#------------------------------------------------------------------------------
#$Date: 2017-03-05 06:26:47 +0100 (dom 05 de mar de 2017) $
#$Revision: 193876 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/59/7055935.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7055935
loop_
_publ_author_name
'Bortoluzzi, Marco'
'Bresciani, Giulio'
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_publ_section_title
;
 Synthesis and structural characterization of mixed
 halide--N,N-diethylcarbamates of group 4 metals, including a case of
 unusual tetrahydrofuran activation
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              1781
_journal_paper_doi               10.1039/C6NJ03489F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C38 H74 Cl4 Hf4 N6 O18'
_chemical_formula_weight         1758.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-27 deposited with the CCDC.
2017-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.888(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5959(12)
_cell_length_b                   18.794(2)
_cell_length_c                   14.5380(16)
_cell_measurement_reflns_used    8312
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.859
_cell_measurement_theta_min      2.309
_cell_volume                     3088.5(6)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CMOS area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28411
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.935
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.3939
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1339 (selected reflections only, before parameter refinement)
 R(int) =  0.0844(selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       cube
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         3.759
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0919P)²+20.1428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4346
_reflns_number_total             6078
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj03489f2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7055933--7055935.cif.'
_cod_database_code               7055935
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.443
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1771(12) 0.5469(7) 0.5302(9) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.0841(19) 0.5536(13) 0.6656(17) 0.096(8) Uani 1 1 d . U . . .
H2A H 0.0021 0.5594 0.6738 0.115 Uiso 1 1 calc R U . . .
H2B H 0.1091 0.5038 0.6808 0.115 Uiso 1 1 calc R U . . .
C3 C 0.159(2) 0.6003(12) 0.7240(17) 0.097(7) Uani 1 1 d . U . . .
H3A H 0.1577 0.5906 0.7899 0.146 Uiso 1 1 calc R U . . .
H3B H 0.2401 0.5940 0.7152 0.146 Uiso 1 1 calc R U . . .
H3C H 0.1336 0.6493 0.7082 0.146 Uiso 1 1 calc R U . . .
C4 C -0.0108(12) 0.6067(8) 0.5056(11) 0.044(4) Uani 1 1 d . . . . .
H4A H -0.0844 0.5874 0.5197 0.053 Uiso 1 1 calc R U . . .
H4B H -0.0116 0.5957 0.4388 0.053 Uiso 1 1 calc R U . . .
C5 C -0.0090(15) 0.6853(9) 0.5183(14) 0.064(5) Uani 1 1 d . . . . .
H5A H -0.0787 0.7062 0.4763 0.096 Uiso 1 1 calc R U . . .
H5B H -0.0100 0.6966 0.5840 0.096 Uiso 1 1 calc R U . . .
H5C H 0.0628 0.7049 0.5031 0.096 Uiso 1 1 calc R U . . .
C6 C 0.1461(11) 0.6313(7) 0.2096(11) 0.041(3) Uani 1 1 d . . . . .
C7 C -0.0503(16) 0.6364(13) 0.1132(15) 0.093(8) Uani 1 1 d . . . . .
H7A H -0.0952 0.6679 0.0633 0.112 Uiso 1 1 calc R U . . .
H7B H -0.0772 0.6467 0.1718 0.112 Uiso 1 1 calc R U . . .
C8 C -0.082(2) 0.5606(16) 0.0854(18) 0.128(11) Uani 1 1 d . . . . .
H8A H -0.1671 0.5539 0.0767 0.192 Uiso 1 1 calc R U . . .
H8B H -0.0580 0.5499 0.0262 0.192 Uiso 1 1 calc R U . . .
H8C H -0.0400 0.5286 0.1350 0.192 Uiso 1 1 calc R U . . .
C9 C 0.1189(15) 0.6943(10) 0.0570(13) 0.068(5) Uani 1 1 d . . . . .
H9A H 0.1840 0.7258 0.0890 0.082 Uiso 1 1 calc R U . . .
H9B H 0.0550 0.7248 0.0208 0.082 Uiso 1 1 calc R U . . .
C10 C 0.163(3) 0.6469(15) -0.0098(16) 0.125(10) Uani 1 1 d . . . . .
H10A H 0.1923 0.6759 -0.0559 0.188 Uiso 1 1 calc R U . . .
H10B H 0.2278 0.6173 0.0254 0.188 Uiso 1 1 calc R U . . .
