# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

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

data_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1908218'
loop_
_audit_author_name
_audit_author_address
'Karl Wilhelm Toernroos'
;University of Bergen
Norway
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2019-05-29 downloaded from the CCDC.
;
#data_Puia123

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H59 Cl Hf N2 O4'
_chemical_formula_sum            'C38 H59 Cl Hf N2 O4'
_chemical_formula_weight         821.81

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.7324(16)
_cell_length_b                   13.8338(14)
_cell_length_c                   19.0436(19)
_cell_angle_alpha                90
_cell_angle_beta                 110.6910(10)
_cell_angle_gamma                90
_cell_volume                     3877.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    9247
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      30.89

_exptl_crystal_description       'long prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   0.49259
_exptl_transmission_factor_max   0.74616
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    2.798
_shelx_estimated_absorpt_T_min   0.441
_shelx_estimated_absorpt_T_max   0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4573
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_process_details   'TWINABS, Bruker AXS,  Version 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker TXS APEX-II Ultra Pt135CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12382
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.864
_diffrn_reflns_theta_max         31.037
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             48754
_reflns_number_gt                10479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Twinning - major component used. 
 Rotated from first domain by 166.1 degrees about
 reciprocal axis  1.000 -0.806  0.173  and real axis  1.000 -0.868  0.393

 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       'Bruker AXS Inc. APEX2 v2008.1-0'
_computing_cell_refinement       'Bruker AXS Inc. SAINT V6.45A'
_computing_data_reduction        'Bruker AXS Inc. SAINT V6.45A'
_computing_structure_solution    'SHELXT v.2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)²+3.2935P] 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         12382
_refine_ls_number_parameters     466
_refine_ls_number_restraints     499
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT971_Compound1           
;
PROBLEM: Check Calcd Resid. Dens.  0.78A   From Hf1             2.92 eA-3  
RESPONSE: The crystal speciment was heavily non-merohedrally twinned. 
Integration was done on the major component only resulting in parts 
of 2nd component being part of the integrated intensity, and therefore 
reflected in residual electron density around primarily the 
heavier elements. Also there is one rotationally disorderded thf ligand 
molecule in the structure.     
;
# end Validation Reply Form

