# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 1419051'
_audit_update_record             
;
2015-08-17 deposited with the CCDC.
2016-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H42 N2 O2 Zr'
_chemical_formula_weight         770.06

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   15.1215(11)
_cell_length_b                   9.6375(7)
_cell_length_c                   26.4463(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.815(2)
_cell_angle_gamma                90.00
_cell_volume                     3818.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23308
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.05
_reflns_number_total             7530
_reflns_number_gt                4365
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0373P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    contra
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7530
_refine_ls_number_parameters     478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1171
_refine_ls_wR_factor_gt          0.0945
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.90301(2) 0.27098(4) 0.583793(13) 0.03303(13) Uani 1 1 d . . .
O1 O 0.96286(16) 0.3552(3) 0.65088(9) 0.0391(7) Uani 1 1 d . . .
C15A C 0.8875(2) 0.2332(4) 0.44759(13) 0.0329(9) Uani 1 1 d . . .
N1A N 0.99994(18) 0.2298(3) 0.52395(10) 0.0324(7) Uani 1 1 d . . .
N1 N 0.7890(2) 0.2656(3) 0.63185(11) 0.0411(8) Uani 1 1 d . . .
C8 C 0.7022(3) 0.2179(5) 0.60988(14) 0.0423(10) Uani 1 1 d . . .
C14A C 0.9756(2) 0.2241(4) 0.47445(13) 0.0341(9) Uani 1 1 d . . .
H14C H 1.0212 0.2128 0.4545 0.041 Uiso 1 1 calc R . .
C8A C 1.0938(2) 0.2201(4) 0.54000(13) 0.0345(9) Uani 1 1 d . . .
C19A C 0.8772(2) 0.2453(4) 0.39013(13) 0.0432(11) Uani 1 1 d . . .
H19C H 0.8728 0.3424 0.3805 0.052 Uiso 1 1 calc R . .
H19D H 0.9295 0.2068 0.3777 0.052 Uiso 1 1 calc R . .
C16A C 0.8125(2) 0.2322(4) 0.47115(13) 0.0359(9) Uani 1 1 d . . .
C18A C 0.6492(3) 0.2719(5) 0.46452(16) 0.0526(12) Uani 1 1 d . . .
H18C H 0.6555 0.2905 0.4993 0.063 Uiso 1 1 calc R . .
C17A C 0.7232(2) 0.2399(4) 0.44129(14) 0.0400(10) Uani 1 1 d . . .
C12 C 0.5453(3) 0.2572(6) 0.58583(17) 0.0647(14) Uani 1 1 d . . .
H12A H 0.4960 0.3155 0.5844 0.078 Uiso 1 1 calc R . .
C23A C 0.5571(3) 0.2478(7) 0.38462(19) 0.092(2) Uani 1 1 d . . .
H23C H 0.5009 0.2519 0.3653 0.110 Uiso 1 1 calc R . .
C2A C 0.8529(3) 0.5630(4) 0.57052(15) 0.0406(10) Uani 1 1 d . . .
C16 C 0.9464(3) 0.3932(4) 0.69547(14) 0.0409(10) Uani 1 1 d . . .
C21A C 0.7144(3) 0.2101(5) 0.38879(15) 0.0504(12) Uani 1 1 d . . .
C24A C 0.5658(3) 0.2762(6) 0.43592(18) 0.0790(17) Uani 1 1 d . . .
H24C H 0.5158 0.2982 0.4513 0.095 Uiso 1 1 calc R . .
C3A C 0.7694(3) 0.5571(4) 0.54086(17) 0.0536(12) Uani 1 1 d . . .
H3C H 0.7638 0.5122 0.5095 0.064 Uiso 1 1 calc R . .
C13 C 0.6281(3) 0.3035(5) 0.60777(15) 0.0527(12) Uani 1 1 d . . .
H13A H 0.6342 0.3927 0.6212 0.063 Uiso 1 1 calc R . .
C1A C 0.9295(2) 0.4907(4) 0.55462(15) 0.0407(10) Uani 1 1 d . . .
H1C H 0.9856 0.5283 0.5711 0.049 Uiso 1 1 calc R . .
H1D H 0.9284 0.4927 0.5179 0.049 Uiso 1 1 calc R . .
C17 C 1.0173(3) 0.4642(5) 0.72883(15) 0.0464(11) Uani 1 1 d . . .
C13A C 1.1327(3) 0.3099(5) 0.57739(15) 0.0511(12) Uani 1 1 d . . .
H13C H 1.0975 0.3743 0.5916 0.061 Uiso 1 1 calc R . .
C21 C 0.9968(3) 0.5421(6) 0.76972(16) 0.0642(14) Uani 1 1 d . . .
C9 C 0.6919(3) 0.0865(5) 0.58965(15) 0.0523(12) Uani 1 1 d . . .
H9A H 0.7413 0.0286 0.5905 0.063 Uiso 1 1 calc R . .
C2 C 0.9778(3) 0.0402(4) 0.66933(16) 0.0479(11) Uani 1 1 d . . .
C22A C 0.6298(3) 0.2133(6) 0.36148(17) 0.0752(16) Uani 1 1 d . . .
H22C H 0.6222 0.1917 0.3269 0.090 Uiso 1 1 calc R . .
C1 C 0.9672(3) 0.0628(4) 0.61319(14) 0.0514(12) Uani 1 1 d . . .
H1A H 0.9311 -0.0122 0.5969 0.062 Uiso 1 1 calc R . .
H1B H 1.0256 0.0562 0.6021 0.062 Uiso 1 1 calc R . .
C15 C 0.8639(3) 0.3709(5) 0.71100(15) 0.0520(12) Uani 1 1 d . . .
C18 C 1.1043(3) 0.4625(5) 0.71762(16) 0.0635(14) Uani 1 1 d . . .
H18A H 1.1180 0.4109 0.6900 0.076 Uiso 1 1 calc R . .
C14 C 0.7930(3) 0.3114(5) 0.67947(15) 0.0550(13) Uani 1 1 d . . .
H14A H 0.7404 0.3024 0.6939 0.066 Uiso 1 1 calc R . .
C7A C 0.8572(3) 0.6325(5) 0.61707(17) 0.0577(13) Uani 1 1 d . . .
H7C H 0.9118 0.6402 0.6379 0.069 Uiso 1 1 calc R . .
C4A C 0.6948(3) 0.6161(6) 0.5568(2) 0.0771(16) Uani 1 1 d . . .
H4C H 0.6399 0.6110 0.5362 0.093 Uiso 1 1 calc R . .
C10 C 0.6088(3) 0.0398(6) 0.56799(16) 0.0638(14) Uani 1 1 d . . .
H10A H 0.6021 -0.0495 0.5546 0.077 Uiso 1 1 calc R . .
C20A C 0.7953(3) 0.1697(5) 0.36584(14) 0.0537(12) Uani 1 1 d . . .
H20C H 0.7856 0.1900 0.3296 0.064 Uiso 1 1 calc R . .
H20D H 0.8047 0.0706 0.3699 0.064 Uiso 1 1 calc R . .
C11 C 0.5356(3) 0.1265(6) 0.56634(18) 0.0713(16) Uani 1 1 d . . .
H11A H 0.4796 0.0954 0.5519 0.086 Uiso 1 1 calc R . .
C20 C 0.9020(4) 0.5458(7) 0.77979(19) 0.097(2) Uani 1 1 d . . .
H20A H 0.8712 0.6214 0.7606 0.117 Uiso 1 1 calc R . .
H20B H 0.9006 0.5638 0.8158 0.117 Uiso 1 1 calc R . .
C3 C 1.0557(3) 0.0708(5) 0.70055(18) 0.0681(15) Uani 1 1 d . . .
H3A H 1.1041 0.1043 0.6860 0.082 Uiso 1 1 calc R . .
C24 C 1.1704(3) 0.5357(6) 0.74676(18) 0.0850(19) Uani 1 1 d . . .
H24A H 1.2288 0.5316 0.7394 0.102 Uiso 1 1 calc R . .
C6A C 0.7823(4) 0.6897(6) 0.6327(2) 0.0835(18) Uani 1 1 d . . .
H6C H 0.7867 0.7345 0.6641 0.100 Uiso 1 1 calc R . .
C19 C 0.8537(3) 0.4124(7) 0.76532(17) 0.091(2) Uani 1 1 d . . .
H19A H 0.7909 0.4234 0.7683 0.109 Uiso 1 1 calc R . .
H19B H 0.8775 0.3395 0.7886 0.109 Uiso 1 1 calc R . .
C5A C 0.7014(4) 0.6817(6) 0.6027(3) 0.093(2) Uani 1 1 d . . .
H5C H 0.6511 0.7208 0.6137 0.112 Uiso 1 1 calc R . .
C7 C 0.9081(4) -0.0045(6) 0.6935(2) 0.089(2) Uani 1 1 d . . .
H7A H 0.8535 -0.0249 0.6742 0.107 Uiso 1 1 calc R . .
C22 C 1.0650(4) 0.6168(7) 0.7977(2) 0.094(2) Uani 1 1 d . . .
H22A H 1.0520 0.6703 0.8250 0.113 Uiso 1 1 calc R . .
C4 C 1.0645(4) 0.0533(7) 0.7529(2) 0.098(2) Uani 1 1 d . . .
H4A H 1.1185 0.0732 0.7728 0.117 Uiso 1 1 calc R . .
C6 C 0.9177(5) -0.0199(7) 0.7462(2) 0.115(3) Uani 1 1 d . . .
H6A H 0.8693 -0.0500 0.7616 0.138 Uiso 1 1 calc R . .
C5 C 0.9948(5) 0.0076(8) 0.7751(2) 0.110(2) Uani 1 1 d . . .
H5A H 1.0005 -0.0046 0.8103 0.132 Uiso 1 1 calc R . .
C23 C 1.1506(4) 0.6146(7) 0.7866(2) 0.100(2) Uani 1 1 d . . .
H23A H 1.1949 0.6663 0.8059 0.120 Uiso 1 1 calc R . .
O1A O 0.81591(15) 0.2238(3) 0.52141(9) 0.0376(6) Uani 1 1 d . . .
C9A C 1.1471(2) 0.1241(4) 0.52029(14) 0.0400(10) Uani 1 1 d . . .
H9C H 1.1218 0.0615 0.4957 0.048 Uiso 1 1 calc R . .
C10A C 1.2380(3) 0.1195(5) 0.53664(17) 0.0544(12) Uani 1 1 d . . .
H10C H 1.2735 0.0550 0.5227 0.065 Uiso 1 1 calc R . .
C11A C 1.2754(3) 0.2094(5) 0.57313(17) 0.0611(13) Uani 1 1 d . . .
H11C H 1.3365 0.2063 0.5840 0.073 Uiso 1 1 calc R . .
C12A C 1.2234(3) 0.3046(5) 0.59381(16) 0.0644(14) Uani 1 1 d . . .
H12C H 1.2490 0.3656 0.6189 0.077 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1A 2.018(2) . ?
Zr1 O1 2.047(2) . ?
Zr1 N1 2.278(3) . ?
Zr1 C1A 2.308(4) . ?
Zr1 C1 2.317(4) . ?
Zr1 N1A 2.333(3) . ?
O1 C16 1.291(4) . ?
C15A C16A 1.366(5) . ?
C15A C14A 1.423(5) . ?
C15A C19A 1.511(4) . ?
N1A C14A 1.312(4) . ?
N1A C8A 1.427(4) . ?
N1 C14 1.328(5) . ?
N1 C8 1.436(5) . ?
C8 C9 1.375(6) . ?
C8 C13 1.386(6) . ?
C8A C9A 1.376(5) . ?
C8A C13A 1.383(5) . ?
C19A C20A 1.504(5) . ?
C16A O1A 1.326(4) . ?
C16A C17A 1.471(5) . ?
C18A C24A 1.379(5) . ?
C18A C17A 1.383(5) . ?
C17A C21A 1.406(5) . ?
C12 C11 1.362(7) . ?
C12 C13 1.381(6) . ?
C23A C22A 1.371(6) . ?
C23A C24A 1.373(6) . ?
C2A C7A 1.395(5) . ?
C2A C3A 1.395(5) . ?
C2A C1A 1.461(5) . ?
C16 C15 1.383(5) . ?
C16 C17 1.462(5) . ?
C21A C22A 1.381(5) . ?
C21A C20A 1.489(5) . ?
C3A C4A 1.379(6) . ?
C17 C21 1.385(6) . ?
C17 C18 1.388(6) . ?
C13A C12A 1.382(5) . ?
C21 C22 1.387(6) . ?
C21 C20 1.495(6) . ?
C9 C10 1.385(6) . ?
C2 C7 1.374(6) . ?
C2 C3 1.375(6) . ?
C2 C1 1.487(5) . ?
C15 C14 1.390(5) . ?
C15 C19 1.519(5) . ?
C18 C24 1.372(6) . ?
C7A C6A 1.374(6) . ?
C4A C5A 1.361(7) . ?
C10 C11 1.382(6) . ?
C20 C19 1.502(7) . ?
C3 C4 1.383(6) . ?
C24 C23 1.365(7) . ?
C6A C5A 1.366(7) . ?
C7 C6 1.389(7) . ?
C22 C23 1.366(7) . ?
C4 C5 1.349(8) . ?
C6 C5 1.330(8) . ?
C9A C10A 1.385(5) . ?
C10A C11A 1.362(6) . ?
C11A C12A 1.370(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
O1A Zr1 O1 163.85(10) . . ?
O1A Zr1 N1 89.51(10) . . ?
O1 Zr1 N1 78.73(10) . . ?
O1A Zr1 C1A 93.26(12) . . ?
O1 Zr1 C1A 81.35(12) . . ?
N1 Zr1 C1A 112.73(13) . . ?
O1A Zr1 C1 106.04(13) . . ?
O1 Zr1 C1 86.38(12) . . ?
N1 Zr1 C1 96.15(14) . . ?
C1A Zr1 C1 145.44(15) . . ?
O1A Zr1 N1A 78.90(9) . . ?
O1 Zr1 N1A 114.27(10) . . ?
N1 Zr1 N1A 165.44(11) . . ?
C1A Zr1 N1A 77.05(12) . . ?
C1 Zr1 N1A 78.89(13) . . ?
C16 O1 Zr1 141.9(2) . . ?
C16A C15A C14A 123.4(3) . . ?
C16A C15A C19A 118.7(3) . . ?
C14A C15A C19A 117.9(3) . . ?
C14A N1A C8A 115.3(3) . . ?
C14A N1A Zr1 124.5(2) . . ?
C8A N1A Zr1 120.0(2) . . ?
C14 N1 C8 114.3(3) . . ?
C14 N1 Zr1 125.5(3) . . ?
C8 N1 Zr1 120.1(2) . . ?
C9 C8 C13 119.0(4) . . ?
C9 C8 N1 120.0(4) . . ?
C13 C8 N1 121.0(4) . . ?
N1A C14A C15A 127.7(3) . . ?
