 2_565 ?
O7 Zr2 N4 72.36(12) 2_565 2_565 ?
N3 Zr2 N3 75.66(17) . 2_565 ?
N4 Zr2 N3 129.31(12) 2_565 . ?
N4 Zr2 N3 129.53(12) . . ?
N4 Zr2 N3 129.53(12) 2_565 2_565 ?
N4 Zr2 N3 129.31(12) . 2_565 ?
N4 Zr2 N4 72.98(17) . 2_565 ?
C1 O1 Zr1 135.5(3) . . ?
C11 O2 C12 103.8(3) . . ?
C18 O3 Zr1 147.1(3) . . ?
C29 O4 C28 104.5(3) . . ?
C35 O5 Zr2 139.4(3) . . ?
C46 O6 C45 104.5(3) . . ?
C52 O7 Zr2 139.3(3) . . ?
C63 O8 C62 104.6(3) . . ?
C11 N1 Zr1 129.2(3) . . ?
C11 N1 C17 104.9(4) . . ?
C17 N1 Zr1 125.9(3) . . ?
C28 N2 Zr1 127.5(3) . . ?
C28 N2 C34 106.9(4) . . ?
C34 N2 Zr1 125.6(3) . . ?
C45 N3 Zr2 126.4(3) . . ?
C45 N3 C51 105.9(3) . . ?
C51 N3 Zr2 127.4(3) . . ?
C62 N4 Zr2 126.4(3) . . ?
C62 N4 C68 105.5(4) . . ?
C68 N4 Zr2 128.0(3) . . ?
O1 C1 C2 117.3(4) . . ?
O1 C1 C10 124.4(4) . . ?
C2 C1 C10 118.3(4) . . ?
C1 C2 H2 118.3 . . ?
C3 C2 C1 123.3(4) . . ?
C3 C2 H2 118.3 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.1(4) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 C9 120.3(4) . . ?
C5 C4 C9 119.8(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(5) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.5(4) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.0(5) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.3(4) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C4 117.3(4) . . ?
C8 C9 C10 124.5(4) . . ?
C10 C9 C4 118.1(4) . . ?
C1 C10 C9 120.6(4) . . ?
C1 C10 C11 116.5(4) . . ?
C9 C10 C11 122.8(4) . . ?
O2 C11 C10 118.8(4) . . ?
N1 C11 O2 115.1(4) . . ?
N1 C11 C10 126.0(4) . . ?
O2 C12 C13 128.4(4) . . ?
C17 C12 O2 108.3(4) . . ?
C17 C12 C13 123.2(4) . . ?
C12 C13 H13 122.3 . . ?
C14 C13 C12 115.4(4) . . ?
C14 C13 H13 122.3 . . ?
C13 C14 H14 118.4 . . ?
C15 C14 C13 123.1(5) . . ?
C15 C14 H14 118.4 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(5) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 121.6 . . ?
C17 C16 C15 116.8(4) . . ?
C17 C16 H16 121.6 . . ?
C12 C17 N1 107.9(4) . . ?
C12 C17 C16 120.2(4) . . ?
C16 C17 N1 131.8(4) . . ?
O3 C18 C19 118.1(4) . . ?
O3 C18 C27 122.1(4) . . ?
C19 C18 C27 119.7(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 121.0(4) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.4(4) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C22 119.9(4) . . ?
C20 C21 C26 120.4(4) . . ?
C22 C21 C26 119.6(4) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.4(5) . . ?
C23 C22 H22 119.3 . . ?
C22 C23 H23 120.7 . . ?
C24 C23 C22 118.6(5) . . ?
C24 C23 H23 120.7 . . ?
C23 C24 H24 118.7 . . ?
C23 C24 C25 122.6(5) . . ?
C25 C24 H24 118.7 . . ?
C24 C25 H25 119.6 . . ?
C24 C25 C26 120.7(5) . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C27 117.2(4) . . ?
C25 C26 C21 117.0(4) . . ?
C25 C26 C27 125.7(4) . . ?
C18 C27 C26 119.6(4) . . ?
C18 C27 C28 116.4(4) . . ?
C28 C27 C26 123.9(4) . . ?
O4 C28 C27 116.7(4) . . ?
N2 C28 O4 112.9(4) . . ?
N2 C28 C27 130.0(4) . . ?
O4 C29 C30 128.1(5) . . ?
O4 C29 C34 108.0(4) . . ?
C30 C29 C34 123.9(4) . . ?
C29 C30 H30 121.3 . . ?
C31 C30 C29 117.5(5) . . ?
C31 C30 H30 121.3 . . ?
C30 C31 H31 120.3 . . ?
C30 C31 C32 119.4(5) . . ?
C32 C31 H31 120.3 . . ?
C31 C32 H32 118.2 . . ?
C33 C32 C31 123.7(5) . . ?
C33 C32 H32 118.2 . . ?
C32 C33 H33 121.6 . . ?
C32 C33 C34 116.8(4) . . ?
C34 C33 H33 121.6 . . ?
N2 C34 C29 107.7(4) . . ?
N2 C34 C33 133.5(4) . . ?
C33 C34 C29 118.7(4) . . ?
O5 C35 C36 118.0(4) . . ?
O5 C35 C44 123.8(4) . . ?
C44 C35 C36 118.2(4) . . ?
C35 C36 H36 118.9 . . ?
C37 C36 C35 122.1(4) . . ?
C37 C36 H36 118.9 . . ?
C36 C37 H37 119.5 . . ?
C36 C37 C38 121.1(4) . . ?
C38 C37 H37 119.5 . . ?
C39 C38 C37 120.6(5) . . ?
C43 C38 C37 118.4(4) . . ?
C43 C38 C39 121.0(5) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.1(5) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 120.3 . . ?
C39 C40 C41 119.5(5) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 119.7 . . ?
C42 C41 C40 120.6(5) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 119.3 . . ?
C41 C42 C43 121.4(4) . . ?
C43 C42 H42 119.3 . . ?
C38 C43 C42 116.3(4) . . ?
C38 C43 C44 120.2(4) . . ?
C42 C43 C44 123.5(4) . . ?
C35 C44 C43 119.6(4) . . ?
C35 C44 C45 116.1(4) . . ?
C45 C44 C43 124.1(4) . . ?
O6 C45 C44 118.3(3) . . ?
N3 C45 O6 112.6(4) . . ?
N3 C45 C44 128.8(4) . . ?
O6 C46 C47 126.3(4) . . ?
C51 C46 O6 108.8(4) . . ?
C51 C46 C47 124.7(5) . . ?
C46 C47 H47 122.8 . . ?
C46 C47 C48 114.4(5) . . ?
C48 C47 H47 122.8 . . ?
C47 C48 H48 119.3 . . ?
C49 C48 C47 121.3(5) . . ?
C49 C48 H48 119.3 . . ?
C48 C49 H49 118.9 . . ?
C48 C49 C50 122.3(5) . . ?
C50 C49 H49 118.9 . . ?
C49 C50 H50 121.8 . . ?
C51 C50 C49 116.4(5) . . ?
C51 C50 H50 121.8 . . ?
C46 C51 N3 108.0(4) . . ?
C46 C51 C50 120.8(4) . . ?
C50 C51 N3 131.2(4) . . ?
O7 C52 C53 115.9(4) . . ?
O7 C52 C61 124.8(4) . . ?
C61 C52 C53 119.3(4) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 C52 120.1(4) . . ?
C54 C53 H53 119.9 . . ?
C53 C54 H54 119.0 . . ?
C53 C54 C55 121.9(4) . . ?
C55 C54 H54 119.0 . . ?
C56 C55 C54 120.0(4) . . ?
C56 C55 C60 120.7(4) . . ?
C60 C55 C54 119.3(4) . . ?
C55 C56 H56 119.3 . . ?
C57 C56 C55 121.4(5) . . ?
C57 C56 H56 119.3 . . ?
C56 C57 H57 120.8 . . ?
C56 C57 C58 118.3(5) . . ?
C58 C57 H57 120.8 . . ?
C57 C58 H58 119.5 . . ?
C59 C58 C57 121.0(5) . . ?
C59 C58 H58 119.5 . . ?
C58 C59 H59 119.3 . . ?
C58 C59 C60 121.5(5) . . ?
C60 C59 H59 119.3 . . ?
C55 C60 C61 118.5(4) . . ?
C59 C60 C55 116.8(4) . . ?
C59 C60 C61 124.4(4) . . ?
C52 C61 C60 120.6(4) . . ?
C52 C61 C62 115.5(4) . . ?
C60 C61 C62 123.4(4) . . ?
O8 C62 C61 117.9(4) . . ?
N4 C62 O8 113.1(4) . . ?
N4 C62 C61 128.7(4) . . ?
O8 C63 C64 127.0(4) . . ?
C68 C63 O8 109.3(4) . . ?
C68 C63 C64 123.7(4) . . ?
C63 C64 H64 122.2 . . ?
C65 C64 C63 115.6(4) . . ?
C65 C64 H64 122.2 . . ?
C64 C65 H65 119.1 . . ?
C64 C65 C66 121.8(4) . . ?
C66 C65 H65 119.1 . . ?
C65 C66 H66 119.8 . . ?
C67 C66 C65 120.5(4) . . ?
C67 C66 H66 119.8 . . ?
C66 C67 H67 121.1 . . ?
C68 C67 C66 117.8(4) . . ?
C68 C67 H67 121.1 . . ?
C63 C68 N4 107.4(4) . . ?
C63 C68 C67 120.6(4) . . ?
C67 C68 N4 131.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 C1 C2 -142.3(4) . . . . ?
Zr1 O1 C1 C10 37.5(7) . . . . ?
Zr1 O3 C18 C19 159.7(4) . . . . ?
Zr1 O3 C18 C27 -23.4(8) . . . . ?
Zr1 N1 C11 O2 -179.3(3) . . . . ?
Zr1 N1 C11 C10 -3.6(6) . . . . ?
Zr1 N1 C17 C12 179.4(3) . . . . ?
Zr1 N1 C17 C16 -0.5(7) . . . . ?
Zr1 N2 C28 O4 179.0(3) . . . . ?
Zr1 N2 C28 C27 6.8(7) . . . . ?
Zr1 N2 C34 C29 -179.1(3) . . . . ?
Zr1 N2 C34 C33 -3.3(7) . . . . ?
Zr2 O5 C35 C36 148.5(3) . . . . ?
Zr2 O5 C35 C44 -33.6(7) . . . . ?
Zr2 O7 C52 C53 -155.0(3) . . . . ?
Zr2 O7 C52 C61 23.8(7) . . . . ?
Zr2 N3 C45 O6 175.8(2) . . . . ?
Zr2 N3 C45 C44 2.0(6) . . . . ?
Zr2 N3 C51 C46 -177.2(3) . . . . ?
Zr2 N3 C51 C50 5.6(7) . . . . ?
Zr2 N4 C62 O8 173.4(3) . . . . ?
Zr2 N4 C62 C61 -13.1(7) . . . . ?
Zr2 N4 C68 C63 -173.0(3) . . . . ?
Zr2 N4 C68 C67 3.9(7) . . . . ?
O1 C1 C2 C3 176.3(4) . . . . ?
O1 C1 C10 C9 -174.3(4) . . . . ?
O1 C1 C10 C11 8.5(7) . . . . ?
O2 C12 C13 C14 -179.5(5) . . . . ?
O2 C12 C17 N1 -0.8(5) . . . . ?
O2 C12 C17 C16 179.1(4) . . . . ?
O3 C18 C19 C20 -173.7(4) . . . . ?
O3 C18 C27 C26 177.0(4) . . . . ?
O3 C18 C27 C28 -5.8(6) . . . . ?
O4 C29 C30 C31 178.6(5) . . . . ?
O4 C29 C34 N2 -1.2(5) . . . . ?
O4 C29 C34 C33 -177.7(4) . . . . ?
O5 C35 C36 C37 179.8(4) . . . . ?
O5 C35 C44 C43 175.8(4) . . . . ?
O5 C35 C44 C45 -9.4(6) . . . . ?
O6 C46 C47 C48 -179.5(5) . . . . ?
O6 C46 C51 N3 3.1(5) . . . . ?
O6 C46 C51 C50 -179.3(4) . . . . ?
O7 C52 C53 C54 176.3(4) . . . . ?
O7 C52 C61 C60 -172.9(4) . . . . ?
O7 C52 C61 C62 14.9(6) . . . . ?
O8 C63 C64 C65 -179.1(5) . . . . ?
O8 C63 C68 N4 -2.8(5) . . . . ?
O8 C63 C68 C67 179.9(4) . . . . ?
C1 C2 C3 C4 -1.1(7) . . . . ?
C1 C10 C11 O2 154.2(4) . . . . ?
C1 C10 C11 N1 -21.3(7) . . . . ?
C2 C1 C10 C9 5.5(6) . . . . ?
C2 C1 C10 C11 -171.7(4) . . . . ?
C2 C3 C4 C5 -176.3(4) . . . . ?
C2 C3 C4 C9 3.6(7) . . . . ?
C3 C4 C5 C6 178.8(4) . . . . ?
C3 C4 C9 C8 -178.6(4) . . . . ?
C3 C4 C9 C10 -1.6(6) . . . . ?
C4 C5 C6 C7 1.3(7) . . . . ?
C4 C9 C10 C1 -3.0(6) . . . . ?
C4 C9 C10 C11 174.0(4) . . . . ?
C5 C4 C9 C8 1.3(6) . . . . ?
C5 C4 C9 C10 178.3(4) . . . . ?
C5 C6 C7 C8 -1.6(8) . . . . ?
C6 C7 C8 C9 1.8(7) . . . . ?
C7 C8 C9 C4 -1.6(7) . . . . ?
C7 C8 C9 C10 -178.4(4) . . . . ?
C8 C9 C10 C1 173.8(4) . . . . ?
C8 C9 C10 C11 -9.2(7) . . . . ?
C9 C4 C5 C6 -1.2(7) . . . . ?
C9 C10 C11 O2 -23.0(6) . . . . ?
C9 C10 C11 N1 161.5(4) . . . . ?
C10 C1 C2 C3 -3.5(7) . . . . ?
C11 O2 C12 C13 -177.9(6) . . . . ?
C11 O2 C12 C17 0.2(5) . . . . ?
C11 N1 C17 C12 1.1(5) . . . . ?
C11 N1 C17 C16 -178.7(5) . . . . ?
C12 O2 C11 N1 0.6(5) . . . . ?
C12 O2 C11 C10 -175.4(4) . . . . ?
C12 C13 C14 C15 -3.2(9) . . . . ?
C13 C12 C17 N1 177.4(5) . . . . ?
C13 C12 C17 C16 -2.8(8) . . . . ?
C13 C14 C15 C16 3.8(9) . . . . ?
C14 C15 C16 C17 -3.5(7) . . . . ?
C15 C16 C17 N1 -177.2(4) . . . . ?
C15 C16 C17 C12 3.0(7) . . . . ?
C17 N1 C11 O2 -1.1(5) . . . . ?
C17 N1 C11 C10 174.6(4) . . . . ?
C17 C12 C13 C14 2.7(9) . . . . ?
C18 C19 C20 C21 -4.6(8) . . . . ?
C18 C27 C28 O4 -162.8(4) . . . . ?
C18 C27 C28 N2 9.0(7) . . . . ?
C19 C18 C27 C26 -6.1(6) . . . . ?
C19 C18 C27 C28 171.1(4) . . . . ?
C19 C20 C21 C22 179.9(5) . . . . ?
C19 C20 C21 C26 -3.4(8) . . . . ?
C20 C21 C22 C23 175.6(5) . . . . ?
C20 C21 C26 C25 -176.1(5) . . . . ?
C20 C21 C26 C27 6.2(7) . . . . ?
C21 C22 C23 C24 0.0(9) . . . . ?
C21 C26 C27 C18 -1.5(6) . . . . ?
C21 C26 C27 C28 -178.4(4) . . . . ?
C22 C21 C26 C25 0.7(7) . . . . ?
C22 C21 C26 C27 -177.0(4) . . . . ?
C22 C23 C24 C25 1.6(10) . . . . ?
C23 C24 C25 C26 -2.1(10) . . . . ?
C24 C25 C26 C21 0.9(8) . . . . ?
C24 C25 C26 C27 178.4(5) . . . . ?
C25 C26 C27 C18 -179.0(5) . . . . ?
C25 C26 C27 C28 4.1(7) . . . . ?
C26 C21 C22 C23 -1.1(8) . . . . ?
C26 C27 C28 O4 14.2(6) . . . . ?
C26 C27 C28 N2 -173.9(4) . . . . ?
C27 C18 C19 C20 9.3(7) . . . . ?
C28 O4 C29 C30 179.7(5) . . . . ?
C28 O4 C29 C34 0.0(5) . . . . ?
C28 N2 C34 C29 2.0(5) . . . . ?
C28 N2 C34 C33 177.8(5) . . . . ?
C29 O4 C28 N2 1.4(5) . . . . ?
C29 O4 C28 C27 174.6(4) . . . . ?
C29 C30 C31 C32 1.2(9) . . . . ?
C30 C29 C34 N2 179.0(5) . . . . ?
C30 C29 C34 C33 2.5(8) . . . . ?
C30 C31 C32 C33 -1.8(9) . . . . ?
C31 C32 C33 C34 2.7(8) . . . . ?
C32 C33 C34 N2 -178.3(5) . . . . ?
C32 C33 C34 C29 -2.9(7) . . . . ?
C34 N2 C28 O4 -2.1(5) . . . . ?
C34 N2 C28 C27 -174.3(4) . . . . ?
C34 C29 C30 C31 -1.6(9) . . . . ?
C35 C36 C37 C38 4.0(7) . . . . ?
C35 C44 C45 O6 -153.0(4) . . . . ?
C35 C44 C45 N3 20.4(6) . . . . ?
C36 C35 C44 C43 -6.3(6) . . . . ?
C36 C35 C44 C45 168.5(4) . . . . ?
C36 C37 C38 C39 176.0(5) . . . . ?
C36 C37 C38 C43 -4.8(7) . . . . ?
C37 C38 C39 C40 178.9(5) . . . . ?
C37 C38 C43 C42 179.0(4) . . . . ?
C37 C38 C43 C44 0.1(7) . . . . ?
C38 C39 C40 C41 1.4(8) . . . . ?
C38 C43 C44 C35 5.4(6) . . . . ?
C38 C43 C44 C45 -169.0(4) . . . . ?
C39 C38 C43 C42 -1.8(7) . . . . ?
C39 C38 C43 C44 179.2(4) . . . . ?
C39 C40 C41 C42 -0.5(8) . . . . ?
C40 C41 C42 C43 -1.7(8) . . . . ?
C41 C42 C43 C38 2.8(7) . . . . ?
C41 C42 C43 C44 -178.3(4) . . . . ?
C42 C43 C44 C35 -173.4(4) . . . . ?
C42 C43 C44 C45 12.2(7) . . . . ?
C43 C38 C39 C40 -0.2(8) . . . . ?
C43 C44 C45 O6 21.6(6) . . . . ?
C43 C44 C45 N3 -165.0(4) . . . . ?
C44 C35 C36 C37 1.7(6) . . . . ?
C45 O6 C46 C47 -179.1(5) . . . . ?
C45 O6 C46 C51 -2.4(5) . . . . ?
C45 N3 C51 C46 -2.6(5) . . . . ?
C45 N3 C51 C50 -179.8(5) . . . . ?
C46 O6 C45 N3 0.7(5) . . . . ?
C46 O6 C45 C44 175.2(4) . . . . ?
C46 C47 C48 C49 -3.7(8) . . . . ?
C47 C46 C51 N3 179.9(4) . . . . ?
C47 C46 C51 C50 -2.5(7) . . . . ?
C47 C48 C49 C50 1.5(8) . . . . ?
C48 C49 C50 C51 0.5(7) . . . . ?
C49 C50 C51 N3 176.9(4) . . . . ?
C49 C50 C51 C46 0.0(7) . . . . ?
C51 N3 C45 O6 1.2(5) . . . . ?
C51 N3 C45 C44 -172.6(4) . . . . ?
C51 C46 C47 C48 4.3(8) . . . . ?
C52 C53 C54 C55 -2.0(7) . . . . ?
C52 C61 C62 O8 157.1(4) . . . . ?
C52 C61 C62 N4 -16.1(7) . . . . ?
C53 C52 C61 C60 5.8(6) . . . . ?
C53 C52 C61 C62 -166.3(4) . . . . ?
C53 C54 C55 C56 -177.2(5) . . . . ?
C53 C54 C55 C60 3.3(7) . . . . ?
C54 C55 C56 C57 179.1(5) . . . . ?
C54 C55 C60 C59 -174.7(5) . . . . ?
C54 C55 C60 C61 0.0(7) . . . . ?
C55 C56 C57 C58 -2.4(8) . . . . ?
C55 C60 C61 C52 -4.6(6) . . . . ?
C55 C60 C61 C62 166.9(4) . . . . ?
C56 C55 C60 C59 5.8(7) . . . . ?
C56 C55 C60 C61 -179.4(4) . . . . ?
C56 C57 C58 C59 1.7(9) . . . . ?
C57 C58 C59 C60 2.9(9) . . . . ?
C58 C59 C60 C55 -6.6(8) . . . . ?
C58 C59 C60 C61 179.1(5) . . . . ?
C59 C60 C61 C52 169.7(5) . . . . ?
C59 C60 C61 C62 -18.8(7) . . . . ?
C60 C55 C56 C57 -1.5(7) . . . . ?
C60 C61 C62 O8 -14.7(6) . . . . ?
C60 C61 C62 N4 172.1(4) . . . . ?
C61 C52 C53 C54 -2.6(7) . . . . ?
C62 O8 C63 C64 -177.7(5) . . . . ?
C62 O8 C63 C68 0.8(5) . . . . ?
C62 N4 C68 C63 3.8(5) . . . . ?
C62 N4 C68 C67 -179.3(5) . . . . ?
C63 O8 C62 N4 1.8(5) . . . . ?
C63 O8 C62 C61 -172.4(4) . . . . ?
C63 C64 C65 C66 -2.8(8) . . . . ?
C64 C63 C68 N4 175.8(4) . . . . ?
C64 C63 C68 C67 -1.5(8) . . . . ?
C64 C65 C66 C67 2.1(8) . . . . ?
C65 C66 C67 C68 -0.9(7) . . . . ?
C66 C67 C68 N4 -175.9(5) . . . . ?
C66 C67 C68 C63 0.6(7) . . . . ?
C68 N4 C62 O8 -3.5(5) . . . . ?
C68 N4 C62 C61 170.0(4) . . . . ?
C68 C63 C64 C65 2.6(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.547 0.751 891.0 61.7 ?
2 0.500 -0.668 0.249 891.0 61.7 ?

_olex2_date_sample_data_collection 2015-11-12
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.768
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound7
_database_code_depnum_ccdc_archive 'CCDC 1816370'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-02-23
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C52 H32 N4 O8 Zr'
_chemical_formula_sum            'C52 H32 N4 O8 Zr'
_chemical_formula_weight         932.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H32 N4 O8 Zr'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.7490(2)
_cell_length_b                   14.56752(12)
_cell_length_c                   16.85932(16)
_cell_angle_alpha                90
_cell_angle_beta                 101.3990(10)
_cell_angle_gamma                90
_cell_volume                     4032.40(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23857
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2110
_cell_measurement_theta_min      4.0250
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0100
-1 0 0 0.0100
1 0 -1 0.0221
-1 0 1 0.0221
-5 -4 -2 0.0096
5 4 2 0.0096

_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.019
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0030 -0.0011 -0.0000 -0.0093 0.0340 0.0872
-1.0030 0.0011 0.0000 0.0093 -0.0340 -0.0872
1.0040 -0.0029 -1.0012 -0.0764 -0.0307 0.0856
-1.0040 0.0029 1.0012 0.0764 0.0307 -0.0856
-5.0081 -4.0124 -1.9995 -0.3644 -0.0098 -0.5807
5.0081 4.0124 1.9995 0.3644 0.0098 0.5807