H10C H 0.0988 0.6163 -0.0428 0.188 Uiso 1 1 calc R U . . .
C11 C 0.3755(12) 0.4490(7) 0.2811(10) 0.037(3) Uani 1 1 d . . . . .
C12 C 0.2252(14) 0.3807(9) 0.1748(12) 0.058(3) Uani 1 1 d . U . . .
H12A H 0.2279 0.3523 0.1180 0.069 Uiso 1 1 calc R U . . .
H12B H 0.1905 0.4277 0.1540 0.069 Uiso 1 1 calc R U . . .
C13 C 0.1491(14) 0.3432(9) 0.2315(12) 0.062(4) Uani 1 1 d . U . . .
H13A H 0.0690 0.3372 0.1926 0.093 Uiso 1 1 calc R U . . .
H13B H 0.1831 0.2965 0.2513 0.093 Uiso 1 1 calc R U . . .
H13C H 0.1458 0.3717 0.2873 0.093 Uiso 1 1 calc R U . . .
C14 C 0.4253(16) 0.3259(10) 0.2429(14) 0.072(3) Uani 1 1 d . U . . .
H14A H 0.4757 0.3242 0.3075 0.086 Uiso 1 1 calc R U . . .
H14B H 0.3772 0.2819 0.2323 0.086 Uiso 1 1 calc R U . . .
C15 C 0.496(3) 0.3304(15) 0.177(2) 0.130(10) Uani 1 1 d . U . . .
H15A H 0.5481 0.2889 0.1833 0.196 Uiso 1 1 calc R U . . .
H15B H 0.4454 0.3316 0.1132 0.196 Uiso 1 1 calc R U . . .
H15C H 0.5437 0.3738 0.1882 0.196 Uiso 1 1 calc R U . . .
C16 C 0.5156(12) 0.6198(8) 0.2651(12) 0.053(4) Uani 1 1 d D U . . .
H16 H 0.4623 0.5960 0.2101 0.064 Uiso 0.5 1 calc R U P A 1
H16' H 0.4625 0.6070 0.2032 0.064 Uiso 0.5 1 calc R U P B 2
C17A C 0.542(3) 0.6914(14) 0.231(3) 0.055(7) Uani 0.5 1 d D U P C 1
H17C H 0.4998 0.7292 0.2579 0.066 Uiso 0.5 1 calc R U P C 1
H17D H 0.5195 0.6941 0.1612 0.066 Uiso 0.5 1 calc R U P C 1
C18A C 0.675(3) 0.6968(13) 0.267(3) 0.072(8) Uani 0.5 1 d D U P C 1
H18C H 0.7118 0.7235 0.2224 0.086 Uiso 0.5 1 calc R U P C 1
H18D H 0.6947 0.7213 0.3293 0.086 Uiso 0.5 1 calc R U P C 1
C17B C 0.567(3) 0.6956(13) 0.266(3) 0.055(7) Uani 0.5 1 d D U P C 2
H17A H 0.5933 0.7133 0.3319 0.066 Uiso 0.5 1 calc R U P C 2
H17B H 0.5075 0.7290 0.2304 0.066 Uiso 0.5 1 calc R U P C 2
C18B C 0.673(3) 0.6866(17) 0.219(3) 0.072(8) Uani 0.5 1 d D U P C 2
H18A H 0.6480 0.6769 0.1504 0.086 Uiso 0.5 1 calc R U P C 2
H18B H 0.7284 0.7272 0.2308 0.086 Uiso 0.5 1 calc R U P C 2
C19 C 0.7196(12) 0.6206(8) 0.2769(13) 0.061(4) Uani 1 1 d D U . . .
H19A H 0.7472 0.6062 0.2199 0.074 Uiso 0.5 1 calc R U P C 1
H19B H 0.7862 0.6157 0.3325 0.074 Uiso 0.5 1 calc R U P C 1
H19C H 0.7719 0.5933 0.2445 0.074 Uiso 0.5 1 calc R U P C 2
H19D H 0.7664 0.6351 0.3397 0.074 Uiso 0.5 1 calc R U P C 2
N1 N 0.0908(11) 0.5713(7) 0.5661(9) 0.047(3) Uani 1 1 d . . . . .
N2 N 0.0736(10) 0.6547(7) 0.1286(9) 0.054(4) Uani 1 1 d . . . . .