C9A C8A C13A 118.5(3) . . ?
C9A C8A N1A 122.8(3) . . ?
C13A C8A N1A 118.7(3) . . ?
C20A C19A C15A 111.0(3) . . ?
O1A C16A C15A 122.4(3) . . ?
O1A C16A C17A 116.7(3) . . ?
C15A C16A C17A 120.9(3) . . ?
C24A C18A C17A 119.9(4) . . ?
C18A C17A C21A 120.7(4) . . ?
C18A C17A C16A 120.8(3) . . ?
C21A C17A C16A 118.5(3) . . ?
C11 C12 C13 120.1(5) . . ?
C22A C23A C24A 120.9(4) . . ?
C7A C2A C3A 116.5(4) . . ?
C7A C2A C1A 122.6(4) . . ?
C3A C2A C1A 120.7(4) . . ?
O1 C16 C15 121.4(4) . . ?
O1 C16 C17 117.9(4) . . ?
C15 C16 C17 120.7(4) . . ?
C22A C21A C17A 117.9(4) . . ?
C22A C21A C20A 123.1(4) . . ?
C17A C21A C20A 118.9(3) . . ?
C23A C24A C18A 119.6(4) . . ?
C4A C3A C2A 121.8(5) . . ?
C12 C13 C8 120.5(4) . . ?
C2A C1A Zr1 99.3(2) . . ?
C21 C17 C18 119.5(4) . . ?
C21 C17 C16 120.1(4) . . ?
C18 C17 C16 120.3(4) . . ?
C12A C13A C8A 120.6(4) . . ?
C17 C21 C22 118.0(5) . . ?
C17 C21 C20 118.3(4) . . ?
C22 C21 C20 123.6(5) . . ?
C8 C9 C10 120.6(5) . . ?
C7 C2 C3 115.9(4) . . ?
C7 C2 C1 121.6(4) . . ?
C3 C2 C1 122.4(4) . . ?
C23A C22A C21A 121.0(4) . . ?
C2 C1 Zr1 116.4(3) . . ?
C16 C15 C14 122.7(4) . . ?
C16 C15 C19 116.9(4) . . ?
C14 C15 C19 120.4(4) . . ?
C24 C18 C17 120.9(4) . . ?
N1 C14 C15 129.6(4) . . ?
C6A C7A C2A 121.1(5) . . ?
C5A C4A C3A 120.0(5) . . ?
C11 C10 C9 119.6(5) . . ?
C21A C20A C19A 111.9(3) . . ?
C12 C11 C10 120.2(5) . . ?
C21 C20 C19 112.3(5) . . ?
C2 C3 C4 122.2(5) . . ?
C23 C24 C18 120.0(5) . . ?
C5A C6A C7A 120.8(5) . . ?
C20 C19 C15 111.0(4) . . ?
C4A C5A C6A 119.7(5) . . ?
C2 C7 C6 121.2(5) . . ?
C23 C22 C21 122.3(5) . . ?
C5 C4 C3 120.1(6) . . ?
C5 C6 C7 121.2(6) . . ?
C6 C5 C4 119.4(6) . . ?
C22 C23 C24 119.3(5) . . ?
C16A O1A Zr1 137.6(2) . . ?
C8A C9A C10A 120.7(4) . . ?
C11A C10A C9A 120.0(4) . . ?
C10A C11A C12A 120.2(4) . . ?
C11A C12A C13A 119.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_5b
_database_code_depnum_ccdc_archive 'CCDC 1419052'
_audit_update_record             
;
2015-08-17 deposited with the CCDC.
2016-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H50 N2 O2 Zr'
_chemical_formula_weight         922.24

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.2590(10)
_cell_length_b                   24.229(2)
_cell_length_c                   17.8544(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.370(2)
_cell_angle_gamma                90.00
_cell_volume                     4869.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8618
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1222
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         25.06
_reflns_number_total             8618
_reflns_number_gt                5461
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0439P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8618
_refine_ls_number_parameters     586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.1363
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.47010(4) 0.861631(17) 0.25164(3) 0.02299(14) Uani 1 1 d . . .
O1 O 0.5405(2) 0.94103(11) 0.25391(16) 0.0225(7) Uani 1 1 d . . .
O1A O 0.4036(3) 0.78341(11) 0.27368(17) 0.0279(8) Uani 1 1 d . . .
N1 N 0.3281(3) 0.91530(15) 0.1863(2) 0.0248(9) Uani 1 1 d . . .
C8A C 0.4982(4) 0.85343(18) 0.0693(3) 0.0269(11) Uani 1 1 d . . .
C16A C 0.4088(4) 0.73338(19) 0.2458(3) 0.0287(12) Uani 1 1 d . . .
C3 C 0.5461(5) 0.9186(2) 0.4228(3) 0.0370(13) Uani 1 1 d . . .
H3A H 0.5241 0.9544 0.4099 0.044 Uiso 1 1 calc R . .
C9A C 0.5635(4) 0.90181(18) 0.0771(3) 0.0322(12) Uani 1 1 d . . .
H9C H 0.5968 0.9111 0.1236 0.039 Uiso 1 1 calc R . .
C2 C 0.4682(4) 0.87462(19) 0.4049(3) 0.0313(12) Uani 1 1 d . . .
C15 C 0.3879(4) 1.00602(18) 0.2349(3) 0.0241(11) Uani 1 1 d . . .
C7 C 0.5049(5) 0.82209(19) 0.4292(3) 0.0354(13) Uani 1 1 d . . .
H7A H 0.4558 0.7919 0.4195 0.042 Uiso 1 1 calc R . .
C14 C 0.3135(4) 0.96895(18) 0.1944(2) 0.0258(11) Uani 1 1 d . . .
H14A H 0.2466 0.9842 0.1708 0.031 Uiso 1 1 calc R . .
C19 C 0.7724(4) 0.99353(18) 0.2639(3) 0.0308(12) Uani 1 1 d . . .
C17 C 0.5730(4) 1.03043(16) 0.3049(2) 0.0223(11) Uani 1 1 d . . .
C5 C 0.6880(5) 0.8572(2) 0.4809(3) 0.0487(15) Uani 1 1 d . . .
H5A H 0.7615 0.8513 0.5044 0.058 Uiso 1 1 calc R . .
C30 C 0.7503(4) 1.05227(19) 0.3762(3) 0.0366(13) Uani 1 1 d . . .
H30A H 0.8313 1.0476 0.3856 0.044 Uiso 1 1 calc R . .
C4 C 0.6533(5) 0.9098(2) 0.4588(3) 0.0480(16) Uani 1 1 d . . .
H4A H 0.7035 0.9396 0.4686 0.058 Uiso 1 1 calc R . .
C10A C 0.5793(5) 0.9360(2) 0.0168(3) 0.0372(13) Uani 1 1 d . . .
H10C H 0.6208 0.9689 0.0233 0.045 Uiso 1 1 calc R . .
C18 C 0.6965(4) 1.02404(17) 0.3164(3) 0.0276(12) Uani 1 1 d . . .
C25 C 0.3474(4) 1.06465(18) 0.2501(3) 0.0326(12) Uani 1 1 d . . .
H25A H 0.2622 1.0677 0.2417 0.039 Uiso 1 1 calc R . .
H25B H 0.3862 1.0901 0.2166 0.039 Uiso 1 1 calc R . .
C27 C 0.5102(4) 1.06910(17) 0.3476(3) 0.0261(11) Uani 1 1 d . . .
C8 C 0.2449(4) 0.88882(19) 0.1363(3) 0.0295(12) Uani 1 1 d . . .
C6 C 0.6114(5) 0.8139(2) 0.4671(3) 0.0441(15) Uani 1 1 d . . .
H6A H 0.6318 0.7787 0.4836 0.053 Uiso 1 1 calc R . .
C16 C 0.4992(4) 0.99062(18) 0.2611(2) 0.0236(11) Uani 1 1 d . . .
C24 C 0.8646(5) 0.9595(2) 0.2903(3) 0.0422(14) Uani 1 1 d . . .
H24A H 0.8753 0.9542 0.3416 0.051 Uiso 1 1 calc R . .
C27A C 0.4485(4) 0.6374(2) 0.2821(3) 0.0369(13) Uani 1 1 d . . .
N1A N 0.4758(3) 0.82057(14) 0.1346(2) 0.0256(9) Uani 1 1 d . . .
C26A C 0.5114(5) 0.6308(2) 0.2102(3) 0.0497(16) Uani 1 1 d . . .
H26C H 0.5118 0.5922 0.1959 0.060 Uiso 1 1 calc R . .
H26D H 0.5931 0.6429 0.2167 0.060 Uiso 1 1 calc R . .
C17A C 0.3857(4) 0.68600(18) 0.2968(3) 0.0285(12) Uani 1 1 d . . .
C1 C 0.3640(4) 0.88329(19) 0.3562(3) 0.0343(13) Uani 1 1 d . . .
H1A H 0.3353 0.9210 0.3564 0.041 Uiso 1 1 calc R . .
H1B H 0.2998 0.8577 0.3656 0.041 Uiso 1 1 calc R . .
C3A C 0.7712(4) 0.7717(2) 0.1821(3) 0.0442(15) Uani 1 1 d . . .
H3C H 0.7732 0.7970 0.1430 0.053 Uiso 1 1 calc R . .
C18A C 0.3138(4) 0.68891(19) 0.3597(3) 0.0336(13) Uani 1 1 d . . .
C7A C 0.7134(5) 0.7461(2) 0.3052(3) 0.0424(14) Uani 1 1 d . . .
H7C H 0.6760 0.7539 0.3499 0.051 Uiso 1 1 calc R . .
C15A C 0.4415(4) 0.72467(19) 0.1740(3) 0.0327(13) Uani 1 1 d . . .
C14A C 0.4707(4) 0.76689(19) 0.1233(3) 0.0330(12) Uani 1 1 d . . .
H14C H 0.4890 0.7552 0.0753 0.040 Uiso 1 1 calc R . .
C19A C 0.2215(5) 0.7322(2) 0.3695(3) 0.0362(13) Uani 1 1 d . . .
C13 C 0.2232(4) 0.9098(2) 0.0646(3) 0.0390(14) Uani 1 1 d . . .
H13A H 0.2622 0.9415 0.0494 0.047 Uiso 1 1 calc R . .
C25A C 0.4503(5) 0.66477(19) 0.1483(3) 0.0454(15) Uani 1 1 d . . .
H25C H 0.4956 0.6627 0.1028 0.055 Uiso 1 1 calc R . .
H25D H 0.3714 0.6502 0.1376 0.055 Uiso 1 1 calc R . .
C20A C 0.1383(5) 0.7431(2) 0.3129(3) 0.0437(15) Uani 1 1 d . . .
H20C H 0.1468 0.7266 0.2663 0.052 Uiso 1 1 calc R . .
C1A C 0.6695(4) 0.84215(17) 0.2613(3) 0.0304(12) Uani 1 1 d . . .
H1C H 0.7086 0.8667 0.2267 0.036 Uiso 1 1 calc R . .
H1D H 0.6954 0.8532 0.3113 0.036 Uiso 1 1 calc R . .
C2A C 0.7188(4) 0.78674(19) 0.2489(3) 0.0332(13) Uani 1 1 d . . .
C28 C 0.5686(5) 1.09619(19) 0.4061(3) 0.0374(13) Uani 1 1 d . . .
H28A H 0.5269 1.1211 0.4353 0.045 Uiso 1 1 calc R . .
C26 C 0.3799(4) 1.07874(18) 0.3312(3) 0.0329(13) Uani 1 1 d . . .
H26A H 0.3608 1.1171 0.3407 0.040 Uiso 1 1 calc R . .
H26B H 0.3332 1.0561 0.3644 0.040 Uiso 1 1 calc R . .
C20 C 0.7593(4) 1.00052(19) 0.1872(3) 0.0344(13) Uani 1 1 d . . .
H20A H 0.6986 1.0228 0.1682 0.041 Uiso 1 1 calc R . .
C11A C 0.5346(5) 0.9222(2) -0.0533(3) 0.0437(14) Uani 1 1 d . . .
H11C H 0.5466 0.9451 -0.0942 0.052 Uiso 1 1 calc R . .
C23 C 0.9398(5) 0.9337(2) 0.2414(4) 0.0507(16) Uani 1 1 d . . .
H23A H 1.0002 0.9110 0.2601 0.061 Uiso 1 1 calc R . .
C30A C 0.3164(5) 0.6453(2) 0.4098(3) 0.0480(16) Uani 1 1 d . . .
H30C H 0.2705 0.6472 0.4524 0.058 Uiso 1 1 calc R . .
C12A C 0.4725(5) 0.8743(2) -0.0611(3) 0.0462(15) Uani 1 1 d . . .
H12C H 0.4427 0.8644 -0.1083 0.055 Uiso 1 1 calc R . .
C21 C 0.8363(5) 0.9745(2) 0.1379(3) 0.0450(15) Uani 1 1 d . . .
H21A H 0.8269 0.9796 0.0865 0.054 Uiso 1 1 calc R . .
C29 C 0.6869(5) 1.0869(2) 0.4218(3) 0.0400(14) Uani 1 1 d . . .
H29A H 0.7241 1.1038 0.4628 0.048 Uiso 1 1 calc R . .
C9 C 0.1883(4) 0.8409(2) 0.1585(3) 0.0398(14) Uani 1 1 d . . .
H9A H 0.2031 0.8263 0.2060 0.048 Uiso 1 1 calc R . .
C28A C 0.4491(5) 0.5944(2) 0.3346(4) 0.0465(16) Uani 1 1 d . . .
H28C H 0.4929 0.5625 0.3261 0.056 Uiso 1 1 calc R . .
C13A C 0.4524(4) 0.8400(2) -0.0016(3) 0.0369(13) Uani 1 1 d . . .
H13C H 0.4082 0.8079 -0.0085 0.044 Uiso 1 1 calc R . .
C12 C 0.1441(5) 0.8837(3) 0.0158(3) 0.0560(18) Uani 1 1 d . . .
H12A H 0.1296 0.8980 -0.0319 0.067 Uiso 1 1 calc R . .
C6A C 0.7630(5) 0.6948(2) 0.2947(4) 0.0485(16) Uani 1 1 d . . .
H6C H 0.7592 0.6688 0.3329 0.058 Uiso 1 1 calc R . .
C21A C 0.0434(5) 0.7779(2) 0.3239(4) 0.0614(19) Uani 1 1 d . . .
H21C H -0.0120 0.7842 0.2853 0.074 Uiso 1 1 calc R . .
C22 C 0.9266(5) 0.9411(2) 0.1663(4) 0.0532(17) Uani 1 1 d . . .
H22A H 0.9782 0.9238 0.1338 0.064 Uiso 1 1 calc R . .
C11 C 0.0871(5) 0.8364(3) 0.0385(4) 0.064(2) Uani 1 1 d . . .
H11A H 0.0335 0.8188 0.0061 0.077 Uiso 1 1 calc R . .