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.348
_diffrn_reflns_theta_min         4.057
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00  31.00   1.00   20.00    --   38.00  82.00 -41.63   25
  2  ω    -53.00 -13.00   1.00   20.00    --  -38.50 -57.00-180.00   40
  3  ω    -37.00 -12.00   1.00   20.00    --  -38.50 -77.00-180.00   25
  4  ω   -109.00 -20.00   1.00   20.00    --  -38.50 -38.00  60.00   89
  5  ω   -106.00 -13.00   1.00   20.00    --  -38.50 -57.00 -30.00   93
  6  ω    -75.00 -43.00   1.00   20.00    --  -38.50 -77.00-180.00   32
  7  ω   -109.00 -78.00   1.00   20.00    --  -38.50 -77.00-180.00   31
  8  ω     32.00  97.00   1.00   20.00    --   43.45-137.00  12.00   65
  9  ω     23.00  84.00   1.00   20.00    --   43.45-125.00-120.00   61
 10  ω    -25.00  72.00   1.00   20.00    --   43.45 -77.00  30.00   97
 11  ω     14.00  39.00   1.00   20.00    --   46.00  83.00-113.75   25
 12  ω     19.00  46.00   1.00   20.00    --   50.00  80.00  82.99   27
 13  ω     18.00  43.00   1.00   20.00    --   50.00  82.00 146.08   25
 14  ω     19.00  44.00   1.00   20.00    --   50.00  81.00-166.78   25
 15  ω     18.00  44.00   1.00   20.00    --   50.00  82.00 -11.59   26
 16  ω     32.00  59.00   1.00   20.00    --   62.00  76.00 120.42   27
 17  ω     94.00 125.00   1.00   20.00    --   62.00  76.00 120.42   31
 18  ω     36.00  67.00   1.00   20.00    --   66.00  75.00  19.17   31
 19  ω     36.00  63.00   1.00   20.00    --   66.00  75.00 -94.50   27
 20  ω    111.00 137.00   1.00   20.00    --   66.00  77.00  68.44   26
 21  ω    107.00 137.00   1.00   20.00    --   66.00  75.00  19.17   30
 22  ω     36.00 115.00   1.00   20.00    --   66.00  76.00 -63.16   79
 23  ω     36.00  64.00   1.00   20.00    --   66.00  77.00  68.44   28
 24  ω     39.00  65.00   1.00   20.00    --   66.00  66.00  -8.30   26
 25  ω     37.00  65.00   1.00   20.00    --   66.00  75.00-135.37   28
 26  ω     37.00  68.00   1.00   20.00    --   66.00  75.00-170.64   31
 27  ω     38.00  65.00   1.00   20.00    --   66.00  75.00 152.94   27
 28  ω     97.00 135.00   1.00   20.00    --   66.00  66.00  -8.30   38
 29  ω     49.00  79.00   1.00   63.00    --   78.00  75.00 113.99   30
 30  ω     49.00  75.00   1.00   63.00    --   78.00  72.00  -6.99   26
 31  ω     61.00  88.00   1.00   63.00    --   86.00  60.00 176.76   27
 32  ω     57.00  85.00   1.00   63.00    --   86.00  74.00   4.26   28
 33  ω     65.00 158.00   1.00   63.00    --   90.00  56.00 -95.18   93
 34  ω     64.00  90.00   1.00   63.00    --   90.00  60.00  79.58   26
 35  ω     66.00 120.00   1.00   63.00    --   94.00  68.00 140.50   54
 36  ω     67.00  94.00   1.00   63.00    --   94.00  70.00 178.21   27
 37  ω     67.00  95.00   1.00   63.00    --   94.00  63.00  90.00   28
 38  ω     72.00  97.00   1.00   63.00    --   98.00  65.00 155.48   25
 39  ω     50.00 132.00   1.00   63.00    --  111.00 -45.00 150.00   82
 40  ω     87.00 114.00   1.00   63.00    --  111.00  61.00-150.00   27
 41  ω     31.00  77.00   1.00   63.00    --  111.00 -94.00 -30.00   46
 42  ω     65.00 106.00   1.00   63.00    --  111.00 -94.00-150.00   41
 43  ω     31.00  89.00   1.00   63.00    --  111.00 -94.00-180.00   58
 44  ω     85.00 120.00   1.00   63.00    --  111.00  61.00 -60.00   35
 45  ω     85.00 119.00   1.00   63.00    --  111.00  61.00 -90.00   34
 46  ω    116.00 168.00   1.00   63.00    --  111.00  77.00   0.00   52
 47  ω     81.00 107.00   1.00   63.00    --  111.00  77.00   0.00   26
 48  ω    116.00 150.00   1.00   63.00    --  111.00  77.00  90.00   34
 49  ω     81.00 107.00   1.00   63.00    --  111.00  77.00  90.00   26
 50  ω     81.00 164.00   1.00   63.00    --  111.00  77.00 -30.00   83
 51  ω     81.00 150.00   1.00   63.00    --  111.00  77.00 -60.00   69
 52  ω     86.00 113.00   1.00   63.00    --  111.00  61.00  30.00   27
 53  ω    129.00 178.00   1.00   63.00    --  111.00  74.00-154.63   49
 54  ω     82.00 159.00   1.00   63.00    --  111.00  77.00  30.00   77
 55  ω     81.00 178.00   1.00   63.00    --  111.00  77.00 150.00   97
 56  ω     83.00 108.00   1.00   63.00    --  111.00  74.00-154.63   25
 57  ω     85.00 164.00   1.00   63.00    --  111.00  61.00-120.00   79
 58  ω     83.00 173.00   1.00   63.00    --  111.00  77.00  60.00   90
 59  ω    112.00 152.00   1.00   63.00    --  111.00  77.00-180.00   40
 60  ω     81.00 107.00   1.00   63.00    --  111.00  77.00-180.00   26
 61  ω     64.00 122.00   1.00   63.00    --  111.00-125.00 -30.00   58
 62  ω     81.00 176.00   1.00   63.00    --  111.00  77.00 -90.00   95
 63  ω     88.00 171.00   1.00   63.00    --  111.00  61.00 120.00   83
 64  ω     32.00  86.00   1.00   63.00    --  111.00 -94.00 120.00   54
 65  ω     40.00 104.00   1.00   63.00    --  111.00 -94.00   0.00   64
 66  ω     83.00 110.00   1.00   63.00    --  111.00  77.00-120.00   27
 67  ω     72.00 120.00   1.00   63.00    --  111.00-125.00-180.00   48
 68  ω     33.00 103.00   1.00   63.00    --  111.00 -94.00  60.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0091478000
_diffrn_orient_matrix_UB_12      0.0688806000
_diffrn_orient_matrix_UB_13      0.0669601000
_diffrn_orient_matrix_UB_21      0.0338363000
_diffrn_orient_matrix_UB_22      -0.0720951000
_diffrn_orient_matrix_UB_23      0.0648178000
_diffrn_orient_matrix_UB_31      0.0870164000
_diffrn_orient_matrix_UB_32      0.0352585000
_diffrn_orient_matrix_UB_33      0.0016963000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3824
_reflns_number_total             3988
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0207
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+3.7676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0505
_refine_special_details          
;
 Disorder of the ligands on a two-fold axis. No larger cell or twinning resolves
 this disorder.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.5000 0.65105(2) 0.2500 0.02099(6) Uani 1 2 d S T P . .
O1A O 0.45558(11) 0.68367(13) 0.34839(11) 0.0234(4) Uani 0.5 1 d . . P A -1
C1A C 0.4761(3) 0.6884(3) 0.4289(3) 0.0202(9) Uani 0.5 1 d . . P A -1
C2A C 0.4362(9) 0.7521(10) 0.4713(6) 0.023(2) Uani 0.5 1 d . . P A -1
H2A H 0.3970 0.7912 0.4426 0.028 Uiso 0.5 1 calc R U P A -1
C3A C 0.4545(3) 0.7568(3) 0.5536(3) 0.0293(8) Uani 0.5 1 d . . P A -1
H3A H 0.4261 0.7972 0.5805 0.035 Uiso 0.5 1 calc R U P A -1
C4A C 0.5159(6) 0.7011(4) 0.5982(5) 0.0327(14) Uani 0.5 1 d . . P A -1
H4A H 0.5293 0.7055 0.6543 0.039 Uiso 0.5 1 calc R U P A -1
C5A C 0.5556(3) 0.6404(4) 0.5579(3) 0.0307(11) Uani 0.5 1 d . . P A -1
H5A H 0.5958 0.6030 0.5873 0.037 Uiso 0.5 1 calc R U P A -1
C6A C 0.5375(2) 0.6329(2) 0.4735(2) 0.0242(6) Uani 0.5 1 d . . P A -1
C7A C 0.5807(4) 0.5617(3) 0.4304(4) 0.0188(7) Uani 0.5 1 d . . P A -1
O2A O 0.62967(12) 0.50538(13) 0.47971(12) 0.0276(4) Uani 0.5 1 d . . P A -1
C8A C 0.6570(3) 0.4490(3) 0.4256(3) 0.0280(9) Uani 0.5 1 d . . P A -1
C9A C 0.7107(16) 0.3757(17) 0.4430(18) 0.035(3) Uani 0.5 1 d . . P A -1
H9A H 0.7346 0.3592 0.4957 0.042 Uiso 0.5 1 calc R U P A -1
C10A C 0.7261(3) 0.3287(4) 0.3757(5) 0.0392(15) Uani 0.5 1 d . . P A -1
H10A H 0.7623 0.2796 0.3831 0.047 Uiso 0.5 1 calc R U P A -1
C11A C 0.6882(3) 0.3537(3) 0.2967(4) 0.0364(8) Uani 0.5 1 d . . P A -1
H11A H 0.6996 0.3201 0.2534 0.044 Uiso 0.5 1 calc R U P A -1
C12A C 0.6343(5) 0.4269(5) 0.2811(4) 0.0289(13) Uani 0.5 1 d . . P A -1
H12A H 0.6097 0.4427 0.2285 0.035 Uiso 0.5 1 calc R U P A -1
C13A C 0.6179(7) 0.4775(7) 0.3494(4) 0.0235(15) Uani 0.5 1 d . . P A -1
N1A N 0.57204(14) 0.55319(16) 0.35429(14) 0.0225(5) Uani 0.5 1 d . . P A -1
O3A O 0.48610(12) 0.78273(12) 0.19844(11) 0.0223(4) Uani 0.5 1 d . . P A -1
C14A C 0.4382(5) 0.8338(5) 0.1431(4) 0.0214(10) Uani 0.5 1 d . . P A -1
C15A C 0.4697(5) 0.9136(5) 0.1159(4) 0.0253(14) Uani 0.5 1 d . . P A -1
H15A H 0.5222 0.9324 0.1390 0.030 Uiso 0.5 1 calc R U P A -1
C16A C 0.4236(5) 0.9652(3) 0.0548(4) 0.0338(14) Uani 0.5 1 d . . P A -1
H16A H 0.4455 1.0184 0.0373 0.041 Uiso 0.5 1 calc R U P A -1
C17A C 0.3445(4) 0.9385(6) 0.0187(4) 0.0337(16) Uani 0.5 1 d . . P A -1
H17A H 0.3148 0.9716 -0.0244 0.040 Uiso 0.5 1 calc R U P A -1
C18A C 0.3113(3) 0.8624(5) 0.0484(4) 0.0277(10) Uani 0.5 1 d . . P A -1
H18A H 0.2578 0.8458 0.0268 0.033 Uiso 0.5 1 calc R U P A -1
C19A C 0.3573(4) 0.8093(3) 0.1111(3) 0.0228(7) Uani 0.5 1 d . . P A -1
C20A C 0.3219(5) 0.7376(5) 0.1484(5) 0.0188(7) Uani 0.5 1 d . . P A -1
O4A O 0.23621(12) 0.73111(15) 0.13129(12) 0.0294(5) Uani 0.5 1 d . . P A -1
C21A C 0.2193(5) 0.6650(5) 0.1834(4) 0.0295(13) Uani 0.5 1 d . . P A -1
C22A C 0.1425(6) 0.6338(5) 0.1904(5) 0.0423(15) Uani 0.5 1 d . . P A -1
H22A H 0.0951 0.6539 0.1564 0.051 Uiso 0.5 1 calc R U P A -1
C23A C 0.1417(4) 0.5708(4) 0.2514(4) 0.0410(11) Uani 0.5 1 d . . P A -1
H23A H 0.0920 0.5477 0.2591 0.049 Uiso 0.5 1 calc R U P A -1
C24A C 0.2131(5) 0.5407(4) 0.3021(4) 0.0343(11) Uani 0.5 1 d . . P A -1
H24A H 0.2101 0.4987 0.3429 0.041 Uiso 0.5 1 calc R U P A -1
C25A C 0.2887(4) 0.5726(4) 0.2923(3) 0.0271(11) Uani 0.5 1 d . . P A -1
H25A H 0.3364 0.5530 0.3262 0.032 Uiso 0.5 1 calc R U P A -1
C26A C 0.2908(3) 0.6344(3) 0.2304(4) 0.0208(8) Uani 0.5 1 d . . P A -1
N2A N 0.35469(14) 0.67915(16) 0.20439(14) 0.0217(5) Uani 0.5 1 d . . P A -1
O5A O 0.44823(12) 0.52062(13) 0.22799(12) 0.0245(4) Uani 0.5 1 d . . P A -1
C27A C 0.3923(7) 0.4705(7) 0.1763(4) 0.0217(13) Uani 0.5 1 d . . P A -1
C28A C 0.3513(4) 0.4006(4) 0.2014(5) 0.0295(14) Uani 0.5 1 d . . P A -1
H28A H 0.3590 0.3883 0.2566 0.035 Uiso 0.5 1 calc R U P A -1
C29A C 0.2981(4) 0.3461(4) 0.1479(4) 0.0331(12) Uani 0.5 1 d . . P A -1
H29A H 0.2701 0.2983 0.1669 0.040 Uiso 0.5 1 calc R U P A -1
C30A C 0.2872(15) 0.3639(16) 0.0662(16) 0.034(4) Uani 0.5 1 d . . P A -1
H30A H 0.2507 0.3285 0.0301 0.040 Uiso 0.5 1 calc R U P A -1
C31A C 0.3289(3) 0.4323(3) 0.0374(3) 0.0289(9) Uani 0.5 1 d . . P A -1
H31A H 0.3222 0.4420 -0.0181 0.035 Uiso 0.5 1 calc R U P A -1
C32A C 0.3821(2) 0.4883(2) 0.0915(3) 0.0250(7) Uani 0.5 1 d . . P A -1
C33A C 0.4290(4) 0.5654(3) 0.0581(4) 0.0188(7) Uani 0.5 1 d . . P A -1
O6A O 0.42183(12) 0.56428(14) -0.02216(12) 0.0275(4) Uani 0.5 1 d . . P A -1
C34A C 0.4713(3) 0.6364(4) -0.0334(3) 0.0269(10) Uani 0.5 1 d . . P A -1
C35A C 0.4887(5) 0.6690(4) -0.1054(5) 0.0353(15) Uani 0.5 1 d . . P A -1
H35A H 0.4664 0.6423 -0.1549 0.042 Uiso 0.5 1 calc R U P A -1
C36A C 0.5406(2) 0.7428(3) -0.0996(3) 0.0366(8) Uani 0.5 1 d . . P A -1
H36A H 0.5526 0.7684 -0.1465 0.044 Uiso 0.5 1 calc R U P A -1
C37A C 0.5757(3) 0.7801(3) -0.0242(4) 0.0307(9) Uani 0.5 1 d . . P A -1
H37A H 0.6106 0.8300 -0.0221 0.037 Uiso 0.5 1 calc R U P A -1
C38A C 0.5597(9) 0.7443(10) 0.0478(8) 0.025(2) Uani 0.5 1 d . . P A -1
H38A H 0.5857 0.7668 0.0979 0.030 Uiso 0.5 1 calc R U P A -1
C39A C 0.5035(3) 0.6736(3) 0.0413(3) 0.0227(10) Uani 0.5 1 d . . P A -1
N3A N 0.47244(14) 0.62506(16) 0.10043(14) 0.0225(5) Uani 0.5 1 d . . P A -1
O7A O 0.60878(11) 0.62108(13) 0.20914(12) 0.0238(4) Uani 0.5 1 d . . P A -1
C40A C 0.6888(3) 0.6179(3) 0.2345(3) 0.0201(7) Uani 0.5 1 d . . P A -1
C41A C 0.7370(4) 0.5667(4) 0.1910(4) 0.0266(11) Uani 0.5 1 d . . P A -1
H41A H 0.7124 0.5375 0.1433 0.032 Uiso 0.5 1 calc R U P A -1
C42A C 0.8195(4) 0.5591(4) 0.2176(4) 0.0319(12) Uani 0.5 1 d . . P A -1
H42A H 0.8500 0.5242 0.1882 0.038 Uiso 0.5 1 calc R U P A -1
C43A C 0.8585(4) 0.6032(5) 0.2882(4) 0.0314(13) Uani 0.5 1 d . . P A -1
H43A H 0.9145 0.5974 0.3063 0.038 Uiso 0.5 1 calc R U P A -1
C44A C 0.8127(5) 0.6556(4) 0.3309(4) 0.0278(11) Uani 0.5 1 d . . P A -1
H44A H 0.8382 0.6859 0.3776 0.033 Uiso 0.5 1 calc R U P A -1
C45A C 0.7285(4) 0.6638(3) 0.3046(3) 0.0223(7) Uani 0.5 1 d . . P A -1
C46A C 0.6853(5) 0.7280(5) 0.3425(5) 0.0188(7) Uani 0.5 1 d . . P A -1
O8A O 0.72566(12) 0.78482(13) 0.40226(12) 0.0263(4) Uani 0.5 1 d . . P A -1
C47A C 0.6683(3) 0.8460(4) 0.4174(4) 0.0246(9) Uani 0.5 1 d . . P A -1
C48A C 0.6805(5) 0.9177(5) 0.4726(4) 0.0315(14) Uani 0.5 1 d . . P A -1
H48A H 0.7300 0.9270 0.5079 0.038 Uiso 0.5 1 calc R U P A -1
C49A C 0.6141(5) 0.9744(5) 0.4719(4) 0.0338(11) Uani 0.5 1 d . . P A -1
H49A H 0.6187 1.0238 0.5075 0.041 Uiso 0.5 1 calc R U P A -1
C50A C 0.5398(4) 0.9587(5) 0.4181(4) 0.0295(10) Uani 0.5 1 d . . P A -1
H50A H 0.4969 0.9994 0.4175 0.035 Uiso 0.5 1 calc R U P A -1
C51A C 0.5286(5) 0.8839(5) 0.3657(5) 0.0234(11) Uani 0.5 1 d . . P A -1
H51A H 0.4790 0.8730 0.3310 0.028 Uiso 0.5 1 calc R U P A -1
C52A C 0.5954(5) 0.8260(5) 0.3675(4) 0.0215(12) Uani 0.5 1 d . . P A -1
N4A N 0.60513(14) 0.74799(16) 0.32349(14) 0.0217(5) Uani 0.5 1 d . . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1A 2.0047(19) . ?
Zr1 N1A 2.396(2) . ?
Zr1 O3A 2.0999(18) . ?
Zr1 N2A 2.438(2) . ?
Zr1 O5A 2.0910(19) . ?
Zr1 N3A 2.501(2) . ?
Zr1 O7A 2.1168(19) . ?
Zr1 N4A 2.401(2) . ?
O1A C1A 1.335(5) . ?
C1A C2A 1.416(12) . ?
C1A C6A 1.404(5) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.362(11) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.405(11) . ?
C4A H4A 0.9300 . ?
C4A C5A 1.366(12) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.399(6) . ?
C6A C7A 1.528(6) . ?
C7A O2A 1.330(6) . ?
C7A C13A 2.023(11) . ?
C7A N1A 1.268(7) . ?
O2A C8A 1.372(5) . ?
C8A C9A 1.39(2) . ?
C8A C13A 1.385(9) . ?
C9A H9A 0.9300 . ?
C9A C10A 1.39(3) . ?
C10A H10A 0.9300 . ?
C10A C11A 1.406(7) . ?
C11A H11A 0.9300 . ?
C11A C12A 1.389(6) . ?
C12A H12A 0.9300 . ?
C12A C13A 1.439(11) . ?
C13A N1A 1.355(12) . ?
O3A C14A 1.331(8) . ?
C14A C15A 1.391(10) . ?
C14A C19A 1.403(6) . ?
C15A H15A 0.9300 . ?
C15A C16A 1.381(7) . ?
C16A H16A 0.9300 . ?
C16A C17A 1.400(9) . ?
C17A H17A 0.9300 . ?
C17A C18A 1.378(8) . ?
C18A H18A 0.9300 . ?
C18A C19A 1.409(6) . ?
C19A C20A 1.408(7) . ?
C20A O4A 1.411(8) . ?
C20A N2A 1.309(6) . ?
O4A C21A 1.371(7) . ?
C21A C22A 1.390(10) . ?
C21A C26A 1.373(7) . ?
C22A H22A 0.9300 . ?
C22A C23A 1.381(7) . ?
C23A H23A 0.9300 . ?
C23A C24A 1.396(7) . ?
C24A H24A 0.9300 . ?
C24A C25A 1.388(7) . ?
C25A H25A 0.9300 . ?
C25A C26A 1.384(7) . ?
C26A N2A 1.396(5) . ?
O5A C27A 1.359(10) . ?
C27A C28A 1.342(14) . ?
C27A C32A 1.430(6) . ?
C28A H28A 0.9300 . ?
C28A C29A 1.386(7) . ?
C29A H29A 0.9300 . ?
C29A C30A 1.38(3) . ?
C30A H30A 0.9300 . ?
C30A C31A 1.36(2) . ?
C31A H31A 0.9300 . ?
C31A C32A 1.403(5) . ?
C32A C33A 1.540(6) . ?
C33A O6A 1.334(7) . ?
C33A N3A 1.261(6) . ?
O6A C34A 1.374(6) . ?
C34A C35A 1.386(11) . ?
C34A C39A 1.380(7) . ?
C35A H35A 0.9300 . ?
C35A C36A 1.374(10) . ?
C36A H36A 0.9300 . ?
C36A C37A 1.401(6) . ?
C37A H37A 0.9300 . ?
C37A C38A 1.395(10) . ?
C38A H38A 0.9300 . ?
C38A C39A 1.384(16) . ?
C39A N3A 1.404(6) . ?
O7A C40A 1.325(5) . ?
C40A C41A 1.407(6) . ?
C40A C45A 1.406(6) . ?
C41A H41A 0.9300 . ?
C41A C42A 1.371(7) . ?
C42A H42A 0.9300 . ?
C42A C43A 1.396(7) . ?
C43A H43A 0.9300 . ?
C43A C44A 1.381(9) . ?
C44A H44A 0.9300 . ?
C44A C45A 1.398(6) . ?
C45A C46A 1.410(7) . ?
C46A O8A 1.374(6) . ?
C46A N4A 1.350(8) . ?
O8A C47A 1.371(5) . ?
C47A C48A 1.387(9) . ?
C47A C52A 1.370(7) . ?
C48A H48A 0.9300 . ?
C48A C49A 1.384(8) . ?
C49A H49A 0.9300 . ?
C49A C50A 1.407(6) . ?
C50A H50A 0.9300 . ?
C50A C51A 1.391(7) . ?
C51A H51A 0.9300 . ?
C51A C52A 1.396(10) . ?
C52A N4A 1.385(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1A Zr1 N1A 75.48(8) . . ?
O1A Zr1 O3A 95.57(7) . . ?
O1A Zr1 N2A 73.17(8) . . ?
O1A Zr1 O5A 98.83(8) . . ?
O1A Zr1 N3A 147.72(7) . . ?
O1A Zr1 O7A 143.35(7) . . ?
O1A Zr1 N4A 77.75(8) . . ?
N1A Zr1 N2A 131.15(8) . . ?
N1A Zr1 N3A 128.00(8) . . ?
N1A Zr1 N4A 76.10(8) . . ?
O3A Zr1 N1A 147.76(7) . . ?
O3A Zr1 N2A 72.18(8) . . ?
O3A Zr1 N3A 74.79(7) . . ?
O3A Zr1 O7A 94.92(7) . . ?
O3A Zr1 N4A 71.72(8) . . ?
N2A Zr1 N3A 74.55(7) . . ?
O5A Zr1 N1A 73.78(7) . . ?
O5A Zr1 O3A 138.45(7) . . ?
O5A Zr1 N2A 75.13(8) . . ?
O5A Zr1 N3A 72.31(8) . . ?
O5A Zr1 O7A 96.22(8) . . ?
O5A Zr1 N4A 149.53(7) . . ?
O7A Zr1 N1A 77.00(8) . . ?
O7A Zr1 N2A 143.31(7) . . ?
O7A Zr1 N3A 68.89(7) . . ?
O7A Zr1 N4A 72.47(8) . . ?
N4A Zr1 N2A 130.43(8) . . ?
N4A Zr1 N3A 125.42(8) . . ?
C1A O1A Zr1 142.3(3) . . ?
O1A C1A C2A 119.7(6) . . ?
O1A C1A C6A 121.9(4) . . ?
C6A C1A C2A 118.5(6) . . ?
C1A C2A H2A 119.6 . . ?
C3A C2A C1A 120.9(10) . . ?
C3A C2A H2A 119.6 . . ?
C2A C3A H3A 119.7 . . ?
C2A C3A C4A 120.6(7) . . ?
C4A C3A H3A 119.7 . . ?
C3A C4A H4A 120.5 . . ?
C5A C4A C3A 119.0(7) . . ?
C5A C4A H4A 120.5 . . ?
C4A C5A H5A 119.1 . . ?
C4A C5A C6A 121.8(5) . . ?
C6A C5A H5A 119.1 . . ?
C1A C6A C7A 120.2(4) . . ?
C5A C6A C1A 119.2(4) . . ?
C5A C6A C7A 120.6(5) . . ?
C6A C7A C13A 166.0(5) . . ?
O2A C7A C6A 114.4(5) . . ?
O2A C7A C13A 79.3(4) . . ?
N1A C7A C6A 125.3(5) . . ?
N1A C7A O2A 120.4(4) . . ?
N1A C7A C13A 41.2(3) . . ?
C7A O2A C8A 101.5(4) . . ?
O2A C8A C9A 127.3(13) . . ?
O2A C8A C13A 106.2(6) . . ?
C13A C8A C9A 126.5(13) . . ?
C8A C9A H9A 122.5 . . ?
C8A C9A C10A 115(2) . . ?
C10A C9A H9A 122.5 . . ?
C9A C10A H10A 119.2 . . ?
C9A C10A C11A 121.5(11) . . ?
C11A C10A H10A 119.2 . . ?
C10A C11A H11A 118.8 . . ?
C12A C11A C10A 122.3(5) . . ?
C12A C11A H11A 118.8 . . ?
C11A C12A H12A 121.3 . . ?
C11A C12A C13A 117.5(6) . . ?
C13A C12A H12A 121.3 . . ?
C8A C13A C7A 73.1(4) . . ?
C8A C13A C12A 117.3(8) . . ?
C12A C13A C7A 169.6(7) . . ?
N1A C13A C7A 38.0(3) . . ?
N1A C13A C8A 110.9(5) . . ?
N1A C13A C12A 131.7(6) . . ?
C7A N1A Zr1 128.6(2) . . ?
C7A N1A C13A 100.8(4) . . ?
C13A N1A Zr1 130.4(3) . . ?
C14A O3A Zr1 143.4(4) . . ?
O3A C14A C15A 118.9(6) . . ?
O3A C14A C19A 122.0(7) . . ?
C15A C14A C19A 119.0(7) . . ?
C14A C15A H15A 119.7 . . ?
C16A C15A C14A 120.6(7) . . ?
C16A C15A H15A 119.7 . . ?
C15A C16A H16A 119.5 . . ?
C15A C16A C17A 121.0(6) . . ?
C17A C16A H16A 119.5 . . ?
C16A C17A H17A 120.6 . . ?
C18A C17A C16A 118.7(6) . . ?
C18A C17A H17A 120.6 . . ?
C17A C18A H18A 119.5 . . ?
C17A C18A C19A 121.0(6) . . ?
C19A C18A H18A 119.5 . . ?
C14A C19A C18A 119.5(6) . . ?
C14A C19A C20A 118.4(6) . . ?
C20A C19A C18A 121.8(7) . . ?
C19A C20A O4A 117.3(5) . . ?
N2A C20A C19A 130.6(6) . . ?
N2A C20A O4A 111.6(4) . . ?
C21A O4A C20A 104.3(4) . . ?
O4A C21A C22A 126.6(6) . . ?
O4A C21A C26A 109.3(7) . . ?
C26A C21A C22A 124.1(6) . . ?
C21A C22A H22A 122.4 . . ?
C23A C22A C21A 115.3(8) . . ?
C23A C22A H22A 122.4 . . ?
C22A C23A H23A 119.0 . . ?
C22A C23A C24A 122.0(8) . . ?
C24A C23A H23A 119.0 . . ?
C23A C24A H24A 119.5 . . ?
C25A C24A C23A 121.0(7) . . ?
C25A C24A H24A 119.5 . . ?
C24A C25A H25A 121.1 . . ?
C26A C25A C24A 117.8(6) . . ?
C26A C25A H25A 121.1 . . ?
C21A C26A C25A 119.8(5) . . ?
C21A C26A N2A 107.6(7) . . ?
C25A C26A N2A 132.5(6) . . ?
C20A N2A Zr1 125.9(4) . . ?
C20A N2A C26A 107.0(5) . . ?
C26A N2A Zr1 127.0(3) . . ?
C27A O5A Zr1 144.2(3) . . ?
O5A C27A C32A 118.3(8) . . ?
C28A C27A O5A 122.4(6) . . ?
C28A C27A C32A 119.0(8) . . ?
C27A C28A H28A 118.9 . . ?
C27A C28A C29A 122.2(7) . . ?
C29A C28A H28A 118.9 . . ?
C28A C29A H29A 120.6 . . ?
C30A C29A C28A 118.9(10) . . ?
C30A C29A H29A 120.6 . . ?
C29A C30A H30A 119.3 . . ?
C31A C30A C29A 121.3(16) . . ?
C31A C30A H30A 119.3 . . ?
C30A C31A H31A 120.1 . . ?
C30A C31A C32A 119.9(11) . . ?
C32A C31A H31A 120.1 . . ?
C27A C32A C33A 122.0(7) . . ?
C31A C32A C27A 118.7(6) . . ?
C31A C32A C33A 119.4(4) . . ?
O6A C33A C32A 114.3(4) . . ?
N3A C33A C32A 125.1(6) . . ?
N3A C33A O6A 120.6(4) . . ?
C33A O6A C34A 101.2(3) . . ?
O6A C34A C35A 128.3(5) . . ?
O6A C34A C39A 108.2(4) . . ?
C39A C34A C35A 123.5(6) . . ?
C34A C35A H35A 121.8 . . ?
C36A C35A C34A 116.5(6) . . ?
C36A C35A H35A 121.8 . . ?
C35A C36A H36A 119.6 . . ?
C35A C36A C37A 120.9(5) . . ?
C37A C36A H36A 119.6 . . ?
C36A C37A H37A 119.1 . . ?
C38A C37A C36A 121.8(7) . . ?
C38A C37A H37A 119.1 . . ?
C37A C38A H38A 121.5 . . ?
C39A C38A C37A 116.9(11) . . ?
C39A C38A H38A 121.5 . . ?
C34A C39A C38A 120.2(7) . . ?
C34A C39A N3A 108.5(4) . . ?
C38A C39A N3A 131.3(7) . . ?
C33A N3A Zr1 130.3(3) . . ?
C33A N3A C39A 101.4(4) . . ?
C39A N3A Zr1 128.3(3) . . ?
C40A O7A Zr1 141.5(3) . . ?
O7A C40A C41A 119.9(5) . . ?
O7A C40A C45A 122.3(5) . . ?
C45A C40A C41A 117.8(5) . . ?
C40A C41A H41A 119.4 . . ?
C42A C41A C40A 121.1(5) . . ?
C42A C41A H41A 119.4 . . ?
C41A C42A H42A 119.5 . . ?
C41A C42A C43A 120.9(5) . . ?
C43A C42A H42A 119.5 . . ?
C42A C43A H43A 120.5 . . ?
C44A C43A C42A 118.9(6) . . ?
C44A C43A H43A 120.5 . . ?
C43A C44A H44A 119.6 . . ?
C43A C44A C45A 120.8(7) . . ?
C45A C44A H44A 119.6 . . ?
C40A C45A C46A 119.8(6) . . ?
C44A C45A C40A 120.4(6) . . ?
C44A C45A C46A 119.3(6) . . ?
O8A C46A C45A 120.7(6) . . ?
N4A C46A C45A 127.6(5) . . ?
N4A C46A O8A 111.5(4) . . ?
C47A O8A C46A 105.5(4) . . ?
O8A C47A C48A 126.8(7) . . ?
C52A C47A O8A 108.7(8) . . ?
C52A C47A C48A 124.5(5) . . ?
C47A C48A H48A 122.2 . . ?
C49A C48A C47A 115.6(8) . . ?
C49A C48A H48A 122.2 . . ?
C48A C49A H49A 119.5 . . ?
C48A C49A C50A 121.0(9) . . ?
C50A C49A H49A 119.5 . . ?
C49A C50A H50A 119.0 . . ?
C51A C50A C49A 121.9(9) . . ?
C51A C50A H50A 119.0 . . ?
C50A C51A H51A 121.6 . . ?
C50A C51A C52A 116.8(8) . . ?
C52A C51A H51A 121.6 . . ?
C47A C52A C51A 120.0(6) . . ?
C47A C52A N4A 108.5(7) . . ?
N4A C52A C51A 131.4(7) . . ?
C46A N4A Zr1 126.1(3) . . ?
C46A N4A C52A 105.5(4) . . ?
C52A N4A Zr1 127.4(3) . . ?