N3 N 0.3455(12) 0.3900(7) 0.2325(10) 0.059(3) Uani 1 1 d . U . . .
O1 O 0.4130(7) 0.5384(4) 0.4647(5) 0.0251(17) Uani 1 1 d . . . . .
O2 O 0.2655(8) 0.5184(5) 0.5883(6) 0.041(2) Uani 1 1 d . . . . .
O3 O 0.1775(7) 0.5537(4) 0.4438(6) 0.031(2) Uani 1 1 d . . . . .
O4 O 0.2601(8) 0.6472(5) 0.2258(6) 0.040(2) Uani 1 1 d . . . . .
O5 O 0.1110(8) 0.5994(5) 0.2727(7) 0.043(2) Uani 1 1 d . . . . .
O6 O 0.2945(8) 0.4966(5) 0.2815(6) 0.038(2) Uani 1 1 d . . . . .
O7 O 0.4843(8) 0.4563(5) 0.3232(6) 0.036(2) Uani 1 1 d . . . . .
O8 O 0.4634(7) 0.6095(5) 0.3405(6) 0.032(2) Uani 1 1 d . . . . .
O9 O 0.6209(8) 0.5764(5) 0.2880(7) 0.045(2) Uani 1 1 d D U . . .
Cl1 Cl 0.3192(3) 0.37453(18) 0.4831(2) 0.0379(7) Uani 1 1 d . . . . .
Cl2 Cl 0.2955(3) 0.70409(17) 0.4431(3) 0.0398(8) Uani 1 1 d . . . . .
Hf1 Hf 0.42668(4) 0.47063(3) 0.57651(4) 0.02985(18) Uani 1 1 d . . . . .
Hf2 Hf 0.29019(4) 0.59002(3) 0.36122(4) 0.03061(18) Uani 1 1 d . . . . .
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'
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'
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
O3 C1 O2 120.9(11) . .
O3 C1 N1 122.2(11) . .
O2 C1 N1 116.8(12) . .
C3 C2 N1 107(2) . .
C3 C2 H2A 110.4 . .
N1 C2 H2A 110.4 . .
C3 C2 H2B 110.4 . .
N1 C2 H2B 110.4 . .
H2A C2 H2B 108.6 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 C5 112.9(13) . .
N1 C4 H4A 109.0 . .
C5 C4 H4A 109.0 . .
N1 C4 H4B 109.0 . .
C5 C4 H4B 109.0 . .
H4A C4 H4B 107.8 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O5 C6 O4 117.2(12) . .
O5 C6 N2 123.8(12) . .
O4 C6 N2 118.8(13) . .
O5 C6 Hf2 58.5(7) . .
O4 C6 Hf2 58.9(7) . .
N2 C6 Hf2 177.7(11) . .
N2 C7 C8 116(2) . .
N2 C7 H7A 108.3 . .
C8 C7 H7A 108.3 . .
N2 C7 H7B 108.3 . .
C8 C7 H7B 108.3 . .
H7A C7 H7B 107.4 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N2 C9 C10 112.9(16) . .
N2 C9 H9A 109.0 . .
C10 C9 H9A 109.0 . .
N2 C9 H9B 109.0 . .
C10 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O7 C11 O6 124.1(13) . .
O7 C11 N3 117.4(12) . .
O6 C11 N3 118.5(13) . .
N3 C12 C13 109.9(14) . .
N3 C12 H12A 109.7 . .
C13 C12 H12A 109.7 . .
N3 C12 H12B 109.7 . .
C13 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
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 . .
C15 C14 N3 108.9(18) . .
C15 C14 H14A 109.9 . .
N3 C14 H14A 109.9 . .
C15 C14 H14B 109.9 . .
N3 C14 H14B 109.9 . .
H14A C14 H14B 108.3 . .
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 . .
O8 C16 O9 103.7(10) . .
O8 C16 C17A 123(2) . .
O9 C16 C17A 111.3(17) . .
O8 C16 C17B 110.8(18) . .
O9 C16 C17B 102.4(17) . .
O8 C16 Hf1 48.2(5) . 3_666
O9 C16 Hf1 55.7(6) . 3_666
C17A C16 Hf1 142.0(17) . 3_666
C17B C16 Hf1 121.7(16) . 3_666
O8 C16 H16 105.8 . .
O9 C16 H16 105.8 . .
