# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_L-H4
_database_code_depnum_ccdc_archive 'CCDC 1950125'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2019-08-29 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H26 O9 Si2'
_chemical_formula_sum            'C30 H26 O9 Si2'
_chemical_formula_weight         586.69

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.1221(5)
_cell_length_b                   10.3996(5)
_cell_length_c                   24.2182(12)
_cell_angle_alpha                83.396(4)
_cell_angle_beta                 80.039(4)
_cell_angle_gamma                79.810(4)
_cell_volume                     2218.7(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    173.00(14)
_cell_measurement_reflns_used    2161
_cell_measurement_theta_min      2.6010
_cell_measurement_theta_max      25.1750

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_F_000             918
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.172
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_T_min  0.95543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.959
_oxdiff_exptl_absorpt_empirical_full_max 1.112
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      173.00(14)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            13006
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.516
_diffrn_reflns_theta_max         28.285
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             8749
_reflns_number_gt                4434
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    Olex-2
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ?

_refine_special_details          
;
Isotropic restraints were used on O4 in order to retain a sensible 
thermal parameter.

Carboxylic acid protons were initially located by searching the difference 
map for areas of residual electron density. H1A, H1C, H1D and H1F were all
refined freely using this method, although DFIX restraints were necessary
in some cases in order to obtain a sensible bond length.