C24A C 0.2064(6) 0.7592(2) 0.4383(3) 0.0549(17) Uani 1 1 d . . .
H24C H 0.2608 0.7528 0.4773 0.066 Uiso 1 1 calc R . .
C10 C 0.1094(5) 0.8153(2) 0.1093(4) 0.0580(19) Uani 1 1 d . . .
H10A H 0.0707 0.7833 0.1241 0.070 Uiso 1 1 calc R . .
C4A C 0.8204(5) 0.7198(2) 0.1726(3) 0.0498(16) Uani 1 1 d . . .
H4C H 0.8556 0.7110 0.1276 0.060 Uiso 1 1 calc R . .
C29A C 0.3848(6) 0.5996(2) 0.3984(4) 0.0558(19) Uani 1 1 d . . .
H29C H 0.3876 0.5717 0.4343 0.067 Uiso 1 1 calc R . .
C5A C 0.8178(5) 0.6808(2) 0.2295(4) 0.0520(17) Uani 1 1 d . . .
H5C H 0.8522 0.6462 0.2237 0.062 Uiso 1 1 calc R . .
C22A C 0.0313(6) 0.8032(3) 0.3924(5) 0.075(2) Uani 1 1 d . . .
H22C H -0.0332 0.8262 0.4004 0.090 Uiso 1 1 calc R . .
C23A C 0.1141(7) 0.7945(3) 0.4492(4) 0.074(2) Uani 1 1 d . . .
H23C H 0.1072 0.8126 0.4948 0.088 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1A 2.079(3) . ?
Zr1 O1 2.081(3) . ?
Zr1 C1A 2.296(4) . ?
Zr1 C1 2.301(5) . ?
Zr1 N1A 2.317(4) . ?
Zr1 N1 2.350(3) . ?
O1 C16 1.296(5) . ?
O1A C16A 1.312(5) . ?
N1 C14 1.319(5) . ?
N1 C8 1.430(5) . ?
C8A C9A 1.389(6) . ?
C8A C13A 1.393(6) . ?
C8A N1A 1.440(6) . ?
C16A C15A 1.360(6) . ?
C16A C17A 1.491(6) . ?
C3 C4 1.370(7) . ?
C3 C2 1.411(6) . ?
C9A C10A 1.374(6) . ?
C2 C7 1.403(6) . ?
C2 C1 1.459(6) . ?
C15 C16 1.379(6) . ?
C15 C14 1.415(6) . ?
C15 C25 1.518(6) . ?
C7 C6 1.378(7) . ?
C19 C20 1.383(6) . ?
C19 C24 1.398(6) . ?
C19 C18 1.482(6) . ?
C17 C18 1.409(6) . ?
C17 C27 1.409(6) . ?
C17 C16 1.484(6) . ?
C5 C6 1.376(6) . ?
C5 C4 1.389(6) . ?
C30 C29 1.380(7) . ?
C30 C18 1.394(6) . ?
C10A C11A 1.378(7) . ?
C25 C26 1.524(6) . ?
C27 C28 1.386(6) . ?
C27 C26 1.508(6) . ?
C8 C9 1.387(6) . ?
C8 C13 1.393(6) . ?
C24 C23 1.381(7) . ?
C27A C28A 1.401(7) . ?
C27A C17A 1.402(6) . ?
C27A C26A 1.489(7) . ?
N1A C14A 1.317(5) . ?
C26A C25A 1.527(7) . ?
C17A C18A 1.403(7) . ?
C3A C4A 1.387(7) . ?
C3A C2A 1.392(7) . ?
C18A C30A 1.384(6) . ?
C18A C19A 1.491(7) . ?
C7A C6A 1.377(6) . ?
C7A C2A 1.410(7) . ?
C15A C14A 1.410(6) . ?
C15A C25A 1.526(6) . ?
C19A C20A 1.386(7) . ?
C19A C24A 1.406(7) . ?
C13 C12 1.382(7) . ?
C20A C21A 1.379(7) . ?
C1A C2A 1.472(6) . ?
C28 C29 1.374(7) . ?
C20 C21 1.400(7) . ?
C11A C12A 1.362(7) . ?
C23 C22 1.358(7) . ?
C30A C29A 1.368(8) . ?
C12A C13A 1.371(7) . ?
C21 C22 1.385(7) . ?
C9 C10 1.382(7) . ?
C28A C29A 1.371(8) . ?
C12 C11 1.379(8) . ?
C6A C5A 1.372(7) . ?
C21A C22A 1.379(9) . ?
C11 C10 1.382(8) . ?
C24A C23A 1.363(8) . ?
C4A C5A 1.388(7) . ?
C22A C23A 1.377(9) . ?

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 O1 167.96(12) . . ?
O1A Zr1 C1A 98.88(14) . . ?
O1 Zr1 C1A 79.48(13) . . ?
O1A Zr1 C1 81.83(15) . . ?
O1 Zr1 C1 88.75(15) . . ?
C1A Zr1 C1 120.76(17) . . ?
O1A Zr1 N1A 78.28(12) . . ?
O1 Zr1 N1A 113.33(12) . . ?
C1A Zr1 N1A 86.07(15) . . ?
C1 Zr1 N1A 148.85(15) . . ?
O1A Zr1 N1 110.77(12) . . ?
O1 Zr1 N1 75.66(11) . . ?
C1A Zr1 N1 143.46(15) . . ?
C1 Zr1 N1 85.22(15) . . ?
N1A Zr1 N1 79.79(12) . . ?
C16 O1 Zr1 136.2(3) . . ?
C16A O1A Zr1 138.7(3) . . ?
C14 N1 C8 115.4(4) . . ?
C14 N1 Zr1 125.2(3) . . ?
C8 N1 Zr1 119.3(3) . . ?
C9A C8A C13A 118.2(5) . . ?
C9A C8A N1A 119.2(4) . . ?
C13A C8A N1A 122.6(4) . . ?
O1A C16A C15A 121.1(4) . . ?
O1A C16A C17A 118.0(4) . . ?
C15A C16A C17A 120.7(4) . . ?
C4 C3 C2 121.7(5) . . ?
C10A C9A C8A 120.5(5) . . ?
C7 C2 C3 116.0(5) . . ?
C7 C2 C1 122.7(4) . . ?
C3 C2 C1 120.9(4) . . ?
C16 C15 C14 121.6(4) . . ?
C16 C15 C25 117.8(4) . . ?
C14 C15 C25 120.6(4) . . ?
C6 C7 C2 121.9(5) . . ?
N1 C14 C15 127.4(4) . . ?
C20 C19 C24 117.8(5) . . ?
C20 C19 C18 121.1(4) . . ?
C24 C19 C18 121.0(5) . . ?
C18 C17 C27 120.1(4) . . ?
C18 C17 C16 122.9(4) . . ?
C27 C17 C16 115.8(4) . . ?
C6 C5 C4 118.6(5) . . ?
C29 C30 C18 121.9(5) . . ?
C3 C4 C5 120.9(5) . . ?
C9A C10A C11A 121.0(5) . . ?
C30 C18 C17 117.8(5) . . ?
C30 C18 C19 118.9(4) . . ?
C17 C18 C19 123.0(4) . . ?
C15 C25 C26 108.3(4) . . ?
C28 C27 C17 119.2(4) . . ?
C28 C27 C26 121.0(4) . . ?
C17 C27 C26 119.8(4) . . ?
C9 C8 C13 119.8(5) . . ?
C9 C8 N1 119.7(5) . . ?
C13 C8 N1 120.5(4) . . ?
C5 C6 C7 120.8(5) . . ?
O1 C16 C15 122.9(4) . . ?
O1 C16 C17 117.2(4) . . ?
C15 C16 C17 119.8(4) . . ?
C23 C24 C19 121.1(5) . . ?
C28A C27A C17A 119.6(5) . . ?
C28A C27A C26A 120.2(5) . . ?
C17A C27A C26A 120.2(5) . . ?
C14A N1A C8A 115.4(4) . . ?
C14A N1A Zr1 124.1(3) . . ?
C8A N1A Zr1 120.2(3) . . ?
C27A C26A C25A 110.6(4) . . ?
C27A C17A C18A 119.7(5) . . ?
C27A C17A C16A 115.9(5) . . ?
C18A C17A C16A 124.2(4) . . ?
C2 C1 Zr1 91.4(3) . . ?
C4A C3A C2A 121.4(5) . . ?
C30A C18A C17A 118.4(5) . . ?
C30A C18A C19A 117.8(5) . . ?
C17A C18A C19A 123.1(4) . . ?
C6A C7A C2A 120.5(5) . . ?
C16A C15A C14A 124.5(4) . . ?
C16A C15A C25A 116.9(4) . . ?
C14A C15A C25A 118.6(5) . . ?
N1A C14A C15A 128.9(5) . . ?
C20A C19A C24A 117.1(6) . . ?
C20A C19A C18A 120.7(5) . . ?
C24A C19A C18A 121.9(5) . . ?
C12 C13 C8 120.6(5) . . ?
C15A C25A C26A 109.0(4) . . ?
C21A C20A C19A 121.7(6) . . ?
C2A C1A Zr1 123.2(3) . . ?
C3A C2A C7A 117.1(5) . . ?
C3A C2A C1A 122.4(5) . . ?
C7A C2A C1A 120.5(5) . . ?
C29 C28 C27 121.1(5) . . ?
C27 C26 C25 111.1(4) . . ?
C19 C20 C21 120.9(5) . . ?
C12A C11A C10A 118.4(5) . . ?
C22 C23 C24 120.6(5) . . ?
C29A C30A C18A 121.7(6) . . ?
C11A C12A C13A 122.0(5) . . ?
C22 C21 C20 119.5(5) . . ?
C28 C29 C30 119.5(5) . . ?
C10 C9 C8 119.1(5) . . ?
C29A C28A C27A 119.6(6) . . ?
C12A C13A C8A 119.9(5) . . ?
C11 C12 C13 119.5(6) . . ?
C5A C6A C7A 122.1(6) . . ?
C22A C21A C20A 119.4(7) . . ?
C23 C22 C21 120.1(6) . . ?
C12 C11 C10 120.0(5) . . ?
C23A C24A C19A 121.7(6) . . ?
C11 C10 C9 121.0(6) . . ?
C3A C4A C5A 120.9(6) . . ?
C30A C29A C28A 120.6(6) . . ?
C6A C5A C4A 118.0(5) . . ?
C23A C22A C21A 120.4(7) . . ?
C24A C23A C22A 119.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_6b
_database_code_depnum_ccdc_archive 'CCDC 1419053'
_audit_update_record             
;
2015-08-17 deposited with the CCDC.
2016-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H54 N2 O2 Zr'
_chemical_formula_weight         950.29

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   22.6289(19)
_cell_length_b                   15.0048(13)
_cell_length_c                   18.0332(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.611(2)
_cell_angle_gamma                90.00
_cell_volume                     5997.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11795
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1354
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         26.05
_reflns_number_total             11795
_reflns_number_gt                6961
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.501 0.000 0.001 827 20 ' '
2 0.358 0.500 0.358 827 20 ' '
_platon_squeeze_details          
;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11795
_refine_ls_number_parameters     604
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1575
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_restrained_S_all      0.932
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.243459(17) 0.96169(3) 0.21420(2) 0.02197(12) Uani 1 1 d . . .
O1 O 0.32138(12) 0.90042(19) 0.27269(14) 0.0281(7) Uani 1 1 d . . .
O1A O 0.15378(12) 1.00246(19) 0.18501(14) 0.0256(7) Uani 1 1 d . . .
N1 N 0.29570(14) 0.9187(2) 0.12038(17) 0.0243(8) Uani 1 1 d . . .
N1A N 0.24980(14) 1.0932(2) 0.15038(18) 0.0262(8) Uani 1 1 d . . .
C16 C 0.36222(17) 0.8420(3) 0.2631(2) 0.0257(10) Uani 1 1 d . . .
C15 C 0.37677(17) 0.8272(3) 0.1940(2) 0.0276(10) Uani 1 1 d . . .
C7 C 0.1403(2) 0.8462(3) 0.2996(3) 0.0350(11) Uani 1 1 d . . .
H3C H 0.1117 0.8786 0.2659 0.042 Uiso 1 1 calc R . .
C17A C 0.05646(17) 1.0681(3) 0.1631(2) 0.0216(9) Uani 1 1 d . . .
C8 C 0.26980(17) 0.9442(3) 0.0440(2) 0.0235(10) Uani 1 1 d . . .
C6 C 0.1338(2) 0.8371(3) 0.3745(3) 0.0409(12) Uani 1 1 d . . .
H6A H 0.1011 0.8631 0.3903 0.049 Uiso 1 1 calc R . .
C14A C 0.20412(18) 1.1423(3) 0.1146(2) 0.0273(10) Uani 1 1 d . . .
H14C H 0.2148 1.1905 0.0877 0.033 Uiso 1 1 calc R . .
C9 C 0.30307(19) 0.9693(3) -0.0087(2) 0.0324(10) Uani 1 1 d . . .
H9A H 0.3449 0.9704 0.0050 0.039 Uiso 1 1 calc R . .
C16A C 0.12002(17) 1.0664(3) 0.1515(2) 0.0236(10) Uani 1 1 d . . .
C21A C 0.06472(18) 0.8372(3) 0.0083(2) 0.0310(11) Uani 1 1 d . . .
H21C H 0.0783 0.8408 -0.0370 0.037 Uiso 1 1 calc R . .
C15A C 0.14242(18) 1.1320(3) 0.1117(2) 0.0257(10) Uani 1 1 d . . .
C2 C 0.18841(18) 0.8083(3) 0.2740(2) 0.0265(10) Uani 1 1 d . . .
C13 C 0.20717(18) 0.9457(3) 0.0227(2) 0.0286(10) Uani 1 1 d . . .
H13A H 0.1837 0.9299 0.0575 0.034 Uiso 1 1 calc R . .
C1A C 0.25533(19) 1.0252(3) 0.3318(2) 0.0319(11) Uani 1 1 d . . .
H1C H 0.2456 0.9791 0.3651 0.038 Uiso 1 1 calc R . .
H1D H 0.2981 1.0370 0.3480 0.038 Uiso 1 1 calc R . .
C7A C 0.1664(2) 1.1055(3) 0.3658(2) 0.0394(12) Uani 1 1 d . . .
H8C H 0.1458 1.0517 0.3643 0.047 Uiso 1 1 calc R . .
C18A C 0.01909(18) 0.9931(3) 0.1531(2) 0.0257(10) Uani 1 1 d . . .
C18 C 0.40729(18) 0.8249(3) 0.4031(2) 0.0335(11) Uani 1 1 d . . .
C8A C 0.30922(19) 1.1245(3) 0.1435(3) 0.0316(11) Uani 1 1 d . . .
C31A C -0.03678(18) 0.9969(3) 0.1757(2) 0.0338(11) Uani 1 1 d . . .
H31C H -0.0611 0.9464 0.1712 0.041 Uiso 1 1 calc R . .