_olex2_date_sample_data_collection 2016-02-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.756
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1816365'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-02-05
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H34 N2 O6 Zr'
_chemical_formula_sum            'C40 H34 N2 O6 Zr'
_chemical_formula_weight         729.91
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H34 N2 O6 Zr'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4580(3)
_cell_length_b                   18.0852(2)
_cell_length_c                   25.5064(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.3075(13)
_cell_angle_gamma                90
_cell_volume                     9870.4(2)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    108020
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.0570
_cell_measurement_theta_min      1.6390
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4512
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 3 5 0.0987
1 -3 -5 0.0987
5 -1 4 0.1902
-3 0 -5 0.1407
-3 -5 4 0.1672
3 5 -4 0.1672
-5 -2 0 0.1841
5 2 0 0.1841
-3 5 0 0.1256
0 5 2 0.1230
4 -5 1 0.1948
0 0 1 0.1378
-4 1 5 0.1436
5 -1 -1 0.1784

_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.197
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9933 2.9993 4.9984 -0.1816 -0.0133 0.0225
0.9933 -2.9993 -4.9984 0.1816 0.0133 -0.0225
5.0007 -0.9996 3.9891 -0.0109 -0.0154 0.2091
-3.0031 -0.0006 -4.9913 0.0704 0.0338 -0.1588
-2.9985 -4.9931 3.9974 0.0487 -0.2378 0.0048
2.9985 4.9931 -3.9974 -0.0487 0.2378 -0.0048
-4.9992 -1.9964 0.0055 0.0231 -0.1259 -0.1311
4.9992 1.9964 -0.0055 -0.0231 0.1259 0.1311
-2.9954 4.9966 0.0068 -0.1609 0.0879 -0.1210
0.0050 4.9962 2.0010 -0.1771 0.1007 -0.0053
3.9959 -4.9966 0.9909 0.1494 -0.0888 0.1643
0.0009 0.0003 0.9991 -0.0181 -0.0155 0.0144
-3.9933 1.0022 5.0012 -0.1451 -0.1099 -0.0507
4.9963 -1.0012 -1.0063 0.0795 0.0623 0.1372