Although the protons attached to O4 and O11 could be found in this manner,
use of DFIX restraints resulted in a high thermal parameter. Thus, they
were added as idealised protons using the AFIX147 command. This worked 
well for H11 but H4 was located in an unusual position, hence AFIX83 was
used instead for this proton. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0777P)²+0.3464P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8749
_refine_ls_number_parameters     576
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.1972
_refine_ls_wR_factor_gt          0.1551
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.036
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0364(5) 0.1640(4) 0.21378(16) 0.0468(10) Uani 1 1 d . . . . .
C2 C 0.0362(6) 0.0500(4) 0.18898(19) 0.0608(13) Uani 1 1 d . . . . .
H2 H 0.050240 0.052269 0.149108 0.073 Uiso 1 1 calc R U . . .
C3 C 0.0161(5) -0.0665(4) 0.22073(19) 0.0619(13) Uani 1 1 d . . . . .
H3 H 0.014550 -0.142262 0.202455 0.074 Uiso 1 1 calc R U . . .
C4 C -0.0016(5) -0.0741(4) 0.27872(18) 0.0515(11) Uani 1 1 d . . . . .
C5 C -0.0088(5) 0.0387(4) 0.30477(18) 0.0598(12) Uani 1 1 d . . . . .
H5 H -0.025715 0.036458 0.344664 0.072 Uiso 1 1 calc R U . . .
C6 C 0.0088(5) 0.1552(4) 0.27214(18) 0.0590(12) Uani 1 1 d . . . . .
H6 H 0.001678 0.232447 0.290576 0.071 Uiso 1 1 calc R U . . .
C7 C -0.0140(5) -0.2009(4) 0.31227(19) 0.0539(11) Uani 1 1 d . . . . .
C8 C 0.1433(5) 0.2844(3) 0.09708(16) 0.0447(10) Uani 1 1 d . . . . .
C9 C 0.2733(5) 0.1920(4) 0.08381(18) 0.0592(12) Uani 1 1 d . . . . .
H9 H 0.324257 0.148156 0.113386 0.071 Uiso 1 1 calc R U . . .
C10 C 0.3286(5) 0.1633(4) 0.03020(18) 0.0585(12) Uani 1 1 d . . . . .
H10 H 0.416203 0.099299 0.022824 0.070 Uiso 1 1 calc R U . . .
C11 C 0.2573(6) 0.2272(4) -0.01405(17) 0.0556(12) Uani 1 1 d . . . . .
C12 C 0.1276(6) 0.3170(4) -0.00146(19) 0.0716(15) Uani 1 1 d . . . . .
H12 H 0.075990 0.360000 -0.031017 0.086 Uiso 1 1 calc R U . . .
C13 C 0.0725(6) 0.3449(4) 0.05265(18) 0.0610(13) Uani 1 1 d . . . . .
H13 H -0.016543 0.407264 0.059960 0.073 Uiso 1 1 calc R U . . .
C14 C 0.3152(6) 0.1957(4) -0.07248(18) 0.0636(14) Uani 1 1 d . . . . .
C15 C -0.1016(5) 0.4454(4) 0.17809(19) 0.0641(13) Uani 1 1 d . . . . .
H15A H -0.135389 0.460675 0.217810 0.096 Uiso 1 1 calc R U . . .
H15B H -0.181156 0.414245 0.163267 0.096 Uiso 1 1 calc R U . . .
H15C H -0.079681 0.527503 0.156679 0.096 Uiso 1 1 calc R U . . .
C16 C 0.5012(5) 0.3665(4) 0.14302(19) 0.0577(12) Uani 1 1 d . . . . .
C17 C 0.5742(5) 0.2505(4) 0.16509(19) 0.0597(12) Uani 1 1 d . . . . .
H17 H 0.548219 0.224346 0.203944 0.072 Uiso 1 1 calc R U . . .
C18 C 0.6861(5) 0.1694(4) 0.1321(2) 0.0650(13) Uani 1 1 d . . . . .
H18 H 0.734130 0.089350 0.148682 0.078 Uiso 1 1 calc R U . . .
C19 C 0.7271(5) 0.2049(5) 0.0755(2) 0.0643(13) Uani 1 1 d . . . . .
C20 C 0.6592(6) 0.3223(5) 0.0527(2) 0.0841(17) Uani 1 1 d . . . . .
H20 H 0.687677 0.348429 0.013979 0.101 Uiso 1 1 calc R U . . .
C21 C 0.5477(6) 0.4046(5) 0.0859(2) 0.0779(16) Uani 1 1 d . . . . .
H21 H 0.503393 0.486657 0.069628 0.094 Uiso 1 1 calc R U . . .
C22 C 0.8435(6) 0.1155(5) 0.0409(2) 0.0700(14) Uani 1 1 d . . . . .
C23 C 0.3813(5) 0.4674(4) 0.25782(18) 0.0499(11) Uani 1 1 d . . . . .
C24 C 0.2951(6) 0.4148(5) 0.3051(2) 0.0741(15) Uani 1 1 d . . . . .
H24 H 0.215129 0.371678 0.300408 0.089 Uiso 1 1 calc R U . . .
C25 C 0.3220(6) 0.4233(5) 0.3589(2) 0.0754(15) Uani 1 1 d . . . . .
H25 H 0.259755 0.387064 0.390299 0.091 Uiso 1 1 calc R U . . .
C26 C 0.4371(5) 0.4832(4) 0.36756(19) 0.0514(11) Uani 1 1 d . . . . .
C27 C 0.5259(6) 0.5350(5) 0.3214(2) 0.0710(14) Uani 1 1 d . . . . .
H27 H 0.606413 0.576823 0.326662 0.085 Uiso 1 1 calc R U . . .
C28 C 0.4989(6) 0.5267(4) 0.2673(2) 0.0684(14) Uani 1 1 d . . . . .
H28 H 0.562157 0.562347 0.236066 0.082 Uiso 1 1 calc R U . . .
C29 C 0.4664(6) 0.4913(4) 0.4252(2) 0.0551(12) Uani 1 1 d . . . . .
C30 C 0.2820(6) 0.6268(4) 0.1519(2) 0.0807(16) Uani 1 1 d . . . . .
H30A H 0.270904 0.620072 0.112839 0.121 Uiso 1 1 calc R U . . .
H30B H 0.360096 0.680136 0.152467 0.121 Uiso 1 1 calc R U . . .
H30C H 0.186025 0.667958 0.172256 0.121 Uiso 1 1 calc R U . . .
C31 C 0.2714(4) 0.8494(4) 0.50980(16) 0.0426(10) Uani 1 1 d . . . . .
C32 C 0.2084(5) 0.7630(4) 0.48404(17) 0.0481(11) Uani 1 1 d . . . . .
H32 H 0.205830 0.777242 0.444739 0.058 Uiso 1 1 calc R U . . .
C33 C 0.1502(5) 0.6581(4) 0.51422(17) 0.0474(11) Uani 1 1 d . . . . .
H33 H 0.109612 0.600486 0.495422 0.057 Uiso 1 1 calc R U . . .
C34 C 0.1502(5) 0.6358(4) 0.57130(17) 0.0451(10) Uani 1 1 d . . . . .
C35 C 0.2110(5) 0.7205(4) 0.59822(17) 0.0529(11) Uani 1 1 d . . . . .
H35 H 0.211479 0.706045 0.637643 0.063 Uiso 1 1 calc R U . . .
C36 C 0.2701(5) 0.8246(4) 0.56820(17) 0.0519(11) Uani 1 1 d . . . . .
H36 H 0.311228 0.881243 0.587307 0.062 Uiso 1 1 calc R U . . .
C37 C 0.0958(5) 0.5203(4) 0.60441(19) 0.0501(11) Uani 1 1 d . . . . .
C38 C 0.4138(5) 0.9692(4) 0.39685(16) 0.0447(10) Uani 1 1 d . . . . .
C39 C 0.3346(6) 1.0308(5) 0.35464(19) 0.0741(15) Uani 1 1 d . . . . .
H39 H 0.246454 1.092716 0.364279 0.089 Uiso 1 1 calc R U . . .
C40 C 0.3798(6) 1.0051(5) 0.2987(2) 0.0776(16) Uani 1 1 d . . . . .
H40 H 0.321553 1.048451 0.271043 0.093 Uiso 1 1 calc R U . . .
C41 C 0.5062(5) 0.9187(4) 0.28298(17) 0.0508(11) Uani 1 1 d . . . . .
C42 C 0.5897(5) 0.8579(4) 0.32379(18) 0.0584(12) Uani 1 1 d . . . . .
H42 H 0.679822 0.798685 0.313485 0.070 Uiso 1 1 calc R U . . .
C43 C 0.5435(5) 0.8823(4) 0.37941(18) 0.0564(12) Uani 1 1 d . . . . .
H43 H 0.602382 0.838316 0.406750 0.068 Uiso 1 1 calc R U . . .
C44 C 0.5542(6) 0.8869(4) 0.22416(18) 0.0547(12) Uani 1 1 d . . . . .
C45 C 0.2129(6) 1.1434(4) 0.48410(19) 0.0708(14) Uani 1 1 d . . . . .
H45A H 0.175576 1.146724 0.524447 0.106 Uiso 1 1 calc R U . . .
H45B H 0.128518 1.142454 0.464098 0.106 Uiso 1 1 calc R U . . .
H45C H 0.260604 1.220537 0.469860 0.106 Uiso 1 1 calc R U . . .
O1 O 0.1997(3) 0.3742(3) 0.19696(12) 0.0582(8) Uani 1 1 d . . . . .
O2 O -0.0091(4) -0.2998(3) 0.28476(13) 0.0669(10) Uani 1 1 d . . . . .
O3 O -0.0271(4) -0.2073(3) 0.36505(13) 0.0704(9) Uani 1 1 d . . . . .
O4 O 0.2438(5) 0.2575(3) -0.11043(14) 0.0946(12) Uani 1 1 d . U . . .
H4 H 0.285526 0.232293 -0.141926 0.142 Uiso 1 1 calc R U . . .
O5 O 0.4289(4) 0.1079(3) -0.08283(12) 0.0711(10) Uani 1 1 d . . . . .
O6 O 0.9146(4) 0.0154(3) 0.06404(14) 0.0810(11) Uani 1 1 d . . . . .
O7 O 0.8624(4) 0.1480(4) -0.01224(16) 0.0925(12) Uani 1 1 d D . . . .
O8 O 0.4002(4) 0.4213(3) 0.46466(15) 0.0694(9) Uani 1 1 d D . . . .
O9 O 0.5542(4) 0.5671(3) 0.43219(13) 0.0657(9) Uani 1 1 d . . . . .
O10 O 0.500000 1.000000 0.500000 0.0673(13) Uani 1 2 d S . P . .
O11 O 0.0644(4) 0.4335(3) 0.57696(13) 0.0664(9) Uani 1 1 d . . . . .
H11 H 0.059951 0.363536 0.597858 0.100 Uiso 1 1 calc R U . . .
O12 O 0.0848(4) 0.5107(3) 0.65735(12) 0.0588(8) Uani 1 1 d . . . . .
O13 O 0.6727(4) 0.8073(3) 0.21230(13) 0.0767(10) Uani 1 1 d . . . . .
O14 O 0.4707(4) 0.9393(3) 0.18821(15) 0.0760(11) Uani 1 1 d . . . . .
SI1 Si 0.07050(14) 0.32074(10) 0.17155(5) 0.0461(3) Uani 1 1 d . . . . .
SI2 Si 0.33739(15) 0.45958(12) 0.18633(5) 0.0561(4) Uani 1 1 d . . . . .
SI3 Si 0.35232(14) 0.99347(11) 0.47264(5) 0.0462(3) Uani 1 1 d . . . . .
H1A H -0.044(7) -0.372(6) 0.305(2) 0.12(2) Uiso 1 1 d . . . . .
H1C H 0.922(4) 0.088(3) -0.0341(16) 0.078(15) Uiso 1 1 d D . . . .
H1D H 0.408(7) 0.434(5) 0.5003(10) 0.14(3) Uiso 1 1 d D . . . .
H1F H 0.499(7) 0.926(5) 0.154(3) 0.12(2) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.387(5) . ?
C1 C2 1.389(5) . ?
C1 SI1 1.867(4) . ?
C2 C3 1.382(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(5) . ?
C4 C7 1.478(6) . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O3 1.258(5) . ?
C7 O2 1.278(5) . ?
C8 C13 1.383(5) . ?
C8 C9 1.402(6) . ?
C8 SI1 1.868(4) . ?
C9 C10 1.356(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(6) . ?
C11 C14 1.475(6) . ?
C12 C13 1.364(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 O5 1.265(5) . ?
C14 O4 1.267(5) . ?
C15 SI1 1.847(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.369(6) . ?
C16 C21 1.407(6) . ?
C16 SI2 1.857(5) . ?
C17 C18 1.401(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.369(6) . ?
C19 C22 1.489(6) . ?
C20 C21 1.408(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O6 1.254(6) . ?
C22 O7 1.281(6) . ?
C23 C24 1.388(6) . ?
C23 C28 1.392(6) . ?
C23 SI2 1.857(4) . ?
C24 C25 1.382(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.369(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.377(6) . ?
C26 C29 1.481(6) . ?
C27 C28 1.390(6) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 O9 1.262(5) . ?
C29 O8 1.266(5) . ?
C30 SI2 1.864(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.400(5) . ?
C31 C36 1.407(5) . ?
C31 SI3 1.858(4) . ?
C32 C33 1.377(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.392(5) . ?
C34 C37 1.478(6) . ?
C35 C36 1.372(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 O12 1.262(5) . ?
C37 O11 1.278(5) . ?
C38 C39 1.385(5) . ?
C38 C43 1.390(6) . ?
C38 SI3 1.857(4) . ?
C39 C40 1.389(6) . ?
C39 H39 0.9500 . ?