C17A C16 H16 105.8 . .
Hf1 C16 H16 112.1 3_666 .
O8 C16 H16' 113.0 . .
O9 C16 H16' 113.0 . .
C17B C16 H16' 113.0 . .
Hf1 C16 H16' 125.3 3_666 .
C16 C17A C18A 102(2) . .
C16 C17A H17C 111.3 . .
C18A C17A H17C 111.3 . .
C16 C17A H17D 111.3 . .
C18A C17A H17D 111.3 . .
H17C C17A H17D 109.2 . .
C19 C18A C17A 105(2) . .
C19 C18A H18C 110.7 . .
C17A C18A H18C 110.7 . .
C19 C18A H18D 110.7 . .
C17A C18A H18D 110.7 . .
H18C C18A H18D 108.8 . .
C16 C17B C18B 104(2) . .
C16 C17B H17A 111.0 . .
C18B C17B H17A 111.0 . .
C16 C17B H17B 111.0 . .
C18B C17B H17B 111.0 . .
H17A C17B H17B 109.0 . .
C19 C18B C17B 94(2) . .
C19 C18B H18A 113.0 . .
C17B C18B H18A 113.0 . .
C19 C18B H18B 113.0 . .
C17B C18B H18B 113.0 . .
H18A C18B H18B 110.4 . .
O9 C19 C18A 107.0(17) . .
O9 C19 C18B 109.4(18) . .
O9 C19 H19A 110.3 . .
C18A C19 H19A 110.3 . .
O9 C19 H19B 110.3 . .
C18A C19 H19B 110.3 . .
H19A C19 H19B 108.6 . .
O9 C19 H19C 109.8 . .
C18B C19 H19C 109.8 . .
O9 C19 H19D 109.8 . .
C18B C19 H19D 109.8 . .
H19C C19 H19D 108.2 . .
C1 N1 C4 120.3(12) . .
C1 N1 C2 120.9(13) . .
C4 N1 C2 118.1(13) . .
C6 N2 C7 117.3(13) . .
C6 N2 C9 121.9(12) . .
C7 N2 C9 120.7(13) . .
C11 N3 C12 120.6(13) . .
C11 N3 C14 122.4(13) . .
C12 N3 C14 116.5(13) . .
Hf1 O1 Hf2 142.2(4) . .
Hf1 O1 Hf1 105.2(3) . 3_666
Hf2 O1 Hf1 110.1(4) . 3_666
C1 O2 Hf1 135.3(8) . .
C1 O3 Hf2 138.6(9) . .
C6 O4 Hf2 90.1(8) . .
C6 O5 Hf2 92.8(8) . .
C11 O6 Hf2 133.0(9) . .
C11 O7 Hf1 133.0(9) . 3_666
C16 O8 Hf2 137.1(8) . .
C16 O8 Hf1 103.5(7) . 3_666
Hf2 O8 Hf1 105.0(3) . 3_666
C16 O9 C19 107.4(10) . .
C16 O9 Hf1 93.5(7) . 3_666
C19 O9 Hf1 130.6(10) . 3_666
O1 Hf1 O1 74.8(3) . 3_666
O1 Hf1 O7 94.8(3) . 3_666
O1 Hf1 O7 85.4(3) 3_666 3_666
O1 Hf1 O2 83.5(3) . .
O1 Hf1 O2 156.9(3) 3_666 .
O7 Hf1 O2 88.5(4) 3_666 .
O1 Hf1 O8 144.2(3) . 3_666
O1 Hf1 O8 69.6(3) 3_666 3_666
O7 Hf1 O8 86.0(3) 3_666 3_666
O2 Hf1 O8 132.3(3) . 3_666
O1 Hf1 O9 156.4(3) . 3_666
O1 Hf1 O9 127.3(3) 3_666 3_666
O7 Hf1 O9 80.4(3) 3_666 3_666
O2 Hf1 O9 73.3(3) . 3_666
O8 Hf1 O9 59.0(3) 3_666 3_666
O1 Hf1 Cl1 94.6(2) . .
O1 Hf1 Cl1 99.1(2) 3_666 .
O7 Hf1 Cl1 170.4(3) 3_666 .
O2 Hf1 Cl1 90.5(3) . .
O8 Hf1 Cl1 87.6(3) 3_666 .
O9 Hf1 Cl1 90.1(3) 3_666 .