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            225130
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         1.474
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  92.90   0.30    5.00    --   25.03  77.00 -30.00  323
  2  ω    -44.00  52.90   0.30    5.00    --   25.03 -77.00 -90.00  323
  3  ω    -43.00  44.00   0.30    5.00    --   25.03 -57.00  60.00  290
  4  ω     -4.00  92.90   0.30    5.00    --   25.03  77.00-150.00  323
  5  ω      7.00  91.90   0.30    5.00    --   25.03  57.00  90.00  283
  6  ω    -20.00  64.90   0.30    5.00    --   25.03 -99.00-180.00  283
  7  ω    -20.00  64.90   0.30    5.00    --   25.03 -99.00  30.00  283
  8  ω      7.00  91.90   0.30    5.00    --   25.03  57.00 120.00  283
  9  ω      3.00  96.00   0.30    5.00    --   25.03  38.00 -30.00  310
 10  ω    -46.00  47.00   0.30    5.00    --   25.03 -38.00-180.00  310
 11  ω    -47.00  61.90   0.30    5.00    --   25.03 -19.00 -60.00  363
 12  ω    -95.00  46.90   0.30    5.00    --  -23.50   0.00-180.00  473
 13  ω    -45.00   6.00   0.30    5.00    --  -23.50 -80.00 -21.00  170
 14  ω    -95.00  46.90   0.30    5.00    --  -23.50   0.00-120.00  473
 15  ω    -95.00  46.90   0.30    5.00    --  -23.50   0.00-150.00  473
 16  ω      7.00  91.90   0.30    5.00    --   25.03  57.00 -90.00  283
 17  ω      7.00  91.90   0.30    5.00    --   25.03  57.00-180.00  283
 18  ω    -20.00  64.90   0.30    5.00    --   25.03 -99.00  90.00  283
 19  ω    -20.00  64.90   0.30    5.00    --   25.03 -99.00 -90.00  283
 20  ω     -4.00  44.00   0.30    5.00    --   25.03  80.00 102.00  160
 21  ω    -95.00 -86.30   0.30    5.00    --  -23.50   0.00 -60.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0066161000
_diffrn_orient_matrix_UB_12      -0.0282051000
_diffrn_orient_matrix_UB_13      -0.0180831000
_diffrn_orient_matrix_UB_21      0.0146255000
_diffrn_orient_matrix_UB_22      0.0263729000
_diffrn_orient_matrix_UB_23      -0.0155832000
_diffrn_orient_matrix_UB_31      0.0289840000
_diffrn_orient_matrix_UB_32      -0.0068539000
_diffrn_orient_matrix_UB_33      0.0143757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13758
_reflns_number_total             14476
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         14476
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0352P)²+12.9089P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0840
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.16174(2) 0.62229(2) 0.56493(2) 0.01718(4) Uani 1 1 d . . . . .
O1 O 0.14099(5) 0.60115(5) 0.64145(4) 0.02182(19) Uani 1 1 d . . . . .
O2 O 0.27251(4) 0.43441(5) 0.64466(4) 0.01903(18) Uani 1 1 d . . . . .
O3 O 0.18509(4) 0.57713(5) 0.49490(4) 0.01880(18) Uani 1 1 d . . . . .
O4 O 0.06280(4) 0.40623(5) 0.52250(4) 0.01728(17) Uani 1 1 d . . . . .
O5 O 0.22688(5) 0.69603(6) 0.57376(5) 0.0288(2) Uani 1 1 d . . . . .
O6 O 0.08988(5) 0.68415(5) 0.54595(4) 0.02272(19) Uani 1 1 d . . . . .
N1 N 0.23308(5) 0.53013(6) 0.59730(4) 0.01695(19) Uani 1 1 d . . . . .
N2 N 0.09667(5) 0.51770(6) 0.55002(4) 0.01590(19) Uani 1 1 d . . . . .
C1 C 0.13511(6) 0.54192(8) 0.67071(5) 0.0207(2) Uani 1 1 d . . . . .
C2 C 0.09210(7) 0.54550(9) 0.71079(6) 0.0264(3) Uani 1 1 d . . . . .
H2 H 0.0696 0.5888 0.7151 0.032 Uiso 1 1 calc R U . . .
C3 C 0.08343(7) 0.48689(10) 0.74264(6) 0.0301(3) Uani 1 1 d . . . . .
H3 H 0.0565 0.4915 0.7693 0.036 Uiso 1 1 calc R U . . .
C4 C 0.11455(7) 0.41884(10) 0.73615(6) 0.0276(3) Uani 1 1 d . . . . .
C5 C 0.10193(8) 0.35660(11) 0.76756(6) 0.0364(4) Uani 1 1 d . . . . .
H5 H 0.0740 0.3613 0.7935 0.044 Uiso 1 1 calc R U . . .
C6 C 0.12993(9) 0.29002(11) 0.76042(7) 0.0393(4) Uani 1 1 d . . . . .
H6 H 0.1216 0.2499 0.7816 0.047 Uiso 1 1 calc R U . . .
C7 C 0.17151(9) 0.28281(10) 0.72080(7) 0.0363(4) Uani 1 1 d . . . . .
H7 H 0.1897 0.2371 0.7151 0.044 Uiso 1 1 calc R U . . .
C8 C 0.18577(8) 0.34226(9) 0.69022(6) 0.0285(3) Uani 1 1 d . . . . .
H8 H 0.2139 0.3362 0.6645 0.034 Uiso 1 1 calc R U . . .
C9 C 0.15833(6) 0.41253(8) 0.69715(5) 0.0225(3) Uani 1 1 d . . . . .
C10 C 0.17053(6) 0.47709(8) 0.66608(5) 0.0189(2) Uani 1 1 d . . . . .
C11 C 0.22324(6) 0.48156(7) 0.63409(5) 0.0171(2) Uani 1 1 d . . . . .
C12 C 0.31719(6) 0.45617(7) 0.61161(5) 0.0176(2) Uani 1 1 d . . . . .
C13 C 0.37541(6) 0.42531(8) 0.60700(6) 0.0216(2) Uani 1 1 d . . . . .
H13 H 0.3901 0.3853 0.6272 0.026 Uiso 1 1 calc R U . . .
C14 C 0.41037(6) 0.45880(8) 0.56974(6) 0.0224(3) Uani 1 1 d . . . . .
H14 H 0.4497 0.4401 0.5643 0.027 Uiso 1 1 calc R U . . .
C15 C 0.38798(6) 0.51979(8) 0.54023(6) 0.0220(3) Uani 1 1 d . . . . .
H15 H 0.4132 0.5410 0.5162 0.026 Uiso 1 1 calc R U . . .
C16 C 0.32909(6) 0.54966(8) 0.54579(5) 0.0205(2) Uani 1 1 d . . . . .
H16 H 0.3143 0.5902 0.5261 0.025 Uiso 1 1 calc R U . . .
C17 C 0.29338(6) 0.51571(7) 0.58227(5) 0.0169(2) Uani 1 1 d . . . . .
C18 C 0.19316(6) 0.51075(7) 0.47519(5) 0.0170(2) Uani 1 1 d . . . . .
C19 C 0.23639(6) 0.50484(8) 0.43554(5) 0.0215(2) Uani 1 1 d . . . . .
H19 H 0.2568 0.5470 0.4249 0.026 Uiso 1 1 calc R U . . .
C20 C 0.24821(6) 0.43880(8) 0.41303(5) 0.0222(3) Uani 1 1 d . . . . .
H20 H 0.2753 0.4369 0.3863 0.027 Uiso 1 1 calc R U . . .
C21 C 0.21989(6) 0.37244(8) 0.42953(5) 0.0195(2) Uani 1 1 d . . . . .
C22 C 0.23701(7) 0.30368(8) 0.40856(6) 0.0251(3) Uani 1 1 d . . . . .
H22 H 0.2658 0.3024 0.3831 0.030 Uiso 1 1 calc R U . . .
C23 C 0.21191(7) 0.23900(8) 0.42507(6) 0.0286(3) Uani 1 1 d . . . . .
H23 H 0.2239 0.1940 0.4114 0.034 Uiso 1 1 calc R U . . .
C24 C 0.16777(7) 0.24144(8) 0.46298(6) 0.0268(3) Uani 1 1 d . . . . .
H24 H 0.1504 0.1976 0.4742 0.032 Uiso 1 1 calc R U . . .
C25 C 0.14975(7) 0.30773(7) 0.48375(5) 0.0217(2) Uani 1 1 d . . . . .
H25 H 0.1203 0.3078 0.5087 0.026 Uiso 1 1 calc R U . . .
C26 C 0.17509(6) 0.37592(7) 0.46801(5) 0.0167(2) Uani 1 1 d . . . . .
C27 C 0.16024(6) 0.44738(7) 0.48964(5) 0.0152(2) Uani 1 1 d . . . . .
C28 C 0.10852(6) 0.45891(7) 0.52202(5) 0.0147(2) Uani 1 1 d . . . . .
C29 C 0.01851(6) 0.43517(7) 0.55338(5) 0.0159(2) Uani 1 1 d . . . . .
C30 C -0.03636(6) 0.40247(7) 0.56651(5) 0.0199(2) Uani 1 1 d . . . . .
H30 H -0.0485 0.3555 0.5549 0.024 Uiso 1 1 calc R U . . .
C31 C -0.07213(6) 0.44505(8) 0.59842(5) 0.0198(2) Uani 1 1 d . . . . .
H31 H -0.1092 0.4256 0.6093 0.024 Uiso 1 1 calc R U . . .
C32 C -0.05389(6) 0.51634(7) 0.61460(5) 0.0195(2) Uani 1 1 d . . . . .
H32 H -0.0796 0.5434 0.6352 0.023 Uiso 1 1 calc R U . . .
C33 C 0.00166(6) 0.54764(7) 0.60073(5) 0.0194(2) Uani 1 1 d . . . . .
H33 H 0.0137 0.5950 0.6115 0.023 Uiso 1 1 calc R U . . .
C34 C 0.03853(6) 0.50453(7) 0.56993(5) 0.0154(2) Uani 1 1 d . . . . .
C35 C 0.04076(7) 0.73545(8) 0.54888(6) 0.0248(3) Uani 1 1 d . . . . .
H35 H 0.0011 0.7103 0.5393 0.030 Uiso 1 1 calc R U . . .
C36 C 0.03978(9) 0.76426(9) 0.60456(7) 0.0375(4) Uani 1 1 d . . . . .
H36A H 0.0364 0.7235 0.6283 0.056 Uiso 1 1 calc R U . . .
H36B H 0.0046 0.7966 0.6069 0.056 Uiso 1 1 calc R U . . .
H36C H 0.0777 0.7910 0.6138 0.056 Uiso 1 1 calc R U . . .
C37 C 0.04839(9) 0.79824(9) 0.51053(7) 0.0357(4) Uani 1 1 d . . . . .
H37A H 0.0878 0.8223 0.5188 0.054 Uiso 1 1 calc R U . . .
H37B H 0.0151 0.8332 0.5131 0.054 Uiso 1 1 calc R U . . .
H37C H 0.0471 0.7790 0.4754 0.054 Uiso 1 1 calc R U . . .
C38 C 0.26056(9) 0.76330(9) 0.58022(7) 0.0273(4) Uani 0.894(4) 1 d . . P A 1
H38 H 0.2491 0.7952 0.5500 0.033 Uiso 0.894(4) 1 calc R U P A 1
C39 C 0.32884(15) 0.74859(19) 0.58203(17) 0.0524(9) Uani 0.894(4) 1 d . . P A 1
H39A H 0.3404 0.7154 0.6105 0.079 Uiso 0.894(4) 1 calc R U P A 1
H39B H 0.3513 0.7942 0.5873 0.079 Uiso 0.894(4) 1 calc R U P A 1
H39C H 0.3389 0.7266 0.5495 0.079 Uiso 0.894(4) 1 calc R U P A 1
C38B C 0.2672(7) 0.7436(8) 0.6110(6) 0.0273(4) Uani 0.106(4) 1 d . . P A 2
H38B H 0.2664 0.7124 0.6424 0.033 Uiso 0.106(4) 1 calc R U P A 2
C39B C 0.3356(12) 0.7278(12) 0.5982(9) 0.026(4) Uani 0.106(4) 1 d . . P A 2
H39D H 0.3498 0.6829 0.6152 0.039 Uiso 0.106(4) 1 calc R U P A 2
H39E H 0.3619 0.7681 0.6107 0.039 Uiso 0.106(4) 1 calc R U P A 2
H39F H 0.3373 0.7228 0.5609 0.039 Uiso 0.106(4) 1 calc R U P A 2
C40 C 0.24238(9) 0.80137(10) 0.62917(8) 0.0393(4) Uani 1 1 d . . . . .
H40A H 0.1983 0.8115 0.6260 0.059 Uiso 0.894(4) 1 calc R U P A 1
H40B H 0.2650 0.8470 0.6337 0.059 Uiso 0.894(4) 1 calc R U P A 1
H40C H 0.2521 0.7700 0.6590 0.059 Uiso 0.894(4) 1 calc R U P A 1
H40D H 0.2285 0.8334 0.6006 0.059 Uiso 0.106(4) 1 calc R U P A 2
H40E H 0.2726 0.8268 0.6523 0.059 Uiso 0.106(4) 1 calc R U P A 2
H40F H 0.2073 0.7874 0.6483 0.059 Uiso 0.106(4) 1 calc R U P A 2
Zr2 Zr 0.5000 0.38556(2) 0.7500 0.02443(5) Uani 1 2 d S T P B .
O7 O 0.52156(5) 0.41867(6) 0.67569(5) 0.0258(2) Uani 1 1 d . . . . .
O8 O 0.39922(4) 0.59201(5) 0.68926(4) 0.01973(18) Uani 1 1 d . . . . .
O9 O 0.43133(6) 0.31904(6) 0.73168(7) 0.0454(4) Uani 1 1 d . . . . .
N3 N 0.43285(5) 0.48622(6) 0.72737(5) 0.0185(2) Uani 1 1 d . . . . .
C41 C 0.53134(6) 0.48296(8) 0.65357(6) 0.0221(3) Uani 1 1 d . . . . .
C42 C 0.57410(7) 0.48554(9) 0.61328(6) 0.0273(3) Uani 1 1 d . . . . .
H42 H 0.5920 0.4419 0.6022 0.033 Uiso 1 1 calc R U . . .
C43 C 0.58908(7) 0.55065(9) 0.59086(6) 0.0276(3) Uani 1 1 d . . . . .
H43 H 0.6155 0.5505 0.5636 0.033 Uiso 1 1 calc R U . . .
C44 C 0.56522(7) 0.61920(9) 0.60828(6) 0.0240(3) Uani 1 1 d . . . . .
C45 C 0.58734(7) 0.68723(10) 0.58982(6) 0.0297(3) Uani 1 1 d . . . . .
H45 H 0.6160 0.6872 0.5643 0.036 Uiso 1 1 calc R U . . .
C46 C 0.56736(8) 0.75303(10) 0.60884(6) 0.0313(3) Uani 1 1 d . . . . .
H46 H 0.5825 0.7974 0.5965 0.038 Uiso 1 1 calc R U . . .
C47 C 0.52358(7) 0.75306(9) 0.64728(6) 0.0287(3) Uani 1 1 d . . . . .
H47 H 0.5102 0.7977 0.6606 0.034 Uiso 1 1 calc R U . . .
C48 C 0.50037(7) 0.68769(8) 0.66529(6) 0.0238(3) Uani 1 1 d . . . . .
H48 H 0.4711 0.6889 0.6904 0.029 Uiso 1 1 calc R U . . .
C49 C 0.52003(6) 0.61843(8) 0.64639(5) 0.0202(2) Uani 1 1 d . . . . .
C50 C 0.50037(6) 0.54840(8) 0.66625(5) 0.0193(2) Uani 1 1 d . . . . .
C51 C 0.44610(6) 0.54070(7) 0.69613(5) 0.0179(2) Uani 1 1 d . . . . .
C52 C 0.35255(6) 0.56650(7) 0.71902(5) 0.0180(2) Uani 1 1 d . . . . .
C53 C 0.29493(6) 0.59837(8) 0.72529(6) 0.0216(2) Uani 1 1 d . . . . .
H53 H 0.2822 0.6421 0.7086 0.026 Uiso 1 1 calc R U . . .
C54 C 0.25756(6) 0.56026(8) 0.75839(6) 0.0220(3) Uani 1 1 d . . . . .
H54 H 0.2186 0.5795 0.7647 0.026 Uiso 1 1 calc R U . . .
C55 C 0.27689(6) 0.49363(8) 0.78257(5) 0.0215(2) Uani 1 1 d . . . . .
H55 H 0.2503 0.4696 0.8041 0.026 Uiso 1 1 calc R U . . .
C56 C 0.33479(6) 0.46252(8) 0.77516(6) 0.0210(2) Uani 1 1 d . . . . .
H56 H 0.3475 0.4182 0.7911 0.025 Uiso 1 1 calc R U . . .
C57 C 0.37279(6) 0.50097(7) 0.74273(5) 0.0179(2) Uani 1 1 d . . . . .
C58 C 0.38063(11) 0.27053(13) 0.71301(11) 0.0241(6) Uani 0.642(5) 1 d . . P B 1
H58 H 0.3505 0.2957 0.6883 0.029 Uiso 0.642(5) 1 calc R U P B 1
C59 C 0.35130(15) 0.24662(15) 0.76213(13) 0.0367(8) Uani 0.642(5) 1 d . . P B 1
H59A H 0.3824 0.2237 0.7858 0.055 Uiso 0.642(5) 1 calc R U P B 1
H59B H 0.3184 0.2119 0.7531 0.055 Uiso 0.642(5) 1 calc R U P B 1
H59C H 0.3344 0.2890 0.7788 0.055 Uiso 0.642(5) 1 calc R U P B 1
C58B C 0.3992(2) 0.2488(2) 0.73934(17) 0.0213(10) Uani 0.358(5) 1 d . . P B 2
H58B H 0.4107 0.2233 0.7726 0.026 Uiso 0.358(5) 1 calc R U P B 2
C59B C 0.3304(2) 0.2683(3) 0.7294(2) 0.0316(12) Uani 0.358(5) 1 d . . P B 2
H59D H 0.3172 0.2962 0.7586 0.047 Uiso 0.358(5) 1 calc R U P B 2
H59E H 0.3062 0.2238 0.7254 0.047 Uiso 0.358(5) 1 calc R U P B 2
H59F H 0.3245 0.2973 0.6979 0.047 Uiso 0.358(5) 1 calc R U P B 2
C60 C 0.41072(11) 0.20358(10) 0.68754(9) 0.0519(6) Uani 1 1 d . . . . .
H60A H 0.4339 0.2201 0.6590 0.078 Uiso 0.642(5) 1 calc R U P B 1
H60B H 0.3786 0.1699 0.6745 0.078 Uiso 0.642(5) 1 calc R U P B 1
H60C H 0.4384 0.1790 0.7133 0.078 Uiso 0.642(5) 1 calc R U P B 1
H60D H 0.3937 0.2305 0.6573 0.078 Uiso 0.358(5) 1 calc R U P B 2
H60E H 0.3906 0.1563 0.6888 0.078 Uiso 0.358(5) 1 calc R U P B 2
H60F H 0.4548 0.1967 0.6852 0.078 Uiso 0.358(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.0701(10) . ?
Zr1 O3 2.0599(9) . ?
Zr1 O5 1.9328(10) . ?
Zr1 O6 1.9369(10) . ?
Zr1 N1 2.3693(11) . ?
Zr1 N2 2.3649(11) . ?
O1 C1 1.3169(17) . ?
O2 C11 1.3692(15) . ?
O2 C12 1.3806(15) . ?
O3 C18 1.3179(15) . ?
O4 C28 1.3681(14) . ?
O4 C29 1.3820(14) . ?
O5 C38 1.4183(18) . ?
O5 C38B 1.507(14) . ?
O6 C35 1.4104(16) . ?
N1 C11 1.3139(17) . ?
N1 C17 1.4012(16) . ?
N2 C28 1.3163(15) . ?
N2 C34 1.4021(15) . ?
C1 C2 1.4294(18) . ?
C1 C10 1.4070(19) . ?
C2 H2 0.9300 . ?
C2 C3 1.357(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.416(2) . ?
C4 C5 1.419(2) . ?
C4 C9 1.4231(19) . ?
C5 H5 0.9300 . ?
C5 C6 1.364(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.404(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.376(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.417(2) . ?
C9 C10 1.4461(19) . ?
C10 C11 1.4457(17) . ?
C12 C13 1.3813(18) . ?
C12 C17 1.3867(18) . ?
C13 H13 0.9300 . ?
C13 C14 1.393(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.400(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.3913(18) . ?
C16 H16 0.9300 . ?
C16 C17 1.3918(18) . ?
C18 C19 1.4267(17) . ?
C18 C27 1.4098(17) . ?
C19 H19 0.9300 . ?
C19 C20 1.3572(19) . ?
C20 H20 0.9300 . ?
C20 C21 1.4230(19) . ?
C21 C22 1.4131(19) . ?
C21 C26 1.4260(17) . ?
C22 H22 0.9300 . ?
C22 C23 1.367(2) . ?
C23 H23 0.9300 . ?
C23 C24 1.404(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.3778(18) . ?
C25 H25 0.9300 . ?
C25 C26 1.4178(18) . ?
C26 C27 1.4500(17) . ?
C27 C28 1.4473(16) . ?
C29 C30 1.3811(17) . ?
C29 C34 1.3817(17) . ?
C30 H30 0.9300 . ?
C30 C31 1.3923(18) . ?
C31 H31 0.9300 . ?
C31 C32 1.4004(19) . ?
C32 H32 0.9300 . ?
C32 C33 1.3890(18) . ?
C33 H33 0.9300 . ?
C33 C34 1.3944(17) . ?
C35 H35 0.9800 . ?
C35 C36 1.514(2) . ?
C35 C37 1.516(2) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38 0.9800 . ?
C38 C39 1.487(4) . ?
C38 C40 1.503(2) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C38B H38B 0.9800 . ?
C38B C39B 1.55(3) . ?
C38B C40 1.275(15) . ?
C39B H39D 0.9600 . ?
C39B H39E 0.9600 . ?
C39B H39F 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C40 H40D 0.9600 . ?
C40 H40E 0.9600 . ?
C40 H40F 0.9600 . ?
Zr2 O7 2.0728(12) . ?
Zr2 O7 2.0728(12) 2_656 ?
Zr2 O9 1.9323(11) 2_656 ?
Zr2 O9 1.9323(11) . ?
Zr2 N3 2.3660(11) . ?
Zr2 N3 2.3660(11) 2_656 ?
O7 C41 1.3161(18) . ?
O8 C51 1.3702(15) . ?
O8 C52 1.3805(15) . ?
O9 C58 1.450(2) . ?
O9 C58B 1.466(4) . ?
N3 C51 1.3116(17) . ?
N3 C57 1.4006(16) . ?
C41 C42 1.4289(19) . ?
C41 C50 1.4068(18) . ?
C42 H42 0.9300 . ?
C42 C43 1.358(2) . ?
C43 H43 0.9300 . ?
C43 C44 1.425(2) . ?
C44 C45 1.412(2) . ?
C44 C49 1.4238(18) . ?
C45 H45 0.9300 . ?
C45 C46 1.366(2) . ?
C46 H46 0.9300 . ?
C46 C47 1.408(2) . ?
C47 H47 0.9300 . ?
C47 C48 1.375(2) . ?
C48 H48 0.9300 . ?
C48 C49 1.4176(19) . ?
C49 C50 1.4388(19) . ?
C50 C51 1.4458(17) . ?
C52 C53 1.3843(17) . ?
C52 C57 1.3854(18) . ?
C53 H53 0.9300 . ?
C53 C54 1.390(2) . ?
C54 H54 0.9300 . ?
C54 C55 1.402(2) . ?
C55 H55 0.9300 . ?
C55 C56 1.3897(18) . ?
C56 H56 0.9300 . ?
C56 C57 1.3907(18) . ?
C58 H58 0.9800 . ?
C58 C59 1.507(4) . ?
C58 C60 1.539(3) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C58B H58B 0.9800 . ?
C58B C59B 1.520(7) . ?
C58B C60 1.589(4) . ?
C59B H59D 0.9600 . ?
C59B H59E 0.9600 . ?
C59B H59F 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C60 H60D 0.9600 . ?
C60 H60E 0.9600 . ?
C60 H60F 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 N1 73.77(4) . . ?
O1 Zr1 N2 80.65(4) . . ?
O3 Zr1 O1 145.89(4) . . ?
O3 Zr1 N1 80.23(4) . . ?
O3 Zr1 N2 73.89(4) . . ?
O5 Zr1 O1 102.85(5) . . ?
O5 Zr1 O3 98.85(4) . . ?
O5 Zr1 O6 100.71(5) . . ?
O5 Zr1 N1 90.12(4) . . ?
O5 Zr1 N2 169.65(4) . . ?
O6 Zr1 O1 96.82(4) . . ?
O6 Zr1 O3 104.67(4) . . ?
O6 Zr1 N1 167.12(4) . . ?
O6 Zr1 N2 88.42(4) . . ?
N2 Zr1 N1 81.46(4) . . ?
C1 O1 Zr1 136.14(8) . . ?
C11 O2 C12 105.28(10) . . ?
C18 O3 Zr1 137.68(8) . . ?
C28 O4 C29 105.41(9) . . ?
C38 O5 Zr1 164.38(11) . . ?
C38B O5 Zr1 147.5(6) . . ?
C35 O6 Zr1 161.95(10) . . ?
C11 N1 Zr1 125.79(8) . . ?
C11 N1 C17 105.79(11) . . ?
C17 N1 Zr1 128.41(8) . . ?
C28 N2 Zr1 126.69(8) . . ?
C28 N2 C34 105.82(10) . . ?
C34 N2 Zr1 127.47(8) . . ?
O1 C1 C2 117.58(13) . . ?
O1 C1 C10 123.70(12) . . ?
C10 C1 C2 118.66(13) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.19(14) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.47(13) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 120.79(14) . . ?
C3 C4 C9 119.55(14) . . ?
C5 C4 C9 119.66(16) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.35(15) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C7 119.23(15) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.06(18) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.17(15) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C10 118.34(14) . . ?
C8 C9 C4 117.47(13) . . ?
C8 C9 C10 124.16(13) . . ?
C1 C10 C9 120.37(12) . . ?
C1 C10 C11 116.82(12) . . ?
C11 C10 C9 122.42(12) . . ?
O2 C11 C10 118.63(11) . . ?
N1 C11 O2 113.19(11) . . ?
N1 C11 C10 127.95(12) . . ?
O2 C12 C13 127.64(12) . . ?
O2 C12 C17 107.84(11) . . ?
C13 C12 C17 124.52(12) . . ?
C12 C13 H13 122.6 . . ?
C12 C13 C14 114.80(13) . . ?
C14 C13 H13 122.6 . . ?
C13 C14 H14 119.0 . . ?
C13 C14 C15 121.91(12) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 121.94(13) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 121.7 . . ?
C15 C16 C17 116.53(13) . . ?
C17 C16 H16 121.7 . . ?
C12 C17 N1 107.89(11) . . ?
C12 C17 C16 120.29(12) . . ?
C16 C17 N1 131.82(12) . . ?
O3 C18 C19 116.72(11) . . ?
O3 C18 C27 123.92(11) . . ?
C27 C18 C19 119.31(12) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.19(12) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.30(12) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C26 119.42(12) . . ?
C22 C21 C20 120.09(12) . . ?
C22 C21 C26 120.48(13) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.11(13) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 H23 120.4 . . ?
C22 C23 C24 119.13(13) . . ?
C24 C23 H23 120.4 . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.02(14) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 119.2 . . ?
C24 C25 C26 121.56(12) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C27 118.69(11) . . ?
C25 C26 C21 116.70(11) . . ?
C25 C26 C27 124.58(11) . . ?
C18 C27 C26 119.76(11) . . ?
C18 C27 C28 116.92(11) . . ?
C28 C27 C26 123.05(11) . . ?
O4 C28 C27 119.07(10) . . ?
N2 C28 O4 112.94(10) . . ?
N2 C28 C27 127.85(11) . . ?
C30 C29 O4 127.69(11) . . ?
C30 C29 C34 124.46(12) . . ?
C34 C29 O4 107.85(10) . . ?
C29 C30 H30 122.5 . . ?
C29 C30 C31 114.99(12) . . ?
C31 C30 H30 122.5 . . ?
C30 C31 H31 119.1 . . ?
C30 C31 C32 121.82(12) . . ?
C32 C31 H31 119.1 . . ?
C31 C32 H32 119.1 . . ?
C33 C32 C31 121.75(12) . . ?
C33 C32 H32 119.1 . . ?
C32 C33 H33 121.6 . . ?
C32 C33 C34 116.73(12) . . ?
C34 C33 H33 121.6 . . ?
C29 C34 N2 107.95(10) . . ?
C29 C34 C33 120.21(11) . . ?
C33 C34 N2 131.84(12) . . ?
O6 C35 H35 108.7 . . ?
O6 C35 C36 109.83(13) . . ?
O6 C35 C37 109.95(12) . . ?
C36 C35 H35 108.7 . . ?
C36 C35 C37 110.94(13) . . ?
C37 C35 H35 108.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O5 C38 H38 108.6 . . ?
O5 C38 C39 110.03(17) . . ?
O5 C38 C40 109.13(14) . . ?
C39 C38 H38 108.6 . . ?
C39 C38 C40 111.9(2) . . ?
C40 C38 H38 108.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O5 C38B H38B 98.1 . . ?
O5 C38B C39B 105.6(12) . . ?
C39B C38B H38B 98.1 . . ?
C40 C38B O5 117.4(12) . . ?
C40 C38B H38B 98.1 . . ?
C40 C38B C39B 130.8(13) . . ?
C38B C39B H39D 109.5 . . ?
C38B C39B H39E 109.5 . . ?
C38B C39B H39F 109.5 . . ?
H39D C39B H39E 109.5 . . ?
H39D C39B H39F 109.5 . . ?
H39E C39B H39F 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
C38B C40 H40D 109.5 . . ?
C38B C40 H40E 109.5 . . ?
C38B C40 H40F 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
H40D C40 H40E 109.5 . . ?
H40D C40 H40F 109.5 . . ?
H40E C40 H40F 109.5 . . ?
O7 Zr2 O7 146.42(5) . 2_656 ?
O7 Zr2 N3 74.24(4) 2_656 2_656 ?
O7 Zr2 N3 80.05(4) . 2_656 ?
O7 Zr2 N3 80.05(4) 2_656 . ?
O7 Zr2 N3 74.24(4) . . ?
O9 Zr2 O7 100.21(6) 2_656 2_656 ?
O9 Zr2 O7 100.21(6) . . ?
O9 Zr2 O7 100.51(5) . 2_656 ?
O9 Zr2 O7 100.51(5) 2_656 . ?
O9 Zr2 O9 102.99(8) 2_656 . ?
O9 Zr2 N3 88.89(5) 2_656 2_656 ?
O9 Zr2 N3 88.89(5) . . ?
O9 Zr2 N3 167.80(5) 2_656 . ?
O9 Zr2 N3 167.80(5) . 2_656 ?
N3 Zr2 N3 79.40(5) 2_656 . ?
C41 O7 Zr2 134.50(9) . . ?
C51 O8 C52 105.02(10) . . ?
C58 O9 Zr2 174.83(16) . . ?
C58B O9 Zr2 149.9(2) . . ?
C51 N3 Zr2 124.77(8) . . ?
C51 N3 C57 105.83(11) . . ?
C57 N3 Zr2 129.39(9) . . ?
O7 C41 C42 117.96(13) . . ?
O7 C41 C50 123.47(12) . . ?
C50 C41 C42 118.53(14) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 C41 121.08(14) . . ?
C43 C42 H42 119.5 . . ?
C42 C43 H43 119.3 . . ?
C42 C43 C44 121.41(13) . . ?
C44 C43 H43 119.3 . . ?
C45 C44 C43 121.10(13) . . ?
C45 C44 C49 119.96(14) . . ?
C49 C44 C43 118.91(14) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 C44 121.22(14) . . ?
C46 C45 H45 119.4 . . ?
C45 C46 H46 120.3 . . ?
C45 C46 C47 119.42(15) . . ?
C47 C46 H46 120.3 . . ?
C46 C47 H47 119.7 . . ?
C48 C47 C46 120.64(15) . . ?
C48 C47 H47 119.7 . . ?
C47 C48 H48 119.3 . . ?
C47 C48 C49 121.44(13) . . ?
C49 C48 H48 119.3 . . ?
C44 C49 C50 118.79(12) . . ?
C48 C49 C44 117.31(13) . . ?
C48 C49 C50 123.75(12) . . ?
C41 C50 C49 120.25(12) . . ?
C41 C50 C51 116.94(12) . . ?
C49 C50 C51 122.64(12) . . ?
O8 C51 C50 118.68(12) . . ?
N3 C51 O8 113.32(11) . . ?
N3 C51 C50 127.78(12) . . ?
O8 C52 C53 127.98(12) . . ?
O8 C52 C57 108.03(11) . . ?
C53 C52 C57 124.00(12) . . ?
C52 C53 H53 122.4 . . ?
C52 C53 C54 115.13(13) . . ?
C54 C53 H53 122.4 . . ?
C53 C54 H54 119.1 . . ?
C53 C54 C55 121.89(12) . . ?
C55 C54 H54 119.1 . . ?
C54 C55 H55 119.1 . . ?
C56 C55 C54 121.73(13) . . ?
C56 C55 H55 119.1 . . ?
C55 C56 H56 121.7 . . ?
C55 C56 C57 116.65(13) . . ?
C57 C56 H56 121.7 . . ?
C52 C57 N3 107.79(11) . . ?
C52 C57 C56 120.59(12) . . ?
C56 C57 N3 131.62(12) . . ?
O9 C58 H58 111.8 . . ?
O9 C58 C59 104.5(2) . . ?
O9 C58 C60 106.66(18) . . ?
C59 C58 H58 111.8 . . ?
C59 C58 C60 109.9(2) . . ?
C60 C58 H58 111.8 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
O9 C58B H58B 115.6 . . ?
O9 C58B C59B 103.7(3) . . ?
O9 C58B C60 103.3(3) . . ?
C59B C58B H58B 115.6 . . ?
C59B C58B C60 101.0(3) . . ?
C60 C58B H58B 115.6 . . ?
C58B C59B H59D 109.5 . . ?
C58B C59B H59E 109.5 . . ?
C58B C59B H59F 109.5 . . ?
H59D C59B H59E 109.5 . . ?
H59D C59B H59F 109.5 . . ?
H59E C59B H59F 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
C58B C60 H60D 109.5 . . ?
C58B C60 H60E 109.5 . . ?
C58B C60 H60F 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
H60D C60 H60E 109.5 . . ?
H60D C60 H60F 109.5 . . ?
H60E C60 H60F 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 C2 -149.37(10) . . . . ?
Zr1 O1 C1 C10 33.4(2) . . . . ?
Zr1 O3 C18 C19 -150.87(10) . . . . ?
Zr1 O3 C18 C27 31.5(2) . . . . ?
Zr1 O5 C38 C39 -178.5(4) . . . . ?
Zr1 O5 C38 C40 58.4(5) . . . . ?
Zr1 O5 C38B C39B 126.6(10) . . . . ?
Zr1 O5 C38B C40 -77.9(16) . . . . ?
Zr1 O6 C35 C36 -2.0(4) . . . . ?
Zr1 O6 C35 C37 120.3(3) . . . . ?
Zr1 N1 C11 O2 179.48(7) . . . . ?
Zr1 N1 C11 C10 -6.07(18) . . . . ?
Zr1 N1 C17 C12 -179.49(8) . . . . ?
Zr1 N1 C17 C16 0.7(2) . . . . ?
Zr1 N2 C28 O4 177.50(7) . . . . ?
Zr1 N2 C28 C27 -6.90(18) . . . . ?
Zr1 N2 C34 C29 -177.07(8) . . . . ?
Zr1 N2 C34 C33 3.4(2) . . . . ?
O1 C1 C2 C3 -179.88(13) . . . . ?
O1 C1 C10 C9 -175.71(12) . . . . ?
O1 C1 C10 C11 11.34(19) . . . . ?
O2 C12 C13 C14 179.45(12) . . . . ?
O2 C12 C17 N1 -0.50(14) . . . . ?
O2 C12 C17 C16 179.29(11) . . . . ?
O3 C18 C19 C20 179.61(13) . . . . ?
O3 C18 C27 C26 -176.36(12) . . . . ?
O3 C18 C27 C28 9.45(19) . . . . ?
O4 C29 C30 C31 -179.92(12) . . . . ?
O4 C29 C34 N2 -1.45(14) . . . . ?
O4 C29 C34 C33 178.16(11) . . . . ?
O5 C38 C40 C38B 62.2(11) . . . . ?
O5 C38B C40 C38 -62.4(11) . . . . ?
C1 C2 C3 C4 -2.7(2) . . . . ?
C1 C10 C11 O2 153.37(12) . . . . ?
C1 C10 C11 N1 -20.83(19) . . . . ?
C2 C1 C10 C9 7.11(19) . . . . ?
C2 C1 C10 C11 -165.85(12) . . . . ?
C2 C3 C4 C5 -175.88(15) . . . . ?
C2 C3 C4 C9 3.2(2) . . . . ?
C3 C4 C5 C6 177.64(16) . . . . ?
C3 C4 C9 C8 -176.69(14) . . . . ?
C3 C4 C9 C10 1.4(2) . . . . ?
C4 C5 C6 C7 -0.7(3) . . . . ?
C4 C9 C10 C1 -6.53(19) . . . . ?
C4 C9 C10 C11 166.02(12) . . . . ?
C5 C4 C9 C8 2.4(2) . . . . ?
C5 C4 C9 C10 -179.52(13) . . . . ?
C5 C6 C7 C8 1.9(3) . . . . ?
C6 C7 C8 C9 -0.9(3) . . . . ?
C7 C8 C9 C4 -1.3(2) . . . . ?
C7 C8 C9 C10 -179.21(15) . . . . ?
C8 C9 C10 C1 171.39(13) . . . . ?
C8 C9 C10 C11 -16.1(2) . . . . ?
C9 C4 C5 C6 -1.5(2) . . . . ?
C9 C10 C11 O2 -19.43(18) . . . . ?
C9 C10 C11 N1 166.38(13) . . . . ?
C10 C1 C2 C3 -2.5(2) . . . . ?
C11 O2 C12 C13 -179.39(13) . . . . ?
C11 O2 C12 C17 0.05(13) . . . . ?
C11 N1 C17 C12 0.77(14) . . . . ?
C11 N1 C17 C16 -178.99(14) . . . . ?
C12 O2 C11 N1 0.47(14) . . . . ?
C12 O2 C11 C10 -174.55(11) . . . . ?
C12 C13 C14 C15 1.1(2) . . . . ?
C13 C12 C17 N1 178.95(12) . . . . ?
C13 C12 C17 C16 -1.3(2) . . . . ?
C13 C14 C15 C16 -1.1(2) . . . . ?
C14 C15 C16 C17 -0.1(2) . . . . ?
C15 C16 C17 N1 -179.09(13) . . . . ?
C15 C16 C17 C12 1.17(19) . . . . ?
C17 N1 C11 O2 -0.78(14) . . . . ?
C17 N1 C11 C10 173.68(12) . . . . ?
C17 C12 C13 C14 0.1(2) . . . . ?
C18 C19 C20 C21 -2.5(2) . . . . ?
C18 C27 C28 O4 157.91(11) . . . . ?
C18 C27 C28 N2 -17.45(19) . . . . ?
C19 C18 C27 C26 6.08(18) . . . . ?
C19 C18 C27 C28 -168.11(12) . . . . ?
C19 C20 C21 C22 -174.67(14) . . . . ?
C19 C20 C21 C26 4.2(2) . . . . ?
C20 C21 C22 C23 177.88(14) . . . . ?
C20 C21 C26 C25 -178.47(13) . . . . ?
C20 C21 C26 C27 -0.66(19) . . . . ?
C21 C22 C23 C24 0.9(2) . . . . ?
C21 C26 C27 C18 -4.41(18) . . . . ?
C21 C26 C27 C28 169.41(12) . . . . ?
C22 C21 C26 C25 0.38(19) . . . . ?
C22 C21 C26 C27 178.19(12) . . . . ?
C22 C23 C24 C25 -0.2(2) . . . . ?
C23 C24 C25 C26 -0.3(2) . . . . ?
C24 C25 C26 C21 0.2(2) . . . . ?
C24 C25 C26 C27 -177.42(14) . . . . ?
C25 C26 C27 C18 173.21(13) . . . . ?
C25 C26 C27 C28 -13.0(2) . . . . ?
C26 C21 C22 C23 -1.0(2) . . . . ?
C26 C27 C28 O4 -16.08(18) . . . . ?
C26 C27 C28 N2 168.56(12) . . . . ?
C27 C18 C19 C20 -2.7(2) . . . . ?
C28 O4 C29 C30 -179.03(13) . . . . ?
C28 O4 C29 C34 0.73(13) . . . . ?
C28 N2 C34 C29 1.60(14) . . . . ?
C28 N2 C34 C33 -177.94(14) . . . . ?
C29 O4 C28 N2 0.30(14) . . . . ?
C29 O4 C28 C27 -175.72(11) . . . . ?
C29 C30 C31 C32 1.5(2) . . . . ?
C30 C29 C34 N2 178.32(12) . . . . ?
C30 C29 C34 C33 -2.1(2) . . . . ?
C30 C31 C32 C33 -1.6(2) . . . . ?
C31 C32 C33 C34 -0.1(2) . . . . ?
C32 C33 C34 N2 -178.64(13) . . . . ?
C32 C33 C34 C29 1.87(19) . . . . ?
C34 N2 C28 O4 -1.18(14) . . . . ?
C34 N2 C28 C27 174.41(12) . . . . ?
C34 C29 C30 C31 0.4(2) . . . . ?
C38 O5 C38B C39B -81.9(12) . . . . ?
C38 O5 C38B C40 73.6(12) . . . . ?
C39 C38 C40 C38B -59.8(11) . . . . ?
C38B O5 C38 C39 73.3(11) . . . . ?
C38B O5 C38 C40 -49.9(11) . . . . ?
C39B C38B C40 C38 85.8(18) . . . . ?
Zr2 O7 C41 C42 148.63(11) . . . . ?
Zr2 O7 C41 C50 -33.6(2) . . . . ?
Zr2 O9 C58B C59B 146.1(3) . . . . ?
Zr2 O9 C58B C60 -108.9(4) . . . . ?
Zr2 N3 C51 O8 179.84(8) . . . . ?
Zr2 N3 C51 C50 5.24(19) . . . . ?
Zr2 N3 C57 C52 -179.79(8) . . . . ?
Zr2 N3 C57 C56 0.1(2) . . . . ?
O7 C41 C42 C43 -176.25(14) . . . . ?
O7 C41 C50 C49 170.67(13) . . . . ?
O7 C41 C50 C51 -13.9(2) . . . . ?
O8 C52 C53 C54 -179.32(12) . . . . ?
O8 C52 C57 N3 0.16(14) . . . . ?
O8 C52 C57 C56 -179.78(12) . . . . ?
O9 C58 C60 C58B 68.9(3) . . . . ?
O9 C58B C60 C58 -65.3(3) . . . . ?
C41 C42 C43 C44 3.1(2) . . . . ?
C41 C50 C51 O8 -150.08(12) . . . . ?
C41 C50 C51 N3 24.3(2) . . . . ?
C42 C41 C50 C49 -11.6(2) . . . . ?
C42 C41 C50 C51 163.82(12) . . . . ?
C42 C43 C44 C45 171.45(15) . . . . ?
C42 C43 C44 C49 -6.2(2) . . . . ?
C43 C44 C45 C46 -175.97(15) . . . . ?
C43 C44 C49 C48 176.02(13) . . . . ?
C43 C44 C49 C50 0.4(2) . . . . ?
C44 C45 C46 C47 -0.4(2) . . . . ?
C44 C49 C50 C41 8.46(19) . . . . ?
C44 C49 C50 C51 -166.68(13) . . . . ?
C45 C44 C49 C48 -1.7(2) . . . . ?
C45 C44 C49 C50 -177.26(13) . . . . ?
C45 C46 C47 C48 -0.7(2) . . . . ?
C46 C47 C48 C49 0.7(2) . . . . ?
C47 C48 C49 C44 0.5(2) . . . . ?
C47 C48 C49 C50 175.87(14) . . . . ?
C48 C49 C50 C41 -166.82(13) . . . . ?
C48 C49 C50 C51 18.0(2) . . . . ?
C49 C44 C45 C46 1.7(2) . . . . ?
C49 C50 C51 O8 25.22(19) . . . . ?
C49 C50 C51 N3 -160.44(13) . . . . ?
C50 C41 C42 C43 5.9(2) . . . . ?
C51 O8 C52 C53 -179.81(13) . . . . ?
C51 O8 C52 C57 0.02(13) . . . . ?
C51 N3 C57 C52 -0.28(14) . . . . ?
C51 N3 C57 C56 179.65(14) . . . . ?
C52 O8 C51 N3 -0.20(14) . . . . ?
C52 O8 C51 C50 174.93(11) . . . . ?
C52 C53 C54 C55 -1.2(2) . . . . ?
C53 C52 C57 N3 180.00(12) . . . . ?
C53 C52 C57 C56 0.1(2) . . . . ?
C53 C54 C55 C56 0.7(2) . . . . ?
C54 C55 C56 C57 0.3(2) . . . . ?
C55 C56 C57 N3 179.43(13) . . . . ?
C55 C56 C57 C52 -0.65(19) . . . . ?
C57 N3 C51 O8 0.30(14) . . . . ?
C57 N3 C51 C50 -174.29(12) . . . . ?
C57 C52 C53 C54 0.9(2) . . . . ?
C58 O9 C58B C59B -40.4(3) . . . . ?
C58 O9 C58B C60 64.6(3) . . . . ?
C59 C58 C60 C58B -43.8(3) . . . . ?
C58B O9 C58 C59 45.1(3) . . . . ?
C58B O9 C58 C60 -71.3(3) . . . . ?
C59B C58B C60 C58 41.8(3) . . . . ?