C40 C41 1.357(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.379(6) . ?
C41 C44 1.474(6) . ?
C42 C43 1.379(5) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 O13 1.251(5) . ?
C44 O14 1.269(5) . ?
C45 SI3 1.844(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
O1 SI1 1.624(3) . ?
O1 SI2 1.632(3) . ?
O2 H1A 0.92(6) . ?
O4 H4 0.8400 . ?
O7 H1C 0.909(10) . ?
O8 H1D 0.904(10) . ?
O10 SI3 1.6155(12) . ?
O10 SI3 1.6155(12) 2_676 ?
O11 H11 0.8400 . ?
O14 H1F 0.84(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
C6 C1 C2 116.1(4) . . ?
C6 C1 SI1 121.5(3) . . ?
C2 C1 SI1 122.4(3) . . ?
C3 C2 C1 121.8(4) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 C7 120.4(4) . . ?
C5 C4 C7 120.7(4) . . ?
C4 C5 C6 119.4(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 122.9(4) . . ?
C5 C6 H6 118.5 . . ?
C1 C6 H6 118.6 . . ?
O3 C7 O2 123.6(4) . . ?
O3 C7 C4 119.9(4) . . ?
O2 C7 C4 116.5(4) . . ?
C13 C8 C9 116.7(4) . . ?
C13 C8 SI1 122.4(3) . . ?
C9 C8 SI1 120.9(3) . . ?
C10 C9 C8 122.2(4) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C11 120.1(4) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 118.2(4) . . ?
C12 C11 C14 121.0(4) . . ?
C10 C11 C14 120.7(4) . . ?
C13 C12 C11 121.2(4) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C8 121.5(4) . . ?
C12 C13 H13 119.2 . . ?
C8 C13 H13 119.2 . . ?
O5 C14 O4 122.8(4) . . ?
O5 C14 C11 120.2(4) . . ?
O4 C14 C11 117.0(5) . . ?
SI1 C15 H15A 109.5 . . ?
SI1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
SI1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 117.3(4) . . ?
C17 C16 SI2 120.0(4) . . ?
C21 C16 SI2 122.5(4) . . ?
C16 C17 C18 121.9(5) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C19 C18 C17 120.5(4) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 118.8(4) . . ?
C20 C19 C22 121.5(5) . . ?
C18 C19 C22 119.6(5) . . ?
C19 C20 C21 120.8(5) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C20 120.6(5) . . ?
C16 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
O6 C22 O7 124.3(5) . . ?
O6 C22 C19 120.0(5) . . ?
O7 C22 C19 115.7(5) . . ?
C24 C23 C28 116.4(4) . . ?
C24 C23 SI2 120.8(3) . . ?
C28 C23 SI2 122.8(4) . . ?
C25 C24 C23 122.0(5) . . ?
C25 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 118.6(4) . . ?
C25 C26 C29 120.7(5) . . ?
C27 C26 C29 120.7(4) . . ?
C26 C27 C28 120.7(5) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C23 121.5(5) . . ?
C27 C28 H28 119.3 . . ?
C23 C28 H28 119.3 . . ?
O9 C29 O8 124.2(4) . . ?
O9 C29 C26 118.6(5) . . ?
O8 C29 C26 117.2(4) . . ?
SI2 C30 H30A 109.5 . . ?
SI2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
SI2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 116.6(4) . . ?
C32 C31 SI3 124.7(3) . . ?
C36 C31 SI3 118.6(3) . . ?
C33 C32 C31 121.7(4) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C34 C33 C32 120.7(4) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C35 119.0(4) . . ?
C33 C34 C37 122.0(4) . . ?
C35 C34 C37 118.9(4) . . ?
C36 C35 C34 120.5(4) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C31 121.5(4) . . ?
C35 C36 H36 119.2 . . ?
C31 C36 H36 119.2 . . ?
O12 C37 O11 123.5(4) . . ?
O12 C37 C34 119.4(4) . . ?
O11 C37 C34 117.1(4) . . ?
C39 C38 C43 115.7(4) . . ?
C39 C38 SI3 123.8(3) . . ?
C43 C38 SI3 120.5(3) . . ?
C38 C39 C40 122.2(4) . . ?
C38 C39 H39 118.9 . . ?
C40 C39 H39 118.9 . . ?
C41 C40 C39 120.8(4) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C40 C41 C42 118.5(4) . . ?
C40 C41 C44 121.8(4) . . ?
C42 C41 C44 119.7(4) . . ?
C43 C42 C41 120.6(4) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C38 122.2(4) . . ?
C42 C43 H43 118.9 . . ?
C38 C43 H43 118.9 . . ?
O13 C44 O14 123.2(4) . . ?
O13 C44 C41 118.8(4) . . ?
O14 C44 C41 118.0(4) . . ?
SI3 C45 H45A 109.5 . . ?
SI3 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
SI3 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
SI1 O1 SI2 148.2(2) . . ?
C7 O2 H1A 116(4) . . ?
C14 O4 H4 109.5 . . ?
C22 O7 H1C 116(3) . . ?
C29 O8 H1D 117(4) . . ?
SI3 O10 SI3 180.00(7) . 2_676 ?
C37 O11 H11 109.5 . . ?
C44 O14 H1F 119(4) . . ?
O1 SI1 C15 108.44(18) . . ?
O1 SI1 C1 107.05(16) . . ?
C15 SI1 C1 111.2(2) . . ?
O1 SI1 C8 109.03(18) . . ?
C15 SI1 C8 112.66(19) . . ?
C1 SI1 C8 108.33(17) . . ?
O1 SI2 C23 104.18(19) . . ?
O1 SI2 C16 107.95(18) . . ?
C23 SI2 C16 109.8(2) . . ?
O1 SI2 C30 111.9(2) . . ?
C23 SI2 C30 111.4(2) . . ?
C16 SI2 C30 111.3(2) . . ?
O10 SI3 C45 110.17(17) . . ?
O10 SI3 C38 108.03(14) . . ?
C45 SI3 C38 112.51(19) . . ?
O10 SI3 C31 106.42(13) . . ?
C45 SI3 C31 109.3(2) . . ?
C38 SI3 C31 110.21(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.7(7) . . . . ?
SI1 C1 C2 C3 177.6(4) . . . . ?
C1 C2 C3 C4 -1.3(7) . . . . ?
C2 C3 C4 C5 4.2(7) . . . . ?
C2 C3 C4 C7 -176.4(4) . . . . ?
C3 C4 C5 C6 -2.9(7) . . . . ?
C7 C4 C5 C6 177.6(4) . . . . ?
C4 C5 C6 C1 -1.2(7) . . . . ?
C2 C1 C6 C5 3.9(7) . . . . ?
SI1 C1 C6 C5 -176.4(4) . . . . ?
C3 C4 C7 O3 178.6(4) . . . . ?
C5 C4 C7 O3 -2.0(7) . . . . ?
C3 C4 C7 O2 -0.8(6) . . . . ?
C5 C4 C7 O2 178.7(4) . . . . ?
C13 C8 C9 C10 0.5(7) . . . . ?
SI1 C8 C9 C10 179.8(4) . . . . ?
C8 C9 C10 C11 0.8(7) . . . . ?
C9 C10 C11 C12 -1.8(7) . . . . ?
C9 C10 C11 C14 -179.2(4) . . . . ?
C10 C11 C12 C13 1.6(7) . . . . ?
C14 C11 C12 C13 179.0(4) . . . . ?
C11 C12 C13 C8 -0.3(8) . . . . ?
C9 C8 C13 C12 -0.7(7) . . . . ?
SI1 C8 C13 C12 180.0(4) . . . . ?
C12 C11 C14 O5 -175.9(4) . . . . ?
C10 C11 C14 O5 1.4(7) . . . . ?
C12 C11 C14 O4 2.3(7) . . . . ?
C10 C11 C14 O4 179.6(5) . . . . ?
C21 C16 C17 C18 -2.8(7) . . . . ?
SI2 C16 C17 C18 172.2(4) . . . . ?
C16 C17 C18 C19 0.3(7) . . . . ?
C17 C18 C19 C20 1.6(7) . . . . ?
C17 C18 C19 C22 -178.4(4) . . . . ?
C18 C19 C20 C21 -1.0(8) . . . . ?
C22 C19 C20 C21 179.0(5) . . . . ?
C17 C16 C21 C20 3.4(7) . . . . ?
SI2 C16 C21 C20 -171.5(4) . . . . ?
C19 C20 C21 C16 -1.5(8) . . . . ?
C20 C19 C22 O6 172.7(5) . . . . ?
C18 C19 C22 O6 -7.3(7) . . . . ?
C20 C19 C22 O7 -8.0(8) . . . . ?
C18 C19 C22 O7 172.1(5) . . . . ?
C28 C23 C24 C25 1.4(7) . . . . ?
SI2 C23 C24 C25 -177.7(4) . . . . ?
C23 C24 C25 C26 -0.8(8) . . . . ?
C24 C25 C26 C27 0.0(7) . . . . ?
C24 C25 C26 C29 -179.6(4) . . . . ?
C25 C26 C27 C28 0.1(7) . . . . ?
C29 C26 C27 C28 179.6(4) . . . . ?
C26 C27 C28 C23 0.6(7) . . . . ?
C24 C23 C28 C27 -1.3(7) . . . . ?
SI2 C23 C28 C27 177.8(3) . . . . ?
C25 C26 C29 O9 -167.2(4) . . . . ?
C27 C26 C29 O9 13.3(6) . . . . ?
C25 C26 C29 O8 12.4(6) . . . . ?
C27 C26 C29 O8 -167.1(4) . . . . ?
C36 C31 C32 C33 -0.9(6) . . . . ?
SI3 C31 C32 C33 -179.9(3) . . . . ?
C31 C32 C33 C34 0.9(6) . . . . ?
C32 C33 C34 C35 -0.4(6) . . . . ?
C32 C33 C34 C37 -176.8(4) . . . . ?
C33 C34 C35 C36 -0.1(6) . . . . ?
C37 C34 C35 C36 176.4(4) . . . . ?
C34 C35 C36 C31 0.1(7) . . . . ?
C32 C31 C36 C35 0.4(6) . . . . ?
SI3 C31 C36 C35 179.5(3) . . . . ?
C33 C34 C37 O12 -173.4(4) . . . . ?
C35 C34 C37 O12 10.3(6) . . . . ?
C33 C34 C37 O11 7.8(6) . . . . ?
C35 C34 C37 O11 -168.6(4) . . . . ?
C43 C38 C39 C40 1.5(7) . . . . ?
SI3 C38 C39 C40 -176.5(4) . . . . ?
C38 C39 C40 C41 -0.9(9) . . . . ?
C39 C40 C41 C42 -0.6(8) . . . . ?
C39 C40 C41 C44 178.2(5) . . . . ?
C40 C41 C42 C43 1.5(7) . . . . ?
C44 C41 C42 C43 -177.4(4) . . . . ?
C41 C42 C43 C38 -0.8(7) . . . . ?
C39 C38 C43 C42 -0.7(7) . . . . ?
SI3 C38 C43 C42 177.5(3) . . . . ?
C40 C41 C44 O13 179.3(5) . . . . ?
C42 C41 C44 O13 -1.8(7) . . . . ?
C40 C41 C44 O14 -2.4(7) . . . . ?
C42 C41 C44 O14 176.4(4) . . . . ?
SI2 O1 SI1 C15 -87.3(4) . . . . ?
SI2 O1 SI1 C1 152.7(3) . . . . ?
SI2 O1 SI1 C8 35.7(4) . . . . ?
C6 C1 SI1 O1 50.5(4) . . . . ?
C2 C1 SI1 O1 -129.9(4) . . . . ?
C6 C1 SI1 C15 -67.8(4) . . . . ?
C2 C1 SI1 C15 111.9(4) . . . . ?
C6 C1 SI1 C8 167.9(4) . . . . ?
C2 C1 SI1 C8 -12.4(4) . . . . ?
C13 C8 SI1 O1 -121.1(4) . . . . ?
C9 C8 SI1 O1 59.6(4) . . . . ?
C13 C8 SI1 C15 -0.7(4) . . . . ?
C9 C8 SI1 C15 -179.9(3) . . . . ?
C13 C8 SI1 C1 122.7(4) . . . . ?
C9 C8 SI1 C1 -56.6(4) . . . . ?
SI1 O1 SI2 C23 170.9(3) . . . . ?
SI1 O1 SI2 C16 -72.4(4) . . . . ?
SI1 O1 SI2 C30 50.4(4) . . . . ?
C24 C23 SI2 O1 -4.3(4) . . . . ?
C28 C23 SI2 O1 176.7(3) . . . . ?
C24 C23 SI2 C16 -119.7(4) . . . . ?
C28 C23 SI2 C16 61.3(4) . . . . ?
C24 C23 SI2 C30 116.5(4) . . . . ?
C28 C23 SI2 C30 -62.5(4) . . . . ?
C17 C16 SI2 O1 -67.5(4) . . . . ?
C21 C16 SI2 O1 107.2(4) . . . . ?
C17 C16 SI2 C23 45.4(4) . . . . ?
C21 C16 SI2 C23 -139.9(4) . . . . ?
C17 C16 SI2 C30 169.2(4) . . . . ?
C21 C16 SI2 C30 -16.1(5) . . . . ?
C39 C38 SI3 O10 -140.2(4) . . . . ?
C43 C38 SI3 O10 41.8(4) . . . . ?
C39 C38 SI3 C45 -18.3(5) . . . . ?
C43 C38 SI3 C45 163.7(3) . . . . ?
C39 C38 SI3 C31 104.0(4) . . . . ?
C43 C38 SI3 C31 -74.0(4) . . . . ?
C32 C31 SI3 O10 -141.2(3) . . . . ?
C36 C31 SI3 O10 39.8(3) . . . . ?
C32 C31 SI3 C45 99.9(4) . . . . ?
C36 C31 SI3 C45 -79.1(4) . . . . ?
C32 C31 SI3 C38 -24.3(4) . . . . ?
C36 C31 SI3 C38 156.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O13_$1 0.84 1.76 2.583(4) 165.6 2_665
O11 H11 O3_$2 0.84 1.81 2.642(4) 169.7 2_556
O2 H1A O12_$2 0.92(6) 1.68(6) 2.598(4) 173(6) 2_556
O7 H1C O6_$3 0.909(10) 1.769(19) 2.642(5) 160(4) 2_755
O8 H1D O9_$4 0.904(10) 1.728(16) 2.622(4) 169(6) 2_666
O14 H1F O5_$1 0.84(6) 1.79(6) 2.630(5) 176(6) 2_665

