# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#
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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_mk236
_database_code_depnum_ccdc_archive 'CCDC 917774'
#TrackingRef 'mk236.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H50 Cl2 Hf N2 O4'
_chemical_formula_sum            'C33 H50 Cl2 Hf N2 O4'
_chemical_formula_weight         788.14
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.09040(10)
_cell_length_b                   13.4696(2)
_cell_length_c                   13.6674(2)
_cell_angle_alpha                114.1734(5)
_cell_angle_beta                 105.5292(6)
_cell_angle_gamma                92.2735(11)
_cell_volume                     1768.57(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6201
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      27.98
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4530
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_diffrn_detector_area_resol_mean 12.8
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19631
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         27.98
_reflns_number_total             8349
_reflns_number_gt                7322
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Collect, Nonius B.V.'
_computing_cell_refinement       Denzo
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_solution    DIRDIF-96
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+3.2771P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8349
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1026
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.160782(14) 0.120346(14) 0.767649(13) 0.01522(7) Uani 1 1 d . . .
O2 O 0.1181(3) 0.2251(2) 0.6986(2) 0.0161(6) Uani 1 1 d . . .
O3 O 0.0702(3) 0.1725(3) 0.8790(2) 0.0183(6) Uani 1 1 d . . .
O4 O 0.3327(3) 0.1798(3) 0.8687(2) 0.0183(6) Uani 1 1 d . . .
O5 O 0.2265(3) 0.0236(2) 0.6321(2) 0.0145(6) Uani 1 1 d . . .
N6 N 0.1293(3) -0.0598(3) 0.7636(3) 0.0158(7) Uani 1 1 d . . .
N7 N -0.0399(3) 0.0355(3) 0.6438(3) 0.0135(7) Uani 1 1 d . . .
C8 C 0.0042(4) 0.2316(4) 0.9533(4) 0.0187(9) Uani 1 1 d . . .
C9 C -0.1366(4) 0.1820(5) 0.9025(4) 0.0323(12) Uani 1 1 d . . .
H9A H -0.1698 0.1823 0.8286 0.048 Uiso 1 1 calc R . .
H9B H -0.1827 0.2258 0.9527 0.048 Uiso 1 1 calc R . .
H9C H -0.1478 0.1059 0.8936 0.048 Uiso 1 1 calc R . .
C10 C 0.0595(4) 0.2231(5) 1.0647(4) 0.0282(11) Uani 1 1 d . . .
H10A H 0.0473 0.1454 1.0508 0.042 Uiso 1 1 calc R . .
H10B H 0.0162 0.2649 1.1185 0.042 Uiso 1 1 calc R . .
H10C H 0.1505 0.2534 1.0960 0.042 Uiso 1 1 calc R . .
C11 C 0.0237(5) 0.3505(4) 0.9730(5) 0.0335(12) Uani 1 1 d . . .
H11A H -0.0214 0.3930 1.0249 0.050 Uiso 1 1 calc R . .
H11B H -0.0095 0.3548 0.9010 0.050 Uiso 1 1 calc R . .
H11C H 0.1146 0.3811 1.0058 0.050 Uiso 1 1 calc R . .
C12 C 0.4490(4) 0.2393(4) 0.9529(4) 0.0218(10) Uani 1 1 d . . .
C13 C 0.5228(4) 0.2964(4) 0.9056(4) 0.0285(11) Uani 1 1 d . . .
H13A H 0.5412 0.2408 0.8404 0.043 Uiso 1 1 calc R . .
H13B H 0.6026 0.3399 0.9639 0.043 Uiso 1 1 calc R . .
H13C H 0.4720 0.3454 0.8822 0.043 Uiso 1 1 calc R . .
C14 C 0.4193(4) 0.3239(5) 1.0542(4) 0.0325(12) Uani 1 1 d . . .
H14A H 0.3742 0.3766 1.0329 0.049 Uiso 1 1 calc R . .
H14B H 0.4987 0.3633 1.1153 0.049 Uiso 1 1 calc R . .
H14C H 0.3660 0.2863 1.0798 0.049 Uiso 1 1 calc R . .
C15 C 0.5230(5) 0.1579(5) 0.9841(4) 0.0322(12) Uani 1 1 d . . .
H15A H 0.4731 0.1203 1.0121 0.048 Uiso 1 1 calc R . .
H15B H 0.6037 0.1979 1.0430 0.048 Uiso 1 1 calc R . .
H15C H 0.5397 0.1034 0.9173 0.048 Uiso 1 1 calc R . .