_olex2_date_sample_data_collection 2016-02-04
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.767
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1816368'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-11-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 Hf N2 O6'
_chemical_formula_sum            'C42 H38 Hf N2 O6'
_chemical_formula_weight         845.23
_chemical_melting_point          ?
_chemical_oxdiff_formula         C43H43HfN4O4
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   10.1170(2)
_cell_length_b                   29.0237(7)
_cell_length_c                   12.8277(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 106.436(3)
_cell_angle_gamma                90.0
_cell_volume                     3612.74(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    77999
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      32.0890
_cell_measurement_theta_min      2.1610
_cell_oxdiff_angle_alpha         89.9284(12)
_cell_oxdiff_angle_beta          106.4191(16)
_cell_oxdiff_angle_gamma         90.0900(12)
_cell_oxdiff_length_a            10.11650(19)
_cell_oxdiff_length_b            29.0286(3)
_cell_oxdiff_length_c            12.8251(2)
_cell_oxdiff_measurement_reflns_used 77999
_cell_oxdiff_volume              3612.74(10)
_exptl_absorpt_coefficient_mu    2.924
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 1 0.1203
-1 0 0 0.0344
1 0 0 0.0084
0 1 0 0.0733
0 -1 0 0.0683
0 2 -1 0.1194
0 -2 1 0.1234
0 -2 -1 0.1263

_exptl_crystal_recrystallization_method 
'non-merohedrically twinned by a rotation of 2.9 deg. around [-0.43 0.01 -0.90] (reciprocal) or [-0.69 0.00 -0.72] (direct), ratio 52:48. Both domains were taken into account during data reduction and refinement'
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.043
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0310 2.0523 0.9672 0.0613 0.0426 -0.0110
-0.9980 0.1116 -0.0013 -0.0543 0.0481 -0.0083
0.9980 -0.1116 0.0013 0.0543 -0.0481 0.0083
0.0154 0.9977 -0.0155 0.0102 0.0079 -0.0207
-0.0154 -0.9977 0.0155 -0.0102 -0.0079 0.0207
0.0306 1.9383 -1.0292 -0.0205 -0.0109 -0.0718
-0.0306 -1.9383 1.0292 0.0205 0.0109 0.0718
-0.0310 -2.0523 -0.9672 -0.0613 -0.0426 0.0110

_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            349734
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.276
_diffrn_reflns_theta_min         1.798
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      3.00  93.00   0.75    8.00    --   24.87  38.00   0.00  120
  2  ω     47.00  90.50   0.75    8.00    --   24.87  57.00  90.00   58
  3  ω      7.00  90.25   0.75    8.00    --   24.87  38.00 -90.00  111
  4  ω     -7.00  31.25   0.75    8.00    --   24.87 -99.00-180.00   51
  5  ω    -10.00  16.25   0.75    8.00    --  -23.50  57.00  60.00   35
  6  ω     37.00  94.00   0.75    8.00    --   24.87 178.00 -30.00   76
  7  ω     35.00  61.25   0.75    8.00    --   24.87 178.00-150.00   35
  8  ω    -61.00 -35.50   0.75    8.00    --  -23.50-178.00  90.00   34
  9  ω    -62.00 -35.00   0.75    8.00    --  -23.50-178.00 120.00   36
 10  ω     34.00 100.00   0.75    8.00    --   24.87-178.00 120.00   88
 11  ω     52.75  85.00   0.75    8.00    --   24.87-133.00  17.27   43
 12  ω     -4.00  90.50   0.75    8.00    --   24.87  77.00  30.00  126
 13  ω     23.50  85.00   0.75    8.00    --   24.87-133.00 179.43   82
 14  ω     -4.00  93.50   0.75    8.00    --   24.87  77.00 150.00  130
 15  ω     -4.00  41.00   0.75    8.00    --   24.87  77.00 -90.00   60
 16  ω     65.00  91.25   0.75    8.00    --   24.87  77.00 -90.00   35
 17  ω     35.00  68.00   0.75    8.00    --   24.87 178.00 150.00   44
 18  ω    -44.00  33.25   0.75    8.00    --   24.87 -57.00 -60.00  103
 19  ω      7.00  34.00   0.75    8.00    --   24.87-133.00  17.27   36
 20  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00 -60.00  189
 21  ω    -85.00  -9.25   0.75    8.00    --  -23.50 135.00-163.61  101
 22  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00   0.00  189
 23  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00 -30.00  189
 24  ω    -92.00  -5.00   0.75    8.00    --  -23.50 -57.00-120.00  116
 25  ω    -97.00 -36.25   0.75    8.00    --  -23.50-178.00 150.00   81
 26  ω    -65.00  19.00   0.75    8.00    --  -23.50 100.00  18.08  112
 27  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00-180.00  189
 28  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00-150.00  189
 29  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00-120.00  189
 30  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00 -90.00  189
 31  ω    -10.00  71.00   0.75    8.00    --   24.87-111.00-104.34  108
 32  ω     -4.00  92.75   0.75    8.00    --   24.87  77.00-180.00  129
 33  ω      6.00  93.00   0.75    8.00    --   24.87  57.00  90.00  116
 34  ω    -44.00  52.75   0.75    8.00    --   24.87 -77.00-150.00  129
 35  ω    -95.00 -68.00   0.75    8.00    --  -23.50   0.00  60.00   36
 36  ω    -95.00  46.75   0.75    8.00    --  -23.50   0.00  30.00  189
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0554486000
_diffrn_orient_matrix_UB_12      0.0099995000
_diffrn_orient_matrix_UB_13      0.0404184000
_diffrn_orient_matrix_UB_21      -0.0472405000
_diffrn_orient_matrix_UB_22      0.0090837000
_diffrn_orient_matrix_UB_23      0.0262719000
_diffrn_orient_matrix_UB_31      0.0060446000
_diffrn_orient_matrix_UB_32      -0.0203603000
_diffrn_orient_matrix_UB_33      0.0316297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                24765
_reflns_number_total             28958
_reflns_special_details          
;
non-merohedrically twinned by a rotation of 2.9 deg.
 around [-0.43 0.01 -0.90] (reciprocal) or 
[-0.69 0.00 -0.72] (direct), ratio 52:48. 
Both domains were taken into account during 
data reduction and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.736
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.110
_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     467
_refine_ls_number_reflns         28958
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²+2.1227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0672
_refine_special_details          
;non-merohedrically twinned by a rotation of 2.9 deg.
 around [-0.43 0.01 -0.90] (reciprocal) or 
[-0.69 0.00 -0.72] (direct), ratio 52:48. 
Both domains were taken into account during 
data reduction and refinement,Twin
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.02498(2) 0.10627(2) 0.20323(2) 0.00940(3) Uani 1 1 d . . . . .
O1 O -0.00727(19) 0.16501(6) 0.28064(14) 0.0124(4) Uani 1 1 d . . . . .
O2 O -0.32234(19) 0.19457(6) 0.00389(15) 0.0132(4) Uani 1 1 d . . . . .
O3 O 0.05158(19) 0.07171(6) 0.07157(15) 0.0123(3) Uani 1 1 d . . . . .
O4 O 0.30167(19) 0.17705(6) 0.02923(15) 0.0134(4) Uani 1 1 d . . . . .
O5 O 0.18208(19) 0.08449(6) 0.31592(15) 0.0140(4) Uani 1 1 d . . . . .
O6 O -0.12445(19) 0.06948(6) 0.22555(15) 0.0132(4) Uani 1 1 d . . . . .
N1 N -0.1523(2) 0.14415(7) 0.07361(17) 0.0109(4) Uani 1 1 d . . . . .
N2 N 0.1714(2) 0.15396(7) 0.13469(17) 0.0106(4) Uani 1 1 d . . . . .
C1 C -0.0627(3) 0.20617(9) 0.2626(2) 0.0115(5) Uani 1 1 d . . . . .
C2 C -0.0409(3) 0.23638(9) 0.3544(2) 0.0137(5) Uani 1 1 d . . . . .
H2 H 0.011334 0.225966 0.424097 0.016 Uiso 1 1 calc R . . . .
C3 C -0.0938(3) 0.27962(9) 0.3430(2) 0.0146(5) Uani 1 1 d . . . . .
H3 H -0.081558 0.298404 0.405645 0.017 Uiso 1 1 calc R . . . .
C4 C -0.1671(3) 0.29760(9) 0.2397(2) 0.0131(5) Uani 1 1 d . . . . .
C5 C -0.2124(3) 0.34375(9) 0.2280(2) 0.0159(5) Uani 1 1 d . . . . .
H5 H -0.197489 0.362768 0.290521 0.019 Uiso 1 1 calc R . . . .
C6 C -0.2778(3) 0.36156(9) 0.1276(2) 0.0195(6) Uani 1 1 d . . . . .
H6 H -0.308437 0.392642 0.120749 0.023 Uiso 1 1 calc R . . . .
C7 C -0.2990(3) 0.33360(9) 0.0353(2) 0.0176(5) Uani 1 1 d . . . . .
H7 H -0.343267 0.346104 -0.034302 0.021 Uiso 1 1 calc R . . . .
C8 C -0.2568(3) 0.28836(9) 0.0437(2) 0.0149(5) Uani 1 1 d . . . . .
H8 H -0.271401 0.270213 -0.020188 0.018 Uiso 1 1 calc R . . . .
C9 C -0.1917(3) 0.26834(8) 0.1466(2) 0.0114(5) Uani 1 1 d . . . . .
C10 C -0.1452(3) 0.22117(8) 0.1611(2) 0.0109(5) Uani 1 1 d . . . . .
C11 C -0.1982(3) 0.18615(9) 0.0790(2) 0.0109(5) Uani 1 1 d . . . . .
C12 C -0.3598(3) 0.15319(9) -0.0501(2) 0.0128(5) Uani 1 1 d . . . . .
C13 C -0.4802(3) 0.14344(10) -0.1293(2) 0.0182(5) Uani 1 1 d . . . . .
H13 H -0.548305 0.166199 -0.157912 0.022 Uiso 1 1 calc R . . . .
C14 C -0.4951(3) 0.09786(10) -0.1644(3) 0.0206(6) Uani 1 1 d . . . . .
H14 H -0.576158 0.088856 -0.218707 0.025 Uiso 1 1 calc R . . . .
C15 C -0.3928(3) 0.06501(10) -0.1212(2) 0.0186(6) Uani 1 1 d . . . . .
H15 H -0.406586 0.034213 -0.147169 0.022 Uiso 1 1 calc R . . . .
C16 C -0.2719(3) 0.07596(9) -0.0417(2) 0.0149(5) Uani 1 1 d . . . . .
H16 H -0.203456 0.053398 -0.012358 0.018 Uiso 1 1 calc R . . . .
C17 C -0.2560(3) 0.12153(9) -0.0073(2) 0.0126(5) Uani 1 1 d . . . . .
C18 C 0.0657(3) 0.08026(8) -0.0256(2) 0.0116(5) Uani 1 1 d . . . . .
C19 C 0.0202(3) 0.04562(9) -0.1072(2) 0.0144(5) Uani 1 1 d . . . . .
H19 H -0.016220 0.017477 -0.089448 0.017 Uiso 1 1 calc R . . . .
C20 C 0.0285(3) 0.05253(9) -0.2095(2) 0.0154(5) Uani 1 1 d . . . . .
H20 H -0.001092 0.028770 -0.261889 0.018 Uiso 1 1 calc R . . . .
C21 C 0.0801(3) 0.09417(9) -0.2410(2) 0.0138(5) Uani 1 1 d . . . . .
C22 C 0.0787(3) 0.10174(10) -0.3500(2) 0.0182(5) Uani 1 1 d . . . . .
H22 H 0.046679 0.077974 -0.401926 0.022 Uiso 1 1 calc R . . . .
C23 C 0.1224(3) 0.14247(10) -0.3827(2) 0.0207(6) Uani 1 1 d . . . . .
H23 H 0.120771 0.147028 -0.456417 0.025 Uiso 1 1 calc R . . . .
C24 C 0.1695(3) 0.17729(10) -0.3055(2) 0.0180(5) Uani 1 1 d . . . . .
H24 H 0.199033 0.205812 -0.327640 0.022 Uiso 1 1 calc R . . . .
C25 C 0.1739(3) 0.17100(9) -0.1985(2) 0.0137(5) Uani 1 1 d . . . . .
H25 H 0.206676 0.195285 -0.148134 0.016 Uiso 1 1 calc R . . . .
C26 C 0.1308(3) 0.12919(9) -0.1611(2) 0.0118(5) Uani 1 1 d . . . . .
C27 C 0.1271(3) 0.12054(9) -0.0517(2) 0.0116(5) Uani 1 1 d . . . . .
C28 C 0.1933(3) 0.15062(8) 0.0387(2) 0.0114(5) Uani 1 1 d . . . . .
C29 C 0.3525(3) 0.19806(9) 0.1291(2) 0.0130(5) Uani 1 1 d . . . . .
C30 C 0.4661(3) 0.22692(9) 0.1616(2) 0.0167(5) Uani 1 1 d . . . . .
H30 H 0.518783 0.235700 0.114227 0.020 Uiso 1 1 calc R . . . .
C31 C 0.4969(3) 0.24198(10) 0.2683(2) 0.0178(5) Uani 1 1 d . . . . .
H31 H 0.573835 0.261723 0.295697 0.021 Uiso 1 1 calc R . . . .
C32 C 0.4176(3) 0.22886(9) 0.3368(2) 0.0164(5) Uani 1 1 d . . . . .
H32 H 0.442371 0.240066 0.409366 0.020 Uiso 1 1 calc R . . . .
C33 C 0.3035(3) 0.19990(9) 0.3023(2) 0.0140(5) Uani 1 1 d . . . . .
H33 H 0.249635 0.191316 0.348966 0.017 Uiso 1 1 calc R . . . .
C34 C 0.2730(3) 0.18423(8) 0.1951(2) 0.0117(5) Uani 1 1 d . . . . .
C35 C 0.2923(3) 0.05760(9) 0.3788(2) 0.0136(5) Uani 1 1 d . . . . .
C36 C 0.2428(3) 0.03063(11) 0.4622(2) 0.0248(6) Uani 1 1 d . . . . .
H36A H 0.214554 0.052127 0.510769 0.037 Uiso 1 1 calc GR . . . .
H36B H 0.317701 0.011068 0.504709 0.037 Uiso 1 1 calc GR . . . .
H36C H 0.164228 0.011312 0.424794 0.037 Uiso 1 1 calc GR . . . .
C37 C 0.3358(3) 0.02458(11) 0.3022(3) 0.0248(6) Uani 1 1 d . . . . .
H37A H 0.258686 0.004179 0.267663 0.037 Uiso 1 1 calc GR . . . .
H37B H 0.414273 0.006107 0.343528 0.037 Uiso 1 1 calc GR . . . .
H37C H 0.362484 0.042226 0.246236 0.037 Uiso 1 1 calc GR . . . .
C38 C 0.4102(3) 0.08949(11) 0.4353(3) 0.0258(7) Uani 1 1 d . . . . .
H38A H 0.437330 0.108012 0.380885 0.039 Uiso 1 1 calc GR . . . .
H38B H 0.489002 0.071082 0.476407 0.039 Uiso 1 1 calc GR . . . .
H38C H 0.380301 0.109901 0.485141 0.039 Uiso 1 1 calc GR . . . .
C39 C -0.2363(3) 0.06517(9) 0.2710(2) 0.0145(5) Uani 1 1 d . . . . .
C40 C -0.1780(3) 0.06800(10) 0.3940(2) 0.0232(6) Uani 1 1 d . . . . .
H40A H -0.117518 0.041552 0.420163 0.035 Uiso 1 1 calc GR . . . .
H40B H -0.253829 0.067689 0.427619 0.035 Uiso 1 1 calc GR . . . .
H40C H -0.125259 0.096587 0.413536 0.035 Uiso 1 1 calc GR . . . .
C41 C -0.3059(3) 0.01873(10) 0.2366(3) 0.0251(7) Uani 1 1 d . . . . .
H41A H -0.337908 0.017104 0.157045 0.038 Uiso 1 1 calc GR . . . .
H41B H -0.384715 0.015419 0.266165 0.038 Uiso 1 1 calc GR . . . .
H41C H -0.239799 -0.006137 0.264326 0.038 Uiso 1 1 calc GR . . . .
C42 C -0.3394(3) 0.10438(10) 0.2299(3) 0.0225(6) Uani 1 1 d . . . . .
H42A H -0.293458 0.134052 0.251192 0.034 Uiso 1 1 calc GR . . . .
H42B H -0.416372 0.101346 0.261748 0.034 Uiso 1 1 calc GR . . . .
H42C H -0.374362 0.102818 0.150528 0.034 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
Hf1 O1 2.0450(19) . ?
Hf1 O3 2.0465(18) . ?
Hf1 O5 1.9274(18) . ?
Hf1 O6 1.9373(18) . ?
Hf1 N1 2.346(2) . ?
Hf1 N2 2.371(2) . ?
O1 C1 1.312(3) . ?
O2 C11 1.372(3) . ?
O2 C12 1.385(3) . ?
O3 C18 1.317(3) . ?
O4 C28 1.371(3) . ?
O4 C29 1.380(3) . ?
O5 C35 1.412(3) . ?
O6 C39 1.418(3) . ?
N1 C11 1.313(3) . ?
N1 C17 1.412(3) . ?
N2 C28 1.315(3) . ?
N2 C34 1.406(3) . ?
C1 C2 1.435(4) . ?
C1 C10 1.402(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.356(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.422(4) . ?
C4 C5 1.410(3) . ?
C4 C9 1.429(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.371(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.401(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.376(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.421(4) . ?
C9 C10 1.442(3) . ?
C10 C11 1.452(3) . ?
C12 C13 1.377(4) . ?
C12 C17 1.387(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.401(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(4) . ?
C18 C19 1.431(4) . ?
C18 C27 1.408(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.353(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.420(4) . ?
C21 C22 1.411(4) . ?
C21 C26 1.432(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.369(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.401(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.374(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.418(4) . ?
C26 C27 1.437(4) . ?
C27 C28 1.454(4) . ?
C29 C30 1.387(4) . ?
C29 C34 1.381(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.400(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.395(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.398(4) . ?
C35 C36 1.520(4) . ?
C35 C37 1.523(4) . ?
C35 C38 1.522(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.522(4) . ?
C39 C41 1.527(4) . ?
C39 C42 1.533(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 O3 152.33(7) . . ?
O1 Hf1 N1 76.03(7) . . ?
O1 Hf1 N2 84.02(7) . . ?
O3 Hf1 N1 84.11(7) . . ?
O3 Hf1 N2 74.82(7) . . ?
O5 Hf1 O1 96.90(7) . . ?
O5 Hf1 O3 100.67(8) . . ?
O5 Hf1 O6 102.75(8) . . ?
O5 Hf1 N1 171.17(7) . . ?
O5 Hf1 N2 90.02(8) . . ?
O6 Hf1 O1 98.59(8) . . ?
O6 Hf1 O3 98.17(8) . . ?
O6 Hf1 N1 83.75(8) . . ?
O6 Hf1 N2 166.49(8) . . ?
N1 Hf1 N2 84.04(7) . . ?
C1 O1 Hf1 142.37(17) . . ?
C11 O2 C12 105.28(19) . . ?
C18 O3 Hf1 139.74(16) . . ?
C28 O4 C29 105.2(2) . . ?
C35 O5 Hf1 163.70(17) . . ?
C39 O6 Hf1 148.92(16) . . ?
C11 N1 Hf1 127.47(17) . . ?
C11 N1 C17 105.7(2) . . ?
C17 N1 Hf1 124.29(16) . . ?
C28 N2 Hf1 126.35(17) . . ?
C28 N2 C34 105.8(2) . . ?
C34 N2 Hf1 126.62(17) . . ?
O1 C1 C2 116.9(2) . . ?
O1 C1 C10 124.0(2) . . ?
C10 C1 C2 119.0(2) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.8(2) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.8(2) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C9 118.8(2) . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 C9 120.1(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.6(3) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.1(3) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C10 118.9(2) . . ?
C8 C9 C4 117.3(2) . . ?
C8 C9 C10 123.8(2) . . ?
C1 C10 C9 120.1(2) . . ?
C1 C10 C11 117.1(2) . . ?
C9 C10 C11 122.0(2) . . ?
O2 C11 C10 117.5(2) . . ?
N1 C11 O2 113.3(2) . . ?
N1 C11 C10 128.7(2) . . ?
O2 C12 C17 107.9(2) . . ?
C13 C12 O2 127.4(2) . . ?
C13 C12 C17 124.7(2) . . ?
C12 C13 H13 122.4 . . ?
C12 C13 C14 115.2(3) . . ?
C14 C13 H13 122.4 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.3(3) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 118.9 . . ?
C16 C15 C14 122.2(3) . . ?
C16 C15 H15 118.9 . . ?
C15 C16 H16 121.6 . . ?
C17 C16 C15 116.7(2) . . ?
C17 C16 H16 121.6 . . ?
C12 C17 N1 107.8(2) . . ?
C12 C17 C16 119.9(2) . . ?
C16 C17 N1 132.2(2) . . ?
O3 C18 C19 117.5(2) . . ?
O3 C18 C27 123.7(2) . . ?
C27 C18 C19 118.8(2) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.7(2) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.0 . . ?
C19 C20 C21 122.1(2) . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C26 119.1(2) . . ?
C22 C21 C20 120.9(2) . . ?
C22 C21 C26 120.0(2) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 C21 121.7(3) . . ?
C23 C22 H22 119.2 . . ?
C22 C23 H23 120.6 . . ?
C22 C23 C24 118.8(3) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 H24 119.4 . . ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H24 119.4 . . ?
C24 C25 H25 119.1 . . ?
C24 C25 C26 121.7(3) . . ?
C26 C25 H25 119.1 . . ?
C21 C26 C27 118.2(2) . . ?
C25 C26 C21 116.6(2) . . ?
C25 C26 C27 125.1(2) . . ?
C18 C27 C26 120.9(2) . . ?
C18 C27 C28 116.3(2) . . ?
C26 C27 C28 122.7(2) . . ?
O4 C28 C27 117.7(2) . . ?
N2 C28 O4 113.1(2) . . ?
N2 C28 C27 129.0(2) . . ?
O4 C29 C30 127.2(3) . . ?
O4 C29 C34 108.2(2) . . ?
C34 C29 C30 124.6(2) . . ?
C29 C30 H30 122.5 . . ?
C31 C30 C29 115.0(3) . . ?
C31 C30 H30 122.5 . . ?
C30 C31 H31 119.2 . . ?
C30 C31 C32 121.7(3) . . ?
C32 C31 H31 119.2 . . ?
C31 C32 H32 118.9 . . ?
C33 C32 C31 122.3(3) . . ?
C33 C32 H32 118.9 . . ?
C32 C33 H33 121.9 . . ?
C32 C33 C34 116.2(3) . . ?
C34 C33 H33 121.9 . . ?
C29 C34 N2 107.8(2) . . ?
C29 C34 C33 120.2(2) . . ?
C33 C34 N2 132.0(2) . . ?
O5 C35 C36 108.8(2) . . ?
O5 C35 C37 107.8(2) . . ?
O5 C35 C38 108.8(2) . . ?
C36 C35 C37 110.0(2) . . ?
C36 C35 C38 110.3(3) . . ?
C38 C35 C37 111.1(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
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 . . ?
O6 C39 C40 107.6(2) . . ?
O6 C39 C41 108.4(2) . . ?
O6 C39 C42 109.7(2) . . ?
C40 C39 C41 111.1(2) . . ?
C40 C39 C42 110.0(2) . . ?
C41 C39 C42 110.0(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 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
Hf1 O1 C1 C2 -173.77(19) . . . . ?
Hf1 O1 C1 C10 8.9(4) . . . . ?
Hf1 O3 C18 C19 -152.0(2) . . . . ?
Hf1 O3 C18 C27 30.3(4) . . . . ?
Hf1 O5 C35 C36 -94.7(6) . . . . ?
Hf1 O5 C35 C37 24.6(7) . . . . ?
Hf1 O5 C35 C38 145.1(5) . . . . ?
Hf1 O6 C39 C40 -62.9(4) . . . . ?
Hf1 O6 C39 C41 177.0(2) . . . . ?
Hf1 O6 C39 C42 56.8(4) . . . . ?
Hf1 N1 C11 O2 -165.43(16) . . . . ?
Hf1 N1 C11 C10 5.5(4) . . . . ?
Hf1 N1 C17 C12 165.25(17) . . . . ?
Hf1 N1 C17 C16 -10.1(4) . . . . ?
Hf1 N2 C28 O4 -168.51(15) . . . . ?
Hf1 N2 C28 C27 5.7(4) . . . . ?
Hf1 N2 C34 C29 168.02(17) . . . . ?
Hf1 N2 C34 C33 -10.5(4) . . . . ?
O1 C1 C2 C3 179.6(2) . . . . ?
O1 C1 C10 C9 -174.5(2) . . . . ?
O1 C1 C10 C11 15.0(4) . . . . ?
O2 C12 C13 C14 -175.7(3) . . . . ?
O2 C12 C17 N1 -0.7(3) . . . . ?
O2 C12 C17 C16 175.4(2) . . . . ?
O3 C18 C19 C20 178.4(2) . . . . ?
O3 C18 C27 C26 -175.7(2) . . . . ?
O3 C18 C27 C28 8.3(4) . . . . ?
O4 C29 C30 C31 -177.8(3) . . . . ?
O4 C29 C34 N2 0.2(3) . . . . ?
O4 C29 C34 C33 178.9(2) . . . . ?
C1 C2 C3 C4 -3.0(4) . . . . ?
C1 C10 C11 O2 150.0(2) . . . . ?
C1 C10 C11 N1 -20.6(4) . . . . ?
C2 C1 C10 C9 8.3(4) . . . . ?
C2 C1 C10 C11 -162.3(2) . . . . ?
C2 C3 C4 C5 -175.1(3) . . . . ?
C2 C3 C4 C9 3.4(4) . . . . ?
C3 C4 C5 C6 177.1(3) . . . . ?
C3 C4 C9 C8 -175.7(2) . . . . ?
C3 C4 C9 C10 2.0(4) . . . . ?
C4 C5 C6 C7 -0.4(4) . . . . ?
C4 C9 C10 C1 -7.8(4) . . . . ?
C4 C9 C10 C11 162.2(2) . . . . ?
C5 C4 C9 C8 2.8(4) . . . . ?
C5 C4 C9 C10 -179.5(2) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
C6 C7 C8 C9 0.7(4) . . . . ?
C7 C8 C9 C4 -2.5(4) . . . . ?
C7 C8 C9 C10 179.9(3) . . . . ?
C8 C9 C10 C1 169.8(3) . . . . ?
C8 C9 C10 C11 -20.2(4) . . . . ?
C9 C4 C5 C6 -1.4(4) . . . . ?
C9 C10 C11 O2 -20.4(4) . . . . ?
C9 C10 C11 N1 169.0(3) . . . . ?
C10 C1 C2 C3 -2.9(4) . . . . ?
C11 O2 C12 C13 176.4(3) . . . . ?
C11 O2 C12 C17 -1.2(3) . . . . ?
C11 N1 C17 C12 2.3(3) . . . . ?
C11 N1 C17 C16 -173.1(3) . . . . ?
C12 O2 C11 N1 2.8(3) . . . . ?
C12 O2 C11 C10 -169.2(2) . . . . ?
C12 C13 C14 C15 -0.3(4) . . . . ?
C13 C12 C17 N1 -178.3(3) . . . . ?
C13 C12 C17 C16 -2.2(4) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C14 C15 C16 C17 -0.6(4) . . . . ?
C15 C16 C17 N1 176.6(3) . . . . ?
C15 C16 C17 C12 1.7(4) . . . . ?
C17 N1 C11 O2 -3.2(3) . . . . ?
C17 N1 C11 C10 167.7(3) . . . . ?
C17 C12 C13 C14 1.5(4) . . . . ?
C18 C19 C20 C21 -1.0(4) . . . . ?
C18 C27 C28 O4 151.4(2) . . . . ?
C18 C27 C28 N2 -22.6(4) . . . . ?
C19 C18 C27 C26 6.7(4) . . . . ?
C19 C18 C27 C28 -169.4(2) . . . . ?
C19 C20 C21 C22 -175.6(3) . . . . ?
C19 C20 C21 C26 2.9(4) . . . . ?
C20 C21 C22 C23 177.1(3) . . . . ?
C20 C21 C26 C25 -176.6(2) . . . . ?
C20 C21 C26 C27 0.0(4) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C21 C26 C27 C18 -4.8(4) . . . . ?
C21 C26 C27 C28 171.0(2) . . . . ?
C22 C21 C26 C25 1.8(4) . . . . ?
C22 C21 C26 C27 178.5(2) . . . . ?
C22 C23 C24 C25 0.7(4) . . . . ?
C23 C24 C25 C26 -0.2(4) . . . . ?
C24 C25 C26 C21 -1.1(4) . . . . ?
C24 C25 C26 C27 -177.5(3) . . . . ?
C25 C26 C27 C18 171.5(3) . . . . ?
C25 C26 C27 C28 -12.6(4) . . . . ?
C26 C21 C22 C23 -1.4(4) . . . . ?
C26 C27 C28 O4 -24.6(4) . . . . ?
C26 C27 C28 N2 161.4(3) . . . . ?
C27 C18 C19 C20 -3.8(4) . . . . ?
C28 O4 C29 C30 177.3(3) . . . . ?
C28 O4 C29 C34 -0.6(3) . . . . ?
C28 N2 C34 C29 0.4(3) . . . . ?
C28 N2 C34 C33 -178.2(3) . . . . ?
C29 O4 C28 N2 0.9(3) . . . . ?
C29 O4 C28 C27 -174.0(2) . . . . ?
C29 C30 C31 C32 -0.3(4) . . . . ?
C30 C29 C34 N2 -177.8(2) . . . . ?
C30 C29 C34 C33 0.9(4) . . . . ?
C30 C31 C32 C33 0.2(4) . . . . ?
C31 C32 C33 C34 0.5(4) . . . . ?
C32 C33 C34 N2 177.4(3) . . . . ?
C32 C33 C34 C29 -1.0(4) . . . . ?
C34 N2 C28 O4 -0.8(3) . . . . ?
C34 N2 C28 C27 173.4(3) . . . . ?
C34 C29 C30 C31 -0.2(4) . . . . ?