_refine_diff_density_max         0.733
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_IMP-32-Zr
_database_code_depnum_ccdc_archive 'CCDC 1950126'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2019-08-29 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H25 N2 O8.5 Si Zr1.5, 1.5(C3 H7 N O)'
_chemical_formula_sum            'C25.50 H35.50 N3.50 O10 Si Zr1.50'
_chemical_formula_weight         715.99

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'

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

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

_cell_length_a                   17.2986(5)
_cell_length_b                   30.7451(6)
_cell_length_c                   27.0210(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14371.0(6)
_cell_formula_units_Z            16
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9137
_cell_measurement_theta_min      2.5520
_cell_measurement_theta_max      28.2030

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_F_000             5872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.526
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67333
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.310
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8406
_reflns_number_gt                5153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1013P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8406
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1826
_refine_ls_wR_factor_gt          0.1665
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.39936(3) 0.49146(2) 0.56573(2) 0.03146(16) Uani 1 1 d . . . . .
Zr2 Zr 0.52222(4) 0.42153(2) 0.500000 0.02581(17) Uani 1 2 d S T P . .
O1 O 0.250000 0.250000 0.750000 0.0654(18) Uani 1 2 d S . P . .
Si2 Si 0.31359(10) 0.23061(5) 0.71255(5) 0.0482(4) Uani 1 1 d . . . . .
C3 C 0.3432(3) 0.27762(16) 0.67248(19) 0.0457(13) Uani 1 1 d . . . . .
C4 C 0.3042(4) 0.3165(2) 0.6750(3) 0.075(2) Uani 1 1 d . . . . .
H4A H 0.260744 0.318882 0.696280 0.090 Uiso 1 1 calc R U . . .
C5 C 0.3266(4) 0.35224(19) 0.6473(2) 0.071(2) Uani 1 1 d . . . . .
H5A H 0.301324 0.379397 0.651626 0.085 Uiso 1 1 calc R U . . .
C6 C 0.3846(3) 0.34831(15) 0.61424(19) 0.0440(13) Uani 1 1 d . . . . .
C7 C 0.4242(4) 0.30982(18) 0.6103(2) 0.0633(18) Uani 1 1 d . . . . .
H7A H 0.466172 0.307178 0.587832 0.076 Uiso 1 1 calc R U . . .
C8 C 0.4025(4) 0.27471(18) 0.6396(2) 0.0661(19) Uani 1 1 d . . . . .
H8A H 0.429750 0.248015 0.636623 0.079 Uiso 1 1 calc R U . . .
C9 C 0.4082(3) 0.38630(15) 0.5831(2) 0.0424(13) Uani 1 1 d . . . . .
O10 O 0.3788(2) 0.42311(11) 0.59321(14) 0.0524(10) Uani 1 1 d . . . . .
O11 O 0.4565(2) 0.37884(9) 0.54894(11) 0.0379(8) Uani 1 1 d . . . . .
C12 C 0.2668(3) 0.18796(16) 0.67304(18) 0.0451(13) Uani 1 1 d . . . . .
C13 C 0.2123(4) 0.20012(17) 0.6385(2) 0.0623(18) Uani 1 1 d . . . . .
H13A H 0.200171 0.230063 0.634700 0.075 Uiso 1 1 calc R U . . .
C14 C 0.1747(4) 0.16956(17) 0.6092(2) 0.0588(17) Uani 1 1 d . . . . .
H14A H 0.137968 0.178871 0.585336 0.071 Uiso 1 1 calc R U . . .
C15 C 0.1903(3) 0.12584(16) 0.61459(19) 0.0448(13) Uani 1 1 d . . . . .
C16 C 0.2415(4) 0.11301(17) 0.6501(2) 0.070(2) Uani 1 1 d . . . . .
H16A H 0.250920 0.082905 0.655243 0.084 Uiso 1 1 calc R U . . .
C17 C 0.2808(4) 0.14414(18) 0.6793(2) 0.071(2) Uani 1 1 d . . . . .
H17A H 0.317148 0.134793 0.703391 0.085 Uiso 1 1 calc R U . . .
C18 C 0.1500(3) 0.09302(16) 0.58384(19) 0.0421(12) Uani 1 1 d . . . . .
O19 O 0.1076(2) 0.10829(10) 0.54895(12) 0.0371(8) Uani 1 1 d . . . . .
O20 O 0.1587(2) 0.05364(11) 0.59307(14) 0.0547(10) Uani 1 1 d . . . . .
C21 C 0.3953(4) 0.2080(2) 0.7465(3) 0.079(2) Uani 1 1 d . . . . .
H21A H 0.433317 0.196378 0.723098 0.118 Uiso 1 1 calc R U . . .
H21B H 0.419386 0.230869 0.766550 0.118 Uiso 1 1 calc R U . . .
H21C H 0.377204 0.184566 0.768226 0.118 Uiso 1 1 calc R U . . .
O30 O 0.2823(3) 0.48251(17) 0.56485(19) 0.0829(15) Uani 1 1 d . . . . .
O40 O 0.4111(4) 0.49285(17) 0.64120(16) 0.106(2) Uani 1 1 d . . . . .
O50 O 0.3873(4) 0.52935(17) 0.500000 0.074(2) Uani 1 2 d S T P . .
O60 O 0.4081(4) 0.4530(2) 0.500000 0.077(2) Uani 1 2 d S T P . .
O70 O 0.4890(2) 0.53848(13) 0.56561(18) 0.0735(15) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O30 2.043(4) . ?
Zr1 O40 2.050(4) . ?
Zr1 O70 2.120(4) . ?
Zr1 O50 2.134(3) . ?
Zr1 O60 2.139(4) . ?
Zr1 O70 2.140(4) 2_665 ?
Zr1 O10 2.257(3) . ?
Zr1 O20 2.282(3) 12_665 ?
Zr1 Zr2 3.4857(6) 9_666 ?
Zr1 Zr2 3.5061(7) . ?
Zr1 Zr1 3.5212(10) 2_665 ?
Zr1 Zr1 3.5520(9) 10_556 ?
Zr2 O70 2.166(4) 2_665 ?
Zr2 O70 2.166(4) 9_666 ?
Zr2 O50 2.175(6) 9_666 ?
Zr2 O11 2.183(3) 10_556 ?
Zr2 O11 2.183(3) . ?
Zr2 O19 2.184(3) 11_665 ?
Zr2 O19 2.184(3) 4_556 ?
Zr2 O60 2.198(6) . ?
O1 Si2 1.6092(18) . ?
O1 Si2 1.6092(18) 13_556 ?
Si2 C21 1.824(7) . ?
Si2 C12 1.875(5) . ?
Si2 C3 1.877(5) . ?
C3 C8 1.359(8) . ?
C3 C4 1.373(8) . ?
C4 C5 1.385(8) . ?
C5 C6 1.348(8) . ?
C6 C7 1.372(8) . ?
C6 C9 1.497(6) . ?
C7 C8 1.391(7) . ?
C9 O11 1.265(6) . ?
C9 O10 1.271(6) . ?
C12 C13 1.377(7) . ?
C12 C17 1.379(7) . ?
C13 C14 1.391(7) . ?
C14 C15 1.379(7) . ?
C15 C16 1.364(7) . ?
C15 C18 1.482(7) . ?
C16 C17 1.414(8) . ?
C18 O20 1.245(6) . ?
C18 O19 1.283(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
O30 Zr1 O40 96.4(2) . . ?
O30 Zr1 O70 144.74(19) . . ?
O40 Zr1 O70 85.1(2) . . ?
O30 Zr1 O50 88.1(2) . . ?
O40 Zr1 O50 145.71(18) . . ?
O70 Zr1 O50 72.41(19) . . ?
O30 Zr1 O60 89.2(2) . . ?