C16 C 0.0138(4) 0.2655(3) 0.6690(3) 0.0133(8) Uani 1 1 d . . .
C17 C 0.0242(4) 0.3732(4) 0.6739(3) 0.0168(8) Uani 1 1 d . . .
C18 C -0.0880(4) 0.4132(4) 0.6495(4) 0.0199(9) Uani 1 1 d . . .
H18 H -0.0818 0.4859 0.6547 0.024 Uiso 1 1 calc R . .
C19 C -0.2103(4) 0.3538(4) 0.6175(4) 0.0180(8) Uani 1 1 d . . .
C20 C -0.2170(4) 0.2472(4) 0.6066(3) 0.0170(8) Uani 1 1 d . . .
H20 H -0.2983 0.2036 0.5815 0.020 Uiso 1 1 calc R . .
C21 C -0.1087(4) 0.2005(3) 0.6311(3) 0.0147(8) Uani 1 1 d . . .
C22 C -0.1274(4) 0.0866(3) 0.6138(3) 0.0143(8) Uani 1 1 d . . .
H22 H -0.2115 0.0463 0.5773 0.017 Uiso 1 1 calc R . .
C23 C -0.0759(4) -0.0807(3) 0.6189(4) 0.0183(9) Uani 1 1 d . . .
H23A H -0.0491 -0.1296 0.5543 0.022 Uiso 1 1 calc R . .
H23B H -0.1692 -0.0994 0.5986 0.022 Uiso 1 1 calc R . .
C24 C -0.0117(4) -0.0975(4) 0.7222(4) 0.0185(9) Uani 1 1 d . . .
H24A H -0.0478 -0.0560 0.7831 0.022 Uiso 1 1 calc R . .
H24B H -0.0296 -0.1768 0.7038 0.022 Uiso 1 1 calc R . .
C25 C 0.1885(4) -0.1452(4) 0.6894(4) 0.0172(8) Uani 1 1 d . . .
H25A H 0.1337 -0.1737 0.6101 0.021 Uiso 1 1 calc R . .
H25B H 0.1924 -0.2077 0.7100 0.021 Uiso 1 1 calc R . .
C26 C 0.3204(4) -0.1021(4) 0.6979(3) 0.0159(8) Uani 1 1 d . . .
C27 C 0.4273(4) -0.1437(4) 0.7338(4) 0.0180(8) Uani 1 1 d . . .
H27 H 0.4218 -0.1978 0.7610 0.022 Uiso 1 1 calc R . .
C28 C 0.5426(4) -0.1046(4) 0.7292(4) 0.0200(9) Uani 1 1 d . . .
C29 C 0.5533(4) -0.0286(4) 0.6880(3) 0.0189(9) Uani 1 1 d . . .
H29 H 0.6327 -0.0048 0.6836 0.023 Uiso 1 1 calc R . .
C30 C 0.4465(4) 0.0128(4) 0.6529(3) 0.0166(8) Uani 1 1 d . . .
C31 C 0.3280(4) -0.0201(3) 0.6594(3) 0.0134(8) Uani 1 1 d . . .
C32 C 0.1548(4) 0.4421(4) 0.7095(4) 0.0216(9) Uani 1 1 d . . .
C33 C 0.2297(4) 0.4659(4) 0.8322(4) 0.0306(11) Uani 1 1 d . . .
H33A H 0.1836 0.5081 0.8831 0.046 Uiso 1 1 calc R . .
H33B H 0.3139 0.5086 0.8538 0.046 Uiso 1 1 calc R . .
H33C H 0.2391 0.3959 0.8372 0.046 Uiso 1 1 calc R . .
C34 C 0.2283(4) 0.3794(4) 0.6291(5) 0.0289(11) Uani 1 1 d . . .
H34A H 0.2417 0.3099 0.6342 0.043 Uiso 1 1 calc R . .
H34B H 0.3107 0.4247 0.6503 0.043 Uiso 1 1 calc R . .
H34C H 0.1794 0.3634 0.5516 0.043 Uiso 1 1 calc R . .
C35 C 0.1441(5) 0.5534(4) 0.7055(5) 0.0311(11) Uani 1 1 d . . .
H35A H 0.0947 0.5410 0.6292 0.047 Uiso 1 1 calc R . .
H35B H 0.2292 0.5937 0.7255 0.047 Uiso 1 1 calc R . .
H35C H 0.1014 0.5967 0.7592 0.047 Uiso 1 1 calc R . .
C36 C -0.3263(4) 0.4089(4) 0.5948(4) 0.0232(9) Uani 1 1 d . . .