_olex2_date_sample_data_collection 2016-10-11
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5217(4) 0.4783(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C30(H30),
  C31(H31), C32(H32), C33(H33)
3.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.094
_oxdiff_exptl_absorpt_empirical_full_min 0.673
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5217(4) 125849 116477 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4783(4) 125677 116476 nmt 0.9994 0.0150 0.0003 -0.1114 0.9988 0.0588 0.0006
-0.0152 0.9996

_twin_special_details            
;
Component 2 rotated by 2.9070° 
 around [-0.43 0.01 -0.90] (reciprocal) or [-0.69 0.00 -0.72] (direct)
;
####################################################################### 
# 
# 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_compound9
_database_code_depnum_ccdc_archive 'CCDC 1816372'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-12-15
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H32 Hf N4 O8'
_chemical_formula_sum            'C52 H32 Hf N4 O8'
_chemical_formula_weight         1019.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H32 O8 N4 Hf'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.69585(13)
_cell_length_b                   14.60495(9)
_cell_length_c                   16.88832(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.3183(7)
_cell_angle_gamma                90
_cell_volume                     4037.99(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    74717
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      30.0690
_cell_measurement_theta_min      1.8600
_exptl_absorpt_coefficient_mu    2.650
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2032
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 3 0.0738
1 5 -5 0.0457
0 0 1 0.1173
4 -5 -4 0.0777
-4 5 4 0.0777
5 1 2 0.1288
-3 -2 -5 0.1349
5 -1 -5 0.1079
-5 1 5 0.1079
5 2 -3 0.1312
-5 -2 3 0.1312

_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.138
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0004 -4.9855 2.9967 -0.1534 -0.2264 0.0190
0.9989 4.9844 -4.9938 0.1192 0.2888 -0.0707
-0.0006 0.0007 0.9984 0.0201 -0.0374 0.0053
3.9968 -4.9892 -3.9931 -0.2699 -0.0140 -0.1824
-3.9968 4.9892 3.9931 0.2699 0.0140 0.1824
4.9882 1.0003 1.9946 0.1128 -0.1133 -0.1951
-2.9899 -1.9993 -4.9901 -0.2038 0.1780 0.0977
4.9936 -0.9996 -4.9932 -0.1131 0.1025 -0.2312
-4.9936 0.9996 4.9932 0.1131 -0.1025 0.2312
4.9909 1.9944 -2.9974 0.0552 0.0963 -0.2223
-4.9909 -1.9944 2.9974 -0.0552 -0.0963 0.2223

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            117598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         1.869
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1901
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  42.00   1.00    5.89    --  -28.55  57.00 -60.00   94
  2  ω    -52.00  42.00   1.00    5.89    --  -28.55  57.00-150.00   94
  3  ω   -111.00 -34.00   1.00    5.89    --  -28.55 178.00-180.00   77
  4  ω   -101.00   5.00   1.00    5.89    --  -28.55 -77.00  90.00  106
  5  ω    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00 150.00   94
  6  ω    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00 -30.00   94
  7  ω    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00-120.00   94
  8  ω    -34.00  -5.00   1.00    5.89    --   28.62 129.00 -80.80   29
  9  ω    -20.00  73.00   1.00    5.89    --   28.62 -99.00  30.00   93
 10  ω     34.00 111.00   1.00    5.89    --   28.62-178.00-120.00   77
 11  ω    -47.00  95.00   1.00    5.89    --   28.62 -19.00   0.00  142
 12  ω   -101.00   5.00   1.00    5.89    --  -28.55 -77.00-180.00  106
 13  ω   -100.00 -53.00   1.00    5.89    --  -28.55-156.00 -79.00   47
 14  ω    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00  30.00   94
 15  ω   -108.00 -35.00   1.00    5.89    --  -28.55-178.00-120.00   73
 16  ω     -3.00 102.00   1.00    5.89    --   28.62  38.00 -60.00  105
 17  ω    -20.00  73.00   1.00    5.89    --   28.62 -99.00-180.00   93
 18  ω     -4.00 101.00   1.00    5.89    --   28.62  77.00  30.00  105
 19  ω     -3.00 102.00   1.00    5.89    --   28.62  38.00  60.00  105
 20  ω    -34.00  -5.00   1.00    5.89    --   28.62 129.00-140.57   29
 21  ω    -46.00 104.00   1.00    5.89    --   28.62   0.00-150.00  150
 22  ω    -46.00 104.00   1.00    5.89    --   28.62   0.00-120.00  150
 23  ω    -46.00 104.00   1.00    5.89    --   28.62   0.00 -90.00  150
 24  ω    -46.00 104.00   1.00    5.89    --   28.62   0.00 -60.00  150
 25  ω    -46.00  92.00   1.00    5.89    --   28.62   0.00 -30.00  138
 26  ω    -46.00 104.00   1.00    5.89    --   28.62   0.00-180.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0060015000
_diffrn_orient_matrix_UB_12      0.0428305000
_diffrn_orient_matrix_UB_13      0.0200754000
_diffrn_orient_matrix_UB_21      -0.0123333000
_diffrn_orient_matrix_UB_22      0.0228902000
_diffrn_orient_matrix_UB_23      -0.0374493000
_diffrn_orient_matrix_UB_31      -0.0411076000
_diffrn_orient_matrix_UB_32      -0.0006293000
_diffrn_orient_matrix_UB_33      0.0053092000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5781
_reflns_number_total             5945
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Disorder of the ligand sphere on the twofold axis of the Hf-complex. 
 No larger cell or twinning resolves this disorder.

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         5945
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0149
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0148P)²+3.4952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0361
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.500000 0.65210(2) 0.250000 0.02256(3) Uani 1 2 d S T P . .
O1A O 0.45602(11) 0.68528(13) 0.34813(11) 0.0238(3) Uani 0.5 1 d . . . A -1
C1A C 0.4755(2) 0.6897(3) 0.4281(2) 0.0229(6) Uani 0.5 1 d . . . A -1
C2A C 0.4341(6) 0.7521(7) 0.4703(4) 0.0232(13) Uani 0.5 1 d . . . A -1
H2A H 0.393943 0.790137 0.441640 0.028 Uiso 0.5 1 calc R . . A -1
C3A C 0.4530(2) 0.7569(2) 0.5532(3) 0.0308(6) Uani 0.5 1 d . . . A -1
H3A H 0.425140 0.797574 0.580529 0.037 Uiso 0.5 1 calc R . . A -1
C4A C 0.5151(6) 0.6997(5) 0.5972(5) 0.0351(13) Uani 0.5 1 d . . . A -1
H4A H 0.528471 0.703851 0.653180 0.042 Uiso 0.5 1 calc R . . A -1
C5A C 0.5546(3) 0.6395(3) 0.5580(2) 0.0320(8) Uani 0.5 1 d . . . A -1
H5A H 0.593970 0.601170 0.587482 0.038 Uiso 0.5 1 calc R . . A -1
C6A C 0.53701(18) 0.63365(19) 0.47312(17) 0.0253(5) Uani 0.5 1 d . . . A -1
C7A C 0.5806(5) 0.5633(3) 0.4300(3) 0.0202(7) Uani 0.5 1 d . . . A -1
O2A O 0.62882(12) 0.50559(13) 0.47910(12) 0.0303(4) Uani 0.5 1 d . . . A -1
C8A C 0.6560(2) 0.4493(2) 0.4252(3) 0.0303(7) Uani 0.5 1 d . . . A -1
C9A C 0.7079(9) 0.3787(7) 0.4430(10) 0.0318(19) Uani 0.5 1 d . . . A -1
H9A H 0.731619 0.363185 0.495813 0.038 Uiso 0.5 1 calc R . . A -1
C10A C 0.7242(3) 0.3288(3) 0.3746(4) 0.0426(11) Uani 0.5 1 d . . . A -1
H10A H 0.759593 0.279046 0.382655 0.051 Uiso 0.5 1 calc R . . A -1
C11A C 0.6875(2) 0.3540(2) 0.2964(3) 0.0390(7) Uani 0.5 1 d . . . A -1
H11A H 0.698530 0.320049 0.253201 0.047 Uiso 0.5 1 calc R . . A -1
C12A C 0.6350(4) 0.4284(3) 0.2810(4) 0.0316(9) Uani 0.5 1 d . . . A -1
H12A H 0.610758 0.444792 0.228605 0.038 Uiso 0.5 1 calc R . . A -1
C13A C 0.6201(3) 0.4776(3) 0.3476(3) 0.0251(9) Uani 0.5 1 d . . . A -1
N1A N 0.57262(13) 0.55462(14) 0.35427(14) 0.0242(4) Uani 0.5 1 d . . . A -1
O3A O 0.48831(11) 0.78324(12) 0.19981(11) 0.0228(3) Uani 0.5 1 d . . . A -1
C14A C 0.4404(3) 0.8336(3) 0.1448(2) 0.0224(6) Uani 0.5 1 d . . . A -1
C15A C 0.4718(4) 0.9154(3) 0.1179(3) 0.0296(9) Uani 0.5 1 d . . . A -1
H15A H 0.523992 0.935020 0.141469 0.036 Uiso 0.5 1 calc R . . A -1
C16A C 0.4254(4) 0.9661(3) 0.0569(4) 0.0364(10) Uani 0.5 1 d . . . A -1
H16A H 0.447183 1.019287 0.039454 0.044 Uiso 0.5 1 calc R . . A -1
C17A C 0.3473(4) 0.9397(4) 0.0211(3) 0.0355(10) Uani 0.5 1 d . . . A -1
H17A H 0.317849 0.973385 -0.021647 0.043 Uiso 0.5 1 calc R . . A -1
C18A C 0.3130(2) 0.8630(3) 0.0491(3) 0.0289(7) Uani 0.5 1 d . . . A -1
H18A H 0.259585 0.846430 0.026857 0.035 Uiso 0.5 1 calc R . . A -1
C19A C 0.3590(3) 0.8103(2) 0.1112(2) 0.0226(5) Uani 0.5 1 d . . . A -1
C20A C 0.3240(5) 0.7370(4) 0.1495(4) 0.0202(7) Uani 0.5 1 d . . . A -1
O4A O 0.23819(12) 0.72999(14) 0.13064(12) 0.0309(4) Uani 0.5 1 d . . . A -1
C21A C 0.2202(3) 0.6640(3) 0.1828(2) 0.0289(7) Uani 0.5 1 d . . . A -1
C22A C 0.1438(3) 0.6331(4) 0.1892(4) 0.0436(11) Uani 0.5 1 d . . . A -1
H22A H 0.096525 0.652632 0.154534 0.052 Uiso 0.5 1 calc R . . A -1
C23A C 0.1421(3) 0.5710(3) 0.2509(4) 0.0432(9) Uani 0.5 1 d . . . A -1
H23A H 0.092201 0.548028 0.258446 0.052 Uiso 0.5 1 calc R . . A -1
C24A C 0.2141(4) 0.5423(3) 0.3021(3) 0.0374(8) Uani 0.5 1 d . . . A -1
H24A H 0.210870 0.501160 0.343400 0.045 Uiso 0.5 1 calc R . . A -1
C25A C 0.2898(3) 0.5735(3) 0.2928(2) 0.0302(8) Uani 0.5 1 d . . . A -1
H25A H 0.337481 0.553836 0.326686 0.036 Uiso 0.5 1 calc R . . A -1
C26A C 0.2920(2) 0.6351(2) 0.2310(3) 0.0236(6) Uani 0.5 1 d . . . A -1
N2A N 0.35647(13) 0.67976(15) 0.20515(13) 0.0220(4) Uani 0.5 1 d . . . A -1
O5A O 0.44996(11) 0.52269(12) 0.22991(11) 0.0253(4) Uani 0.5 1 d . . . A -1
C27A C 0.3973(3) 0.4733(4) 0.1776(3) 0.0258(9) Uani 0.5 1 d . . . A -1
C28A C 0.3541(4) 0.4010(3) 0.2041(4) 0.0327(10) Uani 0.5 1 d . . . A -1
H28A H 0.362064 0.388342 0.259053 0.039 Uiso 0.5 1 calc R . . A -1
C29A C 0.3001(3) 0.3480(3) 0.1507(3) 0.0353(8) Uani 0.5 1 d . . . A -1
H29A H 0.271762 0.301444 0.170904 0.042 Uiso 0.5 1 calc R . . A -1
C30A C 0.2871(9) 0.3617(8) 0.0699(8) 0.0293(18) Uani 0.5 1 d . . . A -1
H30A H 0.251147 0.324675 0.034765 0.035 Uiso 0.5 1 calc R . . A -1
C31A C 0.3295(2) 0.4338(2) 0.0401(2) 0.0297(7) Uani 0.5 1 d . . . A -1
H31A H 0.321811 0.443819 -0.015207 0.036 Uiso 0.5 1 calc R . . A -1
C32A C 0.38315(17) 0.49036(19) 0.09334(19) 0.0263(5) Uani 0.5 1 d . . . A -1
C33A C 0.4296(5) 0.5666(3) 0.0601(3) 0.0202(7) Uani 0.5 1 d . . . A -1
O6A O 0.42191(12) 0.56681(13) -0.02009(11) 0.0279(4) Uani 0.5 1 d . . . A -1
C34A C 0.4713(2) 0.6392(2) -0.0315(2) 0.0259(7) Uani 0.5 1 d . . . A -1
C35A C 0.4888(5) 0.6722(5) -0.1044(5) 0.0350(13) Uani 0.5 1 d . . . A -1
H35A H 0.466562 0.645896 -0.153983 0.042 Uiso 0.5 1 calc R . . A -1
C36A C 0.5405(2) 0.7453(3) -0.0978(2) 0.0360(7) Uani 0.5 1 d . . . A -1
H36A H 0.551800 0.771948 -0.144431 0.043 Uiso 0.5 1 calc R . . A -1
C37A C 0.5769(2) 0.7811(2) -0.0227(3) 0.0306(6) Uani 0.5 1 d . . . A -1
H37A H 0.613402 0.829544 -0.020556 0.037 Uiso 0.5 1 calc R . . A -1
C38A C 0.5603(6) 0.7462(7) 0.0495(5) 0.0252(12) Uani 0.5 1 d . . . A -1
H38A H 0.585279 0.770213 0.099215 0.030 Uiso 0.5 1 calc R . . A -1
C39A C 0.5052(2) 0.6748(2) 0.0440(2) 0.0223(7) Uani 0.5 1 d . . . A -1
N3A N 0.47400(13) 0.62631(15) 0.10204(13) 0.0228(4) Uani 0.5 1 d . . . A -1
O7A O 0.60966(11) 0.62163(13) 0.20948(11) 0.0242(3) Uani 0.5 1 d . . . A -1
C40A C 0.6902(2) 0.6184(2) 0.2348(2) 0.0228(5) Uani 0.5 1 d . . . A -1
C41A C 0.7378(3) 0.5673(3) 0.1914(3) 0.0287(7) Uani 0.5 1 d . . . A -1
H41A H 0.712950 0.538142 0.144003 0.034 Uiso 0.5 1 calc R . . A -1
C42A C 0.8214(4) 0.5596(3) 0.2181(3) 0.0335(8) Uani 0.5 1 d . . . A -1
H42A H 0.851941 0.524264 0.189053 0.040 Uiso 0.5 1 calc R . . A -1
C43A C 0.8604(3) 0.6043(4) 0.2884(3) 0.0323(9) Uani 0.5 1 d . . . A -1
H43A H 0.916530 0.598804 0.306121 0.039 Uiso 0.5 1 calc R . . A -1
C44A C 0.8149(3) 0.6564(2) 0.3309(2) 0.0274(7) Uani 0.5 1 d . . . A -1
H44A H 0.840520 0.686739 0.377445 0.033 Uiso 0.5 1 calc R . . A -1
C45A C 0.7304(3) 0.6643(2) 0.3049(2) 0.0233(5) Uani 0.5 1 d . . . A -1
C46A C 0.6867(5) 0.7287(4) 0.3441(4) 0.0202(7) Uani 0.5 1 d . . . A -1
O8A O 0.72707(12) 0.78470(13) 0.40210(11) 0.0262(4) Uani 0.5 1 d . . . A -1
C47A C 0.6699(2) 0.8467(2) 0.4186(3) 0.0230(6) Uani 0.5 1 d . . . A -1
C48A C 0.6812(3) 0.9170(3) 0.4730(3) 0.0332(8) Uani 0.5 1 d . . . A -1
H48A H 0.730693 0.926306 0.508400 0.040 Uiso 0.5 1 calc R . . A -1
C49A C 0.6146(4) 0.9737(3) 0.4723(3) 0.0355(8) Uani 0.5 1 d . . . A -1
H49A H 0.619364 1.022701 0.508027 0.043 Uiso 0.5 1 calc R . . A -1
C50A C 0.5408(3) 0.9589(3) 0.4193(3) 0.0291(7) Uani 0.5 1 d . . . A -1
H50A H 0.498019 0.999866 0.418958 0.035 Uiso 0.5 1 calc R . . A -1
C51A C 0.5291(3) 0.8846(3) 0.3669(3) 0.0248(8) Uani 0.5 1 d . . . A -1
H51A H 0.479226 0.873818 0.332605 0.030 Uiso 0.5 1 calc R . . A -1
C52A C 0.5962(3) 0.8266(2) 0.3683(2) 0.0222(6) Uani 0.5 1 d . . . A -1
N4A N 0.60614(13) 0.74791(15) 0.32404(13) 0.0232(4) Uani 0.5 1 d . . . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1A 1.9995(18) . ?
Hf1 N1A 2.400(2) . ?
Hf1 O3A 2.0880(17) . ?
Hf1 N2A 2.401(2) . ?
Hf1 O5A 2.0674(18) . ?
Hf1 N3A 2.480(2) . ?
Hf1 O7A 2.1236(18) . ?
Hf1 N4A 2.407(2) . ?
O1A C1A 1.327(4) . ?
C1A C2A 1.417(8) . ?
C1A C6A 1.413(4) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.376(7) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.422(10) . ?
C4A H4A 0.9300 . ?
C4A C5A 1.348(11) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.408(4) . ?
C6A C7A 1.524(6) . ?
C7A O2A 1.336(6) . ?
C7A N1A 1.267(6) . ?
O2A C8A 1.368(4) . ?
C8A C9A 1.343(13) . ?
C8A C13A 1.393(6) . ?
C9A H9A 0.9300 . ?
C9A C10A 1.436(11) . ?
C10A H10A 0.9300 . ?
C10A C11A 1.392(6) . ?
C11A H11A 0.9300 . ?
C11A C12A 1.388(5) . ?
C12A H12A 0.9300 . ?
C12A C13A 1.398(9) . ?
C13A N1A 1.393(6) . ?
O3A C14A 1.323(4) . ?
C14A C15A 1.414(6) . ?
C14A C19A 1.409(5) . ?
C15A H15A 0.9300 . ?
C15A C16A 1.377(7) . ?
C16A H16A 0.9300 . ?
C16A C17A 1.380(7) . ?
C17A H17A 0.9300 . ?
C17A C18A 1.383(6) . ?
C18A H18A 0.9300 . ?
C18A C19A 1.402(5) . ?
C19A C20A 1.434(5) . ?
C20A O4A 1.408(8) . ?
C20A N2A 1.294(6) . ?
O4A C21A 1.378(4) . ?
C21A C22A 1.378(7) . ?
C21A C26A 1.376(6) . ?
C22A H22A 0.9300 . ?
C22A C23A 1.385(6) . ?
C23A H23A 0.9300 . ?
C23A C24A 1.401(6) . ?
C24A H24A 0.9300 . ?
C24A C25A 1.382(6) . ?
C25A H25A 0.9300 . ?
C25A C26A 1.383(6) . ?
C26A N2A 1.399(4) . ?
O5A C27A 1.330(5) . ?
C27A C28A 1.400(9) . ?
C27A C32A 1.419(5) . ?
C28A H28A 0.9300 . ?
C28A C29A 1.381(6) . ?
C29A H29A 0.9300 . ?
C29A C30A 1.355(14) . ?
C30A H30A 0.9300 . ?
C30A C31A 1.414(10) . ?
C31A H31A 0.9300 . ?
C31A C32A 1.406(4) . ?
C32A C33A 1.526(6) . ?
C33A O6A 1.334(6) . ?
C33A N3A 1.267(6) . ?
O6A C34A 1.377(4) . ?
C34A C35A 1.405(10) . ?
C34A C39A 1.392(5) . ?
C35A H35A 0.9300 . ?
C35A C36A 1.364(9) . ?
C36A H36A 0.9300 . ?
C36A C37A 1.396(5) . ?
C37A H37A 0.9300 . ?
C37A C38A 1.398(6) . ?
C38A H38A 0.9300 . ?
C38A C39A 1.382(11) . ?
C39A N3A 1.391(4) . ?
O7A C40A 1.329(4) . ?
C40A C41A 1.397(5) . ?
C40A C45A 1.411(5) . ?
C41A H41A 0.9300 . ?
C41A C42A 1.386(6) . ?
C42A H42A 0.9300 . ?
C42A C43A 1.398(6) . ?
C43A H43A 0.9300 . ?
C43A C44A 1.374(6) . ?
C44A H44A 0.9300 . ?
C44A C45A 1.397(5) . ?
C45A C46A 1.429(6) . ?
C46A O8A 1.351(6) . ?
C46A N4A 1.351(7) . ?
O8A C47A 1.383(4) . ?
C47A C48A 1.366(6) . ?
C47A C52A 1.382(6) . ?
C48A H48A 0.9300 . ?
C48A C49A 1.384(6) . ?
C49A H49A 0.9300 . ?
C49A C50A 1.391(6) . ?
C50A H50A 0.9300 . ?
C50A C51A 1.390(6) . ?
C51A H51A 0.9300 . ?
C51A C52A 1.401(6) . ?
C52A N4A 1.399(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1A Hf1 N1A 75.55(7) . . ?
O1A Hf1 O3A 95.39(7) . . ?
O1A Hf1 N2A 73.42(7) . . ?
O1A Hf1 O5A 98.93(8) . . ?
O1A Hf1 N3A 148.42(7) . . ?
O1A Hf1 O7A 142.93(7) . . ?
O1A Hf1 N4A 77.36(7) . . ?
N1A Hf1 N2A 131.33(7) . . ?
N1A Hf1 N3A 127.78(7) . . ?
N1A Hf1 N4A 75.48(7) . . ?
O3A Hf1 N1A 146.67(7) . . ?
O3A Hf1 N2A 73.12(7) . . ?
O3A Hf1 N3A 75.31(7) . . ?
O3A Hf1 O7A 94.54(7) . . ?
O3A Hf1 N4A 71.23(7) . . ?
N2A Hf1 N3A 75.00(7) . . ?
N2A Hf1 N4A 130.81(7) . . ?
O5A Hf1 N1A 73.01(7) . . ?
O5A Hf1 O3A 140.30(7) . . ?
O5A Hf1 N2A 75.87(7) . . ?
O5A Hf1 N3A 73.17(7) . . ?
O5A Hf1 O7A 95.84(7) . . ?
O5A Hf1 N4A 148.15(7) . . ?
O7A Hf1 N1A 76.63(7) . . ?
O7A Hf1 N2A 143.48(7) . . ?
O7A Hf1 N3A 68.59(7) . . ?
O7A Hf1 N4A 72.29(7) . . ?
N4A Hf1 N3A 125.26(7) . . ?
C1A O1A Hf1 143.0(2) . . ?
O1A C1A C2A 119.7(4) . . ?
O1A C1A C6A 121.8(3) . . ?
C6A C1A C2A 118.5(4) . . ?
C1A C2A H2A 119.7 . . ?
C3A C2A C1A 120.5(7) . . ?
C3A C2A H2A 119.7 . . ?
C2A C3A H3A 120.0 . . ?
C2A C3A C4A 119.9(6) . . ?
C4A C3A H3A 120.0 . . ?
C3A C4A H4A 119.9 . . ?
C5A C4A C3A 120.3(7) . . ?
C5A C4A H4A 119.9 . . ?
C4A C5A H5A 119.5 . . ?
C4A C5A C6A 121.0(5) . . ?
C6A C5A H5A 119.5 . . ?
C1A C6A C7A 119.9(3) . . ?
C5A C6A C1A 119.8(3) . . ?
C5A C6A C7A 120.2(4) . . ?
O2A C7A C6A 114.5(4) . . ?
N1A C7A C6A 125.8(4) . . ?
N1A C7A O2A 119.6(4) . . ?
C7A O2A C8A 101.8(3) . . ?
O2A C8A C13A 108.0(3) . . ?
C9A C8A O2A 126.6(7) . . ?
C9A C8A C13A 125.3(8) . . ?
C8A C9A H9A 122.4 . . ?
C8A C9A C10A 115.2(12) . . ?
C10A C9A H9A 122.4 . . ?
C9A C10A H10A 119.6 . . ?
C11A C10A C9A 120.8(7) . . ?
C11A C10A H10A 119.6 . . ?
C10A C11A H11A 119.1 . . ?
C12A C11A C10A 121.9(4) . . ?
C12A C11A H11A 119.1 . . ?
C11A C12A H12A 121.4 . . ?
C11A C12A C13A 117.3(5) . . ?
C13A C12A H12A 121.4 . . ?
C8A C13A C12A 119.5(4) . . ?
C8A C13A N1A 108.1(4) . . ?
N1A C13A C12A 132.4(4) . . ?
C7A N1A Hf1 128.3(2) . . ?
C7A N1A C13A 102.3(3) . . ?
C13A N1A Hf1 129.3(2) . . ?
C14A O3A Hf1 142.2(2) . . ?
O3A C14A C15A 119.0(4) . . ?
O3A C14A C19A 123.4(4) . . ?
C19A C14A C15A 117.6(4) . . ?
C14A C15A H15A 119.8 . . ?
C16A C15A C14A 120.4(5) . . ?
C16A C15A H15A 119.8 . . ?
C15A C16A H16A 119.3 . . ?
C15A C16A C17A 121.5(4) . . ?
C17A C16A H16A 119.3 . . ?
C16A C17A H17A 120.2 . . ?
C16A C17A C18A 119.6(4) . . ?
C18A C17A H17A 120.2 . . ?
C17A C18A H18A 120.0 . . ?
C17A C18A C19A 119.9(4) . . ?
C19A C18A H18A 120.0 . . ?
C14A C19A C20A 116.5(4) . . ?
C18A C19A C14A 120.8(3) . . ?
C18A C19A C20A 122.4(5) . . ?
O4A C20A C19A 116.0(5) . . ?
N2A C20A C19A 131.3(6) . . ?
N2A C20A O4A 112.4(4) . . ?
C21A O4A C20A 104.2(3) . . ?
C22A C21A O4A 126.9(5) . . ?
C26A C21A O4A 108.6(4) . . ?
C26A C21A C22A 124.5(4) . . ?
C21A C22A H22A 122.3 . . ?
C21A C22A C23A 115.4(5) . . ?
C23A C22A H22A 122.3 . . ?
C22A C23A H23A 119.4 . . ?
C22A C23A C24A 121.3(5) . . ?
C24A C23A H23A 119.4 . . ?
C23A C24A H24A 119.2 . . ?
C25A C24A C23A 121.6(5) . . ?
C25A C24A H24A 119.2 . . ?
C24A C25A H25A 121.3 . . ?
C24A C25A C26A 117.5(4) . . ?
C26A C25A H25A 121.3 . . ?
C21A C26A C25A 119.7(3) . . ?
C21A C26A N2A 107.9(4) . . ?
C25A C26A N2A 132.4(4) . . ?
C20A N2A Hf1 126.0(4) . . ?
C20A N2A C26A 106.8(4) . . ?
C26A N2A Hf1 127.1(2) . . ?
C27A O5A Hf1 143.0(3) . . ?
O5A C27A C28A 120.8(5) . . ?
O5A C27A C32A 121.9(5) . . ?
C28A C27A C32A 117.3(4) . . ?
C27A C28A H28A 119.1 . . ?
C29A C28A C27A 121.7(5) . . ?
C29A C28A H28A 119.1 . . ?
C28A C29A H29A 119.0 . . ?
C30A C29A C28A 122.0(7) . . ?
C30A C29A H29A 119.0 . . ?
C29A C30A H30A 120.8 . . ?
C29A C30A C31A 118.4(11) . . ?
C31A C30A H30A 120.8 . . ?
C30A C31A H31A 119.6 . . ?
C32A C31A C30A 120.7(7) . . ?
C32A C31A H31A 119.6 . . ?
C27A C32A C33A 120.1(4) . . ?
C31A C32A C27A 119.8(3) . . ?
C31A C32A C33A 120.0(3) . . ?
O6A C33A C32A 114.9(4) . . ?
N3A C33A C32A 125.4(4) . . ?
N3A C33A O6A 119.7(4) . . ?
C33A O6A C34A 101.7(3) . . ?
O6A C34A C35A 128.3(4) . . ?
O6A C34A C39A 107.8(3) . . ?
C39A C34A C35A 123.9(4) . . ?
C34A C35A H35A 122.1 . . ?
C36A C35A C34A 115.8(6) . . ?
C36A C35A H35A 122.1 . . ?
C35A C36A H36A 119.2 . . ?
C35A C36A C37A 121.5(5) . . ?
C37A C36A H36A 119.2 . . ?
C36A C37A H37A 119.0 . . ?
C36A C37A C38A 122.0(5) . . ?
C38A C37A H37A 119.0 . . ?
C37A C38A H38A 121.3 . . ?
C39A C38A C37A 117.4(7) . . ?
C39A C38A H38A 121.3 . . ?
C38A C39A C34A 119.3(4) . . ?
C38A C39A N3A 132.4(5) . . ?
N3A C39A C34A 108.3(3) . . ?
C33A N3A Hf1 129.5(3) . . ?
C33A N3A C39A 102.4(3) . . ?
C39A N3A Hf1 128.1(2) . . ?
C40A O7A Hf1 141.8(2) . . ?
O7A C40A C41A 119.6(3) . . ?
O7A C40A C45A 122.5(3) . . ?
C41A C40A C45A 117.8(3) . . ?
C40A C41A H41A 119.5 . . ?
C42A C41A C40A 120.9(4) . . ?
C42A C41A H41A 119.5 . . ?
C41A C42A H42A 119.7 . . ?
C41A C42A C43A 120.6(4) . . ?
C43A C42A H42A 119.7 . . ?
C42A C43A H43A 120.3 . . ?
C44A C43A C42A 119.3(4) . . ?
C44A C43A H43A 120.3 . . ?
C43A C44A H44A 119.7 . . ?
C43A C44A C45A 120.6(4) . . ?
C45A C44A H44A 119.7 . . ?
C40A C45A C46A 119.9(4) . . ?
C44A C45A C40A 120.7(3) . . ?
C44A C45A C46A 119.0(5) . . ?
O8A C46A C45A 120.5(6) . . ?
N4A C46A C45A 126.5(5) . . ?
N4A C46A O8A 112.7(3) . . ?
C46A O8A C47A 106.1(3) . . ?
C48A C47A O8A 128.2(4) . . ?
C48A C47A C52A 124.1(4) . . ?
C52A C47A O8A 107.7(4) . . ?
C47A C48A H48A 122.0 . . ?
C47A C48A C49A 116.1(5) . . ?
C49A C48A H48A 122.0 . . ?
C48A C49A H49A 119.2 . . ?
C48A C49A C50A 121.5(5) . . ?
C50A C49A H49A 119.2 . . ?
C49A C50A H50A 119.1 . . ?
C51A C50A C49A 121.7(5) . . ?
C51A C50A H50A 119.1 . . ?
C50A C51A H51A 121.6 . . ?
C50A C51A C52A 116.7(5) . . ?
C52A C51A H51A 121.6 . . ?
C47A C52A C51A 119.7(3) . . ?
C47A C52A N4A 108.6(4) . . ?
N4A C52A C51A 131.7(5) . . ?
C46A N4A Hf1 127.2(2) . . ?
C46A N4A C52A 104.7(3) . . ?
C52A N4A Hf1 127.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hf1 O1A C1A C2A 154.2(5) . . . . ?
Hf1 O1A C1A C6A -25.8(5) . . . . ?
Hf1 O3A C14A C15A -162.5(3) . . . . ?
Hf1 O3A C14A C19A 17.5(5) . . . . ?
Hf1 O5A C27A C28A -149.3(4) . . . . ?
Hf1 O5A C27A C32A 31.5(8) . . . . ?
Hf1 O7A C40A C41A 160.6(3) . . . . ?
Hf1 O7A C40A C45A -18.9(5) . . . . ?
O1A C1A C2A C3A 179.3(6) . . . . ?
O1A C1A C6A C5A -178.7(3) . . . . ?
O1A C1A C6A C7A -2.3(6) . . . . ?
C1A C2A C3A C4A 0.7(11) . . . . ?
C1A C6A C7A O2A -170.9(4) . . . . ?
C1A C6A C7A N1A 7.0(9) . . . . ?
C2A C1A C6A C5A 1.3(7) . . . . ?
C2A C1A C6A C7A 177.7(6) . . . . ?
C2A C3A C4A C5A -1.2(9) . . . . ?
C3A C4A C5A C6A 1.8(8) . . . . ?
C4A C5A C6A C1A -1.8(6) . . . . ?
C4A C5A C6A C7A -178.3(5) . . . . ?
C5A C6A C7A O2A 5.6(7) . . . . ?
C5A C6A C7A N1A -176.5(5) . . . . ?
C6A C1A C2A C3A -0.7(11) . . . . ?
C6A C7A O2A C8A 177.3(5) . . . . ?
C6A C7A N1A Hf1 7.3(9) . . . . ?
C6A C7A N1A C13A -175.7(6) . . . . ?
C7A O2A C8A C9A 179.2(9) . . . . ?
C7A O2A C8A C13A -1.0(5) . . . . ?
O2A C7A N1A Hf1 -174.9(3) . . . . ?
O2A C7A N1A C13A 2.1(7) . . . . ?
O2A C8A C9A C10A 177.9(6) . . . . ?
O2A C8A C13A C12A -177.1(5) . . . . ?
O2A C8A C13A N1A 2.3(5) . . . . ?
C8A C9A C10A C11A 0.0(15) . . . . ?
C8A C13A N1A Hf1 174.4(2) . . . . ?
C8A C13A N1A C7A -2.5(6) . . . . ?
C9A C8A C13A C12A 2.7(11) . . . . ?
C9A C8A C13A N1A -178.0(8) . . . . ?
C9A C10A C11A C12A 0.8(10) . . . . ?
C10A C11A C12A C13A 0.0(7) . . . . ?
C11A C12A C13A C8A -1.7(8) . . . . ?
C11A C12A C13A N1A 179.2(5) . . . . ?
C12A C13A N1A Hf1 -6.4(8) . . . . ?
C12A C13A N1A C7A 176.7(7) . . . . ?
C13A C8A C9A C10A -1.8(15) . . . . ?
N1A C7A O2A C8A -0.7(7) . . . . ?
O3A C14A C15A C16A 175.6(3) . . . . ?
O3A C14A C19A C18A -175.6(3) . . . . ?
O3A C14A C19A C20A 11.1(6) . . . . ?
C14A C15A C16A C17A 0.8(6) . . . . ?
C14A C19A C20A O4A 163.5(5) . . . . ?
C14A C19A C20A N2A -9.2(12) . . . . ?
C15A C14A C19A C18A 4.4(5) . . . . ?
C15A C14A C19A C20A -168.9(5) . . . . ?
C15A C16A C17A C18A 2.9(6) . . . . ?
C16A C17A C18A C19A -2.8(6) . . . . ?
C17A C18A C19A C14A -0.9(5) . . . . ?
C17A C18A C19A C20A 172.1(5) . . . . ?
C18A C19A C20A O4A -9.8(9) . . . . ?
C18A C19A C20A N2A 177.6(7) . . . . ?
C19A C14A C15A C16A -4.4(5) . . . . ?
C19A C20A O4A C21A -172.0(5) . . . . ?
C19A C20A N2A Hf1 -13.9(12) . . . . ?
C19A C20A N2A C26A 168.6(8) . . . . ?
C20A O4A C21A C22A 178.9(6) . . . . ?
C20A O4A C21A C26A 1.1(5) . . . . ?
O4A C20A N2A Hf1 173.2(3) . . . . ?
O4A C20A N2A C26A -4.3(7) . . . . ?
O4A C21A C22A C23A -175.3(4) . . . . ?
O4A C21A C26A C25A 175.3(3) . . . . ?
O4A C21A C26A N2A -3.6(4) . . . . ?
C21A C22A C23A C24A -0.4(8) . . . . ?
C21A C26A N2A Hf1 -172.6(2) . . . . ?
C21A C26A N2A C20A 4.9(5) . . . . ?
C22A C21A C26A C25A -2.6(6) . . . . ?
C22A C21A C26A N2A 178.5(4) . . . . ?
C22A C23A C24A C25A -0.9(7) . . . . ?
C23A C24A C25A C26A 0.5(6) . . . . ?
C24A C25A C26A C21A 1.2(5) . . . . ?
C24A C25A C26A N2A 179.7(3) . . . . ?
C25A C26A N2A Hf1 8.7(5) . . . . ?
C25A C26A N2A C20A -173.8(5) . . . . ?
C26A C21A C22A C23A 2.1(7) . . . . ?
N2A C20A O4A C21A 2.1(7) . . . . ?
O5A C27A C28A C29A -179.0(5) . . . . ?
O5A C27A C32A C31A 177.2(4) . . . . ?
O5A C27A C32A C33A 0.6(7) . . . . ?
C27A C28A C29A C30A 1.4(11) . . . . ?
C27A C32A C33A O6A 169.4(5) . . . . ?
C27A C32A C33A N3A -9.7(9) . . . . ?
C28A C27A C32A C31A -1.9(7) . . . . ?
C28A C27A C32A C33A -178.5(5) . . . . ?
C28A C29A C30A C31A -1.1(15) . . . . ?
C29A C30A C31A C32A -0.7(15) . . . . ?
C30A C31A C32A C27A 2.2(9) . . . . ?
C30A C31A C32A C33A 178.8(8) . . . . ?
C31A C32A C33A O6A -7.2(7) . . . . ?
C31A C32A C33A N3A 173.7(5) . . . . ?
C32A C27A C28A C29A 0.2(8) . . . . ?
C32A C33A O6A C34A -178.2(5) . . . . ?
C32A C33A N3A Hf1 -3.3(9) . . . . ?
C32A C33A N3A C39A 176.7(6) . . . . ?
C33A O6A C34A C35A 178.9(6) . . . . ?
C33A O6A C34A C39A 0.9(5) . . . . ?
O6A C33A N3A Hf1 177.7(3) . . . . ?
O6A C33A N3A C39A -2.4(7) . . . . ?
O6A C34A C35A C36A -179.7(4) . . . . ?
O6A C34A C39A C38A 177.3(5) . . . . ?
O6A C34A C39A N3A -2.3(4) . . . . ?
C34A C35A C36A C37A 3.5(7) . . . . ?
C34A C39A N3A Hf1 -177.3(2) . . . . ?
C34A C39A N3A C33A 2.7(5) . . . . ?
C35A C34A C39A C38A -0.8(8) . . . . ?
C35A C34A C39A N3A 179.6(4) . . . . ?
C35A C36A C37A C38A -2.3(8) . . . . ?
C36A C37A C38A C39A -0.6(10) . . . . ?
C37A C38A C39A C34A 2.1(10) . . . . ?
C37A C38A C39A N3A -178.5(4) . . . . ?
C38A C39A N3A Hf1 3.2(7) . . . . ?
C38A C39A N3A C33A -176.8(7) . . . . ?
C39A C34A C35A C36A -2.0(7) . . . . ?
N3A C33A O6A C34A 1.0(7) . . . . ?
O7A C40A C41A C42A -177.3(3) . . . . ?
O7A C40A C45A C44A 177.8(3) . . . . ?
O7A C40A C45A C46A -10.4(6) . . . . ?
C40A C41A C42A C43A -1.3(6) . . . . ?
C40A C45A C46A O8A -168.2(5) . . . . ?
C40A C45A C46A N4A 4.6(11) . . . . ?
C41A C40A C45A C44A -1.8(5) . . . . ?
C41A C40A C45A C46A 170.1(5) . . . . ?
C41A C42A C43A C44A -0.1(6) . . . . ?
C42A C43A C44A C45A 0.5(6) . . . . ?
C43A C44A C45A C40A 0.4(5) . . . . ?
C43A C44A C45A C46A -171.5(5) . . . . ?
C44A C45A C46A O8A 3.8(9) . . . . ?
C44A C45A C46A N4A 176.6(6) . . . . ?
C45A C40A C41A C42A 2.2(5) . . . . ?
C45A C46A O8A C47A 171.3(6) . . . . ?
C45A C46A N4A Hf1 22.4(11) . . . . ?
C45A C46A N4A C52A -168.4(7) . . . . ?
C46A O8A C47A C48A -179.9(6) . . . . ?
C46A O8A C47A C52A -1.1(5) . . . . ?
O8A C46A N4A Hf1 -164.3(3) . . . . ?
O8A C46A N4A C52A 4.9(8) . . . . ?
O8A C47A C48A C49A 174.6(4) . . . . ?
O8A C47A C52A C51A -173.9(3) . . . . ?
O8A C47A C52A N4A 4.1(3) . . . . ?
C47A C48A C49A C50A 0.3(7) . . . . ?
C47A C52A N4A Hf1 163.8(2) . . . . ?
C47A C52A N4A C46A -5.4(5) . . . . ?
C48A C47A C52A C51A 5.0(5) . . . . ?
C48A C47A C52A N4A -177.0(3) . . . . ?
C48A C49A C50A C51A 2.7(7) . . . . ?
C49A C50A C51A C52A -1.9(6) . . . . ?
C50A C51A C52A C47A -1.8(5) . . . . ?
C50A C51A C52A N4A -179.3(3) . . . . ?
C51A C52A N4A Hf1 -18.5(5) . . . . ?
C51A C52A N4A C46A 172.3(5) . . . . ?
C52A C47A C48A C49A -4.1(6) . . . . ?
N4A C46A O8A C47A -2.5(8) . . . . ?