O40 Zr1 O60 146.1(2) . . ?
O70 Zr1 O60 108.9(3) . . ?
O50 Zr1 O60 67.53(19) . . ?
O30 Zr1 O70 146.76(18) . 2_665 ?
O40 Zr1 O70 85.5(2) . 2_665 ?
O70 Zr1 O70 68.48(18) . 2_665 ?
O50 Zr1 O70 108.8(2) . 2_665 ?
O60 Zr1 O70 72.4(2) . 2_665 ?
O30 Zr1 O10 73.89(18) . . ?
O40 Zr1 O10 73.00(18) . . ?
O70 Zr1 O10 138.64(15) . . ?
O50 Zr1 O10 140.06(16) . . ?
O60 Zr1 O10 76.67(19) . . ?
O70 Zr1 O10 75.04(16) 2_665 . ?
O30 Zr1 O20 71.38(18) . 12_665 ?
O40 Zr1 O20 72.79(19) . 12_665 ?
O70 Zr1 O20 75.58(16) . 12_665 ?
O50 Zr1 O20 76.66(18) . 12_665 ?
O60 Zr1 O20 139.73(17) . 12_665 ?
O70 Zr1 O20 139.30(15) 2_665 12_665 ?
O10 Zr1 O20 127.17(13) . 12_665 ?
O30 Zr1 Zr2 118.89(15) . 9_666 ?
O40 Zr1 Zr2 116.90(16) . 9_666 ?
O70 Zr1 Zr2 36.02(11) . 9_666 ?
O50 Zr1 Zr2 36.40(16) . 9_666 ?
O60 Zr1 Zr2 88.50(18) . 9_666 ?
O70 Zr1 Zr2 88.75(13) 2_665 9_666 ?
O10 Zr1 Zr2 160.64(9) . 9_666 ?
O20 Zr1 Zr2 72.14(9) 12_665 9_666 ?
O30 Zr1 Zr2 120.80(15) . . ?
O40 Zr1 Zr2 117.18(18) . . ?
O70 Zr1 Zr2 88.51(14) . . ?
O50 Zr1 Zr2 88.41(17) . . ?
O60 Zr1 Zr2 36.63(16) . . ?
O70 Zr1 Zr2 35.73(11) 2_665 . ?
O10 Zr1 Zr2 72.01(9) . . ?
O20 Zr1 Zr2 160.78(9) 12_665 . ?
Zr2 Zr1 Zr2 88.659(16) 9_666 . ?
O30 Zr1 Zr1 178.94(16) . 2_665 ?
O40 Zr1 Zr1 84.2(2) . 2_665 ?
O70 Zr1 Zr1 34.42(11) . 2_665 ?
O50 Zr1 Zr1 90.9(2) . 2_665 ?
O60 Zr1 Zr1 90.7(2) . 2_665 ?
O70 Zr1 Zr1 34.06(11) 2_665 2_665 ?
O10 Zr1 Zr1 107.12(11) . 2_665 ?
O20 Zr1 Zr1 108.07(11) 12_665 2_665 ?
Zr2 Zr1 Zr1 60.050(14) 9_666 2_665 ?
Zr2 Zr1 Zr1 59.473(15) . 2_665 ?
O30 Zr1 Zr1 89.34(15) . 10_556 ?
O40 Zr1 Zr1 174.2(2) . 10_556 ?
O70 Zr1 Zr1 89.91(13) . 10_556 ?
O50 Zr1 Zr1 33.67(13) . 10_556 ?
O60 Zr1 Zr1 33.88(14) . 10_556 ?
O70 Zr1 Zr1 89.91(13) 2_665 10_556 ?
O10 Zr1 Zr1 109.21(10) . 10_556 ?
O20 Zr1 Zr1 108.89(10) 12_665 10_556 ?
Zr2 Zr1 Zr1 59.369(8) 9_666 10_556 ?
Zr2 Zr1 Zr1 59.566(9) . 10_556 ?
Zr1 Zr1 Zr1 90.0 2_665 10_556 ?
O70 Zr2 O70 109.9(3) 2_665 9_666 ?
O70 Zr2 O50 70.75(15) 2_665 9_666 ?
O70 Zr2 O50 70.75(15) 9_666 9_666 ?
O70 Zr2 O11 142.25(14) 2_665 10_556 ?
O70 Zr2 O11 78.40(15) 9_666 10_556 ?
O50 Zr2 O11 142.40(9) 9_666 10_556 ?
O70 Zr2 O11 78.40(15) 2_665 . ?
O70 Zr2 O11 142.25(14) 9_666 . ?
O50 Zr2 O11 142.40(9) 9_666 . ?
O11 Zr2 O11 74.59(17) 10_556 . ?
O70 Zr2 O19 78.64(15) 2_665 11_665 ?
O70 Zr2 O19 142.60(14) 9_666 11_665 ?
O50 Zr2 O19 78.76(18) 9_666 11_665 ?
O11 Zr2 O19 117.80(12) 10_556 11_665 ?
O11 Zr2 O19 74.48(13) . 11_665 ?
O70 Zr2 O19 142.60(14) 2_665 4_556 ?
O70 Zr2 O19 78.64(15) 9_666 4_556 ?
O50 Zr2 O19 78.76(18) 9_666 4_556 ?
O11 Zr2 O19 74.48(13) 10_556 4_556 ?
O11 Zr2 O19 117.80(12) . 4_556 ?
O19 Zr2 O19 74.55(17) 11_665 4_556 ?
O70 Zr2 O60 70.73(15) 2_665 . ?
O70 Zr2 O60 70.73(15) 9_666 . ?
O50 Zr2 O60 109.9(3) 9_666 . ?
O11 Zr2 O60 78.29(18) 10_556 . ?
O11 Zr2 O60 78.29(18) . . ?
O19 Zr2 O60 142.35(9) 11_665 . ?
O19 Zr2 O60 142.35(9) 4_556 . ?
O70 Zr2 Zr1 35.14(11) 2_665 2_665 ?
O70 Zr2 Zr1 90.93(13) 9_666 2_665 ?
O50 Zr2 Zr1 35.61(9) 9_666 2_665 ?
O11 Zr2 Zr1 166.64(9) 10_556 2_665 ?
O11 Zr2 Zr1 110.82(8) . 2_665 ?
O19 Zr2 Zr1 75.56(8) 11_665 2_665 ?
O19 Zr2 Zr1 111.57(9) 4_556 2_665 ?
O60 Zr2 Zr1 90.68(17) . 2_665 ?
O70 Zr2 Zr1 90.93(13) 2_665 9_666 ?
O70 Zr2 Zr1 35.14(11) 9_666 9_666 ?
O50 Zr2 Zr1 35.61(9) 9_666 9_666 ?
O11 Zr2 Zr1 110.82(8) 10_556 9_666 ?
O11 Zr2 Zr1 166.64(9) . 9_666 ?
O19 Zr2 Zr1 111.57(9) 11_665 9_666 ?
O19 Zr2 Zr1 75.56(8) 4_556 9_666 ?
O60 Zr2 Zr1 90.68(17) . 9_666 ?
Zr1 Zr2 Zr1 61.264(17) 2_665 9_666 ?
O70 Zr2 Zr1 90.71(13) 2_665 10_556 ?
O70 Zr2 Zr1 35.23(12) 9_666 10_556 ?
O50 Zr2 Zr1 90.59(17) 9_666 10_556 ?
O11 Zr2 Zr1 75.30(8) 10_556 10_556 ?
O11 Zr2 Zr1 111.11(10) . 10_556 ?
O19 Zr2 Zr1 166.90(8) 11_665 10_556 ?
O19 Zr2 Zr1 111.13(8) 4_556 10_556 ?
O60 Zr2 Zr1 35.50(10) . 10_556 ?
Zr1 Zr2 Zr1 91.343(16) 2_665 10_556 ?
Zr1 Zr2 Zr1 60.479(16) 9_666 10_556 ?
O70 Zr2 Zr1 35.23(12) 2_665 . ?
O70 Zr2 Zr1 90.71(13) 9_666 . ?
O50 Zr2 Zr1 90.59(17) 9_666 . ?
O11 Zr2 Zr1 111.11(10) 10_556 . ?
O11 Zr2 Zr1 75.31(8) . . ?
O19 Zr2 Zr1 111.13(8) 11_665 . ?
O19 Zr2 Zr1 166.90(8) 4_556 . ?
O60 Zr2 Zr1 35.50(10) . . ?
Zr1 Zr2 Zr1 60.478(16) 2_665 . ?
Zr1 Zr2 Zr1 91.343(16) 9_666 . ?
Zr1 Zr2 Zr1 60.867(17) 10_556 . ?
Si2 O1 Si2 180.0 . 13_556 ?
O1 Si2 C21 110.8(3) . . ?
O1 Si2 C12 108.8(2) . . ?
C21 Si2 C12 110.8(3) . . ?
O1 Si2 C3 105.31(19) . . ?
C21 Si2 C3 111.9(3) . . ?
C12 Si2 C3 109.1(2) . . ?
C8 C3 C4 117.4(5) . . ?
C8 C3 Si2 122.1(4) . . ?
C4 C3 Si2 120.5(4) . . ?
C3 C4 C5 121.8(6) . . ?
C6 C5 C4 119.6(6) . . ?
C5 C6 C7 120.0(5) . . ?
C5 C6 C9 120.4(5) . . ?
C7 C6 C9 119.5(5) . . ?
C6 C7 C8 119.4(5) . . ?
C3 C8 C7 121.7(6) . . ?
O11 C9 O10 125.7(4) . . ?
O11 C9 C6 116.7(4) . . ?
O10 C9 C6 117.6(4) . . ?
C9 O10 Zr1 134.0(3) . . ?
C9 O11 Zr2 132.5(3) . . ?
C13 C12 C17 117.9(5) . . ?
C13 C12 Si2 119.4(4) . . ?
C17 C12 Si2 122.6(4) . . ?
C12 C13 C14 121.5(5) . . ?
C15 C14 C13 120.5(5) . . ?
C16 C15 C14 118.9(5) . . ?
C16 C15 C18 120.2(5) . . ?
C14 C15 C18 120.8(5) . . ?
C15 C16 C17 120.6(5) . . ?
C12 C17 C16 120.6(5) . . ?
O20 C18 O19 124.9(5) . . ?
O20 C18 C15 119.5(5) . . ?
O19 C18 C15 115.6(4) . . ?
C18 O19 Zr2 132.6(3) . 11_565 ?
C18 O20 Zr1 134.1(3) . 12_655 ?
Zr1 O50 Zr1 112.7(3) . 10_556 ?
Zr1 O50 Zr2 108.0(2) . 9_666 ?
Zr1 O50 Zr2 108.0(2) 10_556 9_666 ?
Zr1 O60 Zr1 112.2(3) 10_556 . ?
Zr1 O60 Zr2 107.9(2) 10_556 . ?
Zr1 O60 Zr2 107.9(2) . . ?
Zr1 O70 Zr1 111.52(18) . 2_665 ?
Zr1 O70 Zr2 108.84(19) . 9_666 ?
Zr1 O70 Zr2 109.0(2) 2_665 9_666 ?