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 0.41589(2) 0.69600(2) 0.31435(2) 0.02217(4) Uani 1 1 d . . . . .
Cl1 Cl 0.41759(7) 0.83348(6) 0.23281(5) 0.0419(2) Uani 1 1 d . . . . .
O1 O 0.53365(15) 0.71077(15) 0.39855(12) 0.0260(4) Uani 1 1 d . . . . .
N1 N 0.38568(16) 0.46379(17) 0.33820(13) 0.0226(4) Uani 1 1 d . . . . .
C1 C 0.44237(19) 0.5391(2) 0.36208(15) 0.0220(5) Uani 1 1 d . . . . .
O2 O 0.31565(13) 0.62204(15) 0.24182(12) 0.0255(4) Uani 1 1 d . . . . .
N2 N 0.52038(16) 0.50766(17) 0.41408(13) 0.0226(4) Uani 1 1 d . . . . .
C2 C 0.4231(2) 0.3736(2) 0.37880(17) 0.0280(6) Uani 1 1 d . . . . .
H2A H 0.421899 0.320689 0.343502 0.034 Uiso 1 1 calc R U . . .
H2B H 0.388785 0.353317 0.411023 0.034 Uiso 1 1 calc R U . . .
O3 O 0.34269(16) 0.75319(19) 0.37213(18) 0.0454(6) Uani 1 1 d . . . . .
C3 C 0.5199(2) 0.4016(2) 0.42565(16) 0.0256(5) Uani 1 1 d . . . . .
H3A H 0.533966 0.385658 0.479261 0.031 Uiso 1 1 calc R U . . .
H3B H 0.564160 0.368662 0.407578 0.031 Uiso 1 1 calc R U . . .
O4 O 0.50294(15) 0.62904(17) 0.25139(13) 0.0333(5) Uani 1 1 d D . . . .
C4 C 0.60254(19) 0.5603(2) 0.44792(15) 0.0219(5) Uani 1 1 d . . . . .
C5 C 0.60715(18) 0.6614(2) 0.44021(15) 0.0212(5) Uani 1 1 d . . . . .
C6 C 0.6905(2) 0.7103(2) 0.47570(16) 0.0219(5) Uani 1 1 d . . . . .
C7 C 0.76700(19) 0.6551(2) 0.51361(16) 0.0238(5) Uani 1 1 d . . . . .
H7 H 0.823479 0.687295 0.536059 0.029 Uiso 1 1 calc R U . . .
C8 C 0.76473(19) 0.5554(2) 0.52018(17) 0.0256(5) Uani 1 1 d . . . . .
C9 C 0.6809(2) 0.5092(2) 0.48865(17) 0.0257(5) Uani 1 1 d . . . . .
H9 H 0.677122 0.441388 0.495073 0.031 Uiso 1 1 calc R U . . .
C10 C 0.6955(2) 0.8209(2) 0.47194(17) 0.0267(6) Uani 1 1 d . . . . .
C11 C 0.6702(2) 0.8566(2) 0.39071(18) 0.0325(7) Uani 1 1 d . . . . .
H11A H 0.680254 0.926493 0.390694 0.049 Uiso 1 1 calc R U . . .
H11B H 0.606043 0.842385 0.362747 0.049 Uiso 1 1 calc R U . . .
H11C H 0.708079 0.823673 0.366867 0.049 Uiso 1 1 calc R U . . .
C12 C 0.6311(2) 0.8656(3) 0.5076(2) 0.0375(7) Uani 1 1 d . . . . .
H12A H 0.632045 0.936202 0.503316 0.056 Uiso 1 1 calc R U . . .
H12B H 0.651024 0.847476 0.560746 0.056 Uiso 1 1 calc R U . . .
H12C H 0.569262 0.841864 0.481631 0.056 Uiso 1 1 calc R U . . .
C13 C 0.7911(2) 0.8588(2) 0.5152(2) 0.0356(7) Uani 1 1 d . . . . .
H13A H 0.790491 0.929609 0.514525 0.053 Uiso 1 1 calc R U . . .
H13B H 0.833162 0.835061 0.491525 0.053 Uiso 1 1 calc R U . . .
H13C H 0.810750 0.835949 0.567211 0.053 Uiso 1 1 calc R U . . .
C14 C 0.8504(2) 0.4944(2) 0.55696(19) 0.0317(6) Uani 1 1 d . . . . .
C15 C 0.9362(2) 0.5555(3) 0.5823(3) 0.0560(12) Uani 1 1 d . . . . .
H15A H 0.989200 0.513681 0.604513 0.084 Uiso 1 1 calc R U . . .
H15B H 0.933019 0.602636 0.619753 0.084 Uiso 1 1 calc R U . . .
H15C H 0.941658 0.589696 0.539034 0.084 Uiso 1 1 calc R U . . .
C16 C 0.8449(3) 0.4429(3) 0.6267(2) 0.0475(9) Uani 1 1 d . . . . .
H16A H 0.902013 0.408666 0.652390 0.071 Uiso 1 1 calc R U . . .
H16B H 0.794606 0.396414 0.611432 0.071 Uiso 1 1 calc R U . . .
H16C H 0.834497 0.490658 0.660820 0.071 Uiso 1 1 calc R U . . .
C17 C 0.8586(3) 0.4205(4) 0.5006(3) 0.0551(11) Uani 1 1 d . . . . .
H17A H 0.912530 0.380370 0.524243 0.083 Uiso 1 1 calc R U . . .
H17B H 0.864306 0.454077 0.457195 0.083 Uiso 1 1 calc R U . . .
H17C H 0.804354 0.379478 0.484176 0.083 Uiso 1 1 calc R U . . .
C18 C 0.29809(19) 0.4626(2) 0.28076(15) 0.0232(5) Uani 1 1 d . . . . .
C19 C 0.26452(19) 0.5430(2) 0.23377(16) 0.0234(5) Uani 1 1 d . . . . .
C20 C 0.1781(2) 0.5389(2) 0.17793(17) 0.0284(6) Uani 1 1 d . . . . .
C21 C 0.1283(2) 0.4540(2) 0.17023(18) 0.0317(6) Uani 1 1 d . . . . .
H21 H 0.070304 0.450589 0.131611 0.038 Uiso 1 1 calc R U . . .
C22 C 0.1593(2) 0.3740(2) 0.21618(17) 0.0291(6) Uani 1 1 d . . . . .
C23 C 0.2447(2) 0.3793(2) 0.27179(17) 0.0277(6) Uani 1 1 d . . . . .
H23 H 0.267309 0.325627 0.304178 0.033 Uiso 1 1 calc R U . . .
C24 C 0.1397(2) 0.6283(3) 0.1279(2) 0.0369(7) Uani 1 1 d . . . . .
C25 C 0.0435(3) 0.6089(4) 0.0717(3) 0.0682(16) Uani 1 1 d . . . . .
H25A H 0.020043 0.667483 0.042228 0.102 Uiso 1 1 calc R U . . .
H25B H 0.003522 0.590716 0.098961 0.102 Uiso 1 1 calc R U . . .
H25C H 0.045630 0.556220 0.037938 0.102 Uiso 1 1 calc R U . . .
C26 C 0.1321(3) 0.7136(3) 0.1767(3) 0.0506(10) Uani 1 1 d . . . . .
H26A H 0.101191 0.767496 0.144354 0.076 Uiso 1 1 calc R U . . .
H26B H 0.193080 0.733978 0.208937 0.076 Uiso 1 1 calc R U . . .
H26C H 0.097258 0.693808 0.207916 0.076 Uiso 1 1 calc R U . . .
C27 C 0.1997(3) 0.6549(3) 0.0831(2) 0.0461(9) Uani 1 1 d . . . . .
H27A H 0.171630 0.708009 0.048713 0.069 Uiso 1 1 calc R U . . .
H27B H 0.206365 0.598571 0.054237 0.069 Uiso 1 1 calc R U . . .
H27C H 0.259623 0.675028 0.117564 0.069 Uiso 1 1 calc R U . . .
C28 C 0.1006(2) 0.2822(3) 0.2038(2) 0.0373(7) Uani 1 1 d . . . . .
C29 C 0.1261(3) 0.2208(3) 0.2737(3) 0.0516(10) Uani 1 1 d . . . . .
H29A H 0.082268 0.167837 0.265833 0.077 Uiso 1 1 calc R U . . .
H29B H 0.125403 0.260535 0.316056 0.077 Uiso 1 1 calc R U . . .
H29C H 0.187044 0.194032 0.284464 0.077 Uiso 1 1 calc R U . . .
C30 C 0.1115(5) 0.2239(4) 0.1399(3) 0.0733(17) Uani 1 1 d . . . . .
H30A H 0.077128 0.163518 0.133738 0.110 Uiso 1 1 calc R U . . .
H30B H 0.175948 0.209211 0.151288 0.110 Uiso 1 1 calc R U . . .
H30C H 0.088540 0.261522 0.093300 0.110 Uiso 1 1 calc R U . . .
C31 C 0.0004(3) 0.3096(4) 0.1842(4) 0.0665(15) Uani 1 1 d . . . . .
H31A H -0.034510 0.251896 0.186904 0.100 Uiso 1 1 calc R U . . .
H31B H -0.023347 0.336168 0.133241 0.100 Uiso 1 1 calc R U . . .
H31C H -0.004992 0.358062 0.219887 0.100 Uiso 1 1 calc R U . . .
C32 C 0.2967(5) 0.8028(4) 0.4048(4) 0.0741(15) Uani 1 1 d . . . . .
H32 H 0.252701 0.757995 0.415127 0.089 Uiso 1 1 calc R U . . .
C33 C 0.3638(6) 0.8351(5) 0.4786(3) 0.094(2) Uani 1 1 d . . . . .
H33A H 0.331365 0.865218 0.508397 0.141 Uiso 1 1 calc R U . . .
H33B H 0.405623 0.882161 0.469933 0.141 Uiso 1 1 calc R U . . .
H33C H 0.398152 0.779216 0.505649 0.141 Uiso 1 1 calc R U . . .
C34 C 0.2441(4) 0.8837(5) 0.3578(4) 0.090(2) Uani 1 1 d . . . . .
H34A H 0.209509 0.916853 0.384464 0.135 Uiso 1 1 calc R U . . .
H34B H 0.202092 0.857940 0.310205 0.135 Uiso 1 1 calc R U . . .
H34C H 0.285925 0.929404 0.347684 0.135 Uiso 1 1 calc R U . . .
C35 C 0.5981(3) 0.6512(6) 0.2657(4) 0.0370(14) Uani 0.586(7) 1 d D U P A 1
H35A H 0.634647 0.643273 0.319582 0.044 Uiso 0.586(7) 1 calc R U P A 1
H35B H 0.604832 0.718522 0.250699 0.044 Uiso 0.586(7) 1 calc R U P A 1
C36 C 0.6284(10) 0.5806(12) 0.2189(6) 0.046(2) Uani 0.586(7) 1 d D U P A 1
H36A H 0.654353 0.521432 0.247775 0.055 Uiso 0.586(7) 1 calc R U P A 1
H36B H 0.673886 0.609987 0.200427 0.055 Uiso 0.586(7) 1 calc R U P A 1
C37 C 0.5404(9) 0.5588(14) 0.1547(11) 0.0480(18) Uani 0.586(7) 1 d D U P A 1
H37A H 0.527982 0.608418 0.114871 0.058 Uiso 0.586(7) 1 calc R U P A 1
H37B H 0.543059 0.494544 0.132698 0.058 Uiso 0.586(7) 1 calc R U P A 1
C38 C 0.4689(4) 0.5607(5) 0.1905(4) 0.0390(11) Uani 0.586(7) 1 d D U P A 1
H38A H 0.409712 0.582281 0.154056 0.047 Uiso 0.586(7) 1 calc R U P A 1
H38B H 0.461273 0.495965 0.209560 0.047 Uiso 0.586(7) 1 calc R U P A 1
C35A C 0.5985(4) 0.6069(9) 0.2724(5) 0.0374(14) Uani 0.414(7) 1 d D U P A 2
H35C H 0.613847 0.547946 0.303815 0.045 Uiso 0.414(7) 1 calc R U P A 2
H35D H 0.635870 0.661121 0.301219 0.045 Uiso 0.414(7) 1 calc R U P A 2
C36A C 0.6162(15) 0.5914(19) 0.2004(8) 0.046(2) Uani 0.414(7) 1 d D U P A 2
H36C H 0.665774 0.544114 0.207454 0.055 Uiso 0.414(7) 1 calc R U P A 2
H36D H 0.632361 0.652866 0.181582 0.055 Uiso 0.414(7) 1 calc R U P A 2
C37A C 0.5264(13) 0.5525(19) 0.1469(17) 0.0478(18) Uani 0.414(7) 1 d D U P A 2
H37C H 0.519508 0.563413 0.093809 0.057 Uiso 0.414(7) 1 calc R U P A 2
H37D H 0.519069 0.482862 0.155228 0.057 Uiso 0.414(7) 1 calc R U P A 2
C38A C 0.4615(6) 0.6138(8) 0.1700(3) 0.0394(12) Uani 0.414(7) 1 d D U P A 2
H38C H 0.451297 0.676560 0.143330 0.047 Uiso 0.414(7) 1 calc R U P A 2
H38D H 0.402288 0.580511 0.157686 0.047 Uiso 0.414(7) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O2 1.975(2) . ?
Hf1 O1 1.986(2) . ?
Hf1 O3 2.014(3) . ?
Hf1 O4 2.309(2) . ?
Hf1 C1 2.333(3) . ?
Hf1 Cl1 2.4614(9) . ?
O1 C5 1.336(3) . ?
N1 C1 1.343(4) . ?
N1 C18 1.425(4) . ?
N1 C2 1.476(4) . ?
C1 N2 1.348(4) . ?
O2 C19 1.334(3) . ?
N2 C4 1.424(4) . ?
N2 C3 1.485(4) . ?
C2 C3 1.518(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 C32 1.303(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C38 1.444(4) . ?
O4 C35A 1.446(5) . ?
O4 C35 1.457(4) . ?
O4 C38A 1.469(5) . ?
C4 C9 1.395(4) . ?
C4 C5 1.410(4) . ?
C5 C6 1.417(4) . ?
C6 C7 1.392(4) . ?
C6 C10 1.535(4) . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.396(4) . ?
C8 C14 1.533(4) . ?
C9 H9 0.9500 . ?
C10 C13 1.529(4) . ?
C10 C12 1.535(5) . ?
C10 C11 1.537(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C17 1.520(5) . ?
C14 C15 1.520(5) . ?
C14 C16 1.537(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.401(4) . ?
C18 C19 1.408(4) . ?
C19 C20 1.401(4) . ?
C20 C21 1.390(4) . ?
C20 C24 1.547(5) . ?
C21 C22 1.388(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.388(4) . ?
C22 C28 1.539(4) . ?
C23 H23 0.9500 . ?
C24 C27 1.524(6) . ?
C24 C26 1.531(6) . ?
C24 C25 1.538(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.509(6) . ?
C28 C30 1.520(6) . ?
C28 C31 1.533(6) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C34 1.488(9) . ?
C32 C33 1.496(10) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.508(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.518(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.508(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C35A C36A 1.508(7) . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C36A C37A 1.518(9) . ?
C36A H36C 0.9900 . ?
C36A H36D 0.9900 . ?
C37A C38A 1.508(7) . ?
C37A H37C 0.9900 . ?
C37A H37D 0.9900 . ?
C38A H38C 0.9900 . ?
C38A H38D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Hf1 O1 154.71(8) . . ?
O2 Hf1 O3 96.67(10) . . ?
O1 Hf1 O3 93.95(10) . . ?
O2 Hf1 O4 84.40(8) . . ?
O1 Hf1 O4 84.56(9) . . ?
O3 Hf1 O4 178.33(10) . . ?
O2 Hf1 C1 77.24(9) . . ?
O1 Hf1 C1 78.11(9) . . ?
O3 Hf1 C1 102.15(10) . . ?
O4 Hf1 C1 76.82(9) . . ?
O2 Hf1 Cl1 98.22(6) . . ?
O1 Hf1 Cl1 102.41(7) . . ?
O3 Hf1 Cl1 100.19(8) . . ?
O4 Hf1 Cl1 80.89(7) . . ?
C1 Hf1 Cl1 157.57(7) . . ?
C5 O1 Hf1 142.30(19) . . ?
C1 N1 C18 128.0(2) . . ?
C1 N1 C2 112.6(2) . . ?
C18 N1 C2 119.4(2) . . ?
N1 C1 N2 108.7(2) . . ?
N1 C1 Hf1 125.8(2) . . ?
N2 C1 Hf1 125.28(19) . . ?
C19 O2 Hf1 143.61(19) . . ?
C1 N2 C4 127.8(2) . . ?
C1 N2 C3 112.2(2) . . ?
C4 N2 C3 119.3(2) . . ?
N1 C2 C3 103.0(2) . . ?
N1 C2 H2A 111.2 . . ?
C3 C2 H2A 111.2 . . ?
N1 C2 H2B 111.2 . . ?
C3 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
C32 O3 Hf1 171.1(3) . . ?
N2 C3 C2 102.8(2) . . ?
N2 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
N2 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C38 O4 C35 110.7(4) . . ?
C35A O4 C38A 107.0(6) . . ?
C38 O4 Hf1 124.0(3) . . ?
C35A O4 Hf1 133.7(4) . . ?
C35 O4 Hf1 125.3(3) . . ?
C38A O4 Hf1 118.8(4) . . ?
C9 C4 C5 119.5(3) . . ?
C9 C4 N2 118.3(2) . . ?
C5 C4 N2 122.1(2) . . ?
O1 C5 C4 120.2(2) . . ?
O1 C5 C6 120.0(3) . . ?
C4 C5 C6 119.8(2) . . ?
C7 C6 C5 118.1(3) . . ?
C7 C6 C10 121.5(3) . . ?
C5 C6 C10 120.5(3) . . ?
C8 C7 C6 123.2(3) . . ?
C8 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
C7 C8 C9 117.9(3) . . ?
C7 C8 C14 122.8(3) . . ?
C9 C8 C14 119.3(3) . . ?
C4 C9 C8 121.5(3) . . ?
C4 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C13 C10 C6 111.9(3) . . ?
C13 C10 C12 107.4(3) . . ?
C6 C10 C12 109.2(3) . . ?
C13 C10 C11 106.7(3) . . ?
C6 C10 C11 111.6(3) . . ?
C12 C10 C11 109.8(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C14 C15 108.1(3) . . ?
C17 C14 C8 109.1(3) . . ?
C15 C14 C8 112.2(3) . . ?
C17 C14 C16 110.1(3) . . ?
C15 C14 C16 107.4(3) . . ?
C8 C14 C16 110.0(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 119.9(3) . . ?
C23 C18 N1 118.6(3) . . ?
C19 C18 N1 121.5(2) . . ?
O2 C19 C20 120.3(3) . . ?
O2 C19 C18 119.9(2) . . ?
C20 C19 C18 119.8(3) . . ?
C21 C20 C19 118.3(3) . . ?
C21 C20 C24 121.9(3) . . ?
C19 C20 C24 119.9(3) . . ?
C22 C21 C20 123.2(3) . . ?
C22 C21 H21 118.4 . . ?
C20 C21 H21 118.4 . . ?
C21 C22 C23 118.0(3) . . ?
C21 C22 C28 120.2(3) . . ?
C23 C22 C28 121.8(3) . . ?
C22 C23 C18 120.9(3) . . ?
C22 C23 H23 119.6 . . ?
C18 C23 H23 119.6 . . ?
C27 C24 C26 110.5(3) . . ?
C27 C24 C25 107.7(4) . . ?
C26 C24 C25 106.8(4) . . ?
C27 C24 C20 110.7(3) . . ?
C26 C24 C20 109.9(3) . . ?
C25 C24 C20 111.3(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C30 109.7(4) . . ?
C29 C28 C31 106.5(4) . . ?
C30 C28 C31 109.5(4) . . ?
C29 C28 C22 111.8(3) . . ?
C30 C28 C22 109.2(3) . . ?
C31 C28 C22 110.1(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O3 C32 C34 113.2(6) . . ?
O3 C32 C33 106.2(5) . . ?
C34 C32 C33 113.5(5) . . ?
O3 C32 H32 107.9 . . ?
C34 C32 H32 107.9 . . ?
C33 C32 H32 107.9 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O4 C35 C36 105.8(8) . . ?
O4 C35 H35A 110.6 . . ?
C36 C35 H35A 110.6 . . ?
O4 C35 H35B 110.6 . . ?
C36 C35 H35B 110.6 . . ?
H35A C35 H35B 108.7 . . ?
C35 C36 C37 102.5(9) . . ?
C35 C36 H36A 111.3 . . ?
C37 C36 H36A 111.3 . . ?
C35 C36 H36B 111.3 . . ?
C37 C36 H36B 111.3 . . ?
H36A C36 H36B 109.2 . . ?
C38 C37 C36 104.2(12) . . ?
C38 C37 H37A 110.9 . . ?
C36 C37 H37A 110.9 . . ?
C38 C37 H37B 110.9 . . ?
C36 C37 H37B 110.9 . . ?
H37A C37 H37B 108.9 . . ?
O4 C38 C37 104.5(7) . . ?
O4 C38 H38A 110.9 . . ?
C37 C38 H38A 110.9 . . ?
O4 C38 H38B 110.9 . . ?
C37 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
O4 C35A C36A 106.6(10) . . ?
O4 C35A H35C 110.4 . . ?
C36A C35A H35C 110.4 . . ?
O4 C35A H35D 110.4 . . ?
C36A C35A H35D 110.4 . . ?
H35C C35A H35D 108.6 . . ?
C35A C36A C37A 103.5(18) . . ?
C35A C36A H36C 111.1 . . ?
C37A C36A H36C 111.1 . . ?
C35A C36A H36D 111.1 . . ?
C37A C36A H36D 111.1 . . ?
H36C C36A H36D 109.0 . . ?
C38A C37A C36A 99.9(13) . . ?
C38A C37A H37C 111.8 . . ?
C36A C37A H37C 111.8 . . ?
C38A C37A H37D 111.8 . . ?
C36A C37A H37D 111.8 . . ?
H37C C37A H37D 109.5 . . ?
O4 C38A C37A 107.1(12) . . ?
O4 C38A H38C 110.3 . . ?
C37A C38A H38C 110.3 . . ?
O4 C38A H38D 110.3 . . ?
C37A C38A H38D 110.3 . . ?
H38C C38A H38D 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 N1 C1 N2 -176.3(3) . . . . ?
C2 N1 C1 N2 3.7(3) . . . . ?
C18 N1 C1 Hf1 -1.2(4) . . . . ?
C2 N1 C1 Hf1 178.8(2) . . . . ?
N1 C1 N2 C4 172.2(3) . . . . ?
Hf1 C1 N2 C4 -2.9(4) . . . . ?
N1 C1 N2 C3 2.3(3) . . . . ?
Hf1 C1 N2 C3 -172.82(19) . . . . ?
C1 N1 C2 C3 -7.7(3) . . . . ?
C18 N1 C2 C3 172.2(2) . . . . ?
C1 N2 C3 C2 -6.9(3) . . . . ?
C4 N2 C3 C2 -177.8(2) . . . . ?
N1 C2 C3 N2 8.2(3) . . . . ?
C1 N2 C4 C9 -166.9(3) . . . . ?
C3 N2 C4 C9 2.4(4) . . . . ?
C1 N2 C4 C5 11.8(4) . . . . ?
C3 N2 C4 C5 -178.9(3) . . . . ?
Hf1 O1 C5 C4 -23.7(5) . . . . ?
Hf1 O1 C5 C6 155.2(2) . . . . ?
C9 C4 C5 O1 177.0(3) . . . . ?
N2 C4 C5 O1 -1.8(4) . . . . ?
C9 C4 C5 C6 -1.9(4) . . . . ?
N2 C4 C5 C6 179.4(3) . . . . ?
O1 C5 C6 C7 -175.0(3) . . . . ?
C4 C5 C6 C7 3.8(4) . . . . ?
O1 C5 C6 C10 4.9(4) . . . . ?
C4 C5 C6 C10 -176.2(3) . . . . ?
C5 C6 C7 C8 -2.1(4) . . . . ?
C10 C6 C7 C8 178.0(3) . . . . ?
C6 C7 C8 C9 -1.7(5) . . . . ?
C6 C7 C8 C14 175.4(3) . . . . ?
C5 C4 C9 C8 -2.0(4) . . . . ?
N2 C4 C9 C8 176.8(3) . . . . ?
C7 C8 C9 C4 3.7(4) . . . . ?
C14 C8 C9 C4 -173.4(3) . . . . ?
C7 C6 C10 C13 -1.3(4) . . . . ?
C5 C6 C10 C13 178.8(3) . . . . ?
C7 C6 C10 C12 -120.1(3) . . . . ?
C5 C6 C10 C12 60.0(4) . . . . ?
C7 C6 C10 C11 118.3(3) . . . . ?
C5 C6 C10 C11 -61.7(4) . . . . ?
C7 C8 C14 C17 -121.6(4) . . . . ?
C9 C8 C14 C17 55.4(4) . . . . ?
C7 C8 C14 C15 -1.8(5) . . . . ?
C9 C8 C14 C15 175.1(3) . . . . ?
C7 C8 C14 C16 117.6(4) . . . . ?
C9 C8 C14 C16 -65.5(4) . . . . ?
C1 N1 C18 C23 -171.1(3) . . . . ?
C2 N1 C18 C23 8.9(4) . . . . ?
C1 N1 C18 C19 8.5(4) . . . . ?
C2 N1 C18 C19 -171.4(3) . . . . ?
Hf1 O2 C19 C20 155.6(3) . . . . ?
Hf1 O2 C19 C18 -25.4(5) . . . . ?
C23 C18 C19 O2 -179.4(3) . . . . ?
N1 C18 C19 O2 1.0(4) . . . . ?
C23 C18 C19 C20 -0.4(4) . . . . ?
N1 C18 C19 C20 180.0(3) . . . . ?
O2 C19 C20 C21 178.1(3) . . . . ?
C18 C19 C20 C21 -0.8(4) . . . . ?
O2 C19 C20 C24 -3.1(4) . . . . ?
C18 C19 C20 C24 178.0(3) . . . . ?
C19 C20 C21 C22 1.5(5) . . . . ?
C24 C20 C21 C22 -177.3(3) . . . . ?
C20 C21 C22 C23 -0.9(5) . . . . ?
C20 C21 C22 C28 -179.5(3) . . . . ?
C21 C22 C23 C18 -0.4(5) . . . . ?
C28 C22 C23 C18 178.2(3) . . . . ?
C19 C18 C23 C22 1.0(5) . . . . ?
N1 C18 C23 C22 -179.3(3) . . . . ?
C21 C20 C24 C27 -119.8(4) . . . . ?
C19 C20 C24 C27 61.5(4) . . . . ?
C21 C20 C24 C26 117.9(4) . . . . ?
C19 C20 C24 C26 -60.8(4) . . . . ?
C21 C20 C24 C25 -0.1(5) . . . . ?
C19 C20 C24 C25 -178.9(4) . . . . ?
C21 C22 C28 C29 -157.8(4) . . . . ?
C23 C22 C28 C29 23.6(5) . . . . ?
C21 C22 C28 C30 80.6(5) . . . . ?
C23 C22 C28 C30 -98.0(5) . . . . ?
C21 C22 C28 C31 -39.6(5) . . . . ?
C23 C22 C28 C31 141.7(4) . . . . ?
C38 O4 C35 C36 -9.2(9) . . . . ?
Hf1 O4 C35 C36 172.4(6) . . . . ?
O4 C35 C36 C37 27.3(16) . . . . ?
C35 C36 C37 C38 -35.2(18) . . . . ?
C35 O4 C38 C37 -13.1(11) . . . . ?
Hf1 O4 C38 C37 165.3(10) . . . . ?
C36 C37 C38 O4 30.1(17) . . . . ?
C38A O4 C35A C36A 7.7(14) . . . . ?
Hf1 O4 C35A C36A -163.9(11) . . . . ?
O4 C35A C36A C37A -30(2) . . . . ?
C35A C36A C37A C38A 39(3) . . . . ?
C35A O4 C38A C37A 17.8(14) . . . . ?
Hf1 O4 C38A C37A -169.2(11) . . . . ?
C36A C37A C38A O4 -35(2) . . . . ?