_olex2_date_sample_data_collection 2016-12-09
_olex2_date_sample_submission    1480978800
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7A) = Uanis(C46A) = Uanis(C20A) = Uanis(C33A)
3. Others
 Fixed Sof: O1A(0.5) C1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5)
 H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) C7A(0.5) O2A(0.5) C8A(0.5) C9A(0.5)
 H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5)
 N1A(0.5) O3A(0.5) C14A(0.5) C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5)
 H17A(0.5) C18A(0.5) H18A(0.5) C19A(0.5) C20A(0.5) O4A(0.5) C21A(0.5) C22A(0.5)
 H22A(0.5) C23A(0.5) H23A(0.5) C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5)
 C26A(0.5) N2A(0.5) O5A(0.5) C27A(0.5) C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5)
 C30A(0.5) H30A(0.5) C31A(0.5) H31A(0.5) C32A(0.5) C33A(0.5) O6A(0.5) C34A(0.5)
 C35A(0.5) H35A(0.5) C36A(0.5) H36A(0.5) C37A(0.5) H37A(0.5) C38A(0.5)
 H38A(0.5) C39A(0.5) N3A(0.5) O7A(0.5) C40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5)
 H42A(0.5) C43A(0.5) H43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5) C46A(0.5) O8A(0.5)
 C47A(0.5) C48A(0.5) H48A(0.5) C49A(0.5) H49A(0.5) C50A(0.5) H50A(0.5)
 C51A(0.5) H51A(0.5) C52A(0.5) N4A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C9A(H9A), C10A(H10A), C11A(H11A),
 C12A(H12A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C22A(H22A),
 C23A(H23A), C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A),
 C31A(H31A), C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C41A(H41A),
 C42A(H42A), C43A(H43A), C44A(H44A), C48A(H48A), C49A(H49A), C50A(H50A),
 C51A(H51A)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.681

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
####################################################################### 
# 
# 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_compound6
_database_code_depnum_ccdc_archive 'CCDC 1816369'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;

_audit_creation_date             2016-10-06
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C50 H66 Hf N2 O6, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C50.50 H67 Cl Hf N2 O6'
_chemical_formula_weight         1012.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H67 Cl N2 Hf O6'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.62492(9)
_cell_length_b                   13.18535(10)
_cell_length_c                   17.81500(14)
_cell_angle_alpha                91.5475(6)
_cell_angle_beta                 91.2308(7)
_cell_angle_gamma                98.6382(7)
_cell_volume                     2465.73(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    93678
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.8970
_cell_measurement_theta_min      2.2290
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1042
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0336
0 0 -1 0.0336
1 0 -1 0.0965
-1 0 1 0.0965
0 -1 0 0.0974
0 1 0 0.0974

_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.067
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0002 -0.0001 0.9993 0.0269 0.0009 0.0294
-0.0002 0.0001 -0.9993 -0.0269 -0.0009 -0.0294
0.9991 0.0003 -0.9990 0.0233 -0.0142 -0.0725
-0.9991 -0.0003 0.9990 -0.0233 0.0142 0.0725
-0.0010 -0.9963 -0.0019 -0.0142 -0.0509 0.0122
0.0010 0.9963 0.0019 0.0142 0.0509 -0.0122