_refine_diff_density_max         1.105
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.112


####################################################################### 
# 
# 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_IMP-32-Hf
_database_code_depnum_ccdc_archive 'CCDC 1950127'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2019-08-29 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H25 Hf1.5 N2 O8.5 Si, C3 H7 N O'
_chemical_formula_sum            'C24 H32 Hf1.50 N3 O9.50 Si'
_chemical_formula_weight         810.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'

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

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

_cell_length_a                   17.21910(16)
_cell_length_b                   30.6244(2)
_cell_length_c                   27.1584(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14321.3(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    71522
_cell_measurement_theta_min      5.1810
_cell_measurement_theta_max      70.3030

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_F_000             6320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    8.665
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            129803
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         4.193
_diffrn_reflns_theta_max         70.675
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6986
_reflns_number_gt                6809
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0860P)²+93.3056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6986
_refine_ls_number_parameters     262
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1446
_refine_ls_wR_factor_gt          0.1438
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.39925(5) 0.49149(5) 0.56496(4) 0.0368(4) Uani 0.848(15) 1 d . U P A 1
Hf1' Hf 0.3980(5) 0.5032(9) 0.5650(3) 0.077(2) Uani 0.152(15) 1 d . U P A 2
Hf2 Hf 0.52157(9) 0.42146(2) 0.500000 0.0311(3) Uani 0.897(6) 2 d S TU P A 1
Hf2' Hf 0.4793(14) 0.42117(15) 0.500000 0.053(4) Uani 0.103(6) 2 d S TU P A 2
O1 O 0.250000 0.250000 0.750000 0.089(3) Uani 1 2 d S . P . .
Si2 Si 0.31342(13) 0.23067(6) 0.71223(6) 0.0626(5) Uani 1 1 d . . . . .
C3 C 0.3429(4) 0.2784(2) 0.6725(2) 0.0605(16) Uani 1 1 d . . . . .
C4 C 0.3035(6) 0.3174(2) 0.6759(3) 0.088(3) Uani 1 1 d . . . . .
H4A H 0.260579 0.319857 0.697676 0.105 Uiso 1 1 calc R U . . .
C5 C 0.3258(6) 0.3534(3) 0.6476(3) 0.086(3) Uani 1 1 d . . . . .
H5A H 0.300221 0.380694 0.651573 0.103 Uiso 1 1 calc R U . . .
C6 C 0.3844(5) 0.3493(2) 0.6142(2) 0.0610(17) Uani 1 1 d . . . . .
C7 C 0.4240(6) 0.3103(2) 0.6109(3) 0.084(3) Uani 1 1 d . . . . .
H7A H 0.466421 0.307877 0.588691 0.101 Uiso 1 1 calc R U . . .
C8 C 0.4036(6) 0.2745(3) 0.6392(3) 0.086(3) Uani 1 1 d . . . . .
H8A H 0.430718 0.247616 0.635924 0.103 Uiso 1 1 calc R U . . .
C9 C 0.4079(4) 0.38688(19) 0.5820(3) 0.0576(16) Uani 1 1 d . . . . .
O10 O 0.3773(3) 0.42335(13) 0.59194(18) 0.0651(13) Uani 1 1 d . . . . .
O11 O 0.4557(3) 0.37885(12) 0.54899(14) 0.0500(9) Uani 1 1 d . . . . .
C12 C 0.2658(5) 0.1881(2) 0.6726(2) 0.0636(18) Uani 1 1 d . . . . .
C13 C 0.2100(6) 0.2006(2) 0.6386(3) 0.082(3) Uani 1 1 d . . . . .
H13A H 0.196571 0.230546 0.635674 0.098 Uiso 1 1 calc R U . . .
C14 C 0.1733(5) 0.1698(2) 0.6087(3) 0.077(2) Uani 1 1 d . . . . .
H14A H 0.137249 0.179094 0.584331 0.093 Uiso 1 1 calc R U . . .
C15 C 0.1891(4) 0.1270(2) 0.6143(2) 0.0614(17) Uani 1 1 d . . . . .
C16 C 0.2425(6) 0.1136(2) 0.6493(3) 0.085(3) Uani 1 1 d . . . . .
H16A H 0.252839 0.083317 0.653511 0.102 Uiso 1 1 calc R U . . .
C17 C 0.2811(6) 0.1440(2) 0.6784(3) 0.088(3) Uani 1 1 d . . . . .
H17A H 0.317770 0.134556 0.702281 0.105 Uiso 1 1 calc R U . . .
C18 C 0.1481(4) 0.0933(2) 0.5825(2) 0.0523(14) Uani 1 1 d . . . . .
O19 O 0.1060(2) 0.10907(13) 0.54877(15) 0.0498(10) Uani 1 1 d . . . . .
O20 O 0.1582(3) 0.05430(14) 0.59163(18) 0.0686(14) Uani 1 1 d . . . . .
C21 C 0.3946(6) 0.2091(3) 0.7474(3) 0.096(3) Uani 1 1 d . . . . .
H21A H 0.433593 0.197205 0.724743 0.143 Uiso 1 1 calc R U . . .
H21B H 0.417807 0.232506 0.767021 0.143 Uiso 1 1 calc R U . . .
H21C H 0.376122 0.185843 0.769244 0.143 Uiso 1 1 calc R U . . .
O30 O 0.2815(3) 0.4834(2) 0.5641(2) 0.095(2) Uani 1 1 d . . . . .
O40 O 0.4081(5) 0.49434(19) 0.64141(17) 0.096(2) Uani 1 1 d . . . . .
O50 O 0.3886(6) 0.5291(3) 0.500000 0.088(3) Uani 1 2 d S T P . .
O60 O 0.4192(17) 0.4577(7) 0.500000 0.060(5) Uani 0.62(5) 2 d S TU P A 1
O60' O 0.3886(16) 0.4460(9) 0.500000 0.049(5) Uiso 0.38(5) 2 d S U P A 2
O70 O 0.4904(3) 0.53822(17) 0.5645(2) 0.0812(19) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O30 2.044(5) . ?
Hf1 O60 2.074(7) . ?
Hf1 O40 2.084(5) . ?
Hf1 O70 2.107(5) 2_665 ?
Hf1 O50 2.114(5) . ?
Hf1 O70 2.124(5) . ?
Hf1 O10 2.244(4) . ?
Hf1 O20 2.281(4) 12_665 ?
Hf1 Hf2 3.4752(13) 9_666 ?
Hf1 Hf2 3.4855(18) . ?
Hf1 Hf1 3.5085(15) 2_665 ?
Hf1 Hf1 3.529(2) 10_556 ?
Hf1' O70 1.918(18) . ?
Hf1' O50 1.941(14) . ?
Hf1' O20 1.98(2) 12_665 ?
Hf1' O30 2.096(12) . ?
Hf1' O40 2.101(10) . ?
Hf1' O70 2.304(17) 2_665 ?
Hf1' O60' 2.49(3) . ?
Hf1' O10 2.58(3) . ?
Hf1' Hf2' 3.38(2) . ?
Hf1' Hf1' 3.520(16) 2_665 ?
Hf1' Hf1' 3.530(15) 10_556 ?
Hf1' Hf2' 3.60(3) 9_666 ?
Hf2 O60 2.083(19) . ?
Hf2 O70 2.152(5) 2_665 ?
Hf2 O70 2.152(5) 9_666 ?
Hf2 O50 2.165(8) 9_666 ?
Hf2 O19 2.177(4) 11_665 ?