_refine_diff_density_max         3.084
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.137


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

data_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1908220'
loop_
_audit_author_name
_audit_author_address
'Karl Wilhelm Toernroos'
;University of Bergen
Norway
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2019-05-29 downloaded from the CCDC.
;
#data_puia203_a_sq

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C31 H44 Cl3 Hf N2 O2, C36 H30 N P2, 2(C4 H8 O)'
_chemical_formula_sum            'C75 H90 Cl3 Hf N3 O4 P2'
_chemical_formula_weight         1444.27

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.0310(12)
_cell_length_b                   15.1732(12)
_cell_length_c                   20.3432(17)
_cell_angle_alpha                109.7190(10)
_cell_angle_beta                 93.3830(10)
_cell_angle_gamma                116.0500(10)
_cell_volume                     3804.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9938
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.42

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             1492
_exptl_transmission_factor_min   0.85142
_exptl_transmission_factor_max   0.91413
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.087
_exptl_absorpt_coefficient_mu    1.565
_shelx_estimated_absorpt_T_min   0.785
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6294
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker AXS TXS Ultra Rotating Anode'
_diffrn_measurement_device_type  'Bruker AXS APEXII Pt135 CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55516
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.614
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             18138
_reflns_number_gt                15414
_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       'Bruker AXS Inc. APEX2 v2008.1-0'
_computing_cell_refinement       'Bruker AXS Inc. SAINT V6.45A'
_computing_data_reduction        'Bruker AXS Inc. SAINT V6.45A'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0834P)²+7.0140P] 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         18138
_refine_ls_number_parameters     806
_refine_ls_number_restraints     744
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2.00 1.00 0.00 0.0350
2.00 -1.00 0.00 0.0570
1.00 0.00 1.00 0.0660
0.00 1.00 2.00 0.0590
-1.00 0.00 -1.00 0.0450
1.00 -1.00 -1.00 0.0400
-1.00 -1.00 2.00 0.0430
1.00 1.00 -2.00 0.0190
-1.00 1.00 1.00 0.0500
-1.00 2.00 0.00 0.0280
1.00 -2.00 0.00 0.0460
0.00 -1.00 2.00 0.0680

# SQUEEZE RESULTS (Version = 200618)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.679 0.500 450 102 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