C28 C 0.38742(18) 0.6932(3) 0.3210(3) 0.0346(11) Uani 1 1 d . . .
C19A C 0.03332(17) 0.9114(3) 0.1139(2) 0.0243(9) Uani 1 1 d . . .
C13A C 0.35697(19) 1.1139(3) 0.2050(3) 0.0409(12) Uani 1 1 d . . .
H13C H 0.3509 1.0868 0.2492 0.049 Uiso 1 1 calc R . .
C25 C 0.42549(19) 0.7601(3) 0.1871(3) 0.0341(11) Uani 1 1 d . . .
H25A H 0.4392 0.7709 0.1403 0.041 Uiso 1 1 calc R . .
H25B H 0.4596 0.7689 0.2286 0.041 Uiso 1 1 calc R . .
C10 C 0.2758(2) 0.9924(3) -0.0806(2) 0.0314(11) Uani 1 1 d . . .
H10A H 0.2992 1.0078 -0.1155 0.038 Uiso 1 1 calc R . .
C30A C -0.05604(19) 1.0745(3) 0.2043(2) 0.0350(11) Uani 1 1 d . . .
H30C H -0.0927 1.0761 0.2200 0.042 Uiso 1 1 calc R . .
C12 C 0.17985(19) 0.9705(3) -0.0496(2) 0.0364(11) Uani 1 1 d . . .
H12A H 0.1380 0.9718 -0.0632 0.044 Uiso 1 1 calc R . .
C29A C -0.0201(2) 1.1502(3) 0.2095(2) 0.0365(12) Uani 1 1 d . . .
H29C H -0.0342 1.2031 0.2265 0.044 Uiso 1 1 calc R . .
C28A C 0.03633(19) 1.1491(3) 0.1898(2) 0.0321(11) Uani 1 1 d . . .
C21 C 0.4529(2) 1.0668(4) 0.4003(3) 0.0591(16) Uani 1 1 d . . .
H21A H 0.4755 1.1028 0.3747 0.071 Uiso 1 1 calc R . .
C1 C 0.19840(19) 0.8235(3) 0.1961(2) 0.0303(10) Uani 1 1 d . . .
H1A H 0.1608 0.8252 0.1591 0.036 Uiso 1 1 calc R . .
H1B H 0.2250 0.7791 0.1813 0.036 Uiso 1 1 calc R . .
C5A C 0.1685(2) 1.2627(3) 0.3883(3) 0.0438(13) Uani 1 1 d . . .
H6C H 0.1507 1.3137 0.4032 0.053 Uiso 1 1 calc R . .
C24A C 0.02134(19) 0.8274(3) 0.1398(2) 0.0337(11) Uani 1 1 d . . .
H24C H 0.0050 0.8231 0.1831 0.040 Uiso 1 1 calc R . .
C3 C 0.2306(2) 0.7615(3) 0.3270(3) 0.0389(12) Uani 1 1 d . . .
H3A H 0.2637 0.7359 0.3119 0.047 Uiso 1 1 calc R . .
C22A C 0.05463(18) 0.7546(3) 0.0376(2) 0.0330(11) Uani 1 1 d . . .
H22C H 0.0626 0.7029 0.0129 0.040 Uiso 1 1 calc R . .
C25A C 0.0991(2) 1.2014(3) 0.0693(2) 0.0340(11) Uani 1 1 d . . .
H25C H 0.0630 1.1716 0.0427 0.041 Uiso 1 1 calc R . .
H25D H 0.1179 1.2302 0.0317 0.041 Uiso 1 1 calc R . .
C27A C 0.0748(2) 1.2316(3) 0.1984(3) 0.0389(12) Uani 1 1 d . . .
H27C H 0.1146 1.2170 0.2274 0.047 Uiso 1 1 calc R . .
H27D H 0.0571 1.2757 0.2267 0.047 Uiso 1 1 calc R . .
C17 C 0.38784(17) 0.7873(3) 0.3305(2) 0.0281(10) Uani 1 1 d . . .
C23A C 0.03288(19) 0.7492(3) 0.1034(2) 0.0338(11) Uani 1 1 d . . .
H23C H 0.0259 0.6940 0.1233 0.041 Uiso 1 1 calc R . .
C2A C 0.22391(19) 1.1069(3) 0.3495(2) 0.0287(10) Uani 1 1 d . . .
C29 C 0.4058(2) 0.6406(4) 0.3851(3) 0.0448(13) Uani 1 1 d . . .
H29A H 0.4053 0.5789 0.3802 0.054 Uiso 1 1 calc R . .
C9A C 0.3197(2) 1.1627(3) 0.0778(3) 0.0373(12) Uani 1 1 d . . .
H9C H 0.2882 1.1683 0.0361 0.045 Uiso 1 1 calc R . .
C19 C 0.41100(19) 0.9226(4) 0.4180(2) 0.0374(12) Uani 1 1 d . . .
C26 C 0.4044(2) 0.6649(3) 0.1880(3) 0.0430(12) Uani 1 1 d . . .
H26A H 0.4392 0.6259 0.2004 0.052 Uiso 1 1 calc R . .
H26B H 0.3822 0.6489 0.1379 0.052 Uiso 1 1 calc R . .
C27 C 0.3637(2) 0.6509(3) 0.2460(3) 0.0420(12) Uani 1 1 d . . .
H27A H 0.3240 0.6753 0.2254 0.050 Uiso 1 1 calc R . .
H27B H 0.3590 0.5875 0.2533 0.050 Uiso 1 1 calc R . .
C20A C 0.05484(17) 0.9137(3) 0.0454(2) 0.0259(10) Uani 1 1 d . . .
H20C H 0.0624 0.9686 0.0251 0.031 Uiso 1 1 calc R . .
C26A C 0.0814(2) 1.2725(3) 0.1213(3) 0.0421(12) Uani 1 1 d . . .
H26C H 0.0435 1.2995 0.0971 0.051 Uiso 1 1 calc R . .
H26D H 0.1119 1.3188 0.1300 0.051 Uiso 1 1 calc R . .
C11 C 0.2138(2) 0.9932(3) -0.1018(2) 0.0382(12) Uani 1 1 d . . .
H11A H 0.1952 1.0090 -0.1508 0.046 Uiso 1 1 calc R . .
C6A C 0.1393(2) 1.1831(4) 0.3840(2) 0.0403(12) Uani 1 1 d . . .
H7C H 0.1005 1.1806 0.3935 0.048 Uiso 1 1 calc R . .
C3A C 0.2518(2) 1.1913(3) 0.3520(2) 0.0416(12) Uani 1 1 d . . .
H4C H 0.2901 1.1956 0.3409 0.050 Uiso 1 1 calc R . .
C4 C 0.2246(2) 0.7521(3) 0.4017(3) 0.0447(13) Uani 1 1 d . . .
H4A H 0.2533 0.7206 0.4359 0.054 Uiso 1 1 calc R . .
C30 C 0.4247(2) 0.6785(4) 0.4562(3) 0.0490(15) Uani 1 1 d . . .
H30A H 0.4375 0.6422 0.4981 0.059 Uiso 1 1 calc R . .
C5 C 0.1757(2) 0.7896(3) 0.4251(3) 0.0434(13) Uani 1 1 d . . .
H5A H 0.1712 0.7829 0.4749 0.052 Uiso 1 1 calc R . .
C31 C 0.4246(2) 0.7686(4) 0.4645(3) 0.0467(14) Uani 1 1 d . . .
H31A H 0.4364 0.7930 0.5126 0.056 Uiso 1 1 calc R . .
C20 C 0.4450(2) 0.9783(4) 0.3804(3) 0.0469(14) Uani 1 1 d . . .
H20A H 0.4623 0.9555 0.3418 0.056 Uiso 1 1 calc R . .
C24 C 0.3852(2) 0.9600(4) 0.4752(2) 0.0477(14) Uani 1 1 d . . .
H24A H 0.3622 0.9247 0.5010 0.057 Uiso 1 1 calc R . .
C23 C 0.3937(2) 1.0492(5) 0.4935(3) 0.0597(17) Uani 1 1 d . . .
H23A H 0.3758 1.0731 0.5311 0.072 Uiso 1 1 calc R . .
C12A C 0.4142(2) 1.1445(4) 0.1992(3) 0.0577(16) Uani 1 1 d . . .
H12C H 0.4461 1.1378 0.2403 0.069 Uiso 1 1 calc R . .
C10A C 0.3771(2) 1.1931(4) 0.0736(3) 0.0529(15) Uani 1 1 d . . .
H10C H 0.3837 1.2197 0.0294 0.064 Uiso 1 1 calc R . .
C22 C 0.4279(2) 1.1038(4) 0.4575(3) 0.0656(17) Uani 1 1 d . . .
H22A H 0.4342 1.1634 0.4711 0.079 Uiso 1 1 calc R . .
C11A C 0.4241(2) 1.1838(4) 0.1349(3) 0.0584(16) Uani 1 1 d . . .
H11C H 0.4625 1.2042 0.1323 0.070 Uiso 1 1 calc R . .
C4A C 0.2241(2) 1.2666(4) 0.3704(3) 0.0479(13) Uani 1 1 d . . .
H5C H 0.2435 1.3213 0.3707 0.058 Uiso 1 1 calc R . .
C14 C 0.34343(17) 0.8661(3) 0.1269(2) 0.0251(10) Uani 1 1 d . . .
H14A H 0.3565 0.8531 0.0824 0.030 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.078(3) . ?
Zr1 O1A 2.083(3) . ?
Zr1 C1A 2.291(4) . ?
Zr1 N1A 2.303(4) . ?
Zr1 C1 2.305(4) . ?
Zr1 N1 2.341(3) . ?
O1 C16 1.310(5) . ?
O1A C16A 1.297(5) . ?
N1 C14 1.324(5) . ?
N1 C8 1.435(5) . ?
N1A C14A 1.326(5) . ?
N1A C8A 1.453(5) . ?
C16 C15 1.370(5) . ?
C16 C17 1.485(5) . ?
C15 C14 1.416(5) . ?
C15 C25 1.516(5) . ?
C7 C2 1.387(6) . ?
C7 C6 1.396(6) . ?
C17A C18A 1.397(6) . ?
C17A C28A 1.415(6) . ?
C17A C16A 1.494(5) . ?
C8 C9 1.379(5) . ?
C8 C13 1.392(5) . ?
C6 C5 1.375(6) . ?
C14A C15A 1.395(5) . ?
C9 C10 1.364(6) . ?
C16A C15A 1.375(6) . ?
C21A C20A 1.370(6) . ?
C21A C22A 1.385(6) . ?
C15A C25A 1.526(6) . ?
C2 C3 1.397(6) . ?
C2 C1 1.485(5) . ?
C13 C12 1.378(5) . ?
C1A C2A 1.484(6) . ?
C7A C6A 1.385(6) . ?
C7A C2A 1.391(6) . ?
C18A C31A 1.405(5) . ?
C18A C19A 1.483(6) . ?
C18 C31 1.385(6) . ?
C18 C17 1.413(6) . ?
C18 C19 1.489(7) . ?
C8A C9A 1.379(6) . ?
C8A C13A 1.393(6) . ?
C31A C30A 1.379(6) . ?
C28 C29 1.392(6) . ?
C28 C17 1.422(6) . ?
C28 C27 1.494(6) . ?
C19A C24A 1.389(6) . ?
C19A C20A 1.417(5) . ?
C13A C12A 1.397(6) . ?
C25 C26 1.507(6) . ?
C10 C11 1.380(6) . ?
C30A C29A 1.389(6) . ?
C12 C11 1.371(6) . ?
C29A C28A 1.394(6) . ?
C28A C27A 1.504(6) . ?
C21 C20 1.378(7) . ?
C21 C22 1.386(7) . ?
C5A C6A 1.359(7) . ?
C5A C4A 1.363(7) . ?
C24A C23A 1.395(6) . ?
C3 C4 1.388(6) . ?
C22A C23A 1.374(6) . ?
C25A C26A 1.526(6) . ?
C27A C26A 1.554(6) . ?
C2A C3A 1.410(6) . ?
C29 C30 1.389(7) . ?
C9A C10A 1.394(6) . ?
C19 C20 1.399(6) . ?
C19 C24 1.402(6) . ?
C26 C27 1.541(6) . ?
C3A C4A 1.365(6) . ?
C4 C5 1.380(6) . ?
C30 C31 1.361(7) . ?
C24 C23 1.383(8) . ?
C23 C22 1.376(8) . ?
C12A C11A 1.359(7) . ?
C10A C11A 1.379(7) . ?

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 O1A 160.41(10) . . ?
O1 Zr1 C1A 77.57(13) . . ?
O1A Zr1 C1A 92.21(13) . . ?
O1 Zr1 N1A 120.05(11) . . ?
O1A Zr1 N1A 77.15(11) . . ?
C1A Zr1 N1A 95.67(14) . . ?
O1 Zr1 C1 88.85(14) . . ?
O1A Zr1 C1 81.24(13) . . ?
C1A Zr1 C1 118.12(15) . . ?
N1A Zr1 C1 140.38(13) . . ?
O1 Zr1 N1 75.21(10) . . ?
O1A Zr1 N1 120.41(10) . . ?
C1A Zr1 N1 143.26(13) . . ?
N1A Zr1 N1 77.50(11) . . ?
C1 Zr1 N1 85.60(13) . . ?
C16 O1 Zr1 141.1(2) . . ?
C16A O1A Zr1 141.9(3) . . ?
C14 N1 C8 114.4(3) . . ?
C14 N1 Zr1 128.4(3) . . ?
C8 N1 Zr1 116.9(2) . . ?
C14A N1A C8A 115.1(4) . . ?
C14A N1A Zr1 126.7(3) . . ?
C8A N1A Zr1 118.1(3) . . ?
O1 C16 C15 122.2(4) . . ?
O1 C16 C17 115.6(3) . . ?
C15 C16 C17 122.0(4) . . ?
C16 C15 C14 121.8(4) . . ?
C16 C15 C25 119.6(4) . . ?
C14 C15 C25 118.4(4) . . ?
C2 C7 C6 121.7(4) . . ?
C18A C17A C28A 120.5(4) . . ?
C18A C17A C16A 122.9(4) . . ?
C28A C17A C16A 116.6(4) . . ?
C9 C8 C13 118.2(4) . . ?
C9 C8 N1 124.0(4) . . ?
C13 C8 N1 117.8(3) . . ?
C5 C6 C7 120.0(4) . . ?
N1A C14A C15A 129.3(4) . . ?
C10 C9 C8 121.4(4) . . ?
O1A C16A C15A 121.9(4) . . ?
O1A C16A C17A 116.2(3) . . ?
C15A C16A C17A 121.8(4) . . ?
C20A C21A C22A 120.5(4) . . ?
C16A C15A C14A 122.0(4) . . ?
C16A C15A C25A 118.9(4) . . ?
C14A C15A C25A 118.7(4) . . ?
C7 C2 C3 116.9(4) . . ?
C7 C2 C1 122.0(4) . . ?