C37 C -0.4504(4) 0.3335(4) 0.5619(4) 0.0257(10) Uani 1 1 d . . .
H37A H -0.4548 0.3197 0.6260 0.038 Uiso 1 1 calc R . .
H37B H -0.4546 0.2634 0.4977 0.038 Uiso 1 1 calc R . .
H37C H -0.5219 0.3690 0.5407 0.038 Uiso 1 1 calc R . .
C38 C -0.3283(5) 0.4376(5) 0.4962(5) 0.0318(11) Uani 1 1 d . . .
H38A H -0.3298 0.3704 0.4298 0.048 Uiso 1 1 calc R . .
H38B H -0.2522 0.4910 0.5178 0.048 Uiso 1 1 calc R . .
H38C H -0.4041 0.4697 0.4782 0.048 Uiso 1 1 calc R . .
C39 C -0.3157(5) 0.5148(5) 0.6999(5) 0.0374(13) Uani 1 1 d . . .
H39A H -0.3894 0.5504 0.6851 0.056 Uiso 1 1 calc R . .
H39B H -0.2378 0.5650 0.7191 0.056 Uiso 1 1 calc R . .
H39C H -0.3132 0.4969 0.7630 0.056 Uiso 1 1 calc R . .
C40 C 0.1832(4) -0.0482(4) 0.8804(4) 0.0208(9) Uani 1 1 d . . .
H40A H 0.1610 -0.1185 0.8822 0.031 Uiso 1 1 calc R . .
H40B H 0.1483 0.0094 0.9312 0.031 Uiso 1 1 calc R . .
H40C H 0.2758 -0.0278 0.9050 0.031 Uiso 1 1 calc R . .
Cl41 Cl 0.45576(10) 0.11068(9) 0.60183(9) 0.0203(2) Uani 1 1 d . . .
Cl42 Cl 0.67835(11) -0.15618(11) 0.77513(11) 0.0322(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Hf1 0.01054(10) 0.01753(11) 0.01570(10) 0.00585(7) 0.00350(6) 0.00188(6)
O2 0.0112(13) 0.0161(15) 0.0221(15) 0.0100(12) 0.0045(11) 0.0007(11)
O3 0.0139(14) 0.0241(16) 0.0179(15) 0.0081(13) 0.0076(11) 0.0055(12)
O4 0.0106(13) 0.0246(17) 0.0151(14) 0.0067(13) 0.0004(11) 0.0008(11)
O5 0.0134(13) 0.0180(15) 0.0118(13) 0.0051(12) 0.0050(10) 0.0057(11)
N6 0.0110(16) 0.0188(18) 0.0162(17) 0.0076(15) 0.0026(12) 0.0016(13)
N7 0.0132(16) 0.0146(17) 0.0129(16) 0.0066(14) 0.0033(12) 0.0031(13)
C8 0.0146(19) 0.024(2) 0.018(2) 0.0073(18) 0.0089(15) 0.0051(16)
C9 0.015(2) 0.049(3) 0.030(3) 0.013(2) 0.0087(18) 0.006(2)
C10 0.020(2) 0.041(3) 0.024(2) 0.012(2) 0.0105(18) 0.008(2)
C11 0.040(3) 0.028(3) 0.036(3) 0.009(2) 0.024(2) 0.014(2)
C12 0.0109(19) 0.030(3) 0.015(2) 0.0019(18) 0.0026(15) -0.0008(17)
C13 0.018(2) 0.037(3) 0.022(2) 0.006(2) 0.0050(17) -0.0082(19)
C14 0.018(2) 0.039(3) 0.024(2) 0.000(2) 0.0074(18) -0.004(2)
C15 0.024(2) 0.040(3) 0.024(2) 0.010(2) 0.0007(19) 0.009(2)
C16 0.0136(18) 0.015(2) 0.0136(19) 0.0082(16) 0.0047(14) 0.0044(15)
C17 0.0162(19) 0.018(2) 0.018(2) 0.0089(17) 0.0068(15) 0.0027(16)
C18 0.021(2) 0.018(2) 0.024(2) 0.0107(18) 0.0103(17) 0.0078(17)
C19 0.018(2) 0.021(2) 0.018(2) 0.0097(18) 0.0066(15) 0.0067(16)
C20 0.0156(19) 0.018(2) 0.0147(19) 0.0053(17) 0.0041(15) 0.0012(16)
C21 0.0126(18) 0.019(2) 0.0096(18) 0.0037(16) 0.0028(14) 0.0022(15)
C22 0.0131(18) 0.017(2) 0.0102(18) 0.0036(16) 0.0032(14) -0.0022(15)
C23 0.0094(18) 0.015(2) 0.026(2) 0.0070(18) 0.0008(15) -0.0002(15)
C24 0.0074(18) 0.015(2) 0.032(2) 0.0101(18) 0.0050(16) 0.0012(15)
C25 0.0149(19) 0.021(2) 0.018(2) 0.0084(17) 0.0079(15) 0.0031(16)