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 0.55851(2) 0.50775(2) 0.20482(2) 0.01502(7) Uani 1 1 d . . . . .
Cl1 Cl 0.52697(17) 0.51095(19) 0.32388(10) 0.0657(5) Uani 1 1 d . . . . .
Cl2 Cl 0.69843(9) 0.69665(10) 0.27072(8) 0.0358(3) Uani 1 1 d . . . . .
Cl3 Cl 0.40663(9) 0.33104(9) 0.13689(7) 0.0284(3) Uani 1 1 d . . . . .
P1 P 0.12396(8) -0.01584(8) 0.31353(6) 0.0140(2) Uani 1 1 d . . . . .
P2 P 0.02460(8) 0.11993(8) 0.34100(6) 0.0141(2) Uani 1 1 d . . . . .
O1 O 0.6527(2) 0.4468(2) 0.19388(16) 0.0173(6) Uani 1 1 d . . . . .
O2 O 0.4818(2) 0.5722(2) 0.17492(16) 0.0157(6) Uani 1 1 d . . . . .
N1 N 0.6751(3) 0.4930(3) 0.07080(17) 0.0118(6) Uani 1 1 d . . . . .
N2 N 0.6013(3) 0.5899(3) 0.07298(18) 0.0132(6) Uani 1 1 d . . . . .
N3 N 0.0372(3) 0.0162(3) 0.3098(2) 0.0165(7) Uani 1 1 d . . . . .
C1 C 0.6163(3) 0.5308(3) 0.1046(2) 0.0130(7) Uani 1 1 d . . . . .
C2 C 0.6547(3) 0.5970(3) 0.0145(2) 0.0148(8) Uani 1 1 d . . . . .
H2A H 0.709722 0.671207 0.027215 0.018 Uiso 1 1 calc R U . . .
H2AB H 0.606567 0.572553 -0.031246 0.018 Uiso 1 1 calc R U . . .
C3 C 0.6979(3) 0.5224(3) 0.0091(2) 0.0151(8) Uani 1 1 d . . . . .
H3A H 0.664197 0.458293 -0.037114 0.018 Uiso 1 1 calc R U . . .
H3AB H 0.772430 0.559340 0.013319 0.018 Uiso 1 1 calc R U . . .
C4 C 0.7138(3) 0.4307(3) 0.0879(2) 0.0141(7) Uani 1 1 d . . . . .
C5 C 0.7029(3) 0.4106(3) 0.1502(2) 0.0149(8) Uani 1 1 d . . . . .
C6 C 0.7469(3) 0.3528(3) 0.1669(2) 0.0164(8) Uani 1 1 d . . . . .
C7 C 0.7980(3) 0.3164(3) 0.1195(2) 0.0191(8) Uani 1 1 d . . . . .
H7 H 0.827234 0.277157 0.130204 0.023 Uiso 1 1 calc R U . . .
C8 C 0.8088(3) 0.3346(3) 0.0565(2) 0.0187(8) Uani 1 1 d . . . . .
C9 C 0.7655(3) 0.3919(3) 0.0418(2) 0.0172(8) Uani 1 1 d . . . . .
H9 H 0.771084 0.405027 -0.000687 0.021 Uiso 1 1 calc R U . . .
C10 C 0.7390(4) 0.3322(4) 0.2356(2) 0.0205(9) Uani 1 1 d . . . . .
C11 C 0.7855(4) 0.4373(4) 0.3023(3) 0.0262(10) Uani 1 1 d . . . . .
H11A H 0.781790 0.422149 0.345546 0.039 Uiso 1 1 calc R U . . .
H11B H 0.747487 0.475284 0.300552 0.039 Uiso 1 1 calc R U . . .
H11C H 0.857032 0.482017 0.303720 0.039 Uiso 1 1 calc R U . . .
C12 C 0.6252(4) 0.2615(4) 0.2328(3) 0.0302(11) Uani 1 1 d . . . . .
H12A H 0.620999 0.244449 0.275267 0.045 Uiso 1 1 calc R U . . .
H12B H 0.594933 0.194922 0.189121 0.045 Uiso 1 1 calc R U . . .
H12C H 0.588047 0.300651 0.232265 0.045 Uiso 1 1 calc R U . . .
C13 C 0.7965(4) 0.2729(4) 0.2440(3) 0.0319(11) Uani 1 1 d . . . . .
H13A H 0.793193 0.264434 0.289585 0.048 Uiso 1 1 calc R U . . .
H13B H 0.868046 0.314317 0.243735 0.048 Uiso 1 1 calc R U . . .
H13C H 0.765009 0.202012 0.203904 0.048 Uiso 1 1 calc R U . . .
C14 C 0.8717(4) 0.2969(4) 0.0097(3) 0.0261(10) Uani 1 1 d . . . . .
C15 C 0.8512(5) 0.1858(4) 0.0019(3) 0.0369(13) Uani 1 1 d . . . . .
H15A H 0.894092 0.165317 -0.027185 0.055 Uiso 1 1 calc R U . . .
H15B H 0.779060 0.133768 -0.021829 0.055 Uiso 1 1 calc R U . . .
H15C H 0.867116 0.186892 0.049654 0.055 Uiso 1 1 calc R U . . .
C16 C 0.9854(5) 0.3756(5) 0.0490(4) 0.0530(18) Uani 1 1 d . . . . .
H16A H 1.028324 0.361156 0.017234 0.079 Uiso 1 1 calc R U . . .
H16B H 1.000973 0.366119 0.092793 0.079 Uiso 1 1 calc R U . . .
H16C H 0.998980 0.449465 0.061934 0.079 Uiso 1 1 calc R U . . .
C17 C 0.8512(7) 0.2946(7) -0.0646(4) 0.061(2) Uani 1 1 d . . . . .
H17A H 0.895082 0.273144 -0.091965 0.091 Uiso 1 1 calc R U . . .
H17B H 0.865887 0.366137 -0.060460 0.091 Uiso 1 1 calc R U . . .
H17C H 0.779420 0.242987 -0.089526 0.091 Uiso 1 1 calc R U . . .
C18 C 0.5557(3) 0.6561(3) 0.0975(2) 0.0131(7) Uani 1 1 d . . . . .
C19 C 0.4974(3) 0.6462(3) 0.1490(2) 0.0135(7) Uani 1 1 d . . . . .
C20 C 0.4550(3) 0.7143(3) 0.1722(2) 0.0147(8) Uani 1 1 d . . . . .
C21 C 0.4723(3) 0.7900(3) 0.1426(2) 0.0173(8) Uani 1 1 d . . . . .
H21 H 0.444204 0.836452 0.158204 0.021 Uiso 1 1 calc R U . . .
C22 C 0.5285(3) 0.7994(3) 0.0916(2) 0.0176(8) Uani 1 1 d . . . . .
C23 C 0.5685(3) 0.7305(3) 0.0676(2) 0.0161(8) Uani 1 1 d . . . . .
H23 H 0.604525 0.733767 0.030899 0.019 Uiso 1 1 calc R U . . .
C24 C 0.3923(3) 0.7059(4) 0.2286(2) 0.0197(9) Uani 1 1 d . . . . .
C25 C 0.3530(4) 0.7868(4) 0.2469(3) 0.0264(10) Uani 1 1 d . . . . .
H25A H 0.314438 0.778993 0.283669 0.040 Uiso 1 1 calc R U . . .
H25B H 0.308504 0.773417 0.203453 0.040 Uiso 1 1 calc R U . . .
H25C H 0.411053 0.859810 0.265311 0.040 Uiso 1 1 calc R U . . .
C26 C 0.2980(4) 0.5928(4) 0.2006(3) 0.0278(10) Uani 1 1 d . . . . .
H26A H 0.259600 0.587651 0.237711 0.042 Uiso 1 1 calc R U . . .
H26B H 0.320309 0.538823 0.189234 0.042 Uiso 1 1 calc R U . . .
H26C H 0.254209 0.580313 0.157104 0.042 Uiso 1 1 calc R U . . .
C27 C 0.4590(4) 0.7307(4) 0.3004(3) 0.0276(10) Uani 1 1 d . . . . .
H27A H 0.417119 0.721831 0.335301 0.041 Uiso 1 1 calc R U . . .
H27B H 0.515330 0.804743 0.319555 0.041 Uiso 1 1 calc R U . . .
H27C H 0.486719 0.681328 0.291839 0.041 Uiso 1 1 calc R U . . .
C28 C 0.5494(4) 0.8868(4) 0.0624(3) 0.0232(9) Uani 1 1 d . . . . .
C29 C 0.6661(5) 0.9469(6) 0.0669(6) 0.073(3) Uani 1 1 d . . . . .
H29A H 0.681474 1.005653 0.051534 0.109 Uiso 1 1 calc R U . . .
H29B H 0.685252 0.896704 0.035273 0.109 Uiso 1 1 calc R U . . .
H29C H 0.704838 0.976084 0.116602 0.109 Uiso 1 1 calc R U . . .
C30 C 0.4927(6) 0.8368(5) -0.0149(3) 0.0501(17) Uani 1 1 d . . . . .
H30A H 0.509616 0.892685 -0.033288 0.075 Uiso 1 1 calc R U . . .
H30B H 0.419020 0.800268 -0.018672 0.075 Uiso 1 1 calc R U . . .
H30C H 0.512224 0.784702 -0.043204 0.075 Uiso 1 1 calc R U . . .
C31 C 0.5267(8) 0.9716(6) 0.1079(4) 0.069(2) Uani 1 1 d . . . . .
H31A H 0.550814 1.030532 0.091979 0.103 Uiso 1 1 calc R U . . .
H31B H 0.561595 0.999055 0.158454 0.103 Uiso 1 1 calc R U . . .
H31C H 0.452864 0.940785 0.103151 0.103 Uiso 1 1 calc R U . . .
C32 C 0.2140(3) 0.0301(3) 0.2622(2) 0.0195(8) Uani 1 1 d . . . . .
C33 C 0.3122(4) 0.0434(4) 0.2777(3) 0.0264(10) Uani 1 1 d . . . . .
H33 H 0.333489 0.031081 0.317078 0.032 Uiso 1 1 calc R U . . .
C34 C 0.3781(4) 0.0744(4) 0.2352(3) 0.0363(12) Uani 1 1 d . . . . .
H34 H 0.444362 0.082422 0.245156 0.044 Uiso 1 1 calc R U . . .
C35 C 0.3485(4) 0.0938(4) 0.1788(3) 0.0355(12) Uani 1 1 d . . . . .
H35 H 0.394873 0.116861 0.150699 0.043 Uiso 1 1 calc R U . . .
C36 C 0.2511(4) 0.0799(4) 0.1627(3) 0.0328(11) Uani 1 1 d . . . . .
H36 H 0.230553 0.092646 0.123247 0.039 Uiso 1 1 calc R U . . .
C37 C 0.1834(4) 0.0474(4) 0.2042(3) 0.0243(9) Uani 1 1 d . . . . .
H37 H 0.116382 0.036967 0.192813 0.029 Uiso 1 1 calc R U . . .
C38 C 0.1962(3) 0.0318(4) 0.4038(2) 0.0204(9) Uani 1 1 d . . . . .
C39 C 0.2704(4) 0.1396(4) 0.4400(3) 0.0274(10) Uani 1 1 d . . . . .
H39 H 0.289706 0.185339 0.415021 0.033 Uiso 1 1 calc R U . . .
C40 C 0.3160(4) 0.1797(5) 0.5125(3) 0.0346(12) Uani 1 1 d . . . . .
H40 H 0.366026 0.253207 0.537202 0.042 Uiso 1 1 calc R U . . .
C41 C 0.2892(4) 0.1141(5) 0.5487(3) 0.0394(13) Uani 1 1 d . . . . .
H41 H 0.320644 0.142672 0.598469 0.047 Uiso 1 1 calc R U . . .
C42 C 0.2175(4) 0.0075(5) 0.5140(3) 0.0363(12) Uani 1 1 d . . . . .
H42 H 0.199787 -0.037558 0.539451 0.044 Uiso 1 1 calc R U . . .
C43 C 0.1703(4) -0.0345(4) 0.4406(3) 0.0269(10) Uani 1 1 d . . . . .
H43 H 0.120823 -0.108229 0.416161 0.032 Uiso 1 1 calc R U . . .
C44 C 0.0620(3) -0.1602(3) 0.2745(2) 0.0156(8) Uani 1 1 d . . . . .
C45 C -0.0428(3) -0.2208(3) 0.2641(2) 0.0193(9) Uani 1 1 d . . . . .
H45 H -0.082377 -0.186361 0.278321 0.023 Uiso 1 1 calc R U . . .
C46 C -0.0893(3) -0.3318(4) 0.2329(3) 0.0236(9) Uani 1 1 d . . . . .
H46 H -0.160996 -0.373484 0.225462 0.028 Uiso 1 1 calc R U . . .
C47 C -0.0318(4) -0.3823(3) 0.2124(3) 0.0216(9) Uani 1 1 d . . . . .
H47 H -0.063965 -0.458400 0.190451 0.026 Uiso 1 1 calc R U . . .
C48 C 0.0726(4) -0.3216(4) 0.2239(3) 0.0255(10) Uani 1 1 d . . . . .
H48 H 0.112405 -0.356037 0.210741 0.031 Uiso 1 1 calc R U . . .
C49 C 0.1196(3) -0.2105(4) 0.2546(3) 0.0238(10) Uani 1 1 d . . . . .
H49 H 0.191303 -0.168965 0.262023 0.029 Uiso 1 1 calc R U . . .
C50 C 0.0753(4) 0.2066(3) 0.2947(2) 0.0208(9) Uani 1 1 d . . . . .
C51 C 0.1811(4) 0.2642(4) 0.3039(3) 0.0333(12) Uani 1 1 d . . . . .
H51 H 0.226455 0.263519 0.338031 0.040 Uiso 1 1 calc R U . . .
C52 C 0.2196(6) 0.3238(5) 0.2616(4) 0.0499(16) Uani 1 1 d . . . . .
H52 H 0.291261 0.363803 0.267737 0.060 Uiso 1 1 calc R U . . .
C53 C 0.1548(7) 0.3239(5) 0.2128(4) 0.0588(18) Uani 1 1 d . . . . .
H53 H 0.180946 0.363155 0.184211 0.071 Uiso 1 1 calc R U . . .
C54 C 0.0524(7) 0.2679(6) 0.2044(4) 0.0572(18) Uani 1 1 d . . . . .
H54 H 0.007923 0.268594 0.169638 0.069 Uiso 1 1 calc R U . . .
C55 C 0.0106(5) 0.2095(5) 0.2451(3) 0.0339(12) Uani 1 1 d . . . . .
H55 H -0.061229 0.172139 0.238936 0.041 Uiso 1 1 calc R U . . .
C56 C -0.1094(3) 0.0770(3) 0.3284(2) 0.0165(8) Uani 1 1 d . . . . .
C57 C -0.1822(3) -0.0277(4) 0.2836(3) 0.0217(9) Uani 1 1 d . . . . .
H57 H -0.161232 -0.078233 0.259718 0.026 Uiso 1 1 calc R U . . .
C58 C -0.2852(4) -0.0586(4) 0.2738(3) 0.0283(10) Uani 1 1 d . . . . .
H58 H -0.334994 -0.129975 0.242851 0.034 Uiso 1 1 calc R U . . .
C59 C -0.3150(4) 0.0160(4) 0.3097(3) 0.0299(11) Uani 1 1 d . . . . .
H59 H -0.385563 -0.004577 0.302453 0.036 Uiso 1 1 calc R U . . .
C60 C -0.2434(4) 0.1191(4) 0.3555(3) 0.0258(10) Uani 1 1 d . . . . .
H60 H -0.264719 0.168752 0.380698 0.031 Uiso 1 1 calc R U . . .
C61 C -0.1405(4) 0.1507(4) 0.3648(3) 0.0212(9) Uani 1 1 d . . . . .
H61 H -0.090994 0.222123 0.395928 0.025 Uiso 1 1 calc R U . . .
C62 C 0.0792(4) 0.1965(4) 0.4358(2) 0.0214(9) Uani 1 1 d . . . . .
C63 C 0.1491(4) 0.3066(4) 0.4666(3) 0.0341(12) Uani 1 1 d . . . . .
H63 H 0.167777 0.345612 0.437098 0.041 Uiso 1 1 calc R U . . .
C64 C 0.1909(5) 0.3583(5) 0.5402(3) 0.0438(14) Uani 1 1 d . . . . .
H64 H 0.237983 0.433025 0.561270 0.053 Uiso 1 1 calc R U . . .
C65 C 0.1645(5) 0.3018(5) 0.5830(3) 0.0411(13) Uani 1 1 d . . . . .
H65 H 0.193572 0.338104 0.633521 0.049 Uiso 1 1 calc R U . . .
C66 C 0.0967(4) 0.1937(4) 0.5536(3) 0.0290(10) Uani 1 1 d . . . . .
H66 H 0.078757 0.155539 0.583605 0.035 Uiso 1 1 calc R U . . .
C67 C 0.0544(4) 0.1403(4) 0.4798(2) 0.0224(9) Uani 1 1 d . . . . .
H67 H 0.008300 0.065299 0.459266 0.027 Uiso 1 1 calc R U . . .
O3 O 0.1157(7) 0.6364(5) 0.4983(4) 0.097(2) Uani 1 1 d . . . . .
C68 C 0.1233(8) 0.5428(7) 0.4753(5) 0.071(2) Uani 1 1 d . . . . .
H68A H 0.082173 0.494455 0.497427 0.085 Uiso 1 1 calc R U . . .
H68B H 0.195248 0.559770 0.488059 0.085 Uiso 1 1 calc R U . . .
C69 C 0.0827(8) 0.4921(7) 0.3954(4) 0.073(2) Uani 1 1 d . . . . .
H69A H 0.116429 0.451126 0.371714 0.087 Uiso 1 1 calc R U . . .
H69B H 0.008128 0.442965 0.382143 0.087 Uiso 1 1 calc R U . . .
C70 C 0.1061(7) 0.5820(8) 0.3741(5) 0.076(2) Uani 1 1 d . . . . .
H70A H 0.056070 0.559709 0.329919 0.091 Uiso 1 1 calc R U . . .
H70B H 0.175753 0.612021 0.366278 0.091 Uiso 1 1 calc R U . . .
C71 C 0.0974(8) 0.6610(7) 0.4383(6) 0.080(3) Uani 1 1 d . . . . .
H71A H 0.148625 0.735305 0.447219 0.096 Uiso 1 1 calc R U . . .
H71B H 0.028484 0.653668 0.430216 0.096 Uiso 1 1 calc R U . . .
O4 O 0.8884(3) 0.7611(4) 0.0243(2) 0.0464(10) Uani 1 1 d . . . . .
C72 C 0.9116(5) 0.8119(6) 0.1002(4) 0.0501(15) Uani 1 1 d . . . . .