C3 C2 C1 120.8(4) . . ?
C12 C13 C8 120.3(4) . . ?
C2A C1A Zr1 124.8(3) . . ?
C6A C7A C2A 120.9(5) . . ?
C17A C18A C31A 119.1(4) . . ?
C17A C18A C19A 122.9(4) . . ?
C31A C18A C19A 117.7(4) . . ?
C31 C18 C17 118.9(5) . . ?
C31 C18 C19 117.4(4) . . ?
C17 C18 C19 123.7(4) . . ?
C9A C8A C13A 119.5(4) . . ?
C9A C8A N1A 121.9(4) . . ?
C13A C8A N1A 118.6(4) . . ?
C30A C31A C18A 120.8(4) . . ?
C29 C28 C17 118.0(5) . . ?
C29 C28 C27 120.3(5) . . ?
C17 C28 C27 121.5(4) . . ?
C24A C19A C20A 116.1(4) . . ?
C24A C19A C18A 121.0(4) . . ?
C20A C19A C18A 122.7(4) . . ?
C8A C13A C12A 119.0(5) . . ?
C26 C25 C15 113.0(4) . . ?
C9 C10 C11 120.4(4) . . ?
C31A C30A C29A 119.4(4) . . ?
C11 C12 C13 120.7(4) . . ?
C30A C29A C28A 121.8(4) . . ?
C29A C28A C17A 118.2(4) . . ?
C29A C28A C27A 120.3(4) . . ?
C17A C28A C27A 121.5(4) . . ?
C20 C21 C22 121.9(5) . . ?
C2 C1 Zr1 98.7(3) . . ?
C6A C5A C4A 119.0(5) . . ?
C19A C24A C23A 122.4(4) . . ?
C4 C3 C2 121.9(4) . . ?
C23A C22A C21A 119.8(4) . . ?
C15A C25A C26A 113.0(4) . . ?
C28A C27A C26A 112.9(4) . . ?
C18 C17 C28 120.1(4) . . ?
C18 C17 C16 122.4(4) . . ?
C28 C17 C16 117.3(4) . . ?
C22A C23A C24A 119.4(4) . . ?
C7A C2A C3A 116.0(4) . . ?
C7A C2A C1A 122.8(4) . . ?
C3A C2A C1A 121.2(4) . . ?
C30 C29 C28 121.2(5) . . ?
C8A C9A C10A 120.4(4) . . ?
C20 C19 C24 117.9(5) . . ?
C20 C19 C18 121.2(4) . . ?
C24 C19 C18 120.6(5) . . ?
C25 C26 C27 111.7(4) . . ?
C28 C27 C26 113.7(4) . . ?
C21A C20A C19A 121.6(4) . . ?
C25A C26A C27A 111.0(4) . . ?
C12 C11 C10 119.2(4) . . ?
C5A C6A C7A 121.3(4) . . ?
C4A C3A C2A 121.8(5) . . ?
C5 C4 C3 119.8(4) . . ?
C31 C30 C29 120.2(5) . . ?
C6 C5 C4 119.8(4) . . ?
C30 C31 C18 121.6(5) . . ?
C21 C20 C19 120.3(5) . . ?
C23 C24 C19 120.3(5) . . ?
C22 C23 C24 121.9(5) . . ?
C11A C12A C13A 121.4(5) . . ?
C11A C10A C9A 120.1(5) . . ?
C23 C22 C21 117.6(6) . . ?
C12A C11A C10A 119.6(5) . . ?
C5A C4A C3A 120.8(5) . . ?
N1 C14 C15 127.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.05
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_7b
_database_code_depnum_ccdc_archive 'CCDC 1419054'
_audit_update_record             
;
2015-08-17 deposited with the CCDC.
2016-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H50 Hf N2 O2'
_chemical_formula_weight         1009.51

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.8992(11)
_cell_length_b                   19.3310(12)
_cell_length_c                   20.5734(13)
_cell_angle_alpha                97.5330(10)
_cell_angle_beta                 94.4190(10)
_cell_angle_gamma                116.1370(10)
_cell_volume                     6262.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5875
_exptl_absorpt_correction_T_max  0.7845
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21784
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         25.06
_reflns_number_total             21784
_reflns_number_gt                15061
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.208 0.339 2128 114 ' '
_platon_squeeze_details          
;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0807P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         21784
_refine_ls_number_parameters     1171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1579
_refine_ls_wR_factor_gt          0.1422
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.141019(18) 0.796208(15) 0.036034(13) 0.02647(9) Uani 1 1 d . . .
O1A O 0.0593(3) 0.8239(2) -0.0152(2) 0.0253(10) Uani 1 1 d . . .
O1 O 0.2146(3) 0.7466(2) 0.0555(2) 0.0330(11) Uani 1 1 d . . .
N1 N 0.0561(4) 0.6654(3) -0.0151(3) 0.0265(13) Uani 1 1 d . . .
N1A N 0.1835(4) 0.8016(3) -0.0706(3) 0.0298(13) Uani 1 1 d . . .
C15 C 0.1510(4) 0.6089(4) 0.0144(3) 0.0273(15) Uani 1 1 d . . .
C16A C 0.0386(4) 0.8365(4) -0.0707(3) 0.0303(16) Uani 1 1 d . . .
C1 C 0.2366(5) 0.9216(4) 0.0800(4) 0.0408(19) Uani 1 1 d . . .
H1A H 0.2059 0.9465 0.1035 0.049 Uiso 1 1 calc R . .
H1B H 0.2767 0.9189 0.1143 0.049 Uiso 1 1 calc R . .
C8A C 0.2404(5) 0.7689(4) -0.0869(4) 0.0357(17) Uani 1 1 d . . .
C19A C -0.0523(5) 0.8795(4) 0.0376(4) 0.0377(18) Uani 1 1 d . . .
C27A C -0.0825(6) 0.8157(4) -0.1525(4) 0.046(2) Uani 1 1 d . . .
C1A C 0.0766(5) 0.7794(4) 0.1261(3) 0.0410(19) Uani 1 1 d . . .
H1D H 0.1210 0.8120 0.1644 0.049 Uiso 1 1 calc R . .
H1C H 0.0386 0.8041 0.1225 0.049 Uiso 1 1 calc R . .
C14 C 0.0765(5) 0.6082(4) -0.0156(4) 0.042(2) Uani 1 1 d . . .
H14A H 0.0352 0.5588 -0.0397 0.051 Uiso 1 1 calc R . .
C8 C -0.0221(4) 0.6483(4) -0.0556(3) 0.0300(16) Uani 1 1 d . . .
C15A C 0.0861(5) 0.8423(4) -0.1219(3) 0.0361(17) Uani 1 1 d . . .
C9A C 0.2131(5) 0.7061(5) -0.1396(4) 0.043(2) Uani 1 1 d . . .
H9C H 0.1578 0.6840 -0.1636 0.052 Uiso 1 1 calc R . .
C2A C 0.0242(5) 0.6995(4) 0.1472(3) 0.0365(18) Uani 1 1 d . . .
C3A C 0.0560(5) 0.6495(4) 0.1580(4) 0.044(2) Uani 1 1 d . . .
H3C H 0.1130 0.6645 0.1526 0.052 Uiso 1 1 calc R . .
C26A C -0.0335(6) 0.8087(5) -0.2071(4) 0.052(2) Uani 1 1 d . . .
H26C H -0.0438 0.7536 -0.2190 0.062 Uiso 1 1 calc R . .
H26D H -0.0530 0.8234 -0.2470 0.062 Uiso 1 1 calc R . .
C18A C -0.0903(5) 0.8482(4) -0.0354(4) 0.0347(17) Uani 1 1 d . . .
C13A C 0.3192(5) 0.8020(5) -0.0542(4) 0.053(2) Uani 1 1 d . . .
H13C H 0.3399 0.8499 -0.0234 0.064 Uiso 1 1 calc R . .
C19 C 0.3590(5) 0.8052(4) 0.1584(4) 0.0364(17) Uani 1 1 d . . .
C17A C -0.0441(5) 0.8371(4) -0.0863(3) 0.0307(16) Uani 1 1 d . . .
C7A C -0.0604(5) 0.6750(5) 0.1527(4) 0.047(2) Uani 1 1 d . . .
H7C H -0.0845 0.7087 0.1447 0.056 Uiso 1 1 calc R . .
C17 C 0.2998(5) 0.6791(4) 0.0673(4) 0.0357(18) Uani 1 1 d . . .
C16 C 0.2183(5) 0.6767(4) 0.0476(4) 0.0361(18) Uani 1 1 d . . .
C20A C -0.0975(5) 0.8502(5) 0.0849(4) 0.049(2) Uani 1 1 d . . .
H20C H -0.1513 0.8060 0.0726 0.059 Uiso 1 1 calc R . .
C26 C 0.2436(5) 0.5504(4) -0.0130(4) 0.051(2) Uani 1 1 d . . .
H26A H 0.2456 0.5625 -0.0583 0.061 Uiso 1 1 calc R . .
H26B H 0.2511 0.5026 -0.0136 0.061 Uiso 1 1 calc R . .
C6A C -0.1100(6) 0.6045(6) 0.1692(4) 0.056(2) Uani 1 1 d . . .
H6C H -0.1675 0.5896 0.1724 0.067 Uiso 1 1 calc R . .
C30A C -0.1722(5) 0.8324(4) -0.0522(4) 0.044(2) Uani 1 1 d . . .
H30C H -0.2037 0.8384 -0.0187 0.052 Uiso 1 1 calc R . .
C20 C 0.4190(5) 0.8838(5) 0.1640(4) 0.053(2) Uani 1 1 d . . .
H20A H 0.4611 0.8970 0.1359 0.063 Uiso 1 1 calc R . .
C7 C 0.2527(6) 1.0094(4) -0.0027(4) 0.055(2) Uani 1 1 d . . .
H7A H 0.1946 0.9954 -0.0041 0.065 Uiso 1 1 calc R . .
C13 C -0.0839(5) 0.6600(4) -0.0264(4) 0.0345(17) Uani 1 1 d . . .
H13A H -0.0751 0.6791 0.0199 0.041 Uiso 1 1 calc R . .
C18 C 0.3666(5) 0.7421(4) 0.1129(4) 0.0391(18) Uani 1 1 d . . .
C29A C -0.2097(6) 0.8074(5) -0.1183(5) 0.059(3) Uani 1 1 d . . .
H29C H -0.2674 0.7946 -0.1294 0.071 Uiso 1 1 calc R . .
C24A C 0.0230(5) 0.9472(4) 0.0555(4) 0.0387(18) Uani 1 1 d . . .
H24C H 0.0539 0.9706 0.0221 0.046 Uiso 1 1 calc R . .
C28A C -0.1646(6) 0.8008(5) -0.1680(4) 0.056(2) Uani 1 1 d . . .
H28C H -0.1904 0.7859 -0.2131 0.067 Uiso 1 1 calc R . .
C12 C -0.1575(5) 0.6440(4) -0.0647(4) 0.050(2) Uani 1 1 d . . .
H12A H -0.2001 0.6509 -0.0441 0.060 Uiso 1 1 calc R . .
C27 C 0.3146(5) 0.6178(4) 0.0345(4) 0.0429(19) Uani 1 1 d . . .
C23 C 0.2949(6) 0.8432(5) 0.2448(4) 0.058(2) Uani 1 1 d . . .
H23A H 0.2508 0.8299 0.2710 0.070 Uiso 1 1 calc R . .
C11 C -0.1720(5) 0.6177(5) -0.1329(4) 0.052(2) Uani 1 1 d . . .
H11A H -0.2236 0.6065 -0.1588 0.062 Uiso 1 1 calc R . .
C25 C 0.1590(5) 0.5352(4) 0.0065(4) 0.046(2) Uani 1 1 d . . .
H25A H 0.1137 0.4949 -0.0281 0.055 Uiso 1 1 calc R . .
H25B H 0.1533 0.5152 0.0487 0.055 Uiso 1 1 calc R . .
C2 C 0.2877(5) 0.9766(4) 0.0385(4) 0.0389(19) Uani 1 1 d . . .
C14A C 0.1536(5) 0.8196(4) -0.1173(4) 0.042(2) Uani 1 1 d . . .
H14C H 0.1783 0.8185 -0.1565 0.051 Uiso 1 1 calc R . .
C23A C 0.0542(6) 0.9817(5) 0.1222(4) 0.044(2) Uani 1 1 d . . .
H23C H 0.1083 1.0255 0.1352 0.053 Uiso 1 1 calc R . .
C5 C 0.3816(8) 1.0820(7) -0.0427(7) 0.096(4) Uani 1 1 d . . .
H5A H 0.4136 1.1161 -0.0704 0.115 Uiso 1 1 calc R . .
C9 C -0.0361(5) 0.6214(4) -0.1235(4) 0.050(2) Uani 1 1 d . . .
H9A H 0.0052 0.6118 -0.1437 0.060 Uiso 1 1 calc R . .
C30 C 0.4465(5) 0.7413(5) 0.1209(4) 0.055(2) Uani 1 1 d . . .
H30A H 0.4918 0.7817 0.1518 0.066 Uiso 1 1 calc R . .
C10A C 0.2679(6) 0.6766(6) -0.1562(5) 0.075(3) Uani 1 1 d . . .
H10C H 0.2519 0.6386 -0.1956 0.090 Uiso 1 1 calc R . .
C10 C -0.1091(6) 0.6084(5) -0.1618(4) 0.054(2) Uani 1 1 d . . .
H10A H -0.1163 0.5929 -0.2085 0.065 Uiso 1 1 calc R . .
C25A C 0.0588(6) 0.8607(5) -0.1859(4) 0.053(2) Uani 1 1 d . . .
H25C H 0.0704 0.9163 -0.1795 0.063 Uiso 1 1 calc R . .
H25D H 0.0906 0.8517 -0.2206 0.063 Uiso 1 1 calc R . .
C29 C 0.4589(6) 0.6828(6) 0.0845(5) 0.064(3) Uani 1 1 d . . .
H29A H 0.5132 0.6852 0.0884 0.076 Uiso 1 1 calc R . .
C21 C 0.4178(6) 0.9414(5) 0.2091(5) 0.060(2) Uani 1 1 d . . .
H21A H 0.4579 0.9946 0.2118 0.072 Uiso 1 1 calc R . .
C4 C 0.4198(7) 1.0477(6) 0.0022(7) 0.093(4) Uani 1 1 d . . .
H4A H 0.4780 1.0612 0.0054 0.111 Uiso 1 1 calc R . .
C11A C 0.3469(6) 0.7002(5) -0.1174(5) 0.068(3) Uani 1 1 d . . .
H11C H 0.3799 0.6737 -0.1261 0.082 Uiso 1 1 calc R . .
C28 C 0.3935(6) 0.6217(5) 0.0431(5) 0.055(2) Uani 1 1 d . . .
H28A H 0.4025 0.5810 0.0197 0.066 Uiso 1 1 calc R . .