C26 0.0129(18) 0.020(2) 0.0140(19) 0.0065(17) 0.0052(14) 0.0030(15)
C27 0.019(2) 0.019(2) 0.018(2) 0.0084(17) 0.0080(16) 0.0046(16)
C28 0.0130(19) 0.029(2) 0.021(2) 0.0110(19) 0.0084(16) 0.0087(17)
C29 0.0109(18) 0.026(2) 0.016(2) 0.0051(18) 0.0043(15) 0.0044(16)
C30 0.019(2) 0.019(2) 0.0134(19) 0.0069(17) 0.0077(15) 0.0042(16)
C31 0.0129(18) 0.0128(19) 0.0110(18) 0.0021(15) 0.0036(14) -0.0005(14)
C32 0.016(2) 0.018(2) 0.032(2) 0.0112(19) 0.0093(17) 0.0029(16)
C33 0.021(2) 0.026(3) 0.036(3) 0.007(2) 0.0067(19) -0.0028(19)
C34 0.024(2) 0.026(3) 0.046(3) 0.018(2) 0.021(2) 0.0070(19)
C35 0.022(2) 0.019(2) 0.054(3) 0.014(2) 0.016(2) 0.0050(18)
C36 0.018(2) 0.023(2) 0.030(2) 0.011(2) 0.0105(18) 0.0077(17)
C37 0.018(2) 0.026(2) 0.034(3) 0.013(2) 0.0074(18) 0.0072(18)
C38 0.025(2) 0.040(3) 0.040(3) 0.024(3) 0.011(2) 0.012(2)
C39 0.029(3) 0.030(3) 0.044(3) 0.006(2) 0.010(2) 0.014(2)
C40 0.019(2) 0.031(3) 0.020(2) 0.0164(19) 0.0073(16) 0.0073(18)
Cl41 0.0201(5) 0.0208(5) 0.0236(5) 0.0112(4) 0.0100(4) 0.0025(4)
Cl42 0.0176(5) 0.0453(8) 0.0454(7) 0.0295(6) 0.0108(5) 0.0148(5)
_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 O4 1.936(3) . ?
Hf1 O3 1.954(3) . ?
Hf1 O2 2.003(3) . ?
Hf1 O5 2.117(3) . ?
Hf1 N7 2.307(3) . ?
Hf1 N6 2.414(4) . ?
O2 C16 1.333(5) . ?
O3 C8 1.408(5) . ?
O4 C12 1.413(5) . ?
O5 C31 1.327(5) . ?
N6 C40 1.486(5) . ?
N6 C25 1.498(5) . ?
N6 C24 1.501(5) . ?
N7 C22 1.286(5) . ?
N7 C23 1.471(5) . ?
C8 C11 1.508(7) . ?
C8 C9 1.525(6) . ?
C8 C10 1.535(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.518(6) . ?
C12 C13 1.523(7) . ?
C12 C15 1.524(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.423(6) . ?
C16 C21 1.427(5) . ?
C17 C18 1.389(6) . ?
C17 C32 1.530(6) . ?
C18 C19 1.408(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(6) . ?
C19 C36 1.534(6) . ?
C20 C21 1.402(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.451(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.513(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.508(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.389(6) . ?
C26 C31 1.412(6) . ?
C27 C28 1.390(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.371(7) . ?
C28 Cl42 1.754(4) . ?
C29 C30 1.383(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.408(6) . ?
C30 Cl41 1.736(4) . ?
C32 C35 1.532(7) . ?
C32 C34 1.536(6) . ?
C32 C33 1.548(7) . ?
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 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.521(6) . ?
C36 C39 1.527(7) . ?
C36 C38 1.542(7) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
O4 Hf1 O3 98.72(12) . . ?
O4 Hf1 O2 104.95(12) . . ?
O3 Hf1 O2 98.36(12) . . ?
O4 Hf1 O5 91.63(11) . . ?
O3 Hf1 O5 164.64(12) . . ?
O2 Hf1 O5 89.81(11) . . ?
O4 Hf1 N7 175.37(12) . . ?
O3 Hf1 N7 83.33(12) . . ?
O2 Hf1 N7 78.77(12) . . ?