Hf2 O19 2.177(4) 4_556 ?
Hf2 O11 2.182(4) . ?
Hf2 O11 2.182(4) 10_556 ?
Hf2' O60' 1.74(3) . ?
Hf2' O11 1.901(8) . ?
Hf2' O11 1.901(8) 10_556 ?
Hf2' O70 2.210(9) 2_665 ?
Hf2' O70 2.210(9) 9_666 ?
Hf2' O19 2.71(2) 11_665 ?
Hf2' O19 2.71(2) 4_556 ?
Hf2' C9 2.753(13) . ?
Hf2' C9 2.753(13) 10_556 ?
O1 Si2 1.611(2) 13_556 ?
O1 Si2 1.611(2) . ?
Si2 C21 1.817(10) . ?
Si2 C12 1.880(6) . ?
Si2 C3 1.887(6) . ?
C3 C4 1.377(11) . ?
C3 C8 1.386(11) . ?
C4 C5 1.399(10) . ?
C5 C6 1.362(11) . ?
C6 C7 1.379(10) . ?
C6 C9 1.501(8) . ?
C7 C8 1.385(9) . ?
C9 O11 1.242(8) . ?
C9 O10 1.264(8) . ?
C12 C17 1.385(10) . ?
C12 C13 1.385(10) . ?
C13 C14 1.396(9) . ?
C14 C15 1.350(10) . ?
C15 C16 1.386(10) . ?
C15 C18 1.517(8) . ?
C16 C17 1.391(10) . ?
C18 O20 1.234(7) . ?
C18 O19 1.264(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
O30 Hf1 O60 95.4(9) . . ?
O30 Hf1 O40 95.1(3) . . ?
O60 Hf1 O40 148.9(3) . . ?
O30 Hf1 O70 147.4(3) . 2_665 ?
O60 Hf1 O70 68.3(7) . 2_665 ?
O40 Hf1 O70 87.6(3) . 2_665 ?
O30 Hf1 O50 88.3(3) . . ?
O60 Hf1 O50 64.9(4) . . ?
O40 Hf1 O50 144.6(2) . . ?
O70 Hf1 O50 107.9(3) 2_665 . ?
O30 Hf1 O70 144.6(3) . . ?
O60 Hf1 O70 102.0(9) . . ?
O40 Hf1 O70 85.7(3) . . ?
O70 Hf1 O70 67.9(2) 2_665 . ?
O50 Hf1 O70 72.1(3) . . ?
O30 Hf1 O10 73.9(3) . . ?
O60 Hf1 O10 80.9(6) . . ?
O40 Hf1 O10 74.1(2) . . ?
O70 Hf1 O10 75.7(2) 2_665 . ?
O50 Hf1 O10 139.8(2) . . ?
O70 Hf1 O10 138.9(2) . . ?
O30 Hf1 O20 71.1(3) . 12_665 ?
O60 Hf1 O20 139.7(3) . 12_665 ?
O40 Hf1 O20 71.3(2) . 12_665 ?
O70 Hf1 O20 139.2(2) 2_665 12_665 ?
O50 Hf1 O20 76.6(3) . 12_665 ?
O70 Hf1 O20 75.8(2) . 12_665 ?
O10 Hf1 O20 127.40(17) . 12_665 ?
O30 Hf1 Hf2 118.5(2) . 9_666 ?
O60 Hf1 Hf2 83.4(7) . 9_666 ?
O40 Hf1 Hf2 116.43(19) . 9_666 ?
O70 Hf1 Hf2 88.52(18) 2_665 9_666 ?
O50 Hf1 Hf2 36.2(2) . 9_666 ?
O70 Hf1 Hf2 35.91(14) . 9_666 ?
O10 Hf1 Hf2 160.95(13) . 9_666 ?
O20 Hf1 Hf2 71.62(12) 12_665 9_666 ?
O30 Hf1 Hf2 121.2(2) . . ?
O60 Hf1 Hf2 33.1(6) . . ?
O40 Hf1 Hf2 119.1(2) . . ?
O70 Hf1 Hf2 35.51(14) 2_665 . ?
O50 Hf1 Hf2 88.0(2) . . ?
O70 Hf1 Hf2 87.98(18) . . ?
O10 Hf1 Hf2 72.23(12) . . ?
O20 Hf1 Hf2 160.35(12) 12_665 . ?
Hf2 Hf1 Hf2 88.74(2) 9_666 . ?
O30 Hf1 Hf1 178.3(2) . 2_665 ?
O60 Hf1 Hf1 84.8(9) . 2_665 ?
O40 Hf1 Hf1 85.5(2) . 2_665 ?
O70 Hf1 Hf1 34.13(14) 2_665 2_665 ?
O50 Hf1 Hf1 90.3(3) . 2_665 ?
O70 Hf1 Hf1 33.82(14) . 2_665 ?
O10 Hf1 Hf1 107.74(16) . 2_665 ?
O20 Hf1 Hf1 107.69(15) 12_665 2_665 ?
Hf2 Hf1 Hf1 59.88(4) 9_666 2_665 ?
Hf2 Hf1 Hf1 59.59(4) . 2_665 ?
O30 Hf1 Hf1 89.31(19) . 10_556 ?
O60 Hf1 Hf1 31.7(3) . 10_556 ?
O40 Hf1 Hf1 175.2(2) . 10_556 ?
O70 Hf1 Hf1 89.63(18) 2_665 10_556 ?
O50 Hf1 Hf1 33.45(19) . 10_556 ?
O70 Hf1 Hf1 89.64(17) . 10_556 ?
O10 Hf1 Hf1 109.06(13) . 10_556 ?
O20 Hf1 Hf1 108.51(13) 12_665 10_556 ?
Hf2 Hf1 Hf1 59.49(2) 9_666 10_556 ?
Hf2 Hf1 Hf1 59.59(2) . 10_556 ?
Hf1 Hf1 Hf1 90.0 2_665 10_556 ?
O70 Hf1' O50 80.5(8) . . ?
O70 Hf1' O20 88.1(11) . 12_665 ?
O50 Hf1' O20 88.3(10) . 12_665 ?
O70 Hf1' O30 162.9(14) . . ?
O50 Hf1' O30 91.6(5) . . ?
O20 Hf1' O30 76.4(4) 12_665 . ?
O70 Hf1' O40 90.6(5) . . ?
O50 Hf1' O40 163.4(15) . . ?
O20 Hf1' O40 77.4(5) 12_665 . ?
O30 Hf1' O40 93.1(6) . . ?
O70 Hf1' O70 67.4(4) . 2_665 ?
O50 Hf1' O70 106.7(5) . 2_665 ?
O20 Hf1' O70 147.9(7) 12_665 2_665 ?
O30 Hf1' O70 129.7(13) . 2_665 ?
O40 Hf1' O70 82.3(6) . 2_665 ?
O70 Hf1' O60' 116.2(8) . . ?
O50 Hf1' O60' 68.8(6) . . ?
O20 Hf1' O60' 141.6(7) 12_665 . ?
O30 Hf1' O60' 74.1(9) . . ?
O40 Hf1' O60' 127.8(13) . . ?
O70 Hf1' O60' 70.2(8) 2_665 . ?
O70 Hf1' O10 130.3(8) . . ?
O50 Hf1' O10 129.3(9) . . ?
O20 Hf1' O10 125.4(5) 12_665 . ?
O30 Hf1' O10 66.2(7) . . ?
O40 Hf1' O10 66.9(6) . . ?
O70 Hf1' O10 66.0(7) 2_665 . ?
O60' Hf1' O10 61.6(8) . . ?
O70 Hf1' Hf2' 93.9(6) . . ?
O50 Hf1' Hf2' 82.1(5) . . ?
O20 Hf1' Hf2' 169.7(5) 12_665 . ?
O30 Hf1' Hf2' 100.1(9) . . ?
O40 Hf1' Hf2' 112.7(9) . . ?
O70 Hf1' Hf2' 40.6(5) 2_665 . ?
O60' Hf1' Hf2' 29.9(7) . . ?
O10 Hf1' Hf2' 59.9(5) . . ?
O70 Hf1' Hf1' 37.2(3) . 2_665 ?
O50 Hf1' Hf1' 96.1(5) . 2_665 ?
O20 Hf1' Hf1' 122.2(12) 12_665 2_665 ?
O30 Hf1' Hf1' 159.9(16) . 2_665 ?
O40 Hf1' Hf1' 84.8(3) . 2_665 ?
O70 Hf1' Hf1' 30.2(4) 2_665 2_665 ?
O10 Hf1' Hf1' 94.8(10) . 2_665 ?
O70 Hf1' Hf1' 89.6(3) . 10_556 ?
O50 Hf1' Hf1' 24.6(8) . 10_556 ?
O20 Hf1' Hf1' 111.5(4) 12_665 10_556 ?
O30 Hf1' Hf1' 89.3(3) . 10_556 ?
O40 Hf1' Hf1' 171.1(7) . 10_556 ?
O70 Hf1' Hf1' 89.6(2) 2_665 10_556 ?
O10 Hf1' Hf1' 106.5(2) . 10_556 ?
O70 Hf1' Hf2' 31.8(4) . 9_666 ?
O50 Hf1' Hf2' 48.7(6) . 9_666 ?
O20 Hf1' Hf2' 87.6(9) 12_665 9_666 ?
O30 Hf1' Hf2' 138.0(8) . 9_666 ?
O40 Hf1' Hf2' 121.3(7) . 9_666 ?
O70 Hf1' Hf2' 82.0(5) 2_665 9_666 ?
O10 Hf1' Hf2' 146.2(6) . 9_666 ?
O60 Hf2 O70 67.2(4) . 2_665 ?
O60 Hf2 O70 67.2(4) . 9_666 ?
O70 Hf2 O70 108.9(4) 2_665 9_666 ?
O60 Hf2 O50 103.4(9) . 9_666 ?
O70 Hf2 O50 70.5(2) 2_665 9_666 ?
O70 Hf2 O50 70.5(2) 9_666 9_666 ?
O60 Hf2 O19 142.53(11) . 11_665 ?
O70 Hf2 O19 79.4(2) 2_665 11_665 ?
O70 Hf2 O19 143.6(2) 9_666 11_665 ?
O50 Hf2 O19 79.9(2) 9_666 11_665 ?
O60 Hf2 O19 142.53(11) . 4_556 ?
O70 Hf2 O19 143.6(2) 2_665 4_556 ?
O70 Hf2 O19 79.4(2) 9_666 4_556 ?
O50 Hf2 O19 79.9(2) 9_666 4_556 ?
O19 Hf2 O19 74.9(2) 11_665 4_556 ?
O60 Hf2 O11 83.1(7) . . ?
O70 Hf2 O11 78.3(2) 2_665 . ?
O70 Hf2 O11 142.1(2) 9_666 . ?
O50 Hf2 O11 142.18(11) 9_666 . ?
O19 Hf2 O11 73.69(17) 11_665 . ?
O19 Hf2 O11 117.46(15) 4_556 . ?
O60 Hf2 O11 83.1(7) . 10_556 ?