C24 C 0.2982(5) 0.7857(5) 0.2001(4) 0.047(2) Uani 1 1 d . . .
H24A H 0.2588 0.7324 0.1976 0.056 Uiso 1 1 calc R . .
C4A C 0.0100(7) 0.5771(5) 0.1765(4) 0.064(3) Uani 1 1 d . . .
H4C H 0.0352 0.5445 0.1855 0.077 Uiso 1 1 calc R . .
C21A C -0.0681(7) 0.8824(7) 0.1508(4) 0.067(3) Uani 1 1 d . . .
H21C H -0.0979 0.8579 0.1843 0.080 Uiso 1 1 calc R . .
C22A C 0.0051(7) 0.9508(7) 0.1669(4) 0.076(3) Uani 1 1 d . . .
H22C H 0.0218 0.9774 0.2117 0.091 Uiso 1 1 calc R . .
C22 C 0.3559(6) 0.9210(5) 0.2521(4) 0.052(2) Uani 1 1 d . . .
H22A H 0.3561 0.9600 0.2854 0.062 Uiso 1 1 calc R . .
C3 C 0.3717(6) 0.9989(5) 0.0369(4) 0.056(2) Uani 1 1 d . . .
H3A H 0.3973 0.9765 0.0638 0.067 Uiso 1 1 calc R . .
C6 C 0.2986(8) 1.0622(6) -0.0423(5) 0.083(3) Uani 1 1 d . . .
H6A H 0.2719 1.0841 -0.0687 0.100 Uiso 1 1 calc R . .
C12A C 0.3738(5) 0.7637(5) -0.0661(5) 0.061(3) Uani 1 1 d . . .
H12C H 0.4267 0.7825 -0.0389 0.074 Uiso 1 1 calc R . .
C5A C -0.0757(7) 0.5547(6) 0.1812(5) 0.078(4) Uani 1 1 d . . .
H5C H -0.1099 0.5055 0.1926 0.094 Uiso 1 1 calc R . .
Hf2 Hf 0.111687(19) 0.302310(16) 0.487426(13) 0.02994(10) Uani 1 1 d . . .
O1D O 0.1935(3) 0.4131(2) 0.4858(2) 0.0315(11) Uani 1 1 d . . .
O1C O 0.0277(3) 0.2128(2) 0.5243(2) 0.0346(12) Uani 1 1 d . . .
C1C C 0.0455(5) 0.2706(4) 0.3824(3) 0.0387(19) Uani 1 1 d . . .
H1E H 0.0878 0.2730 0.3533 0.046 Uiso 1 1 calc R . .
H1F H 0.0032 0.2149 0.3757 0.046 Uiso 1 1 calc R . .
N1D N 0.0374(4) 0.3689(3) 0.5242(3) 0.0314(14) Uani 1 1 d . . .
C16D C 0.2042(5) 0.4870(4) 0.4974(3) 0.0317(16) Uani 1 1 d . . .
C15D C 0.1402(5) 0.5025(4) 0.5162(4) 0.0349(17) Uani 1 1 d . . .
C19D C 0.3373(5) 0.4680(4) 0.4186(3) 0.0341(17) Uani 1 1 d . . .
C20C C -0.1525(5) 0.0667(4) 0.3955(4) 0.043(2) Uani 1 1 d . . .
H20E H -0.1992 0.0770 0.4003 0.052 Uiso 1 1 calc R . .
C4C C -0.1274(6) 0.3166(5) 0.3089(4) 0.053(2) Uani 1 1 d . . .
H4E H -0.1864 0.2893 0.2946 0.064 Uiso 1 1 calc R . .
C27D C 0.3079(5) 0.6264(5) 0.5331(4) 0.046(2) Uani 1 1 d . . .
C18C C -0.1303(5) 0.0721(5) 0.5185(4) 0.049(2) Uani 1 1 d . . .
C13D C -0.1085(5) 0.2679(4) 0.5053(4) 0.0426(19) Uani 1 1 d . . .
H13G H -0.1042 0.2555 0.4599 0.051 Uiso 1 1 calc R . .
C24D C 0.2775(5) 0.4416(4) 0.3596(4) 0.0419(19) Uani 1 1 d . . .
H24G H 0.2428 0.4662 0.3518 0.050 Uiso 1 1 calc R . .
C18D C 0.3513(5) 0.5395(4) 0.4662(4) 0.0374(18) Uani 1 1 d . . .
C17C C -0.0756(5) 0.1200(4) 0.5782(3) 0.0387(19) Uani 1 1 d . . .
C15C C 0.0633(6) 0.2187(5) 0.6385(4) 0.044(2) Uani 1 1 d . . .
C7C C 0.0432(5) 0.3933(4) 0.3506(3) 0.0411(19) Uani 1 1 d . . .
H7E H 0.1024 0.4209 0.3642 0.049 Uiso 1 1 calc R . .
C9C C 0.2343(6) 0.4630(5) 0.6722(5) 0.076(3) Uani 1 1 d . . .
H9E H 0.1846 0.4511 0.6916 0.091 Uiso 1 1 calc R . .
C2C C 0.0007(5) 0.3140(4) 0.3548(3) 0.0369(18) Uani 1 1 d . . .
C16C C 0.0089(5) 0.1860(4) 0.5780(4) 0.047(2) Uani 1 1 d . . .
C8C C 0.2414(5) 0.4070(5) 0.6279(4) 0.047(2) Uani 1 1 d . . .
C14D C 0.0629(5) 0.4438(4) 0.5308(4) 0.044(2) Uani 1 1 d . . .
H14G H 0.0257 0.4622 0.5476 0.053 Uiso 1 1 calc R . .
C19C C -0.1026(5) 0.0667(4) 0.4524(4) 0.0358(17) Uani 1 1 d . . .
C6C C -0.0002(6) 0.4341(5) 0.3262(4) 0.054(2) Uani 1 1 d . . .
H6E H 0.0307 0.4881 0.3245 0.064 Uiso 1 1 calc R . .
C26D C 0.2411(5) 0.6389(4) 0.5655(4) 0.046(2) Uani 1 1 d . . .
H26G H 0.2531 0.6945 0.5692 0.055 Uiso 1 1 calc R . .
H26H H 0.2424 0.6271 0.6109 0.055 Uiso 1 1 calc R . .
C3C C -0.0865(5) 0.2762(5) 0.3325(3) 0.043(2) Uani 1 1 d . . .
H3E H -0.1180 0.2220 0.3335 0.051 Uiso 1 1 calc R . .
C17D C 0.2877(4) 0.5504(4) 0.4968(4) 0.0363(18) Uani 1 1 d . . .
C20D C 0.3903(5) 0.4323(4) 0.4296(4) 0.0412(19) Uani 1 1 d . . .
H20G H 0.4300 0.4502 0.4690 0.049 Uiso 1 1 calc R . .
C25D C 0.1543(5) 0.5869(4) 0.5261(4) 0.0421(19) Uani 1 1 d . . .
H25G H 0.1501 0.6026 0.4826 0.051 Uiso 1 1 calc R . .
H25H H 0.1109 0.5922 0.5504 0.051 Uiso 1 1 calc R . .
C12D C -0.1838(5) 0.2238(5) 0.5289(4) 0.051(2) Uani 1 1 d . . .
H12G H -0.2302 0.1821 0.4999 0.062 Uiso 1 1 calc R . .
C13C C 0.3154(6) 0.4235(6) 0.6053(5) 0.079(4) Uani 1 1 d . . .
H13E H 0.3218 0.3840 0.5772 0.095 Uiso 1 1 calc R . .
C8D C -0.0409(5) 0.3287(4) 0.5468(4) 0.0380(18) Uani 1 1 d . . .
C23C C -0.0147(5) 0.0380(4) 0.3794(4) 0.042(2) Uani 1 1 d . . .
H23E H 0.0324 0.0285 0.3744 0.051 Uiso 1 1 calc R . .
C28D C 0.3881(5) 0.6874(4) 0.5409(4) 0.049(2) Uani 1 1 d . . .
H28G H 0.4001 0.7375 0.5649 0.059 Uiso 1 1 calc R . .
C2D C 0.2364(5) 0.2206(4) 0.5068(4) 0.0429(19) Uani 1 1 d . . .
C3D C 0.1937(6) 0.1633(4) 0.5484(4) 0.051(2) Uani 1 1 d . . .
H3G H 0.1339 0.1373 0.5413 0.061 Uiso 1 1 calc R . .
C5C C -0.0837(6) 0.3972(5) 0.3057(4) 0.056(2) Uani 1 1 d . . .
H5E H -0.1124 0.4243 0.2896 0.068 Uiso 1 1 calc R . .
C25C C 0.0393(7) 0.1843(5) 0.6976(4) 0.063(3) Uani 1 1 d . . .
H25E H 0.0753 0.2224 0.7377 0.075 Uiso 1 1 calc R . .
H25F H 0.0479 0.1369 0.6955 0.075 Uiso 1 1 calc R . .
C27C C -0.1069(6) 0.1121(5) 0.6385(4) 0.052(2) Uani 1 1 d . . .
C21C C -0.1334(6) 0.0518(5) 0.3333(4) 0.053(2) Uani 1 1 d . . .
H21E H -0.1670 0.0524 0.2955 0.064 Uiso 1 1 calc R . .
C11C C 0.3814(7) 0.5595(6) 0.6675(5) 0.073(3) Uani 1 1 d . . .
H11E H 0.4288 0.6094 0.6822 0.088 Uiso 1 1 calc R . .
C7D C 0.3242(6) 0.2533(5) 0.5203(4) 0.057(2) Uani 1 1 d . . .
H7G H 0.3573 0.2917 0.4961 0.068 Uiso 1 1 calc R . .
C23D C 0.2713(5) 0.3801(5) 0.3147(4) 0.053(2) Uani 1 1 d . . .
H23G H 0.2298 0.3605 0.2763 0.064 Uiso 1 1 calc R . .
C22C C -0.0661(6) 0.0360(4) 0.3250(4) 0.049(2) Uani 1 1 d . . .
H22E H -0.0553 0.0238 0.2816 0.059 Uiso 1 1 calc R . .
C10D C -0.1213(6) 0.2997(6) 0.6376(5) 0.061(3) Uani 1 1 d . . .
H10G H -0.1260 0.3113 0.6830 0.073 Uiso 1 1 calc R . .
C21D C 0.3836(5) 0.3708(4) 0.3818(4) 0.045(2) Uani 1 1 d . . .
H21G H 0.4186 0.3461 0.3881 0.054 Uiso 1 1 calc R . .
C5D C 0.3209(7) 0.1805(6) 0.6071(5) 0.068(3) Uani 1 1 d . . .
H5G H 0.3498 0.1691 0.6415 0.082 Uiso 1 1 calc R . .
C26C C -0.0513(7) 0.1628(5) 0.7019(4) 0.066(3) Uani 1 1 d . . .
H26E H -0.0686 0.1345 0.7391 0.079 Uiso 1 1 calc R . .
H26F H -0.0581 0.2112 0.7109 0.079 Uiso 1 1 calc R . .
C28C C -0.1892(7) 0.0599(6) 0.6396(5) 0.070(3) Uani 1 1 d . . .
H28E H -0.2103 0.0566 0.6807 0.084 Uiso 1 1 calc R . .
C4D C 0.2343(7) 0.1454(5) 0.5962(5) 0.063(3) Uani 1 1 d . . .
H4G H 0.2032 0.1086 0.6223 0.076 Uiso 1 1 calc R . .
C30D C 0.4319(5) 0.6038(5) 0.4761(4) 0.052(2) Uani 1 1 d . . .
H30G H 0.4752 0.5976 0.4561 0.062 Uiso 1 1 calc R . .
C30C C -0.2133(6) 0.0192(5) 0.5218(5) 0.062(3) Uani 1 1 d . . .
H30E H -0.2504 -0.0121 0.4823 0.075 Uiso 1 1 calc R . .
C9D C -0.0474(5) 0.3405(5) 0.6157(4) 0.044(2) Uani 1 1 d . . .
H9G H 0.0005 0.3773 0.6465 0.053 Uiso 1 1 calc R . .
C6D C 0.3647(6) 0.2312(6) 0.5685(5) 0.066(3) Uani 1 1 d . . .
H6G H 0.4243 0.2523 0.5742 0.080 Uiso 1 1 calc R . .
C29D C 0.4510(5) 0.6760(5) 0.5138(4) 0.056(2) Uani 1 1 d . . .
H29G H 0.5069 0.7173 0.5211 0.067 Uiso 1 1 calc R . .
C24C C -0.0340(5) 0.0544(4) 0.4414(4) 0.047(2) Uani 1 1 d . . .
H24E H 0.0024 0.0575 0.4790 0.056 Uiso 1 1 calc R . .
C12C C 0.3843(6) 0.5012(6) 0.6242(5) 0.081(4) Uani 1 1 d . . .
H12E H 0.4344 0.5126 0.6055 0.097 Uiso 1 1 calc R . .
C11D C -0.1892(6) 0.2420(5) 0.5949(5) 0.063(3) Uani 1 1 d . . .
H11G H -0.2406 0.2142 0.6109 0.075 Uiso 1 1 calc R . .
C29C C -0.2415(7) 0.0125(6) 0.5826(6) 0.076(3) Uani 1 1 d . . .
H29E H -0.2973 -0.0250 0.5848 0.091 Uiso 1 1 calc R . .
C10C C 0.3055(8) 0.5409(6) 0.6882(5) 0.087(4) Uani 1 1 d . . .
H10E H 0.2987 0.5813 0.7148 0.104 Uiso 1 1 calc R . .
N1C N 0.1699(4) 0.3328(3) 0.6018(3) 0.0380(15) Uani 1 1 d . . .
C22D C 0.3232(6) 0.3455(5) 0.3234(4) 0.055(2) Uani 1 1 d . . .
H22G H 0.3187 0.3044 0.2900 0.066 Uiso 1 1 calc R . .
C1D C 0.1913(5) 0.2422(6) 0.4601(5) 0.061(3) Uani 1 1 d . . .
H1G H 0.1538 0.1935 0.4283 0.073 Uiso 1 1 calc R . .
H1H H 0.2334 0.2763 0.4350 0.073 Uiso 1 1 calc R . .
C14C C 0.1365(6) 0.2930(5) 0.6452(4) 0.062(3) Uani 1 1 d . . .
H14E H 0.1644 0.3160 0.6894 0.075 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1 1.987(5) . ?
Hf1 O1A 2.033(4) . ?
Hf1 C1A 2.243(7) . ?
Hf1 C1 2.270(7) . ?
Hf1 N1 2.341(5) . ?
Hf1 N1A 2.376(5) . ?
O1A C16A 1.259(8) . ?
O1 C16 1.372(8) . ?
N1 C14 1.307(9) . ?
N1 C8 1.451(9) . ?
N1A C14A 1.227(9) . ?
N1A C8A 1.453(9) . ?
C15 C16 1.372(10) . ?
C15 C14 1.420(10) . ?
C15 C25 1.484(9) . ?