H72A H 0.983982 0.837709 0.121406 0.060 Uiso 1 1 calc R U . . .
H72B H 0.867709 0.761725 0.120225 0.060 Uiso 1 1 calc R U . . .
C73 C 0.8912(5) 0.9045(6) 0.1160(4) 0.0523(16) Uani 1 1 d . . . . .
H73A H 0.818333 0.881911 0.115007 0.063 Uiso 1 1 calc R U . . .
H73B H 0.934000 0.963464 0.163298 0.063 Uiso 1 1 calc R U . . .
C74 C 0.9205(6) 0.9370(6) 0.0553(4) 0.0545(17) Uani 1 1 d . . . . .
H74A H 0.995235 0.983762 0.065851 0.065 Uiso 1 1 calc R U . . .
H74B H 0.885389 0.974914 0.045629 0.065 Uiso 1 1 calc R U . . .
C75 C 0.8850(5) 0.8301(6) -0.0079(4) 0.0484(15) Uani 1 1 d . . . . .
H75A H 0.814677 0.801651 -0.035294 0.058 Uiso 1 1 calc R U . . .
H75B H 0.931019 0.837950 -0.040930 0.058 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1 1.989(3) . ?
Hf1 O2 1.991(3) . ?
Hf1 C1 2.337(4) . ?
Hf1 Cl3 2.4620(12) . ?
Hf1 Cl1 2.4841(19) . ?
Hf1 Cl2 2.4931(13) . ?
P1 N3 1.586(4) . ?
P1 C32 1.799(4) . ?
P1 C44 1.801(4) . ?
P1 C38 1.805(5) . ?
P2 N3 1.587(4) . ?
P2 C62 1.790(5) . ?
P2 C56 1.795(4) . ?
P2 C50 1.800(4) . ?
O1 C5 1.333(5) . ?
O2 C19 1.333(5) . ?
N1 C1 1.354(5) . ?
N1 C4 1.426(5) . ?
N1 C3 1.480(5) . ?
N2 C1 1.348(5) . ?
N2 C18 1.426(5) . ?
N2 C2 1.481(5) . ?
C2 C3 1.511(6) . ?
C2 H2A 0.9900 . ?
C2 H2AB 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3AB 0.9900 . ?
C4 C9 1.395(6) . ?
C4 C5 1.403(6) . ?
C5 C6 1.416(6) . ?
C6 C7 1.388(6) . ?
C6 C10 1.531(6) . ?
C7 C8 1.403(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(6) . ?
C8 C14 1.530(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.524(6) . ?
C10 C13 1.534(6) . ?
C10 C12 1.553(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C17 1.510(8) . ?
C14 C15 1.522(7) . ?
C14 C16 1.546(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.402(6) . ?
C18 C19 1.409(6) . ?
C19 C20 1.408(6) . ?
C20 C21 1.405(6) . ?
C20 C24 1.529(6) . ?
C21 C22 1.382(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(6) . ?
C22 C28 1.549(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.533(6) . ?
C24 C26 1.545(6) . ?
C24 C27 1.550(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.497(8) . ?
C28 C31 1.499(8) . ?
C28 C29 1.562(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C37 1.387(7) . ?
C32 C33 1.400(6) . ?
C33 C34 1.384(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.373(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.390(7) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C43 1.385(7) . ?
C38 C39 1.397(7) . ?
C39 C40 1.387(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.369(9) . ?
C40 H40 0.9500 . ?
C41 C42 1.373(9) . ?
C41 H41 0.9500 . ?
C42 C43 1.406(7) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C49 1.380(6) . ?
C44 C45 1.389(6) . ?
C45 C46 1.386(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.385(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.381(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.386(6) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C55 1.385(7) . ?
C50 C51 1.400(7) . ?
C51 C52 1.420(8) . ?
C51 H51 0.9500 . ?
C52 C53 1.350(11) . ?
C52 H52 0.9500 . ?
C53 C54 1.358(11) . ?
C53 H53 0.9500 . ?
C54 C55 1.389(8) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.388(6) . ?
C56 C61 1.399(6) . ?
C57 C58 1.385(6) . ?
C57 H57 0.9500 . ?
C58 C59 1.394(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.376(8) . ?
C59 H59 0.9500 . ?
C60 C61 1.383(6) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 C67 1.393(7) . ?
C62 C63 1.401(7) . ?
C63 C64 1.384(8) . ?
C63 H63 0.9500 . ?
C64 C65 1.377(9) . ?
C64 H64 0.9500 . ?
C65 C66 1.373(8) . ?
C65 H65 0.9500 . ?
C66 C67 1.389(7) . ?
C66 H66 0.9500 . ?
C67 H67 0.9500 . ?
O3 C68 1.396(10) . ?
O3 C71 1.437(11) . ?
C68 C69 1.493(11) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.472(12) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.502(13) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
O4 C72 1.414(8) . ?
O4 C75 1.427(8) . ?
C72 C73 1.502(10) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.499(10) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.523(10) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 O2 153.96(12) . . ?
O1 Hf1 C1 76.74(13) . . ?
O2 Hf1 C1 77.31(13) . . ?
O1 Hf1 Cl3 92.95(9) . . ?
O2 Hf1 Cl3 87.61(9) . . ?
C1 Hf1 Cl3 96.15(10) . . ?
O1 Hf1 Cl1 100.81(10) . . ?
O2 Hf1 Cl1 105.14(10) . . ?
C1 Hf1 Cl1 169.88(11) . . ?
Cl3 Hf1 Cl1 93.77(6) . . ?
O1 Hf1 Cl2 94.05(9) . . ?
O2 Hf1 Cl2 85.13(9) . . ?
C1 Hf1 Cl2 83.32(10) . . ?
Cl3 Hf1 Cl2 172.66(4) . . ?
Cl1 Hf1 Cl2 87.09(7) . . ?
N3 P1 C32 113.2(2) . . ?
N3 P1 C44 107.04(19) . . ?
C32 P1 C44 107.1(2) . . ?
N3 P1 C38 113.9(2) . . ?
C32 P1 C38 107.3(2) . . ?
C44 P1 C38 108.1(2) . . ?
N3 P2 C62 113.8(2) . . ?
N3 P2 C56 108.0(2) . . ?
C62 P2 C56 105.8(2) . . ?
N3 P2 C50 112.4(2) . . ?
C62 P2 C50 109.1(2) . . ?
C56 P2 C50 107.3(2) . . ?
C5 O1 Hf1 145.6(3) . . ?
C19 O2 Hf1 138.6(3) . . ?
C1 N1 C4 127.9(3) . . ?
C1 N1 C3 112.4(3) . . ?
C4 N1 C3 119.7(3) . . ?
C1 N2 C18 126.8(3) . . ?
C1 N2 C2 112.7(3) . . ?
C18 N2 C2 119.7(3) . . ?
P1 N3 P2 138.7(2) . . ?
N2 C1 N1 108.2(3) . . ?
N2 C1 Hf1 125.3(3) . . ?
N1 C1 Hf1 126.4(3) . . ?
N2 C2 C3 103.0(3) . . ?
N2 C2 H2A 111.2 . . ?
C3 C2 H2A 111.2 . . ?
N2 C2 H2AB 111.2 . . ?
C3 C2 H2AB 111.2 . . ?
H2A C2 H2AB 109.1 . . ?
N1 C3 C2 103.2(3) . . ?
N1 C3 H3A 111.1 . . ?
C2 C3 H3A 111.1 . . ?
N1 C3 H3AB 111.1 . . ?
C2 C3 H3AB 111.1 . . ?
H3A C3 H3AB 109.1 . . ?
C9 C4 C5 120.3(4) . . ?
C9 C4 N1 118.2(4) . . ?
C5 C4 N1 121.5(4) . . ?
O1 C5 C4 120.3(4) . . ?
O1 C5 C6 120.1(4) . . ?
C4 C5 C6 119.6(4) . . ?
C7 C6 C5 117.8(4) . . ?
C7 C6 C10 121.3(4) . . ?
C5 C6 C10 120.9(4) . . ?
C6 C7 C8 123.5(4) . . ?
C6 C7 H7 118.3 . . ?
C8 C7 H7 118.3 . . ?
C9 C8 C7 117.3(4) . . ?
C9 C8 C14 122.9(4) . . ?
C7 C8 C14 119.7(4) . . ?
C8 C9 C4 121.4(4) . . ?
C8 C9 H9 119.3 . . ?
C4 C9 H9 119.3 . . ?
C11 C10 C6 111.0(4) . . ?
C11 C10 C13 107.0(4) . . ?
C6 C10 C13 111.5(4) . . ?
C11 C10 C12 109.6(4) . . ?
C6 C10 C12 109.9(4) . . ?
C13 C10 C12 107.8(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C14 C15 108.5(5) . . ?
C17 C14 C8 112.1(4) . . ?
C15 C14 C8 111.8(4) . . ?
C17 C14 C16 110.1(6) . . ?
C15 C14 C16 107.1(5) . . ?
C8 C14 C16 107.1(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.5(4) . . ?
C23 C18 N2 117.9(4) . . ?
C19 C18 N2 121.6(3) . . ?
O2 C19 C20 120.3(4) . . ?
O2 C19 C18 120.2(4) . . ?
C20 C19 C18 119.5(4) . . ?
C21 C20 C19 118.2(4) . . ?
C21 C20 C24 121.3(4) . . ?
C19 C20 C24 120.5(4) . . ?
C22 C21 C20 122.6(4) . . ?
C22 C21 H21 118.7 . . ?
C20 C21 H21 118.7 . . ?
C21 C22 C23 119.1(4) . . ?
C21 C22 C28 120.9(4) . . ?
C23 C22 C28 120.0(4) . . ?
C22 C23 C18 120.1(4) . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
C20 C24 C25 112.6(4) . . ?
C20 C24 C26 110.2(4) . . ?
C25 C24 C26 107.1(4) . . ?
C20 C24 C27 110.4(4) . . ?
C25 C24 C27 105.9(4) . . ?
C26 C24 C27 110.5(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C30 C28 C31 112.0(5) . . ?
C30 C28 C22 110.4(4) . . ?
C31 C28 C22 112.4(4) . . ?
C30 C28 C29 108.2(6) . . ?
C31 C28 C29 105.2(6) . . ?
C22 C28 C29 108.3(4) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C37 C32 C33 119.7(4) . . ?
C37 C32 P1 119.1(3) . . ?
C33 C32 P1 121.1(4) . . ?
C34 C33 C32 119.6(5) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C35 C34 C33 120.6(5) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 120.2(5) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C37 120.0(5) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C32 C37 C36 119.9(5) . . ?
C32 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C43 C38 C39 119.5(4) . . ?
C43 C38 P1 120.4(4) . . ?
C39 C38 P1 119.7(4) . . ?
C40 C39 C38 119.8(5) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C41 C40 C39 120.5(5) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C42 120.7(5) . . ?
C40 C41 H41 119.6 . . ?
C42 C41 H41 119.6 . . ?
C41 C42 C43 119.6(5) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
C38 C43 C42 119.9(5) . . ?
C38 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C49 C44 C45 120.1(4) . . ?
C49 C44 P1 119.4(3) . . ?
C45 C44 P1 120.5(3) . . ?
C46 C45 C44 119.6(4) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C47 C46 C45 120.4(4) . . ?
C47 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C48 C47 C46 119.7(4) . . ?
C48 C47 H47 120.1 . . ?
C46 C47 H47 120.1 . . ?
C47 C48 C49 120.3(4) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 H48 119.9 . . ?
C44 C49 C48 120.0(4) . . ?
C44 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C55 C50 C51 119.5(5) . . ?
C55 C50 P2 120.6(4) . . ?
C51 C50 P2 119.7(4) . . ?
C50 C51 C52 119.1(6) . . ?
C50 C51 H51 120.5 . . ?
C52 C51 H51 120.4 . . ?
C53 C52 C51 120.2(6) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C52 C53 C54 120.2(6) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C53 C54 C55 122.0(7) . . ?
C53 C54 H54 119.0 . . ?
C55 C54 H54 119.0 . . ?
C50 C55 C54 119.0(6) . . ?
C50 C55 H55 120.5 . . ?
C54 C55 H55 120.5 . . ?
C57 C56 C61 119.8(4) . . ?
C57 C56 P2 121.2(3) . . ?
C61 C56 P2 119.0(3) . . ?
C58 C57 C56 120.2(4) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C57 C58 C59 119.4(5) . . ?
C57 C58 H58 120.3 . . ?
C59 C58 H58 120.3 . . ?
C60 C59 C58 120.7(4) . . ?
C60 C59 H59 119.7 . . ?
C58 C59 H59 119.7 . . ?
C59 C60 C61 120.1(4) . . ?
C59 C60 H60 120.0 . . ?
C61 C60 H60 120.0 . . ?
C60 C61 C56 119.8(4) . . ?
C60 C61 H61 120.1 . . ?
C56 C61 H61 120.1 . . ?
C67 C62 C63 119.2(4) . . ?
C67 C62 P2 117.0(3) . . ?
C63 C62 P2 123.7(4) . . ?
C64 C63 C62 119.7(5) . . ?
C64 C63 H63 120.2 . . ?
C62 C63 H63 120.2 . . ?
C65 C64 C63 120.3(5) . . ?
C65 C64 H64 119.8 . . ?
C63 C64 H64 119.8 . . ?
C66 C65 C64 120.7(5) . . ?
C66 C65 H65 119.7 . . ?
C64 C65 H65 119.7 . . ?
C65 C66 C67 119.8(5) . . ?
C65 C66 H66 120.1 . . ?
C67 C66 H66 120.1 . . ?
C66 C67 C62 120.2(5) . . ?
C66 C67 H67 119.9 . . ?
C62 C67 H67 119.9 . . ?
C68 O3 C71 110.6(7) . . ?
O3 C68 C69 104.9(7) . . ?
O3 C68 H68A 110.8 . . ?
C69 C68 H68A 110.8 . . ?
O3 C68 H68B 110.8 . . ?
C69 C68 H68B 110.8 . . ?
H68A C68 H68B 108.8 . . ?
C70 C69 C68 105.3(7) . . ?
C70 C69 H69A 110.7 . . ?
C68 C69 H69A 110.7 . . ?
C70 C69 H69B 110.7 . . ?
C68 C69 H69B 110.7 . . ?
H69A C69 H69B 108.8 . . ?
C69 C70 C71 102.0(7) . . ?
C69 C70 H70A 111.4 . . ?
C71 C70 H70A 111.4 . . ?
C69 C70 H70B 111.4 . . ?
C71 C70 H70B 111.4 . . ?
H70A C70 H70B 109.2 . . ?
O3 C71 C70 106.2(7) . . ?
O3 C71 H71A 110.5 . . ?
C70 C71 H71A 110.5 . . ?
O3 C71 H71B 110.5 . . ?
C70 C71 H71B 110.5 . . ?
H71A C71 H71B 108.7 . . ?
C72 O4 C75 111.0(5) . . ?
O4 C72 C73 105.5(5) . . ?
O4 C72 H72A 110.6 . . ?
C73 C72 H72A 110.6 . . ?
O4 C72 H72B 110.6 . . ?
C73 C72 H72B 110.6 . . ?
H72A C72 H72B 108.8 . . ?
C74 C73 C72 101.7(6) . . ?
C74 C73 H73A 111.4 . . ?
C72 C73 H73A 111.4 . . ?
C74 C73 H73B 111.4 . . ?
C72 C73 H73B 111.4 . . ?
H73A C73 H73B 109.3 . . ?
C73 C74 C75 103.1(6) . . ?
C73 C74 H74A 111.1 . . ?
C75 C74 H74A 111.1 . . ?
C73 C74 H74B 111.1 . . ?
C75 C74 H74B 111.1 . . ?
H74A C74 H74B 109.1 . . ?
O4 C75 C74 104.5(5) . . ?
O4 C75 H75A 110.8 . . ?
C74 C75 H75A 110.8 . . ?
O4 C75 H75B 110.8 . . ?
C74 C75 H75B 110.8 . . ?
H75A C75 H75B 108.9 . . ?