O5 Hf1 N7 85.57(11) . . ?
O4 Hf1 N6 101.63(12) . . ?
O3 Hf1 N6 88.41(12) . . ?
O2 Hf1 N6 151.16(12) . . ?
O5 Hf1 N6 78.36(12) . . ?
N7 Hf1 N6 74.21(12) . . ?
C16 O2 Hf1 134.5(3) . . ?
C8 O3 Hf1 166.5(3) . . ?
C12 O4 Hf1 169.9(3) . . ?
C31 O5 Hf1 115.5(2) . . ?
C40 N6 C25 108.0(3) . . ?
C40 N6 C24 110.1(3) . . ?
C25 N6 C24 109.0(3) . . ?
C40 N6 Hf1 108.4(3) . . ?
C25 N6 Hf1 115.3(3) . . ?
C24 N6 Hf1 106.0(2) . . ?
C22 N7 C23 118.4(3) . . ?
C22 N7 Hf1 124.6(3) . . ?
C23 N7 Hf1 115.6(2) . . ?
O3 C8 C11 108.4(4) . . ?
O3 C8 C9 109.8(4) . . ?
C11 C8 C9 110.6(4) . . ?
O3 C8 C10 107.9(3) . . ?
C11 C8 C10 110.2(4) . . ?
C9 C8 C10 109.8(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C12 C14 108.1(3) . . ?
O4 C12 C13 108.5(4) . . ?
C14 C12 C13 110.5(4) . . ?
O4 C12 C15 108.3(4) . . ?
C14 C12 C15 110.8(4) . . ?
C13 C12 C15 110.5(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 C16 C17 120.0(4) . . ?
O2 C16 C21 120.2(4) . . ?
C17 C16 C21 119.7(3) . . ?
C18 C17 C16 117.1(4) . . ?
C18 C17 C32 122.4(4) . . ?
C16 C17 C32 120.4(4) . . ?
C17 C18 C19 124.7(4) . . ?
C17 C18 H18 117.7 . . ?
C19 C18 H18 117.7 . . ?
C20 C19 C18 116.5(4) . . ?
C20 C19 C36 124.3(4) . . ?
C18 C19 C36 119.2(4) . . ?
C19 C20 C21 122.7(4) . . ?
C19 C20 H20 118.7 . . ?
C21 C20 H20 118.7 . . ?
C20 C21 C16 119.1(4) . . ?
C20 C21 C22 117.8(4) . . ?
C16 C21 C22 123.1(3) . . ?
N7 C22 C21 125.6(4) . . ?
N7 C22 H22 117.2 . . ?
C21 C22 H22 117.2 . . ?
N7 C23 C24 108.9(3) . . ?
N7 C23 H23A 109.9 . . ?
C24 C23 H23A 109.9 . . ?
N7 C23 H23B 109.9 . . ?
C24 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
N6 C24 C23 112.1(4) . . ?
N6 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
N6 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
N6 C25 C26 113.5(3) . . ?
N6 C25 H25A 108.9 . . ?
C26 C25 H25A 108.9 . . ?
N6 C25 H25B 108.9 . . ?
C26 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C27 C26 C31 121.2(4) . . ?
C27 C26 C25 123.4(4) . . ?
C31 C26 C25 115.4(4) . . ?
C26 C27 C28 118.6(4) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 H27 120.7 . . ?
C29 C28 C27 122.2(4) . . ?
C29 C28 Cl42 118.8(3) . . ?
C27 C28 Cl42 118.9(4) . . ?
C28 C29 C30 118.8(4) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C29 C30 C31 121.8(4) . . ?
C29 C30 Cl41 120.5(3) . . ?
C31 C30 Cl41 117.7(3) . . ?
O5 C31 C30 122.4(4) . . ?
O5 C31 C26 120.3(3) . . ?
C30 C31 C26 117.3(4) . . ?
C17 C32 C35 111.8(4) . . ?
C17 C32 C34 109.5(4) . . ?
C35 C32 C34 107.9(4) . . ?
C17 C32 C33 110.0(4) . . ?
C35 C32 C33 107.6(4) . . ?
C34 C32 C33 110.1(4) . . ?
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 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C39 109.3(4) . . ?
C37 C36 C19 112.3(4) . . ?
C39 C36 C19 109.5(4) . . ?
C37 C36 C38 108.0(4) . . ?
C39 C36 C38 109.3(4) . . ?
C19 C36 C38 108.5(4) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N6 C40 H40A 109.5 . . ?
N6 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N6 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.98
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         2.945
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.164