O70 Hf2 O11 142.1(2) 2_665 10_556 ?
O70 Hf2 O11 78.3(2) 9_666 10_556 ?
O50 Hf2 O11 142.18(11) 9_666 10_556 ?
O19 Hf2 O11 117.46(15) 11_665 10_556 ?
O19 Hf2 O11 73.69(17) 4_556 10_556 ?
O11 Hf2 O11 75.2(2) . 10_556 ?
O60 Hf2 Hf1 85.6(7) . 2_665 ?
O70 Hf2 Hf1 35.36(15) 2_665 2_665 ?
O70 Hf2 Hf1 90.60(17) 9_666 2_665 ?
O50 Hf2 Hf1 35.21(13) 9_666 2_665 ?
O19 Hf2 Hf1 76.04(11) 11_665 2_665 ?
O19 Hf2 Hf1 112.12(13) 4_556 2_665 ?
O11 Hf2 Hf1 110.68(10) . 2_665 ?
O11 Hf2 Hf1 166.50(12) 10_556 2_665 ?
O60 Hf2 Hf1 85.6(7) . 9_666 ?
O70 Hf2 Hf1 90.60(17) 2_665 9_666 ?
O70 Hf2 Hf1 35.36(15) 9_666 9_666 ?
O50 Hf2 Hf1 35.21(13) 9_666 9_666 ?
O19 Hf2 Hf1 112.12(13) 11_665 9_666 ?
O19 Hf2 Hf1 76.04(11) 4_556 9_666 ?
O11 Hf2 Hf1 166.50(12) . 9_666 ?
O11 Hf2 Hf1 110.68(10) 10_556 9_666 ?
Hf1 Hf2 Hf1 61.02(4) 2_665 9_666 ?
O60 Hf2 Hf1 32.9(3) . 10_556 ?
O70 Hf2 Hf1 90.05(17) 2_665 10_556 ?
O70 Hf2 Hf1 34.65(15) 9_666 10_556 ?
O50 Hf2 Hf1 90.1(2) 9_666 10_556 ?
O19 Hf2 Hf1 167.30(11) 11_665 10_556 ?
O19 Hf2 Hf1 111.08(11) 4_556 10_556 ?
O11 Hf2 Hf1 111.26(14) . 10_556 ?
O11 Hf2 Hf1 75.23(11) 10_556 10_556 ?
Hf1 Hf2 Hf1 91.26(2) 2_665 10_556 ?
Hf1 Hf2 Hf1 60.53(2) 9_666 10_556 ?
O60 Hf2 Hf1 32.9(3) . . ?
O70 Hf2 Hf1 34.65(15) 2_665 . ?
O70 Hf2 Hf1 90.05(17) 9_666 . ?
O50 Hf2 Hf1 90.1(2) 9_666 . ?
O19 Hf2 Hf1 111.08(11) 11_665 . ?
O19 Hf2 Hf1 167.30(11) 4_556 . ?
O11 Hf2 Hf1 75.23(11) . . ?
O11 Hf2 Hf1 111.26(14) 10_556 . ?
Hf1 Hf2 Hf1 60.53(2) 2_665 . ?
Hf1 Hf2 Hf1 91.26(2) 9_666 . ?
Hf1 Hf2 Hf1 60.82(4) 10_556 . ?
O60' Hf2' O11 96.1(12) . . ?
O11 Hf2' O11 88.8(5) . 10_556 ?
O60' Hf2' O70 88.1(7) . 2_665 ?
O11 Hf2' O70 83.1(2) . 2_665 ?
O11 Hf2' O70 171.3(3) 10_556 2_665 ?
O11 Hf2' O70 171.3(3) . 9_666 ?
O11 Hf2' O70 83.1(2) 10_556 9_666 ?
O70 Hf2' O70 104.8(6) 2_665 9_666 ?
O11 Hf2' O19 66.3(4) . 11_665 ?
O11 Hf2' O19 106.3(6) 10_556 11_665 ?
O70 Hf2' O19 67.4(5) 2_665 11_665 ?
O70 Hf2' O19 112.9(10) 9_666 11_665 ?
O11 Hf2' O19 106.3(6) . 4_556 ?
O11 Hf2' O19 66.3(4) 10_556 4_556 ?
O70 Hf2' O19 112.9(10) 2_665 4_556 ?
O70 Hf2' O19 67.4(5) 9_666 4_556 ?
O19 Hf2' O19 58.4(5) 11_665 4_556 ?
O60' Hf2' C9 76.4(9) . . ?
O11 Hf2' C9 22.8(3) . . ?
O11 Hf2' C9 102.2(6) 10_556 . ?
O70 Hf2' C9 71.3(3) 2_665 . ?
O70 Hf2' C9 164.0(9) 9_666 . ?
O19 Hf2' C9 80.4(2) 11_665 . ?
O19 Hf2' C9 128.6(4) 4_556 . ?
O11 Hf2' C9 102.2(6) . 10_556 ?
O11 Hf2' C9 22.8(3) 10_556 10_556 ?
O70 Hf2' C9 164.0(9) 2_665 10_556 ?
O70 Hf2' C9 71.3(3) 9_666 10_556 ?
O19 Hf2' C9 128.6(4) 11_665 10_556 ?
O19 Hf2' C9 80.4(2) 4_556 10_556 ?
C9 Hf2' C9 108.1(7) . 10_556 ?
O11 Hf2' Hf1' 141.7(11) . 10_556 ?
O11 Hf2' Hf1' 93.0(5) 10_556 10_556 ?
O70 Hf2' Hf1' 95.3(4) 2_665 10_556 ?
O70 Hf2' Hf1' 42.7(3) 9_666 10_556 ?
O19 Hf2' Hf1' 147.4(7) 11_665 10_556 ?
O19 Hf2' Hf1' 109.4(3) 4_556 10_556 ?
C9 Hf2' Hf1' 121.5(7) . 10_556 ?
C9 Hf2' Hf1' 71.1(4) 10_556 10_556 ?
O60' Hf2' Hf1' 45.7(7) . . ?
O11 Hf2' Hf1' 93.0(5) . . ?
O11 Hf2' Hf1' 141.7(11) 10_556 . ?
O70 Hf2' Hf1' 42.7(3) 2_665 . ?
O70 Hf2' Hf1' 95.3(4) 9_666 . ?
O19 Hf2' Hf1' 109.4(3) 11_665 . ?
O19 Hf2' Hf1' 147.4(7) 4_556 . ?
C9 Hf2' Hf1' 71.1(4) . . ?
C9 Hf2' Hf1' 121.5(7) 10_556 . ?
Hf1' Hf2' Hf1' 63.0(6) 10_556 . ?
O11 Hf2' Hf1' 102.8(5) . 2_665 ?
O11 Hf2' Hf1' 155.2(10) 10_556 2_665 ?
O70 Hf2' Hf1' 27.2(4) 2_665 2_665 ?
O70 Hf2' Hf1' 83.6(6) 9_666 2_665 ?
O19 Hf2' Hf1' 60.5(5) 11_665 2_665 ?
O19 Hf2' Hf1' 89.2(7) 4_556 2_665 ?
C9 Hf2' Hf1' 96.4(3) . 2_665 ?
C9 Hf2' Hf1' 154.8(4) 10_556 2_665 ?
Si2 O1 Si2 180.00(9) 13_556 . ?
O1 Si2 C21 108.7(4) . . ?
O1 Si2 C12 108.9(3) . . ?
C21 Si2 C12 112.6(4) . . ?
O1 Si2 C3 105.2(3) . . ?
C21 Si2 C3 112.1(4) . . ?
C12 Si2 C3 109.1(3) . . ?
C4 C3 C8 119.4(6) . . ?
C4 C3 Si2 120.1(6) . . ?
C8 C3 Si2 120.5(5) . . ?
C3 C4 C5 120.8(8) . . ?
C6 C5 C4 119.7(8) . . ?
C5 C6 C7 119.4(6) . . ?
C5 C6 C9 121.0(6) . . ?
C7 C6 C9 119.6(6) . . ?
C6 C7 C8 121.6(8) . . ?
C7 C8 C3 119.0(8) . . ?
O11 C9 O10 127.2(5) . . ?
O11 C9 C6 116.6(6) . . ?
O10 C9 C6 116.2(6) . . ?
O11 C9 Hf2' 36.4(4) . . ?
O10 C9 Hf2' 91.2(4) . . ?
C6 C9 Hf2' 152.2(5) . . ?
C9 O10 Hf1 133.0(4) . . ?
C9 O10 Hf1' 136.1(5) . . ?
C9 O11 Hf2' 120.8(6) . . ?
C9 O11 Hf2 131.8(4) . . ?
C17 C12 C13 118.5(6) . . ?
C17 C12 Si2 121.9(5) . . ?
C13 C12 Si2 119.5(5) . . ?
C12 C13 C14 121.1(7) . . ?
C15 C14 C13 120.0(7) . . ?
C14 C15 C16 119.9(6) . . ?
C14 C15 C18 120.2(6) . . ?
C16 C15 C18 119.9(6) . . ?
C15 C16 C17 120.6(7) . . ?
C12 C17 C16 119.8(7) . . ?
O20 C18 O19 126.6(5) . . ?
O20 C18 C15 118.5(5) . . ?
O19 C18 C15 114.9(5) . . ?
C18 O19 Hf2 131.3(4) . 11_565 ?
C18 O19 Hf2' 133.2(4) . 11_565 ?
Hf2 O19 Hf2' 11.6(3) 11_565 11_565 ?
C18 O20 Hf1' 128.6(7) . 12_655 ?
C18 O20 Hf1 133.8(4) . 12_655 ?
Hf1 O50 Hf1 113.1(4) . 10_556 ?
Hf1 O50 Hf2 108.6(3) . 9_666 ?
Hf1 O50 Hf2 108.6(3) 10_556 9_666 ?
Hf1 O60 Hf1 116.6(6) . 10_556 ?
Hf1 O60 Hf2 114.0(8) . . ?
Hf1 O60 Hf2 114.0(8) 10_556 . ?
Hf2' O60' Hf1' 104.5(12) . . ?
Hf1' O60' Hf1' 90.1(13) 10_556 . ?
Hf1 O70 Hf1 112.1(2) 2_665 . ?
Hf1 O70 Hf2 109.8(3) 2_665 9_666 ?
Hf1 O70 Hf2 108.7(3) . 9_666 ?
Hf1 O70 Hf2' 92.0(6) 2_665 9_666 ?
Hf1 O70 Hf2' 124.0(6) . 9_666 ?
Hf2 O70 Hf2' 19.2(6) 9_666 9_666 ?
Hf1 O70 Hf1' 7.9(6) 2_665 2_665 ?
Hf1 O70 Hf1' 104.2(6) . 2_665 ?
Hf2 O70 Hf1' 113.6(4) 9_666 2_665 ?

_refine_diff_density_max         1.863
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.163



#===END