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
C32 P1 N3 P2 -73.7(4) . . . . ?
C44 P1 N3 P2 168.6(4) . . . . ?
C38 P1 N3 P2 49.2(4) . . . . ?
C62 P2 N3 P1 -47.6(4) . . . . ?
C56 P2 N3 P1 -164.8(3) . . . . ?
C50 P2 N3 P1 77.0(4) . . . . ?
C18 N2 C1 N1 -170.9(4) . . . . ?
C2 N2 C1 N1 -1.6(5) . . . . ?
C18 N2 C1 Hf1 5.6(6) . . . . ?
C2 N2 C1 Hf1 175.0(3) . . . . ?
C4 N1 C1 N2 177.1(4) . . . . ?
C3 N1 C1 N2 -3.4(5) . . . . ?
C4 N1 C1 Hf1 0.6(6) . . . . ?
C3 N1 C1 Hf1 -179.9(3) . . . . ?
C1 N2 C2 C3 5.6(4) . . . . ?
C18 N2 C2 C3 175.7(3) . . . . ?
C1 N1 C3 C2 6.6(4) . . . . ?
C4 N1 C3 C2 -173.8(3) . . . . ?
N2 C2 C3 N1 -6.8(4) . . . . ?
C1 N1 C4 C9 174.3(4) . . . . ?
C3 N1 C4 C9 -5.2(5) . . . . ?
C1 N1 C4 C5 -7.2(6) . . . . ?
C3 N1 C4 C5 173.3(4) . . . . ?
Hf1 O1 C5 C4 14.3(7) . . . . ?
Hf1 O1 C5 C6 -166.5(3) . . . . ?
C9 C4 C5 O1 -179.3(4) . . . . ?
N1 C4 C5 O1 2.2(6) . . . . ?
C9 C4 C5 C6 1.5(6) . . . . ?
N1 C4 C5 C6 -176.9(4) . . . . ?
O1 C5 C6 C7 179.7(4) . . . . ?
C4 C5 C6 C7 -1.1(6) . . . . ?
O1 C5 C6 C10 -0.9(6) . . . . ?
C4 C5 C6 C10 178.3(4) . . . . ?
C5 C6 C7 C8 0.5(6) . . . . ?
C10 C6 C7 C8 -179.0(4) . . . . ?
C6 C7 C8 C9 -0.1(7) . . . . ?
C6 C7 C8 C14 176.5(4) . . . . ?
C7 C8 C9 C4 0.5(6) . . . . ?
C14 C8 C9 C4 -176.1(4) . . . . ?
C5 C4 C9 C8 -1.2(6) . . . . ?
N1 C4 C9 C8 177.3(4) . . . . ?
C7 C6 C10 C11 121.4(5) . . . . ?
C5 C6 C10 C11 -58.1(5) . . . . ?
C7 C6 C10 C13 2.1(6) . . . . ?
C5 C6 C10 C13 -177.3(4) . . . . ?
C7 C6 C10 C12 -117.3(5) . . . . ?
C5 C6 C10 C12 63.3(5) . . . . ?
C9 C8 C14 C17 -19.6(7) . . . . ?
C7 C8 C14 C17 164.0(5) . . . . ?
C9 C8 C14 C15 -141.7(5) . . . . ?
C7 C8 C14 C15 41.8(6) . . . . ?
C9 C8 C14 C16 101.3(6) . . . . ?
C7 C8 C14 C16 -75.2(6) . . . . ?
C1 N2 C18 C23 165.1(4) . . . . ?
C2 N2 C18 C23 -3.5(5) . . . . ?
C1 N2 C18 C19 -16.3(6) . . . . ?
C2 N2 C18 C19 175.0(4) . . . . ?
Hf1 O2 C19 C20 -141.9(3) . . . . ?
Hf1 O2 C19 C18 38.8(6) . . . . ?
C23 C18 C19 O2 177.0(4) . . . . ?
N2 C18 C19 O2 -1.5(6) . . . . ?
C23 C18 C19 C20 -2.3(6) . . . . ?
N2 C18 C19 C20 179.2(4) . . . . ?
O2 C19 C20 C21 -179.0(4) . . . . ?
C18 C19 C20 C21 0.3(6) . . . . ?
O2 C19 C20 C24 1.3(6) . . . . ?
C18 C19 C20 C24 -179.4(4) . . . . ?
C19 C20 C21 C22 0.4(6) . . . . ?
C24 C20 C21 C22 180.0(4) . . . . ?
C20 C21 C22 C23 1.0(6) . . . . ?
C20 C21 C22 C28 -177.6(4) . . . . ?
C21 C22 C23 C18 -3.0(6) . . . . ?
C28 C22 C23 C18 175.6(4) . . . . ?
C19 C18 C23 C22 3.7(6) . . . . ?
N2 C18 C23 C22 -177.8(4) . . . . ?
C21 C20 C24 C25 0.2(6) . . . . ?
C19 C20 C24 C25 179.8(4) . . . . ?
C21 C20 C24 C26 119.8(4) . . . . ?
C19 C20 C24 C26 -60.6(5) . . . . ?
C21 C20 C24 C27 -118.0(4) . . . . ?
C19 C20 C24 C27 61.7(5) . . . . ?
C21 C22 C28 C30 -111.2(5) . . . . ?
C23 C22 C28 C30 70.2(6) . . . . ?
C21 C22 C28 C31 14.6(7) . . . . ?
C23 C22 C28 C31 -163.9(6) . . . . ?
C21 C22 C28 C29 130.5(6) . . . . ?
C23 C22 C28 C29 -48.1(7) . . . . ?
N3 P1 C32 C37 -25.6(4) . . . . ?
C44 P1 C32 C37 92.1(4) . . . . ?
C38 P1 C32 C37 -152.1(4) . . . . ?
N3 P1 C32 C33 157.7(4) . . . . ?
C44 P1 C32 C33 -84.6(4) . . . . ?
C38 P1 C32 C33 31.2(4) . . . . ?
C37 C32 C33 C34 0.6(7) . . . . ?
P1 C32 C33 C34 177.2(4) . . . . ?
C32 C33 C34 C35 0.9(8) . . . . ?
C33 C34 C35 C36 -1.6(9) . . . . ?
C34 C35 C36 C37 0.7(8) . . . . ?
C33 C32 C37 C36 -1.4(7) . . . . ?
P1 C32 C37 C36 -178.2(4) . . . . ?
C35 C36 C37 C32 0.8(8) . . . . ?
N3 P1 C38 C43 95.8(4) . . . . ?
C32 P1 C38 C43 -138.2(4) . . . . ?
C44 P1 C38 C43 -23.0(4) . . . . ?
N3 P1 C38 C39 -76.5(4) . . . . ?
C32 P1 C38 C39 49.5(4) . . . . ?
C44 P1 C38 C39 164.7(4) . . . . ?
C43 C38 C39 C40 -1.3(7) . . . . ?
P1 C38 C39 C40 171.0(4) . . . . ?
C38 C39 C40 C41 0.5(8) . . . . ?
C39 C40 C41 C42 0.4(9) . . . . ?
C40 C41 C42 C43 -0.5(9) . . . . ?
C39 C38 C43 C42 1.1(7) . . . . ?
P1 C38 C43 C42 -171.2(4) . . . . ?
C41 C42 C43 C38 -0.2(8) . . . . ?
N3 P1 C44 C49 164.3(4) . . . . ?
C32 P1 C44 C49 42.7(4) . . . . ?
C38 P1 C44 C49 -72.6(4) . . . . ?
N3 P1 C44 C45 -15.4(4) . . . . ?
C32 P1 C44 C45 -137.0(4) . . . . ?
C38 P1 C44 C45 107.7(4) . . . . ?
C49 C44 C45 C46 -0.8(7) . . . . ?
P1 C44 C45 C46 178.9(4) . . . . ?
C44 C45 C46 C47 0.3(7) . . . . ?
C45 C46 C47 C48 0.7(7) . . . . ?
C46 C47 C48 C49 -1.2(8) . . . . ?
C45 C44 C49 C48 0.3(7) . . . . ?
P1 C44 C49 C48 -179.4(4) . . . . ?
C47 C48 C49 C44 0.7(8) . . . . ?
N3 P2 C50 C55 103.7(4) . . . . ?
C62 P2 C50 C55 -129.2(4) . . . . ?
C56 P2 C50 C55 -14.9(5) . . . . ?
N3 P2 C50 C51 -70.5(4) . . . . ?
C62 P2 C50 C51 56.6(4) . . . . ?
C56 P2 C50 C51 170.9(4) . . . . ?
C55 C50 C51 C52 -0.5(7) . . . . ?
P2 C50 C51 C52 173.7(4) . . . . ?
C50 C51 C52 C53 -0.6(9) . . . . ?
C51 C52 C53 C54 0.7(10) . . . . ?
C52 C53 C54 C55 0.2(11) . . . . ?
C51 C50 C55 C54 1.4(8) . . . . ?
P2 C50 C55 C54 -172.8(5) . . . . ?
C53 C54 C55 C50 -1.3(10) . . . . ?
N3 P2 C56 C57 -13.2(4) . . . . ?
C62 P2 C56 C57 -135.4(4) . . . . ?
C50 P2 C56 C57 108.2(4) . . . . ?
N3 P2 C56 C61 166.3(3) . . . . ?
C62 P2 C56 C61 44.2(4) . . . . ?
C50 P2 C56 C61 -72.3(4) . . . . ?
C61 C56 C57 C58 1.5(7) . . . . ?
P2 C56 C57 C58 -179.0(4) . . . . ?
C56 C57 C58 C59 -0.6(7) . . . . ?
C57 C58 C59 C60 -1.0(8) . . . . ?
C58 C59 C60 C61 1.8(7) . . . . ?
C59 C60 C61 C56 -0.9(7) . . . . ?
C57 C56 C61 C60 -0.7(7) . . . . ?
P2 C56 C61 C60 179.7(3) . . . . ?
N3 P2 C62 C67 -48.9(4) . . . . ?
C56 P2 C62 C67 69.5(4) . . . . ?
C50 P2 C62 C67 -175.3(4) . . . . ?
N3 P2 C62 C63 127.1(4) . . . . ?
C56 P2 C62 C63 -114.5(4) . . . . ?
C50 P2 C62 C63 0.7(5) . . . . ?
C67 C62 C63 C64 -1.2(8) . . . . ?
P2 C62 C63 C64 -177.1(5) . . . . ?
C62 C63 C64 C65 0.4(10) . . . . ?
C63 C64 C65 C66 0.1(10) . . . . ?
C64 C65 C66 C67 0.2(9) . . . . ?
C65 C66 C67 C62 -1.1(8) . . . . ?
C63 C62 C67 C66 1.5(7) . . . . ?
P2 C62 C67 C66 177.7(4) . . . . ?
C71 O3 C68 C69 -14.1(11) . . . . ?
O3 C68 C69 C70 29.9(11) . . . . ?
C68 C69 C70 C71 -32.9(10) . . . . ?
C68 O3 C71 C70 -6.6(11) . . . . ?
C69 C70 C71 O3 24.5(10) . . . . ?
C75 O4 C72 C73 17.3(7) . . . . ?
O4 C72 C73 C74 -33.7(7) . . . . ?
C72 C73 C74 C75 36.7(7) . . . . ?
C72 O4 C75 C74 6.3(7) . . . . ?
C73 C74 C75 O4 -27.3(7) . . . . ?