C16A C15A 1.390(9) . ?
C16A C17A 1.495(10) . ?
C1 C2 1.483(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C8A C13A 1.341(11) . ?
C8A C9A 1.393(10) . ?
C19A C20A 1.336(10) . ?
C19A C24A 1.381(10) . ?
C19A C18A 1.525(10) . ?
C27A C28A 1.368(12) . ?
C27A C17A 1.399(10) . ?
C27A C26A 1.507(11) . ?
C1A C2A 1.554(10) . ?
C1A H1D 0.9900 . ?
C1A H1C 0.9900 . ?
C14 H14A 0.9500 . ?
C8 C13 1.386(10) . ?
C8 C9 1.387(10) . ?
C15A C14A 1.459(11) . ?
C15A C25A 1.508(10) . ?
C9A C10A 1.376(11) . ?
C9A H9C 0.9500 . ?
C2A C3A 1.352(10) . ?
C2A C7A 1.392(11) . ?
C3A C4A 1.397(11) . ?
C3A H3C 0.9500 . ?
C26A C25A 1.496(12) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C18A C30A 1.365(10) . ?
C18A C17A 1.436(10) . ?
C13A C12A 1.481(11) . ?
C13A H13C 0.9500 . ?
C19 C24 1.389(10) . ?
C19 C20 1.406(10) . ?
C19 C18 1.499(10) . ?
C7A C6A 1.365(11) . ?
C7A H7C 0.9500 . ?
C17 C27 1.423(10) . ?
C17 C18 1.427(10) . ?
C17 C16 1.462(10) . ?
C20A C21A 1.372(12) . ?
C20A H20C 0.9500 . ?
C26 C25 1.507(10) . ?
C26 C27 1.510(11) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C6A C5A 1.385(14) . ?
C6A H6C 0.9500 . ?
C30A C29A 1.392(11) . ?
C30A H30C 0.9500 . ?
C20 C21 1.361(11) . ?
C20 H20A 0.9500 . ?
C7 C2 1.385(11) . ?
C7 C6 1.400(12) . ?
C7 H7A 0.9500 . ?
C13 C12 1.368(11) . ?
C13 H13A 0.9500 . ?
C18 C30 1.436(11) . ?
C29A C28A 1.378(12) . ?
C29A H29C 0.9500 . ?
C24A C23A 1.397(10) . ?
C24A H24C 0.9500 . ?
C28A H28C 0.9500 . ?
C12 C11 1.391(11) . ?
C12 H12A 0.9500 . ?
C27 C28 1.377(11) . ?
C23 C24 1.372(11) . ?
C23 C22 1.395(11) . ?
C23 H23A 0.9500 . ?
C11 C10 1.380(12) . ?
C11 H11A 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C2 C3 1.375(11) . ?
C14A H14C 0.9500 . ?
C23A C22A 1.335(12) . ?
C23A H23C 0.9500 . ?
C5 C6 1.362(15) . ?
C5 C4 1.490(17) . ?
C5 H5A 0.9500 . ?
C9 C10 1.375(11) . ?
C9 H9A 0.9500 . ?
C30 C29 1.383(11) . ?
C30 H30A 0.9500 . ?
C10A C11A 1.418(13) . ?
C10A H10C 0.9500 . ?
C10 H10A 0.9500 . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C29 C28 1.361(12) . ?
C29 H29A 0.9500 . ?
C21 C22 1.422(12) . ?
C21 H21A 0.9500 . ?
C4 C3 1.302(13) . ?
C4 H4A 0.9500 . ?
C11A C12A 1.382(12) . ?
C11A H11C 0.9500 . ?
C28 H28A 0.9500 . ?
C24 H24A 0.9500 . ?
C4A C5A 1.415(14) . ?
C4A H4C 0.9500 . ?
C21A C22A 1.366(14) . ?
C21A H21C 0.9500 . ?
C22A H22C 0.9500 . ?
C22 H22A 0.9500 . ?
C3 H3A 0.9500 . ?
C6 H6A 0.9500 . ?
C12A H12C 0.9500 . ?
C5A H5C 0.9500 . ?
Hf2 O1D 1.999(4) . ?
Hf2 O1C 2.015(4) . ?
Hf2 C1C 2.251(7) . ?
Hf2 C1D 2.261(8) . ?
Hf2 N1D 2.326(6) . ?
Hf2 N1C 2.385(6) . ?
O1D C16D 1.341(7) . ?
O1C C16C 1.287(9) . ?
C1C C2C 1.521(11) . ?
C1C H1E 0.9900 . ?
C1C H1F 0.9900 . ?
N1D C14D 1.294(9) . ?
N1D C8D 1.421(9) . ?
C16D C15D 1.376(10) . ?
C16D C17D 1.460(9) . ?
C15D C14D 1.436(10) . ?
C15D C25D 1.518(9) . ?
C19D C20D 1.419(10) . ?
C19D C24D 1.427(10) . ?
C19D C18D 1.495(10) . ?
C20C C21C 1.375(11) . ?
C20C C19C 1.417(10) . ?
C20C H20E 0.9500 . ?
C4C C3C 1.388(12) . ?
C4C C5C 1.418(12) . ?
C4C H4E 0.9500 . ?
C27D C28D 1.378(10) . ?
C27D C17D 1.432(10) . ?
C27D C26D 1.505(10) . ?
C18C C30C 1.397(11) . ?
C18C C17C 1.429(11) . ?
C18C C19C 1.491(10) . ?
C13D C8D 1.378(10) . ?
C13D C12D 1.406(10) . ?
C13D H13G 0.9500 . ?
C24D C23D 1.362(10) . ?
C24D H24G 0.9500 . ?
C18D C30D 1.406(10) . ?
C18D C17D 1.423(10) . ?
C17C C27C 1.399(10) . ?
C17C C16C 1.489(10) . ?
C15C C16C 1.400(11) . ?
C15C C14C 1.436(11) . ?
C15C C25C 1.464(10) . ?
C7C C2C 1.398(10) . ?
C7C C6C 1.436(12) . ?
C7C H7E 0.9500 . ?
C9C C8C 1.378(10) . ?
C9C C10C 1.455(13) . ?
C9C H9E 0.9500 . ?
C2C C3C 1.407(11) . ?
C8C C13C 1.354(12) . ?
C8C N1C 1.436(9) . ?
C14D H14G 0.9500 . ?
C19C C24C 1.378(11) . ?
C6C C5C 1.344(12) . ?
C6C H6E 0.9500 . ?
C26D C25D 1.517(10) . ?
C26D H26G 0.9900 . ?
C26D H26H 0.9900 . ?
C3C H3E 0.9500 . ?
C20D C21D 1.395(10) . ?
C20D H20G 0.9500 . ?
C25D H25G 0.9900 . ?
C25D H25H 0.9900 . ?
C12D C11D 1.378(12) . ?
C12D H12G 0.9500 . ?
C13C C12C 1.438(12) . ?
C13C H13E 0.9500 . ?
C8D C9D 1.428(10) . ?
C23C C22C 1.378(11) . ?
C23C C24C 1.379(10) . ?
C23C H23E 0.9500 . ?
C28D C29D 1.383(11) . ?
C28D H28G 0.9500 . ?
C2D C7D 1.398(11) . ?
C2D C1D 1.424(12) . ?
C2D C3D 1.466(11) . ?
C3D C4D 1.347(12) . ?
C3D H3G 0.9500 . ?
C5C H5E 0.9500 . ?
C25C C26C 1.500(13) . ?
C25C H25E 0.9900 . ?
C25C H25F 0.9900 . ?
C27C C28C 1.375(13) . ?
C27C C26C 1.503(13) . ?
C21C C22C 1.384(12) . ?
C21C H21E 0.9500 . ?
C11C C10C 1.362(14) . ?
C11C C12C 1.365(13) . ?
C11C H11E 0.9500 . ?
C7D C6D 1.402(12) . ?
C7D H7G 0.9500 . ?
C23D C22D 1.376(12) . ?
C23D H23G 0.9500 . ?
C22C H22E 0.9500 . ?
C10D C9D 1.357(11) . ?
C10D C11D 1.371(13) . ?
C10D H10G 0.9500 . ?
C21D C22D 1.427(11) . ?
C21D H21G 0.9500 . ?
C5D C6D 1.352(12) . ?
C5D C4D 1.376(13) . ?
C5D H5G 0.9500 . ?
C26C H26E 0.9900 . ?
C26C H26F 0.9900 . ?
C28C C29C 1.373(14) . ?
C28C H28E 0.9500 . ?
C4D H4G 0.9500 . ?
C30D C29D 1.385(10) . ?
C30D H30G 0.9500 . ?
C30C C29C 1.385(12) . ?
C30C H30E 0.9500 . ?
C9D H9G 0.9500 . ?
C6D H6G 0.9500 . ?
C29D H29G 0.9500 . ?
C24C H24E 0.9500 . ?
C12C H12E 0.9500 . ?
C11D H11G 0.9500 . ?
C29C H29E 0.9500 . ?
C10C H10E 0.9500 . ?
N1C C14C 1.266(10) . ?
C22D H22G 0.9500 . ?
C1D H1G 0.9900 . ?
C1D H1H 0.9900 . ?
C14C H14E 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 O1A 160.07(17) . . ?
O1 Hf1 C1A 98.6(2) . . ?
O1A Hf1 C1A 95.5(2) . . ?
O1 Hf1 C1 97.0(2) . . ?
O1A Hf1 C1 96.1(2) . . ?
C1A Hf1 C1 93.6(3) . . ?
O1 Hf1 N1 77.85(18) . . ?
O1A Hf1 N1 87.70(18) . . ?
C1A Hf1 N1 92.0(2) . . ?
C1 Hf1 N1 172.9(2) . . ?
O1 Hf1 N1A 87.5(2) . . ?
O1A Hf1 N1A 76.54(19) . . ?
C1A Hf1 N1A 169.4(3) . . ?
C1 Hf1 N1A 94.2(2) . . ?
N1 Hf1 N1A 80.73(17) . . ?
C16A O1A Hf1 144.1(4) . . ?
C16 O1 Hf1 143.6(4) . . ?
C14 N1 C8 117.1(6) . . ?
C14 N1 Hf1 125.8(5) . . ?
C8 N1 Hf1 116.7(4) . . ?
C14A N1A C8A 114.8(6) . . ?
C14A N1A Hf1 126.3(5) . . ?
C8A N1A Hf1 118.2(4) . . ?
C16 C15 C14 122.1(6) . . ?
C16 C15 C25 118.5(7) . . ?
C14 C15 C25 119.4(6) . . ?
O1A C16A C15A 122.4(7) . . ?
O1A C16A C17A 120.4(6) . . ?
C15A C16A C17A 116.9(6) . . ?
C2 C1 Hf1 122.1(5) . . ?
C2 C1 H1A 106.8 . . ?
Hf1 C1 H1A 106.8 . . ?
C2 C1 H1B 106.8 . . ?
Hf1 C1 H1B 106.8 . . ?
H1A C1 H1B 106.7 . . ?
C13A C8A C9A 121.0(7) . . ?
C13A C8A N1A 120.1(7) . . ?
C9A C8A N1A 118.7(7) . . ?
C20A C19A C24A 118.8(8) . . ?
C20A C19A C18A 120.3(7) . . ?
C24A C19A C18A 119.9(7) . . ?
C28A C27A C17A 120.5(8) . . ?
C28A C27A C26A 119.7(8) . . ?
C17A C27A C26A 119.8(8) . . ?
C2A C1A Hf1 125.7(5) . . ?
C2A C1A H1D 105.9 . . ?
Hf1 C1A H1D 105.9 . . ?
C2A C1A H1C 105.9 . . ?
Hf1 C1A H1C 105.9 . . ?
H1D C1A H1C 106.2 . . ?
N1 C14 C15 129.7(7) . . ?
N1 C14 H14A 115.1 . . ?
C15 C14 H14A 115.1 . . ?
C13 C8 C9 119.1(7) . . ?
C13 C8 N1 119.6(6) . . ?
C9 C8 N1 121.3(7) . . ?
C16A C15A C14A 120.0(6) . . ?
C16A C15A C25A 119.2(7) . . ?
C14A C15A C25A 120.2(6) . . ?
C10A C9A C8A 118.7(8) . . ?
C10A C9A H9C 120.7 . . ?
C8A C9A H9C 120.7 . . ?
C3A C2A C7A 117.0(7) . . ?
C3A C2A C1A 122.9(7) . . ?
C7A C2A C1A 120.0(7) . . ?
C2A C3A C4A 124.0(9) . . ?
C2A C3A H3C 118.0 . . ?
C4A C3A H3C 118.0 . . ?
C25A C26A C27A 110.9(6) . . ?
C25A C26A H26C 109.5 . . ?
C27A C26A H26C 109.5 . . ?
C25A C26A H26D 109.5 . . ?
C27A C26A H26D 109.5 . . ?
H26C C26A H26D 108.1 . . ?
C30A C18A C17A 119.4(7) . . ?
C30A C18A C19A 117.0(7) . . ?
C17A C18A C19A 123.6(7) . . ?
C8A C13A C12A 119.8(7) . . ?
C8A C13A H13C 120.1 . . ?
C12A C13A H13C 120.1 . . ?
C24 C19 C20 119.5(7) . . ?
C24 C19 C18 120.3(7) . . ?
C20 C19 C18 119.9(7) . . ?
C27A C17A C18A 118.8(7) . . ?
C27A C17A C16A 118.5(7) . . ?
C18A C17A C16A 122.1(6) . . ?
C6A C7A C2A 122.5(8) . . ?
C6A C7A H7C 118.7 . . ?
C2A C7A H7C 118.7 . . ?
C27 C17 C18 118.9(7) . . ?
C27 C17 C16 117.1(7) . . ?
C18 C17 C16 123.8(7) . . ?
O1 C16 C15 120.8(7) . . ?
O1 C16 C17 117.4(6) . . ?
C15 C16 C17 121.2(7) . . ?
C19A C20A C21A 121.6(9) . . ?
C19A C20A H20C 119.2 . . ?
C21A C20A H20C 119.2 . . ?
C25 C26 C27 111.6(6) . . ?
C25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C7A C6A C5A 119.5(9) . . ?
C7A C6A H6C 120.3 . . ?
C5A C6A H6C 120.3 . . ?
C18A C30A C29A 120.1(8) . . ?
C18A C30A H30C 120.0 . . ?
C29A C30A H30C 120.0 . . ?
C21 C20 C19 121.1(8) . . ?
C21 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C2 C7 C6 123.4(9) . . ?
C2 C7 H7A 118.3 . . ?
C6 C7 H7A 118.3 . . ?
C12 C13 C8 119.6(7) . . ?
C12 C13 H13A 120.2 . . ?
C8 C13 H13A 120.2 . . ?
C17 C18 C30 117.5(7) . . ?
C17 C18 C19 125.9(7) . . ?
C30 C18 C19 116.3(7) . . ?
C28A C29A C30A 121.1(8) . . ?