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            144424
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         1.563
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9424
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  96.00   1.00   10.00    --   25.97  77.00  60.00  100
  2  ω    -44.00  56.00   1.00   10.00    --   25.97 -77.00-150.00  100
  3  ω     -4.00  96.00   1.00   10.00    --   25.97  77.00 -30.00  100
  4  ω    -44.00  56.00   1.00   10.00    --   25.97 -77.00 120.00  100
  5  ω     -4.00  96.00   1.00   10.00    --   25.97  77.00-180.00  100
  6  ω      0.00  98.00   1.00   10.00    --   25.97  38.00-180.00   98
  7  ω     -4.00  96.00   1.00   10.00    --   25.97  77.00-120.00  100
  8  ω    -20.00  68.00   1.00   10.00    --   25.97 -99.00 -30.00   88
  9  ω    -20.00  68.00   1.00   10.00    --   25.97 -99.00  60.00   88
 10  ω    -99.00 -35.00   1.00   10.00    --  -23.50-178.00 -30.00   64
 11  ω    -92.00  -2.00   1.00   10.00    --  -23.50 -57.00  30.00   90
 12  ω    -20.00  68.00   1.00   10.00    --   25.97 -99.00 150.00   88
 13  ω      0.00  98.00   1.00   10.00    --   25.97  38.00 -30.00   98
 14  ω    -43.00  47.00   1.00   10.00    --   25.97 -57.00 -60.00   90
 15  ω    -47.00  99.00   1.00   10.00    --   25.97   0.00-180.00  146
 16  ω    -46.00  51.00   1.00   10.00    --   25.97 -38.00   0.00   97
 17  ω    -46.00  51.00   1.00   10.00    --   25.97 -38.00-150.00   97
 18  ω    -47.00  99.00   1.00   10.00    --   25.97   0.00-120.00  146
 19  ω    -47.00  99.00   1.00   10.00    --   25.97   0.00 -90.00  146
 20  ω    -47.00  99.00   1.00   10.00    --   25.97   0.00 -60.00  146
 21  ω    -47.00  99.00   1.00   10.00    --   25.97   0.00 -30.00  146
 22  ω    -47.00  57.00   1.00   10.00    --   25.97   0.00   0.00  104
 23  ω    -47.00  99.00   1.00   10.00    --   25.97   0.00-150.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0502222000
_diffrn_orient_matrix_UB_12      0.0141440000
_diffrn_orient_matrix_UB_13      0.0268782000
_diffrn_orient_matrix_UB_21      -0.0133566000
_diffrn_orient_matrix_UB_22      0.0511276000
_diffrn_orient_matrix_UB_23      0.0008882000
_diffrn_orient_matrix_UB_31      -0.0431496000
_diffrn_orient_matrix_UB_32      -0.0122200000
_diffrn_orient_matrix_UB_33      0.0293973000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13944
_reflns_number_total             14456
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         14456
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+1.9476P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0506
_refine_special_details          
;
 Disorder of CH2Cl2 near an center of inversion. One t-butylgroup is
 influenced by this disorder and shows the same occupation factor (0.5).
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.76739(2) 0.67751(2) 0.74426(2) 0.01161(2) Uani 1 1 d . . . . .
O1 O 0.74751(10) 0.80285(8) 0.68115(6) 0.0143(2) Uani 1 1 d . . . . .
O2 O 0.42317(11) 0.61752(8) 0.59114(6) 0.0144(2) Uani 1 1 d . . . . .
O3 O 0.77998(11) 0.52814(9) 0.76838(7) 0.0153(2) Uani 1 1 d . . . . .
O4 O 1.06685(11) 0.54784(9) 0.61172(6) 0.0159(2) Uani 1 1 d . . . . .
O5 O 0.91526(11) 0.73927(10) 0.80164(7) 0.0193(2) Uani 1 1 d . . . . .
O6 O 0.62890(11) 0.69175(9) 0.80867(7) 0.0174(2) Uani 1 1 d . . . . .
N1 N 0.61081(13) 0.61313(10) 0.65088(7) 0.0132(2) Uani 1 1 d . . . . .
N2 N 0.90373(13) 0.62407(10) 0.65194(7) 0.0138(2) Uani 1 1 d . . . . .
C1 C 0.64462(14) 0.84384(11) 0.66310(8) 0.0124(3) Uani 1 1 d . . . . .
C2 C 0.64511(14) 0.95185(11) 0.67121(8) 0.0125(3) Uani 1 1 d . . . . .
C3 C 0.53398(15) 0.98928(11) 0.65179(9) 0.0131(3) Uani 1 1 d . . . . .
H3 H 0.5337 1.0595 0.6576 0.016 Uiso 1 1 calc R . . . .
C4 C 0.42132(14) 0.92826(11) 0.62380(8) 0.0126(3) Uani 1 1 d . . . . .
C5 C 0.42254(14) 0.82408(11) 0.61551(9) 0.0135(3) Uani 1 1 d . . . . .
H5 H 0.3503 0.7815 0.5967 0.016 Uiso 1 1 calc R . . . .
C6 C 0.53239(14) 0.78146(11) 0.63534(9) 0.0126(3) Uani 1 1 d . . . . .
C7 C 0.52804(14) 0.67126(11) 0.62750(8) 0.0127(3) Uani 1 1 d . . . . .
C8 C 0.44362(15) 0.51660(11) 0.59046(9) 0.0139(3) Uani 1 1 d . . . . .
C9 C 0.36577(16) 0.43231(12) 0.55869(9) 0.0168(3) Uani 1 1 d . . . . .
H9 H 0.2878 0.4372 0.5355 0.020 Uiso 1 1 calc R . . . .
C10 C 0.41256(17) 0.33942(12) 0.56393(10) 0.0187(3) Uani 1 1 d . . . . .
H10 H 0.3648 0.2800 0.5432 0.022 Uiso 1 1 calc R . . . .
C11 C 0.52972(17) 0.33334(12) 0.59967(10) 0.0184(3) Uani 1 1 d . . . . .
H11 H 0.5579 0.2700 0.6016 0.022 Uiso 1 1 calc R . . . .
C12 C 0.60542(16) 0.41918(12) 0.63241(9) 0.0161(3) Uani 1 1 d . . . . .
H12 H 0.6826 0.4145 0.6567 0.019 Uiso 1 1 calc R . . . .
C13 C 0.55948(15) 0.51263(11) 0.62689(9) 0.0135(3) Uani 1 1 d . . . . .
C14 C 0.76364(15) 1.02325(12) 0.70210(9) 0.0148(3) Uani 1 1 d . . . . .
C15 C 0.79097(17) 0.99685(13) 0.78407(10) 0.0205(3) Uani 1 1 d . . . . .
H15A H 0.8655 1.0411 0.8032 0.031 Uiso 1 1 calc GR . . . .
H15B H 0.8050 0.9267 0.7859 0.031 Uiso 1 1 calc GR . . . .
H15C H 0.7195 1.0063 0.8141 0.031 Uiso 1 1 calc GR . . . .
C16 C 0.74436(17) 1.13640(12) 0.70231(11) 0.0210(3) Uani 1 1 d . . . . .
H16A H 0.6750 1.1461 0.7341 0.032 Uiso 1 1 calc GR . . . .
H16B H 0.7253 1.1551 0.6521 0.032 Uiso 1 1 calc GR . . . .
H16C H 0.8207 1.1787 0.7209 0.032 Uiso 1 1 calc GR . . . .
C17 C 0.87959(16) 1.01285(13) 0.65362(10) 0.0199(3) Uani 1 1 d . . . . .
H17A H 0.9523 1.0587 0.6732 0.030 Uiso 1 1 calc GR . . . .
H17B H 0.8616 1.0298 0.6028 0.030 Uiso 1 1 calc GR . . . .
H17C H 0.8971 0.9435 0.6547 0.030 Uiso 1 1 calc GR . . . .
C18 C 0.30665(15) 0.98002(11) 0.60213(9) 0.0140(3) Uani 1 1 d . . . . .
C19 C 0.27332(17) 1.04807(13) 0.66764(10) 0.0205(3) Uani 1 1 d . . . . .
H19A H 0.2550 1.0071 0.7109 0.031 Uiso 1 1 calc GR . . . .
H19B H 0.2000 1.0788 0.6539 0.031 Uiso 1 1 calc GR . . . .
H19C H 0.3440 1.1010 0.6791 0.031 Uiso 1 1 calc GR . . . .
C20 C 0.34087(18) 1.04711(14) 0.53401(10) 0.0220(3) Uani 1 1 d . . . . .
H20A H 0.4140 1.0973 0.5465 0.033 Uiso 1 1 calc GR . . . .
H20B H 0.2703 1.0812 0.5206 0.033 Uiso 1 1 calc GR . . . .
H20C H 0.3597 1.0047 0.4924 0.033 Uiso 1 1 calc GR . . . .
C21 C 0.18873(16) 0.90198(13) 0.58096(12) 0.0243(4) Uani 1 1 d . . . . .
H21A H 0.2063 0.8611 0.5381 0.036 Uiso 1 1 calc GR . . . .
H21B H 0.1188 0.9376 0.5690 0.036 Uiso 1 1 calc GR . . . .
H21C H 0.1671 0.8583 0.6225 0.036 Uiso 1 1 calc GR . . . .
C22 C 0.87250(14) 0.47186(11) 0.77519(8) 0.0129(3) Uani 1 1 d . . . . .
C23 C 0.86824(15) 0.39646(12) 0.83132(9) 0.0135(3) Uani 1 1 d . . . . .
C24 C 0.97234(15) 0.34508(12) 0.83851(9) 0.0146(3) Uani 1 1 d . . . . .
H24 H 0.9711 0.2975 0.8762 0.017 Uiso 1 1 calc R . . . .
C25 C 1.07959(15) 0.35973(11) 0.79301(9) 0.0137(3) Uani 1 1 d . . . . .
C26 C 1.07949(15) 0.42888(12) 0.73615(9) 0.0144(3) Uani 1 1 d . . . . .
H26 H 1.1474 0.4387 0.7037 0.017 Uiso 1 1 calc R . . . .
C27 C 0.97700(15) 0.48486(11) 0.72684(9) 0.0136(3) Uani 1 1 d . . . . .
C28 C 0.97840(15) 0.55508(12) 0.66579(9) 0.0134(3) Uani 1 1 d . . . . .
C29 C 1.04162(16) 0.61565(12) 0.55780(9) 0.0152(3) Uani 1 1 d . . . . .
C30 C 1.10011(17) 0.63257(13) 0.48974(10) 0.0194(3) Uani 1 1 d . . . . .
H30 H 1.1680 0.6000 0.4754 0.023 Uiso 1 1 calc R . . . .
C31 C 1.05032(18) 0.70185(13) 0.44418(9) 0.0201(3) Uani 1 1 d . . . . .
H31 H 1.0847 0.7152 0.3973 0.024 Uiso 1 1 calc R . . . .
C32 C 0.94965(17) 0.75204(13) 0.46730(9) 0.0190(3) Uani 1 1 d . . . . .
H32 H 0.9194 0.7982 0.4354 0.023 Uiso 1 1 calc R . . . .
C33 C 0.89377(16) 0.73461(12) 0.53663(9) 0.0169(3) Uani 1 1 d . . . . .
H33 H 0.8279 0.7688 0.5521 0.020 Uiso 1 1 calc R . . . .
C34 C 0.94097(15) 0.66358(12) 0.58185(9) 0.0137(3) Uani 1 1 d . . . . .
C35 C 0.75691(16) 0.37808(13) 0.88520(9) 0.0166(3) Uani 1 1 d . . . . .
C36 C 0.62728(16) 0.36104(14) 0.84305(10) 0.0211(3) Uani 1 1 d . . . . .
H36A H 0.6154 0.4224 0.8177 0.032 Uiso 1 1 calc GR . . . .
H36B H 0.5606 0.3447 0.8782 0.032 Uiso 1 1 calc GR . . . .
H36C H 0.6249 0.3054 0.8069 0.032 Uiso 1 1 calc GR . . . .
C37 C 0.7656(2) 0.47147(15) 0.93964(11) 0.0276(4) Uani 1 1 d . . . . .
H37A H 0.8437 0.4780 0.9687 0.041 Uiso 1 1 calc GR . . . .
H37B H 0.6948 0.4623 0.9727 0.041 Uiso 1 1 calc GR . . . .
H37C H 0.7636 0.5324 0.9116 0.041 Uiso 1 1 calc GR . . . .
C38 C 0.76239(18) 0.28182(15) 0.93135(11) 0.0264(4) Uani 1 1 d . . . . .
H38A H 0.7613 0.2233 0.8980 0.040 Uiso 1 1 calc GR . . . .
H38B H 0.6901 0.2710 0.9631 0.040 Uiso 1 1 calc GR . . . .
H38C H 0.8392 0.2911 0.9617 0.040 Uiso 1 1 calc GR . . . .
C39 C 1.19093(15) 0.30184(12) 0.81034(9) 0.0141(3) Uani 1 1 d . . . . .
C40 C 1.25137(17) 0.34102(14) 0.88704(10) 0.0210(3) Uani 1 1 d . . . . .
H40A H 1.2814 0.4133 0.8852 0.031 Uiso 1 1 calc GR . . . .
H40B H 1.3215 0.3054 0.8985 0.031 Uiso 1 1 calc GR . . . .
H40C H 1.1889 0.3288 0.9252 0.031 Uiso 1 1 calc GR . . . .
C41 C 1.14195(17) 0.18620(13) 0.81467(11) 0.0217(3) Uani 1 1 d . . . . .
H41A H 1.0852 0.1746 0.8558 0.033 Uiso 1 1 calc GR . . . .
H41B H 1.2127 0.1498 0.8223 0.033 Uiso 1 1 calc GR . . . .
H41C H 1.0974 0.1621 0.7686 0.033 Uiso 1 1 calc GR . . . .
C42 C 1.29266(16) 0.31721(13) 0.75062(10) 0.0193(3) Uani 1 1 d . . . . .
H42A H 1.2555 0.2932 0.7026 0.029 Uiso 1 1 calc GR . . . .
H42B H 1.3601 0.2793 0.7632 0.029 Uiso 1 1 calc GR . . . .
H42C H 1.3263 0.3888 0.7485 0.029 Uiso 1 1 calc GR . . . .
C43 C 1.01874(16) 0.77499(14) 0.85105(10) 0.0199(3) Uani 1 1 d . . . . .
C44 C 1.1046(2) 0.8605(2) 0.81261(15) 0.0442(6) Uani 1 1 d . . . . .
H44A H 1.1337 0.8342 0.7664 0.066 Uiso 1 1 calc GR . . . .
H44B H 1.1765 0.8857 0.8450 0.066 Uiso 1 1 calc GR . . . .
H44C H 1.0575 0.9155 0.8023 0.066 Uiso 1 1 calc GR . . . .
C45 C 0.9672(2) 0.8154(2) 0.92302(12) 0.0372(5) Uani 1 1 d . . . . .
H45A H 0.9218 0.8711 0.9118 0.056 Uiso 1 1 calc GR . . . .
H45B H 1.0366 0.8391 0.9576 0.056 Uiso 1 1 calc GR . . . .
H45C H 0.9105 0.7613 0.9452 0.056 Uiso 1 1 calc GR . . . .
C46 C 1.0903(2) 0.68583(17) 0.86704(13) 0.0330(5) Uani 1 1 d . . . . .
H46A H 1.0349 0.6328 0.8910 0.049 Uiso 1 1 calc GR . . . .
H46B H 1.1627 0.7093 0.8995 0.049 Uiso 1 1 calc GR . . . .
H46C H 1.1186 0.6592 0.8207 0.049 Uiso 1 1 calc GR . . . .
C47 C 0.52196(18) 0.69872(16) 0.85302(12) 0.0276(4) Uani 1 1 d . . . . .
C48 C 0.4847(16) 0.7994(13) 0.8519(7) 0.026(2) Uani 0.5 1 d . . P A 1
H48A H 0.5500 0.8483 0.8762 0.039 Uiso 0.5 1 calc GR . P A 1
H48B H 0.4064 0.7988 0.8779 0.039 Uiso 0.5 1 calc GR . P A 1
H48C H 0.4729 0.8182 0.8008 0.039 Uiso 0.5 1 calc GR . P A 1
C48B C 0.4712(15) 0.8003(13) 0.8344(7) 0.026(2) Uani 0.5 1 d . . P A 2
H48D H 0.5400 0.8566 0.8386 0.039 Uiso 0.5 1 calc GR . P A 2
H48E H 0.4065 0.8117 0.8691 0.039 Uiso 0.5 1 calc GR . P A 2
H48F H 0.4359 0.7953 0.7842 0.039 Uiso 0.5 1 calc GR . P A 2
C49 C 0.5391(5) 0.6564(4) 0.9269(2) 0.0293(9) Uani 0.5 1 d . . P A 1
H49A H 0.5495 0.5855 0.9211 0.044 Uiso 0.5 1 calc GR . P A 1
H49B H 0.4656 0.6617 0.9564 0.044 Uiso 0.5 1 calc GR . P A 1
H49C H 0.6134 0.6941 0.9518 0.044 Uiso 0.5 1 calc GR . P A 1
C49B C 0.5865(6) 0.7265(7) 0.9384(3) 0.064(2) Uani 0.5 1 d . . P A 2
H49D H 0.6388 0.6759 0.9514 0.096 Uiso 0.5 1 calc GR . P A 2
H49E H 0.5202 0.7266 0.9741 0.096 Uiso 0.5 1 calc GR . P A 2
H49F H 0.6378 0.7930 0.9388 0.096 Uiso 0.5 1 calc GR . P A 2
C50 C 0.4086(4) 0.6191(4) 0.8077(3) 0.0294(9) Uani 0.5 1 d . . P A 1
H50A H 0.3912 0.6463 0.7597 0.044 Uiso 0.5 1 calc GR . P A 1
H50B H 0.3327 0.6112 0.8366 0.044 Uiso 0.5 1 calc GR . P A 1
H50C H 0.4361 0.5535 0.8004 0.044 Uiso 0.5 1 calc GR . P A 1
C50B C 0.4335(6) 0.6097(4) 0.8535(5) 0.059(2) Uani 0.5 1 d . . P A 2
H50D H 0.3928 0.5974 0.8048 0.089 Uiso 0.5 1 calc GR . P A 2
H50E H 0.3706 0.6174 0.8903 0.089 Uiso 0.5 1 calc GR . P A 2
H50F H 0.4759 0.5527 0.8658 0.089 Uiso 0.5 1 calc GR . P A 2
Cl1 Cl 0.69168(17) 1.00638(17) 1.00763(9) 0.0766(6) Uani 0.5 1 d . . P B -1
Cl2 Cl 0.55076(11) 0.93238(8) 1.13899(7) 0.0373(2) Uani 0.5 1 d . . P B -1
C51 C 0.5937(8) 0.9038(4) 1.0506(4) 0.069(2) Uani 0.5 1 d . . P B -1
H51A H 0.5172 0.8842 1.0196 0.082 Uiso 0.5 1 calc R . P B -1
H51B H 0.6388 0.8452 1.0521 0.082 Uiso 0.5 1 calc R . P B -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1 2.0579(11) . ?
Hf1 O3 2.0504(11) . ?
Hf1 O5 1.9178(12) . ?
Hf1 O6 1.9134(12) . ?
Hf1 N1 2.3742(13) . ?
Hf1 N2 2.3762(14) . ?
O1 C1 1.3275(18) . ?
O2 C7 1.3676(18) . ?
O2 C8 1.3799(17) . ?
O3 C22 1.3231(18) . ?
O4 C28 1.3715(19) . ?
O4 C29 1.3789(18) . ?
O5 C43 1.4092(19) . ?
O6 C47 1.411(2) . ?
N1 C7 1.3184(19) . ?
N1 C13 1.4066(19) . ?
N2 C28 1.3185(19) . ?
N2 C34 1.408(2) . ?
C1 C2 1.427(2) . ?
C1 C6 1.415(2) . ?
C2 C3 1.387(2) . ?
C2 C14 1.537(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.411(2) . ?
C4 C5 1.380(2) . ?
C4 C18 1.531(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.412(2) . ?
C6 C7 1.450(2) . ?
C8 C9 1.382(2) . ?
C8 C13 1.388(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.394(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.400(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.392(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.397(2) . ?
C14 C15 1.542(2) . ?
C14 C16 1.536(2) . ?
C14 C17 1.540(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.533(2) . ?
C18 C20 1.539(2) . ?
C18 C21 1.530(2) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.426(2) . ?
C22 C27 1.413(2) . ?
C23 C24 1.387(2) . ?
C23 C35 1.534(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.405(2) . ?
C25 C26 1.381(2) . ?
C25 C39 1.531(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.414(2) . ?
C27 C28 1.446(2) . ?
C29 C30 1.383(2) . ?
C29 C34 1.391(2) . ?
C30 H30 0.9300 . ?
C30 C31 1.393(2) . ?
C31 H31 0.9300 . ?
C31 C32 1.403(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.392(2) . ?
C33 H33 0.9300 . ?
C33 C34 1.394(2) . ?
C35 C36 1.538(2) . ?
C35 C37 1.537(2) . ?
C35 C38 1.538(2) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.540(2) . ?
C39 C41 1.540(2) . ?
C39 C42 1.529(2) . ?
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 C44 1.527(3) . ?
C43 C45 1.519(3) . ?
C43 C46 1.523(3) . ?
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 C48 1.442(16) . ?
C47 C48B 1.558(15) . ?
C47 C49 1.463(4) . ?
C47 C49B 1.663(6) . ?
C47 C50 1.655(5) . ?
C47 C50B 1.390(6) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C48B H48D 0.9600 . ?
C48B H48E 0.9600 . ?
C48B H48F 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C49B H49D 0.9600 . ?
C49B H49E 0.9600 . ?
C49B H49F 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C50B H50D 0.9600 . ?
C50B H50E 0.9600 . ?
C50B H50F 0.9600 . ?
Cl1 C51 1.779(8) . ?
Cl2 C51 1.697(7) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?

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 N1 75.71(4) . . ?
O1 Hf1 N2 89.11(4) . . ?
O3 Hf1 O1 158.87(5) . . ?
O3 Hf1 N1 87.63(4) . . ?
O3 Hf1 N2 75.38(4) . . ?
O5 Hf1 O1 96.96(5) . . ?
O5 Hf1 O3 96.99(5) . . ?
O5 Hf1 N1 167.72(5) . . ?
O5 Hf1 N2 88.88(5) . . ?
O6 Hf1 O1 95.45(5) . . ?
O6 Hf1 O3 96.49(5) . . ?
O6 Hf1 O5 103.99(5) . . ?
O6 Hf1 N1 86.69(5) . . ?
O6 Hf1 N2 165.67(5) . . ?
N1 Hf1 N2 81.27(5) . . ?
C1 O1 Hf1 130.58(10) . . ?
C7 O2 C8 105.00(11) . . ?
C22 O3 Hf1 136.16(10) . . ?
C28 O4 C29 105.10(12) . . ?
C43 O5 Hf1 172.39(12) . . ?
C47 O6 Hf1 176.61(13) . . ?
C7 N1 Hf1 119.96(10) . . ?
C7 N1 C13 105.30(12) . . ?
C13 N1 Hf1 132.09(10) . . ?
C28 N2 Hf1 121.81(10) . . ?
C28 N2 C34 105.34(13) . . ?
C34 N2 Hf1 132.05(10) . . ?
O1 C1 C2 120.61(13) . . ?
O1 C1 C6 120.75(13) . . ?
C6 C1 C2 118.64(13) . . ?
C1 C2 C14 120.97(13) . . ?
C3 C2 C1 117.50(13) . . ?
C3 C2 C14 121.52(13) . . ?
C2 C3 H3 117.7 . . ?
C2 C3 C4 124.62(14) . . ?
C4 C3 H3 117.7 . . ?
C3 C4 C18 119.23(13) . . ?
C5 C4 C3 117.28(14) . . ?
C5 C4 C18 123.46(13) . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.59(14) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C7 120.05(13) . . ?
C5 C6 C1 121.35(13) . . ?
C5 C6 C7 118.60(13) . . ?
O2 C7 C6 116.72(13) . . ?
N1 C7 O2 113.69(13) . . ?
N1 C7 C6 129.59(14) . . ?
O2 C8 C9 127.42(14) . . ?
O2 C8 C13 108.19(13) . . ?
C9 C8 C13 124.39(14) . . ?
C8 C9 H9 122.4 . . ?
C8 C9 C10 115.19(15) . . ?
C10 C9 H9 122.4 . . ?
C9 C10 H10 119.2 . . ?
C9 C10 C11 121.63(15) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 H11 119.0 . . ?
C12 C11 C10 122.07(14) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 H12 121.7 . . ?
C11 C12 C13 116.58(14) . . ?
C13 C12 H12 121.7 . . ?
C8 C13 N1 107.81(13) . . ?
C8 C13 C12 120.13(14) . . ?
C12 C13 N1 132.04(14) . . ?
C2 C14 C15 109.51(13) . . ?
C2 C14 C17 110.57(13) . . ?
C16 C14 C2 111.78(13) . . ?
C16 C14 C15 107.23(13) . . ?
C16 C14 C17 107.45(14) . . ?
C17 C14 C15 110.23(13) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 C18 C19 110.18(13) . . ?
C4 C18 C20 108.74(13) . . ?
C19 C18 C20 109.06(13) . . ?
C21 C18 C4 112.23(13) . . ?
C21 C18 C19 108.27(14) . . ?
C21 C18 C20 108.31(14) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C22 C23 120.55(14) . . ?
O3 C22 C27 120.74(13) . . ?
C27 C22 C23 118.71(13) . . ?
C22 C23 C35 121.25(13) . . ?
C24 C23 C22 117.41(14) . . ?
C24 C23 C35 121.21(14) . . ?
C23 C24 H24 117.6 . . ?
C23 C24 C25 124.74(14) . . ?
C25 C24 H24 117.6 . . ?
C24 C25 C39 118.93(13) . . ?
C26 C25 C24 117.29(14) . . ?
C26 C25 C39 123.74(14) . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.54(15) . . ?
C27 C26 H26 119.7 . . ?
C22 C27 C26 121.14(14) . . ?
C22 C27 C28 119.63(13) . . ?
C26 C27 C28 119.21(14) . . ?
O4 C28 C27 116.55(13) . . ?
N2 C28 O4 113.57(13) . . ?
N2 C28 C27 129.83(14) . . ?
O4 C29 C30 127.62(15) . . ?
O4 C29 C34 108.10(13) . . ?
C30 C29 C34 124.23(15) . . ?
C29 C30 H30 122.3 . . ?
C29 C30 C31 115.31(16) . . ?
C31 C30 H30 122.3 . . ?
C30 C31 H31 119.2 . . ?
C30 C31 C32 121.67(16) . . ?
C32 C31 H31 119.2 . . ?
C31 C32 H32 119.1 . . ?
C33 C32 C31 121.76(15) . . ?
C33 C32 H32 119.1 . . ?
C32 C33 H33 121.5 . . ?
C32 C33 C34 116.96(15) . . ?
C34 C33 H33 121.5 . . ?
C29 C34 N2 107.84(13) . . ?
C29 C34 C33 120.03(15) . . ?
C33 C34 N2 132.10(15) . . ?
C23 C35 C36 111.97(13) . . ?
C23 C35 C37 108.36(14) . . ?
C23 C35 C38 111.43(13) . . ?
C36 C35 C38 106.41(14) . . ?
C37 C35 C36 110.12(15) . . ?
C37 C35 C38 108.50(15) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
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 . . ?
C25 C39 C40 108.66(13) . . ?
C25 C39 C41 109.80(13) . . ?
C40 C39 C41 108.69(14) . . ?
C42 C39 C25 112.07(13) . . ?
C42 C39 C40 109.04(14) . . ?
C42 C39 C41 108.52(13) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C43 C44 107.89(15) . . ?
O5 C43 C45 108.49(15) . . ?
O5 C43 C46 108.38(15) . . ?
C45 C43 C44 110.69(19) . . ?
C45 C43 C46 110.65(17) . . ?
C46 C43 C44 110.64(18) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O6 C47 C48 112.1(7) . . ?
O6 C47 C48B 108.1(6) . . ?
O6 C47 C49 110.5(2) . . ?
O6 C47 C49B 102.9(2) . . ?
O6 C47 C50 102.3(2) . . ?
C48 C47 C49 116.6(6) . . ?
C48 C47 C50 107.1(6) . . ?
C48B C47 C49B 101.6(5) . . ?
C49 C47 C50 107.0(3) . . ?
C50B C47 O6 114.8(3) . . ?
C50B C47 C48B 117.3(7) . . ?
C50B C47 C49B 110.5(5) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C48B H48D 109.5 . . ?
C47 C48B H48E 109.5 . . ?
C47 C48B H48F 109.5 . . ?
H48D C48B H48E 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C49B H49D 109.5 . . ?
C47 C49B H49E 109.5 . . ?
C47 C49B H49F 109.5 . . ?
H49D C49B H49E 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C50B H50D 109.5 . . ?
C47 C50B H50E 109.5 . . ?
C47 C50B H50F 109.5 . . ?
H50D C50B H50E 109.5 . . ?
H50D C50B H50F 109.5 . . ?
H50E C50B H50F 109.5 . . ?
Cl1 C51 H51A 108.7 . . ?
Cl1 C51 H51B 108.7 . . ?
Cl2 C51 Cl1 114.0(3) . . ?
Cl2 C51 H51A 108.7 . . ?
Cl2 C51 H51B 108.7 . . ?
H51A C51 H51B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hf1 O1 C1 C2 132.60(13) . . . . ?
Hf1 O1 C1 C6 -47.5(2) . . . . ?
Hf1 O3 C22 C23 142.26(13) . . . . ?
Hf1 O3 C22 C27 -38.1(2) . . . . ?
Hf1 N1 C7 O2 -162.21(10) . . . . ?
Hf1 N1 C7 C6 17.3(2) . . . . ?
Hf1 N1 C13 C8 159.75(11) . . . . ?
Hf1 N1 C13 C12 -21.9(3) . . . . ?
Hf1 N2 C28 O4 -168.42(9) . . . . ?
Hf1 N2 C28 C27 14.3(2) . . . . ?
Hf1 N2 C34 C29 168.17(11) . . . . ?
Hf1 N2 C34 C33 -13.8(3) . . . . ?
O1 C1 C2 C3 -179.54(14) . . . . ?
O1 C1 C2 C14 -1.0(2) . . . . ?
O1 C1 C6 C5 -179.62(14) . . . . ?
O1 C1 C6 C7 1.0(2) . . . . ?
O2 C8 C9 C10 177.63(16) . . . . ?
O2 C8 C13 N1 0.41(18) . . . . ?
O2 C8 C13 C12 -178.20(14) . . . . ?
O3 C22 C23 C24 -175.83(14) . . . . ?
O3 C22 C23 C35 0.1(2) . . . . ?
O3 C22 C27 C26 176.69(14) . . . . ?
O3 C22 C27 C28 -4.5(2) . . . . ?
O4 C29 C30 C31 176.50(15) . . . . ?
O4 C29 C34 N2 -0.09(17) . . . . ?
O4 C29 C34 C33 -178.44(14) . . . . ?
C1 C2 C3 C4 -0.8(2) . . . . ?
C1 C2 C14 C15 -64.01(19) . . . . ?
C1 C2 C14 C16 177.30(15) . . . . ?
C1 C2 C14 C17 57.65(19) . . . . ?
C1 C6 C7 O2 -171.53(14) . . . . ?
C1 C6 C7 N1 9.0(3) . . . . ?
C2 C1 C6 C5 0.3(2) . . . . ?
C2 C1 C6 C7 -179.06(14) . . . . ?
C2 C3 C4 C5 0.2(2) . . . . ?
C2 C3 C4 C18 -178.03(15) . . . . ?
C3 C2 C14 C15 114.51(16) . . . . ?
C3 C2 C14 C16 -4.2(2) . . . . ?
C3 C2 C14 C17 -123.83(16) . . . . ?
C3 C4 C5 C6 0.7(2) . . . . ?
C3 C4 C18 C19 -53.16(19) . . . . ?
C3 C4 C18 C20 66.31(18) . . . . ?
C3 C4 C18 C21 -173.89(15) . . . . ?
C4 C5 C6 C1 -0.9(2) . . . . ?
C4 C5 C6 C7 178.40(15) . . . . ?
C5 C4 C18 C19 128.76(16) . . . . ?
C5 C4 C18 C20 -111.77(17) . . . . ?
C5 C4 C18 C21 8.0(2) . . . . ?
C5 C6 C7 O2 9.1(2) . . . . ?
C5 C6 C7 N1 -170.37(16) . . . . ?
C6 C1 C2 C3 0.6(2) . . . . ?
C6 C1 C2 C14 179.15(14) . . . . ?
C7 O2 C8 C9 -178.61(16) . . . . ?
C7 O2 C8 C13 0.46(17) . . . . ?
C7 N1 C13 C8 -1.14(17) . . . . ?
C7 N1 C13 C12 177.25(18) . . . . ?
C8 O2 C7 N1 -1.26(18) . . . . ?
C8 O2 C7 C6 179.16(14) . . . . ?
C8 C9 C10 C11 0.6(3) . . . . ?
C9 C8 C13 N1 179.51(15) . . . . ?
C9 C8 C13 C12 0.9(3) . . . . ?
C9 C10 C11 C12 0.5(3) . . . . ?
C10 C11 C12 C13 -0.9(3) . . . . ?
C11 C12 C13 N1 -177.96(16) . . . . ?
C11 C12 C13 C8 0.3(2) . . . . ?
C13 N1 C7 O2 1.51(18) . . . . ?
C13 N1 C7 C6 -178.99(16) . . . . ?
C13 C8 C9 C10 -1.3(3) . . . . ?
C14 C2 C3 C4 -179.39(15) . . . . ?
C18 C4 C5 C6 178.83(15) . . . . ?
C22 C23 C24 C25 -2.1(2) . . . . ?
C22 C23 C35 C36 51.5(2) . . . . ?
C22 C23 C35 C37 -70.19(19) . . . . ?
C22 C23 C35 C38 170.51(15) . . . . ?
C22 C27 C28 O4 -166.16(14) . . . . ?
C22 C27 C28 N2 11.1(3) . . . . ?
C23 C22 C27 C26 -3.6(2) . . . . ?
C23 C22 C27 C28 175.15(14) . . . . ?
C23 C24 C25 C26 -1.4(2) . . . . ?
C23 C24 C25 C39 176.59(14) . . . . ?
C24 C23 C35 C36 -132.75(16) . . . . ?
C24 C23 C35 C37 105.60(17) . . . . ?
C24 C23 C35 C38 -13.7(2) . . . . ?
C24 C25 C26 C27 2.4(2) . . . . ?
C24 C25 C39 C40 -65.78(18) . . . . ?
C24 C25 C39 C41 52.97(19) . . . . ?
C24 C25 C39 C42 173.65(14) . . . . ?
C25 C26 C27 C22 0.1(2) . . . . ?
C25 C26 C27 C28 -178.69(14) . . . . ?
C26 C25 C39 C40 112.06(17) . . . . ?
C26 C25 C39 C41 -129.19(16) . . . . ?
C26 C25 C39 C42 -8.5(2) . . . . ?
C26 C27 C28 O4 12.6(2) . . . . ?
C26 C27 C28 N2 -170.13(16) . . . . ?
C27 C22 C23 C24 4.5(2) . . . . ?
C27 C22 C23 C35 -179.57(14) . . . . ?
C28 O4 C29 C30 -176.12(16) . . . . ?
C28 O4 C29 C34 1.49(16) . . . . ?
C28 N2 C34 C29 -1.40(17) . . . . ?
C28 N2 C34 C33 176.67(17) . . . . ?
C29 O4 C28 N2 -2.54(17) . . . . ?
C29 O4 C28 C27 175.13(13) . . . . ?
C29 C30 C31 C32 1.3(2) . . . . ?
C30 C29 C34 N2 177.62(15) . . . . ?
C30 C29 C34 C33 -0.7(2) . . . . ?
C30 C31 C32 C33 -0.5(3) . . . . ?
C31 C32 C33 C34 -1.0(2) . . . . ?
C32 C33 C34 N2 -176.30(16) . . . . ?
C32 C33 C34 C29 1.6(2) . . . . ?
C34 N2 C28 O4 2.47(17) . . . . ?
C34 N2 C28 C27 -174.82(15) . . . . ?
C34 C29 C30 C31 -0.8(2) . . . . ?
C35 C23 C24 C25 -178.03(15) . . . . ?
C39 C25 C26 C27 -175.50(14) . . . . ?

_olex2_date_sample_data_collection 2016-09-30
_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. Others
 Fixed Sof: C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C48B(0.5) H48D(0.5)
 H48E(0.5) H48F(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C49B(0.5) H49D(0.5)
 H49E(0.5) H49F(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C50B(0.5) H50D(0.5)
 H50E(0.5) H50F(0.5) Cl1(0.5) Cl2(0.5) C51(0.5) H51A(0.5) H51B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C33(H33)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C48B(H48D,H48E,H48F), C49(H49A,H49B,H49C),
 C49B(H49D,H49E,H49F), C50(H50A,H50B,H50C), C50B(H50D,H50E,H50F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.792

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-3