_refine_diff_density_max         4.278
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.158



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

data_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1908219'
loop_
_audit_author_name
_audit_author_address
'Karl Wilhelm Toernroos'
;University of Bergen
Norway
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2019-05-29 downloaded from the CCDC.
;
#data_Puia177_a

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H52 Cl2 Hf N2 O3, C4 H10 O'
_chemical_formula_sum            'C39 H62 Cl2 Hf N2 O4'
_chemical_formula_weight         872.29

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.5953(6)
_cell_length_b                   14.0285(5)
_cell_length_c                   17.4961(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.2400(10)
_cell_angle_gamma                90
_cell_volume                     4049.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      30.02

_exptl_crystal_description       'thin prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   0.74142
_exptl_transmission_factor_max   0.89552
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    2.748
_shelx_estimated_absorpt_T_min   0.607
_shelx_estimated_absorpt_T_max   0.866
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6319
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker AXS TXS Ultra Rotating Anode'
_diffrn_measurement_device_type  'Bruker AXS APEXII Pt135 CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67447
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.906
_diffrn_reflns_theta_max         30.049
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11853
_reflns_number_gt                10059
_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       'Bruker AXS Inc. APEX2 v2008.1-0'
_computing_cell_refinement       'Bruker AXS Inc. SAINT V6.45A'
_computing_data_reduction        'Bruker AXS Inc. SAINT V6.45A'
_computing_structure_solution    'SHELXT v.2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+2.7030P] 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         11853
_refine_ls_number_parameters     447
_refine_ls_number_restraints     426
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 -1.00 -1.00 0.0820
-2.00 1.00 1.00 0.0320
-1.00 1.00 -1.00 0.0440
2.00 0.00 -1.00 0.0900
0.00 1.00 -2.00 0.0420
0.00 -1.00 2.00 0.0500
2.00 -1.00 2.00 0.0910
1.00 0.00 0.00 0.1020
0.00 2.00 1.00 0.0270
0.00 -2.00 -1.00 0.0180
1.00 2.00 1.00 0.0470
-1.00 -2.00 -1.00 0.0260
0.00 1.00 1.00 0.0320