C28A C29A H29C 119.5 . . ?
C30A C29A H29C 119.5 . . ?
C19A C24A C23A 120.8(7) . . ?
C19A C24A H24C 119.6 . . ?
C23A C24A H24C 119.6 . . ?
C27A C28A C29A 120.0(8) . . ?
C27A C28A H28C 120.0 . . ?
C29A C28A H28C 120.0 . . ?
C13 C12 C11 121.9(8) . . ?
C13 C12 H12A 119.1 . . ?
C11 C12 H12A 119.1 . . ?
C28 C27 C17 120.6(7) . . ?
C28 C27 C26 120.3(7) . . ?
C17 C27 C26 119.0(7) . . ?
C24 C23 C22 120.4(8) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C10 C11 C12 118.1(8) . . ?
C10 C11 H11A 121.0 . . ?
C12 C11 H11A 121.0 . . ?
C15 C25 C26 109.5(6) . . ?
C15 C25 H25A 109.8 . . ?
C26 C25 H25A 109.8 . . ?
C15 C25 H25B 109.8 . . ?
C26 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
C3 C2 C7 114.7(7) . . ?
C3 C2 C1 123.9(7) . . ?
C7 C2 C1 121.4(8) . . ?
N1A C14A C15A 129.8(7) . . ?
N1A C14A H14C 115.1 . . ?
C15A C14A H14C 115.1 . . ?
C22A C23A C24A 117.3(9) . . ?
C22A C23A H23C 121.3 . . ?
C24A C23A H23C 121.3 . . ?
C6 C5 C4 116.9(11) . . ?
C6 C5 H5A 121.5 . . ?
C4 C5 H5A 121.5 . . ?
C10 C9 C8 120.7(8) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C29 C30 C18 121.1(8) . . ?
C29 C30 H30A 119.4 . . ?
C18 C30 H30A 119.4 . . ?
C9A C10A C11A 123.2(8) . . ?
C9A C10A H10C 118.4 . . ?
C11A C10A H10C 118.4 . . ?
C9 C10 C11 120.6(8) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C26A C25A C15A 108.8(7) . . ?
C26A C25A H25C 109.9 . . ?
C15A C25A H25C 109.9 . . ?
C26A C25A H25D 109.9 . . ?
C15A C25A H25D 109.9 . . ?
H25C C25A H25D 108.3 . . ?
C28 C29 C30 120.3(8) . . ?
C28 C29 H29A 119.8 . . ?
C30 C29 H29A 119.8 . . ?
C20 C21 C22 119.1(8) . . ?
C20 C21 H21A 120.4 . . ?
C22 C21 H21A 120.4 . . ?
C3 C4 C5 118.6(10) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
C12A C11A C10A 116.9(9) . . ?
C12A C11A H11C 121.6 . . ?
C10A C11A H11C 121.6 . . ?
C29 C28 C27 121.4(8) . . ?
C29 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
C23 C24 C19 120.2(8) . . ?
C23 C24 H24A 119.9 . . ?
C19 C24 H24A 119.9 . . ?
C3A C4A C5A 116.8(10) . . ?
C3A C4A H4C 121.6 . . ?
C5A C4A H4C 121.6 . . ?
C22A C21A C20A 118.1(9) . . ?
C22A C21A H21C 121.0 . . ?
C20A C21A H21C 121.0 . . ?
C23A C22A C21A 122.7(9) . . ?
C23A C22A H22C 118.6 . . ?
C21A C22A H22C 118.6 . . ?
C23 C22 C21 119.5(8) . . ?
C23 C22 H22A 120.2 . . ?
C21 C22 H22A 120.2 . . ?
C4 C3 C2 126.5(10) . . ?
C4 C3 H3A 116.7 . . ?
C2 C3 H3A 116.7 . . ?
C5 C6 C7 119.8(11) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C11A C12A C13A 119.2(8) . . ?
C11A C12A H12C 120.4 . . ?
C13A C12A H12C 120.4 . . ?
C6A C5A C4A 120.1(9) . . ?
C6A C5A H5C 120.0 . . ?
C4A C5A H5C 119.9 . . ?
O1D Hf2 O1C 157.08(18) . . ?
O1D Hf2 C1C 97.9(2) . . ?
O1C Hf2 C1C 99.1(2) . . ?
O1D Hf2 C1D 99.6(3) . . ?
O1C Hf2 C1D 95.0(3) . . ?
C1C Hf2 C1D 92.0(3) . . ?
O1D Hf2 N1D 78.68(19) . . ?
O1C Hf2 N1D 85.21(19) . . ?
C1C Hf2 N1D 92.8(2) . . ?
C1D Hf2 N1D 175.1(3) . . ?
O1D Hf2 N1C 84.92(19) . . ?
O1C Hf2 N1C 77.1(2) . . ?
C1C Hf2 N1C 174.9(2) . . ?
C1D Hf2 N1C 91.8(3) . . ?
N1D Hf2 N1C 83.5(2) . . ?
C16D O1D Hf2 143.0(4) . . ?
C16C O1C Hf2 143.8(5) . . ?
C2C C1C Hf2 123.5(5) . . ?
C2C C1C H1E 106.5 . . ?
Hf2 C1C H1E 106.5 . . ?
C2C C1C H1F 106.5 . . ?
Hf2 C1C H1F 106.5 . . ?
H1E C1C H1F 106.5 . . ?
C14D N1D C8D 113.3(6) . . ?
C14D N1D Hf2 126.0(5) . . ?
C8D N1D Hf2 120.5(4) . . ?
O1D C16D C15D 120.4(6) . . ?
O1D C16D C17D 118.2(6) . . ?
C15D C16D C17D 121.1(6) . . ?
C16D C15D C14D 123.2(7) . . ?
C16D C15D C25D 118.2(6) . . ?
C14D C15D C25D 118.4(7) . . ?
C20D C19D C24D 120.8(7) . . ?
C20D C19D C18D 118.8(7) . . ?
C24D C19D C18D 120.0(6) . . ?
C21C C20C C19C 120.1(8) . . ?
C21C C20C H20E 120.0 . . ?
C19C C20C H20E 120.0 . . ?
C3C C4C C5C 122.1(8) . . ?
C3C C4C H4E 119.0 . . ?
C5C C4C H4E 119.0 . . ?
C28D C27D C17D 121.1(7) . . ?
C28D C27D C26D 119.6(7) . . ?
C17D C27D C26D 119.2(7) . . ?
C30C C18C C17C 119.4(7) . . ?
C30C C18C C19C 115.9(8) . . ?
C17C C18C C19C 124.3(7) . . ?
C8D C13D C12D 121.2(7) . . ?
C8D C13D H13G 119.4 . . ?
C12D C13D H13G 119.4 . . ?
C23D C24D C19D 118.4(7) . . ?
C23D C24D H24G 120.8 . . ?
C19D C24D H24G 120.8 . . ?
C30D C18D C17D 117.5(7) . . ?
C30D C18D C19D 117.0(7) . . ?
C17D C18D C19D 125.2(7) . . ?
C27C C17C C18C 118.7(8) . . ?
C27C C17C C16C 118.1(7) . . ?
C18C C17C C16C 122.6(6) . . ?
C16C C15C C14C 119.5(7) . . ?
C16C C15C C25C 120.4(8) . . ?
C14C C15C C25C 119.3(8) . . ?
C2C C7C C6C 121.7(8) . . ?
C2C C7C H7E 119.1 . . ?
C6C C7C H7E 119.1 . . ?
C8C C9C C10C 117.7(9) . . ?
C8C C9C H9E 121.1 . . ?
C10C C9C H9E 121.1 . . ?
C7C C2C C3C 116.2(8) . . ?
C7C C2C C1C 122.3(7) . . ?
C3C C2C C1C 121.5(7) . . ?
O1C C16C C15C 122.9(7) . . ?
O1C C16C C17C 119.8(7) . . ?
C15C C16C C17C 117.2(7) . . ?
C13C C8C C9C 119.9(8) . . ?
C13C C8C N1C 119.0(7) . . ?
C9C C8C N1C 121.0(8) . . ?
N1D C14D C15D 128.5(7) . . ?
N1D C14D H14G 115.8 . . ?
C15D C14D H14G 115.8 . . ?
C24C C19C C20C 116.4(7) . . ?
C24C C19C C18C 123.8(7) . . ?
C20C C19C C18C 119.6(7) . . ?
C5C C6C C7C 121.3(8) . . ?
C5C C6C H6E 119.4 . . ?
C7C C6C H6E 119.4 . . ?
C27D C26D C25D 111.3(6) . . ?
C27D C26D H26G 109.4 . . ?
C25D C26D H26G 109.4 . . ?
C27D C26D H26H 109.4 . . ?
C25D C26D H26H 109.4 . . ?
H26G C26D H26H 108.0 . . ?
C4C C3C C2C 121.2(8) . . ?
C4C C3C H3E 119.4 . . ?
C2C C3C H3E 119.4 . . ?
C18D C17D C27D 118.7(6) . . ?
C18D C17D C16D 123.6(6) . . ?
C27D C17D C16D 117.5(7) . . ?
C21D C20D C19D 119.2(7) . . ?
C21D C20D H20G 120.4 . . ?
C19D C20D H20G 120.4 . . ?
C26D C25D C15D 108.4(6) . . ?
C26D C25D H25G 110.0 . . ?
C15D C25D H25G 110.0 . . ?
C26D C25D H25H 110.0 . . ?
C15D C25D H25H 110.0 . . ?
H25G C25D H25H 108.4 . . ?
C11D C12D C13D 118.9(8) . . ?
C11D C12D H12G 120.6 . . ?
C13D C12D H12G 120.5 . . ?
C8C C13C C12C 119.6(9) . . ?
C8C C13C H13E 120.2 . . ?
C12C C13C H13E 120.2 . . ?
C13D C8D N1D 121.0(6) . . ?
C13D C8D C9D 117.4(7) . . ?
N1D C8D C9D 120.6(7) . . ?
C22C C23C C24C 117.8(8) . . ?
C22C C23C H23E 121.1 . . ?
C24C C23C H23E 121.1 . . ?
C27D C28D C29D 120.2(7) . . ?
C27D C28D H28G 119.9 . . ?
C29D C28D H28G 119.9 . . ?
C7D C2D C1D 124.8(8) . . ?
C7D C2D C3D 113.0(8) . . ?
C1D C2D C3D 122.1(8) . . ?
C4D C3D C2D 123.9(9) . . ?
C4D C3D H3G 118.1 . . ?
C2D C3D H3G 118.1 . . ?
C6C C5C C4C 117.5(9) . . ?
C6C C5C H5E 121.2 . . ?
C4C C5C H5E 121.2 . . ?
C15C C25C C26C 110.1(8) . . ?
C15C C25C H25E 109.6 . . ?
C26C C25C H25E 109.6 . . ?
C15C C25C H25F 109.6 . . ?
C26C C25C H25F 109.6 . . ?
H25E C25C H25F 108.2 . . ?
C28C C27C C17C 120.2(9) . . ?
C28C C27C C26C 119.9(8) . . ?
C17C C27C C26C 119.9(8) . . ?
C20C C21C C22C 121.1(8) . . ?
C20C C21C H21E 119.5 . . ?
C22C C21C H21E 119.5 . . ?
C10C C11C C12C 115.0(10) . . ?
C10C C11C H11E 122.5 . . ?
C12C C11C H11E 122.5 . . ?
C6D C7D C2D 121.9(9) . . ?
C6D C7D H7G 119.0 . . ?
C2D C7D H7G 119.0 . . ?
C24D C23D C22D 122.0(8) . . ?
C24D C23D H23G 119.0 . . ?
C22D C23D H23G 119.0 . . ?
C23C C22C C21C 120.3(8) . . ?
C23C C22C H22E 119.9 . . ?
C21C C22C H22E 119.9 . . ?
C9D C10D C11D 120.6(8) . . ?
C9D C10D H10G 119.7 . . ?
C11D C10D H10G 119.7 . . ?
C20D C21D C22D 118.7(8) . . ?
C20D C21D H21G 120.6 . . ?
C22D C21D H21G 120.6 . . ?
C6D C5D C4D 119.7(10) . . ?
C6D C5D H5G 120.1 . . ?
C4D C5D H5G 120.1 . . ?
C27C C26C C25C 111.0(7) . . ?
C27C C26C H26E 109.4 . . ?
C25C C26C H26E 109.4 . . ?
C27C C26C H26F 109.4 . . ?
C25C C26C H26F 109.4 . . ?
H26E C26C H26F 108.0 . . ?
C29C C28C C27C 121.3(8) . . ?
C29C C28C H28E 119.3 . . ?
C27C C28C H28E 119.3 . . ?
C3D C4D C5D 119.9(9) . . ?
C3D C4D H4G 120.1 . . ?
C5D C4D H4G 120.1 . . ?
C29D C30D C18D 122.8(7) . . ?
C29D C30D H30G 118.6 . . ?
C18D C30D H30G 118.6 . . ?
C29C C30C C18C 120.1(9) . . ?
C29C C30C H30E 120.0 . . ?
C18C C30C H30E 120.0 . . ?
C10D C9D C8D 120.6(8) . . ?
C10D C9D H9G 119.7 . . ?
C8D C9D H9G 119.7 . . ?
C5D C6D C7D 121.5(10) . . ?
C5D C6D H6G 119.3 . . ?
C7D C6D H6G 119.3 . . ?
C28D C29D C30D 119.5(7) . . ?
C28D C29D H29G 120.2 . . ?
C30D C29D H29G 120.2 . . ?
C19C C24C C23C 124.3(8) . . ?
C19C C24C H24E 117.8 . . ?
C23C C24C H24E 117.8 . . ?
C11C C12C C13C 123.4(9) . . ?
C11C C12C H12E 118.3 . . ?
C13C C12C H12E 118.3 . . ?
C10D C11D C12D 120.8(8) . . ?
C10D C11D H11G 119.6 . . ?
C12D C11D H11G 119.6 . . ?
C28C C29C C30C 120.2(9) . . ?
C28C C29C H29E 119.9 . . ?
C30C C29C H29E 119.9 . . ?
C11C C10C C9C 123.9(10) . . ?
C11C C10C H10E 118.1 . . ?
C9C C10C H10E 118.1 . . ?
C14C N1C C8C 114.6(7) . . ?
C14C N1C Hf2 125.1(6) . . ?
C8C N1C Hf2 119.6(5) . . ?
C23D C22D C21D 120.8(8) . . ?
C23D C22D H22G 119.6 . . ?
C21D C22D H22G 119.6 . . ?
C2D C1D Hf2 124.4(6) . . ?
C2D C1D H1G 106.2 . . ?
Hf2 C1D H1G 106.2 . . ?
C2D C1D H1H 106.2 . . ?
Hf2 C1D H1H 106.2 . . ?
H1G C1D H1H 106.4 . . ?
N1C C14C C15C 130.6(8) . . ?
N1C C14C H14E 114.7 . . ?
C15C C14C H14E 114.7 . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.154