# start Validation Reply Form
_vrf_PLAT971_Compound2           
;
PROBLEM: Check Calcd Resid. Dens.  0.78A   From Hf1             3.66 eA-3  
RESPONSE: The platelike crystal specimen suffers from lammelar twinning 
visible down the b* axis. The (rotational) twinning can only be partially 
deconvoluted, resulting in a degree of disorder expressed as residual density
around the heavy Hf site. 
;
_vrf_PLAT094_Compound2           
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.07 Report
RESPONSE: The platelike crystal specimen suffers from lammelar twinning 
visible down the b* axis. The (rotational) twinning can only be partially 
deconvoluted, resulting in a degree of disorder expressed as residual density
around the heavy Hf site.  
;
# end Validation Reply Form

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 0.59163(2) 0.68653(2) 0.34806(2) 0.01602(4) Uani 1 1 d . . . . .
Cl1 Cl 0.60538(5) 0.83210(5) 0.27356(5) 0.02817(16) Uani 1 1 d . . . . .
Cl2 Cl 0.62912(4) 0.75558(5) 0.47265(4) 0.02553(14) Uani 1 1 d . . . . .
O1 O 0.47632(12) 0.68846(13) 0.36429(12) 0.0193(4) Uani 1 1 d . . . . .
O2 O 0.69744(11) 0.62691(14) 0.34154(12) 0.0194(4) Uani 1 1 d . . . . .
N1 N 0.49667(13) 0.49211(16) 0.39852(13) 0.0155(4) Uani 1 1 d . . . . .
N2 N 0.62482(13) 0.45913(15) 0.39075(13) 0.0144(4) Uani 1 1 d . . . . .
C1 C 0.56873(15) 0.52931(19) 0.38354(15) 0.0156(4) Uani 1 1 d . . . . .
C2 C 0.59179(16) 0.36779(18) 0.41560(16) 0.0163(5) Uani 1 1 d . . . . .
H2A H 0.617136 0.349435 0.467345 0.020 Uiso 1 1 calc R U . . .
H2B H 0.600353 0.316069 0.378840 0.020 Uiso 1 1 calc R U . . .
C3 C 0.50207(16) 0.38899(19) 0.41653(16) 0.0167(5) Uani 1 1 d . . . . .
H3A H 0.468757 0.351046 0.377194 0.020 Uiso 1 1 calc R U . . .
H3B H 0.484295 0.375567 0.467663 0.020 Uiso 1 1 calc R U . . .
C4 C 0.41983(15) 0.53799(19) 0.39189(15) 0.0159(4) Uani 1 1 d . . . . .
C5 C 0.41130(16) 0.6360(2) 0.37639(15) 0.0173(5) Uani 1 1 d . . . . .
C6 C 0.33422(18) 0.6796(2) 0.37309(16) 0.0189(5) Uani 1 1 d . . . . .
C7 C 0.26748(17) 0.6207(2) 0.37795(16) 0.0214(5) Uani 1 1 d . . . . .
H7 H 0.215131 0.648811 0.374263 0.026 Uiso 1 1 calc R U . . .
C8 C 0.27388(16) 0.5220(2) 0.38799(16) 0.0192(5) Uani 1 1 d . . . . .
C9 C 0.35090(16) 0.4820(2) 0.39771(16) 0.0185(5) Uani 1 1 d . . . . .
H9 H 0.356868 0.415793 0.408420 0.022 Uiso 1 1 calc R U . . .
C10 C 0.32563(19) 0.7883(2) 0.36473(18) 0.0239(5) Uani 1 1 d . . . . .
C11 C 0.3736(2) 0.8374(2) 0.43463(19) 0.0289(6) Uani 1 1 d . . . . .
H11A H 0.368159 0.906763 0.429311 0.043 Uiso 1 1 calc R U . . .
H11B H 0.430915 0.819785 0.436928 0.043 Uiso 1 1 calc R U . . .
H11C H 0.352004 0.816949 0.481945 0.043 Uiso 1 1 calc R U . . .
C12 C 0.3562(2) 0.8229(2) 0.2896(2) 0.0296(7) Uani 1 1 d . . . . .
H12A H 0.344433 0.890986 0.282647 0.044 Uiso 1 1 calc R U . . .
H12B H 0.328841 0.787152 0.246127 0.044 Uiso 1 1 calc R U . . .
H12C H 0.414846 0.812564 0.292076 0.044 Uiso 1 1 calc R U . . .
C13 C 0.2367(2) 0.8205(2) 0.3632(3) 0.0366(8) Uani 1 1 d . . . . .
H13A H 0.233709 0.890073 0.358680 0.055 Uiso 1 1 calc R U . . .
H13B H 0.215473 0.800545 0.410815 0.055 Uiso 1 1 calc R U . . .
H13C H 0.204328 0.791371 0.319102 0.055 Uiso 1 1 calc R U . . .
C14 C 0.19680(16) 0.4611(2) 0.38245(16) 0.0212(5) Uani 1 1 d . . . . .
C15 C 0.1565(2) 0.4664(3) 0.29928(18) 0.0317(7) Uani 1 1 d . . . . .
H15A H 0.108995 0.424434 0.293378 0.048 Uiso 1 1 calc R U . . .
H15B H 0.195231 0.445935 0.264090 0.048 Uiso 1 1 calc R U . . .
H15C H 0.139552 0.532090 0.287300 0.048 Uiso 1 1 calc R U . . .
C16 C 0.13759(18) 0.4991(3) 0.43692(19) 0.0288(6) Uani 1 1 d . . . . .
H16A H 0.087010 0.462565 0.429579 0.043 Uiso 1 1 calc R U . . .
H16B H 0.126119 0.566488 0.425651 0.043 Uiso 1 1 calc R U . . .
H16C H 0.161882 0.492523 0.490266 0.043 Uiso 1 1 calc R U . . .
C17 C 0.21392(19) 0.3570(2) 0.4036(2) 0.0289(6) Uani 1 1 d . . . . .
H17A H 0.163341 0.320435 0.395975 0.043 Uiso 1 1 calc R U . . .
H17B H 0.236632 0.352738 0.457568 0.043 Uiso 1 1 calc R U . . .
H17C H 0.252782 0.330815 0.370771 0.043 Uiso 1 1 calc R U . . .
C18 C 0.70824(15) 0.46415(19) 0.37861(15) 0.0153(4) Uani 1 1 d . . . . .
C19 C 0.74292(15) 0.54841(19) 0.35428(15) 0.0165(4) Uani 1 1 d . . . . .
C20 C 0.82644(16) 0.5509(2) 0.34461(16) 0.0193(5) Uani 1 1 d . . . . .
C21 C 0.87000(17) 0.4659(2) 0.35405(17) 0.0208(5) Uani 1 1 d . . . . .
H21 H 0.925662 0.466330 0.345868 0.025 Uiso 1 1 calc R U . . .
C22 C 0.83560(16) 0.3801(2) 0.37496(16) 0.0180(5) Uani 1 1 d . . . . .
C23 C 0.75516(16) 0.38141(19) 0.38934(15) 0.0169(5) Uani 1 1 d . . . . .
H23 H 0.731370 0.324982 0.406832 0.020 Uiso 1 1 calc R U . . .
C24 C 0.86735(18) 0.6453(2) 0.32668(19) 0.0252(5) Uani 1 1 d . . . . .
C25 C 0.8599(2) 0.7163(3) 0.3927(2) 0.0323(7) Uani 1 1 d . . . . .
H25A H 0.889536 0.774809 0.383316 0.048 Uiso 1 1 calc R U . . .
H25B H 0.882845 0.687779 0.441424 0.048 Uiso 1 1 calc R U . . .
H25C H 0.802647 0.731408 0.395412 0.048 Uiso 1 1 calc R U . . .
C26 C 0.95837(19) 0.6312(3) 0.3202(2) 0.0325(7) Uani 1 1 d . . . . .
H26A H 0.982750 0.692317 0.308467 0.049 Uiso 1 1 calc R U . . .
H26B H 0.965364 0.585491 0.279089 0.049 Uiso 1 1 calc R U . . .
H26C H 0.984939 0.606664 0.369070 0.049 Uiso 1 1 calc R U . . .
C27 C 0.8293(2) 0.6884(2) 0.2502(2) 0.0323(7) Uani 1 1 d . . . . .
H27A H 0.861030 0.743872 0.237210 0.049 Uiso 1 1 calc R U . . .
H27B H 0.773513 0.708217 0.255382 0.049 Uiso 1 1 calc R U . . .
H27C H 0.829101 0.640603 0.209344 0.049 Uiso 1 1 calc R U . . .
C28 C 0.88688(18) 0.2886(2) 0.38558(18) 0.0233(5) Uani 1 1 d . . . . .
C29 C 0.8357(3) 0.1999(3) 0.3755(4) 0.0585(15) Uani 1 1 d . . . . .
H29A H 0.870976 0.143718 0.377955 0.088 Uiso 1 1 calc R U . . .
H29B H 0.802822 0.201878 0.325517 0.088 Uiso 1 1 calc R U . . .
H29C H 0.800055 0.196434 0.416558 0.088 Uiso 1 1 calc R U . . .
C30 C 0.9342(3) 0.2898(3) 0.4653(2) 0.0532(12) Uani 1 1 d . . . . .
H30A H 0.972801 0.236763 0.469856 0.080 Uiso 1 1 calc R U . . .
H30B H 0.896483 0.283274 0.504385 0.080 Uiso 1 1 calc R U . . .
H30C H 0.963638 0.350222 0.472896 0.080 Uiso 1 1 calc R U . . .
C31 C 0.9491(3) 0.2847(3) 0.3269(3) 0.0425(9) Uani 1 1 d . . . . .
H31A H 0.980322 0.225422 0.333779 0.064 Uiso 1 1 calc R U . . .
H31B H 0.985894 0.339311 0.334639 0.064 Uiso 1 1 calc R U . . .
H31C H 0.920849 0.286786 0.274723 0.064 Uiso 1 1 calc R U . . .
O3 O 0.55075(12) 0.62285(16) 0.23164(12) 0.0229(4) Uani 1 1 d . . . . .
C32 C 0.6011(2) 0.6184(3) 0.1672(2) 0.0345(7) Uani 1 1 d . . . . .
H32A H 0.641477 0.566384 0.174977 0.041 Uiso 1 1 calc R U . . .
H32B H 0.629775 0.679416 0.161575 0.041 Uiso 1 1 calc R U . . .
C33 C 0.5404(3) 0.5990(4) 0.0972(2) 0.0486(10) Uani 1 1 d . . . . .
H33A H 0.517697 0.659217 0.074524 0.058 Uiso 1 1 calc R U . . .
H33B H 0.565983 0.563197 0.057420 0.058 Uiso 1 1 calc R U . . .
C34 C 0.4763(3) 0.5409(4) 0.1284(2) 0.0483(10) Uani 1 1 d . . . . .
H34A H 0.492734 0.473176 0.134040 0.058 Uiso 1 1 calc R U . . .
H34B H 0.424348 0.544927 0.094873 0.058 Uiso 1 1 calc R U . . .
C35 C 0.4694(2) 0.5859(3) 0.2054(2) 0.0367(8) Uani 1 1 d . . . . .
H35A H 0.429255 0.638345 0.200551 0.044 Uiso 1 1 calc R U . . .
H35B H 0.452449 0.538204 0.242110 0.044 Uiso 1 1 calc R U . . .
O4 O 0.12812(17) -0.0082(2) 0.47040(16) 0.0413(6) Uani 1 1 d . . . . .
C36 C 0.0151(3) -0.0638(4) 0.3862(3) 0.0618(13) Uani 1 1 d . . . . .
H36A H -0.017974 -0.050435 0.337516 0.093 Uiso 1 1 calc R U . . .
H36B H -0.019564 -0.064482 0.428111 0.093 Uiso 1 1 calc R U . . .
H36C H 0.041333 -0.126095 0.383116 0.093 Uiso 1 1 calc R U . . .
C37 C 0.0779(3) 0.0111(3) 0.4011(3) 0.0497(10) Uani 1 1 d . . . . .
H37A H 0.111539 0.013732 0.357738 0.060 Uiso 1 1 calc R U . . .
H37B H 0.051507 0.073960 0.404998 0.060 Uiso 1 1 calc R U . . .
C38 C 0.1899(3) 0.0594(3) 0.4898(3) 0.0512(10) Uani 1 1 d . . . . .
H38A H 0.165390 0.123191 0.494353 0.061 Uiso 1 1 calc R U . . .
H38B H 0.226076 0.062140 0.448471 0.061 Uiso 1 1 calc R U . . .
C39 C 0.2378(3) 0.0340(3) 0.5634(3) 0.0538(11) Uani 1 1 d . . . . .
H39A H 0.281561 0.080379 0.574812 0.081 Uiso 1 1 calc R U . . .
H39B H 0.260933 -0.029829 0.559286 0.081 Uiso 1 1 calc R U . . .
H39C H 0.202465 0.034594 0.604824 0.081 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O2 1.9595(19) . ?
Hf1 O1 1.965(2) . ?
Hf1 O3 2.260(2) . ?
Hf1 C1 2.334(3) . ?
Hf1 Cl2 2.4046(7) . ?
Hf1 Cl1 2.4466(7) . ?
O1 C5 1.342(3) . ?
O2 C19 1.340(3) . ?
N1 C1 1.356(3) . ?
N1 C4 1.422(3) . ?
N1 C3 1.481(3) . ?
N2 C1 1.351(3) . ?
N2 C18 1.425(3) . ?
N2 C2 1.478(3) . ?
C2 C3 1.520(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.401(4) . ?
C4 C5 1.405(4) . ?
C5 C6 1.414(4) . ?
C6 C7 1.392(4) . ?
C6 C10 1.536(4) . ?
C7 C8 1.398(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(4) . ?
C8 C14 1.533(4) . ?
C9 H9 0.9500 . ?
C10 C12 1.539(5) . ?
C10 C13 1.541(5) . ?
C10 C11 1.547(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C17 1.526(4) . ?
C14 C15 1.536(4) . ?
C14 C16 1.537(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.399(4) . ?
C18 C19 1.401(4) . ?
C19 C20 1.415(4) . ?
C20 C21 1.395(4) . ?
C20 C24 1.535(4) . ?
C21 C22 1.398(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(4) . ?
C22 C28 1.540(4) . ?
C23 H23 0.9500 . ?
C24 C26 1.540(4) . ?
C24 C27 1.540(5) . ?
C24 C25 1.540(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.506(5) . ?
C28 C30 1.524(5) . ?
C28 C31 1.535(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
O3 C35 1.472(4) . ?
O3 C32 1.475(4) . ?
C32 C33 1.524(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.490(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.503(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
O4 C38 1.410(5) . ?
O4 C37 1.420(5) . ?
C36 C37 1.484(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.481(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Hf1 O1 155.12(8) . . ?
O2 Hf1 O3 87.82(8) . . ?
O1 Hf1 O3 86.22(8) . . ?
O2 Hf1 C1 77.58(8) . . ?
O1 Hf1 C1 77.60(8) . . ?
O3 Hf1 C1 79.89(8) . . ?
O2 Hf1 Cl2 94.56(6) . . ?
O1 Hf1 Cl2 91.35(6) . . ?
O3 Hf1 Cl2 177.54(6) . . ?
C1 Hf1 Cl2 99.97(7) . . ?
O2 Hf1 Cl1 100.91(6) . . ?
O1 Hf1 Cl1 102.37(6) . . ?
O3 Hf1 Cl1 83.45(6) . . ?
C1 Hf1 Cl1 163.32(7) . . ?
Cl2 Hf1 Cl1 96.71(3) . . ?
C5 O1 Hf1 145.85(17) . . ?
C19 O2 Hf1 146.44(17) . . ?
C1 N1 C4 127.7(2) . . ?
C1 N1 C3 112.5(2) . . ?
C4 N1 C3 119.5(2) . . ?
C1 N2 C18 128.4(2) . . ?
C1 N2 C2 112.7(2) . . ?
C18 N2 C2 119.0(2) . . ?
N2 C1 N1 108.3(2) . . ?
N2 C1 Hf1 125.65(18) . . ?
N1 C1 Hf1 125.99(18) . . ?
N2 C2 C3 103.2(2) . . ?
N2 C2 H2A 111.1 . . ?
C3 C2 H2A 111.1 . . ?
N2 C2 H2B 111.1 . . ?
C3 C2 H2B 111.1 . . ?
H2A C2 H2B 109.1 . . ?
N1 C3 C2 103.0(2) . . ?
N1 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
N1 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C9 C4 C5 119.8(2) . . ?
C9 C4 N1 118.2(2) . . ?
C5 C4 N1 121.9(2) . . ?
O1 C5 C4 120.1(2) . . ?
O1 C5 C6 119.7(2) . . ?
C4 C5 C6 120.2(2) . . ?
C7 C6 C5 117.5(3) . . ?
C7 C6 C10 121.9(3) . . ?
C5 C6 C10 120.5(3) . . ?
C6 C7 C8 123.1(3) . . ?
C6 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
C9 C8 C7 118.2(3) . . ?
C9 C8 C14 122.2(3) . . ?
C7 C8 C14 119.5(2) . . ?
C8 C9 C4 120.8(3) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
C6 C10 C12 111.0(3) . . ?
C6 C10 C13 111.8(3) . . ?
C12 C10 C13 107.3(3) . . ?
C6 C10 C11 109.4(2) . . ?
C12 C10 C11 110.2(3) . . ?
C13 C10 C11 107.0(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C14 C8 112.7(2) . . ?
C17 C14 C15 109.0(3) . . ?
C8 C14 C15 107.9(2) . . ?
C17 C14 C16 107.3(3) . . ?
C8 C14 C16 110.6(2) . . ?
C15 C14 C16 109.2(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.0(2) . . ?
C23 C18 N2 118.3(2) . . ?
C19 C18 N2 121.6(2) . . ?
O2 C19 C18 120.1(2) . . ?
O2 C19 C20 120.1(2) . . ?
C18 C19 C20 119.8(2) . . ?
C21 C20 C19 117.8(3) . . ?
C21 C20 C24 121.8(2) . . ?
C19 C20 C24 120.4(3) . . ?
C20 C21 C22 123.1(3) . . ?
C20 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C23 C22 C21 117.7(3) . . ?
C23 C22 C28 121.3(3) . . ?
C21 C22 C28 120.9(2) . . ?
C22 C23 C18 121.3(3) . . ?
C22 C23 H23 119.3 . . ?
C18 C23 H23 119.3 . . ?
C20 C24 C26 111.3(3) . . ?
C20 C24 C27 111.6(3) . . ?
C26 C24 C27 107.5(3) . . ?
C20 C24 C25 109.3(3) . . ?
C26 C24 C25 107.3(3) . . ?
C27 C24 C25 109.8(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C30 110.1(4) . . ?
C29 C28 C31 107.7(3) . . ?
C30 C28 C31 107.2(3) . . ?
C29 C28 C22 112.2(3) . . ?
C30 C28 C22 108.9(3) . . ?
C31 C28 C22 110.7(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C35 O3 C32 108.8(2) . . ?
C35 O3 Hf1 126.57(19) . . ?
C32 O3 Hf1 124.48(19) . . ?
O3 C32 C33 104.0(3) . . ?
O3 C32 H32A 111.0 . . ?
C33 C32 H32A 111.0 . . ?
O3 C32 H32B 111.0 . . ?
C33 C32 H32B 111.0 . . ?
H32A C32 H32B 109.0 . . ?
C34 C33 C32 103.8(3) . . ?
C34 C33 H33A 111.0 . . ?
C32 C33 H33A 111.0 . . ?
C34 C33 H33B 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
C33 C34 C35 103.0(3) . . ?
C33 C34 H34A 111.2 . . ?
C35 C34 H34A 111.2 . . ?
C33 C34 H34B 111.2 . . ?
C35 C34 H34B 111.2 . . ?
H34A C34 H34B 109.1 . . ?
O3 C35 C34 105.8(3) . . ?
O3 C35 H35A 110.6 . . ?
C34 C35 H35A 110.6 . . ?
O3 C35 H35B 110.6 . . ?
C34 C35 H35B 110.6 . . ?
H35A C35 H35B 108.7 . . ?
C38 O4 C37 114.9(3) . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O4 C37 C36 110.5(4) . . ?
O4 C37 H37A 109.5 . . ?
C36 C37 H37A 109.5 . . ?
O4 C37 H37B 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
O4 C38 C39 110.8(4) . . ?
O4 C38 H38A 109.5 . . ?
C39 C38 H38A 109.5 . . ?
O4 C38 H38B 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 N2 C1 N1 178.3(2) . . . . ?
C2 N2 C1 N1 -2.7(3) . . . . ?
C18 N2 C1 Hf1 -0.2(4) . . . . ?
C2 N2 C1 Hf1 178.84(17) . . . . ?
C4 N1 C1 N2 -174.6(2) . . . . ?
C3 N1 C1 N2 -0.7(3) . . . . ?
C4 N1 C1 Hf1 3.8(4) . . . . ?
C3 N1 C1 Hf1 177.75(17) . . . . ?
C1 N2 C2 C3 4.8(3) . . . . ?
C18 N2 C2 C3 -176.1(2) . . . . ?
C1 N1 C3 C2 3.6(3) . . . . ?
C4 N1 C3 C2 178.0(2) . . . . ?
N2 C2 C3 N1 -4.7(3) . . . . ?
C1 N1 C4 C9 169.4(3) . . . . ?
C3 N1 C4 C9 -4.2(4) . . . . ?
C1 N1 C4 C5 -7.7(4) . . . . ?
C3 N1 C4 C5 178.7(2) . . . . ?
Hf1 O1 C5 C4 9.1(5) . . . . ?
Hf1 O1 C5 C6 -170.6(2) . . . . ?
C9 C4 C5 O1 -174.3(2) . . . . ?
N1 C4 C5 O1 2.7(4) . . . . ?
C9 C4 C5 C6 5.3(4) . . . . ?
N1 C4 C5 C6 -177.6(2) . . . . ?
O1 C5 C6 C7 173.4(3) . . . . ?
C4 C5 C6 C7 -6.3(4) . . . . ?
O1 C5 C6 C10 -6.8(4) . . . . ?
C4 C5 C6 C10 173.5(3) . . . . ?
C5 C6 C7 C8 1.9(4) . . . . ?
C10 C6 C7 C8 -177.9(3) . . . . ?
C6 C7 C8 C9 3.6(4) . . . . ?
C6 C7 C8 C14 -172.2(3) . . . . ?
C7 C8 C9 C4 -4.6(4) . . . . ?
C14 C8 C9 C4 171.1(2) . . . . ?
C5 C4 C9 C8 0.3(4) . . . . ?
N1 C4 C9 C8 -176.9(2) . . . . ?
C7 C6 C10 C12 -119.4(3) . . . . ?
C5 C6 C10 C12 60.9(4) . . . . ?
C7 C6 C10 C13 0.4(4) . . . . ?
C5 C6 C10 C13 -179.4(3) . . . . ?
C7 C6 C10 C11 118.7(3) . . . . ?
C5 C6 C10 C11 -61.0(4) . . . . ?
C9 C8 C14 C17 10.8(4) . . . . ?
C7 C8 C14 C17 -173.6(3) . . . . ?
C9 C8 C14 C15 -109.7(3) . . . . ?
C7 C8 C14 C15 65.9(3) . . . . ?
C9 C8 C14 C16 130.9(3) . . . . ?
C7 C8 C14 C16 -53.5(4) . . . . ?
C1 N2 C18 C23 -179.8(3) . . . . ?
C2 N2 C18 C23 1.3(4) . . . . ?
C1 N2 C18 C19 -1.7(4) . . . . ?
C2 N2 C18 C19 179.3(2) . . . . ?
Hf1 O2 C19 C18 6.1(5) . . . . ?
Hf1 O2 C19 C20 -172.6(2) . . . . ?
C23 C18 C19 O2 177.8(2) . . . . ?
N2 C18 C19 O2 -0.2(4) . . . . ?
C23 C18 C19 C20 -3.4(4) . . . . ?
N2 C18 C19 C20 178.6(2) . . . . ?
O2 C19 C20 C21 -176.2(3) . . . . ?
C18 C19 C20 C21 5.0(4) . . . . ?
O2 C19 C20 C24 5.6(4) . . . . ?
C18 C19 C20 C24 -173.2(3) . . . . ?
C19 C20 C21 C22 -2.2(4) . . . . ?
C24 C20 C21 C22 176.0(3) . . . . ?
C20 C21 C22 C23 -2.2(4) . . . . ?
C20 C21 C22 C28 -179.2(3) . . . . ?
C21 C22 C23 C18 4.0(4) . . . . ?
C28 C22 C23 C18 -179.0(3) . . . . ?
C19 C18 C23 C22 -1.3(4) . . . . ?
N2 C18 C23 C22 176.9(2) . . . . ?
C21 C20 C24 C26 0.7(4) . . . . ?
C19 C20 C24 C26 178.8(3) . . . . ?
C21 C20 C24 C27 120.7(3) . . . . ?
C19 C20 C24 C27 -61.1(4) . . . . ?
C21 C20 C24 C25 -117.7(3) . . . . ?
C19 C20 C24 C25 60.5(4) . . . . ?
C23 C22 C28 C29 26.7(5) . . . . ?
C21 C22 C28 C29 -156.4(4) . . . . ?
C23 C22 C28 C30 -95.4(4) . . . . ?
C21 C22 C28 C30 81.5(4) . . . . ?
C23 C22 C28 C31 147.0(3) . . . . ?
C21 C22 C28 C31 -36.1(4) . . . . ?
C35 O3 C32 C33 12.8(4) . . . . ?
Hf1 O3 C32 C33 -163.2(2) . . . . ?
O3 C32 C33 C34 -31.8(4) . . . . ?
C32 C33 C34 C35 38.4(5) . . . . ?
C32 O3 C35 C34 11.0(4) . . . . ?
Hf1 O3 C35 C34 -173.1(3) . . . . ?
C33 C34 C35 O3 -30.7(5) . . . . ?
C38 O4 C37 C36 -179.9(4) . . . . ?
C37 O4 C38 C39 179.0(4) . . . . ?

_refine_diff_density_max         3.521
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.153


_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