O1 Hf1 C16 171.0(3) . 3_666
O1 Hf1 C16 96.9(3) 3_666 3_666
O7 Hf1 C16 80.6(4) 3_666 3_666
O2 Hf1 C16 104.1(4) . 3_666
O8 Hf1 C16 28.4(3) 3_666 3_666
O9 Hf1 C16 30.8(3) 3_666 3_666
Cl1 Hf1 C16 90.4(4) . 3_666
O1 Hf1 Hf1 37.8(2) . 3_666
O1 Hf1 Hf1 37.0(2) 3_666 3_666
O7 Hf1 Hf1 90.1(2) 3_666 3_666
O2 Hf1 Hf1 120.9(2) . 3_666
O8 Hf1 Hf1 106.5(2) 3_666 3_666
O9 Hf1 Hf1 162.9(2) 3_666 3_666
Cl1 Hf1 Hf1 98.64(8) . 3_666
C16 Hf1 Hf1 133.8(3) 3_666 3_666
O1 Hf1 Hf2 108.7(2) . 3_666
O1 Hf1 Hf2 34.8(2) 3_666 3_666
O7 Hf1 Hf2 74.8(2) 3_666 3_666
O2 Hf1 Hf2 159.9(3) . 3_666
O8 Hf1 Hf2 37.2(2) 3_666 3_666
O9 Hf1 Hf2 92.5(2) 3_666 3_666
Cl1 Hf1 Hf2 104.11(8) . 3_666
C16 Hf1 Hf2 62.7(3) 3_666 3_666
Hf1 Hf1 Hf2 71.184(19) 3_666 3_666
O1 Hf2 O3 81.1(3) . .
O1 Hf2 O6 85.0(3) . .
O3 Hf2 O6 98.0(4) . .
O1 Hf2 O8 70.5(3) . .
O3 Hf2 O8 150.9(3) . .
O6 Hf2 O8 85.8(4) . .
O1 Hf2 O5 150.8(3) . .
O3 Hf2 O5 74.3(3) . .
O6 Hf2 O5 83.1(4) . .
O8 Hf2 O5 134.7(3) . .
O1 Hf2 O4 145.7(3) . .
O3 Hf2 O4 133.1(3) . .
O6 Hf2 O4 86.2(3) . .
O8 Hf2 O4 75.9(3) . .
O5 Hf2 O4 59.7(3) . .
O1 Hf2 Cl2 96.8(2) . .
O3 Hf2 Cl2 87.6(3) . .
O6 Hf2 Cl2 174.4(3) . .
O8 Hf2 Cl2 89.8(3) . .
O5 Hf2 Cl2 97.6(3) . .
O4 Hf2 Cl2 89.4(3) . .
O1 Hf2 C6 167.3(4) . .
O3 Hf2 C6 102.9(4) . .
O6 Hf2 C6 82.6(4) . .
O8 Hf2 C6 106.2(4) . .
O5 Hf2 C6 28.7(4) . .
O4 Hf2 C6 31.0(4) . .
Cl2 Hf2 C6 95.4(3) . .
O1 Hf2 Hf1 35.1(2) . 3_666
O3 Hf2 Hf1 115.5(2) . 3_666
O6 Hf2 Hf1 74.2(2) . 3_666
O8 Hf2 Hf1 37.8(2) . 3_666
O5 Hf2 Hf1 156.2(3) . 3_666
O4 Hf2 Hf1 110.7(2) . 3_666
Cl2 Hf2 Hf1 104.26(8) . 3_666
C6 Hf2 Hf1 137.2(3) . 3_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O3 1.263(15) .
C1 O2 1.290(15) .
C1 N1 1.310(16) .
C2 C3 1.39(3) .
C2 N1 1.50(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 N1 1.463(17) .
C4 C5 1.49(2) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 O5 1.238(17) .
C6 O4 1.324(15) .
C6 N2 1.358(18) .
C6 Hf2 2.571(14) .
C7 N2 1.45(2) .
C7 C8 1.50(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 N2 1.47(2) .
C9 C10 1.49(3) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 O7 1.280(16) .
C11 O6 1.298(15) .
C11 N3 1.320(18) .
C12 N3 1.469(19) .
C12 C13 1.51(2) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.40(3) .
C14 N3 1.51(2) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 O8 1.377(16) .
C16 O9 1.445(13) .
C16 C17A 1.489(18) .
C16 C17B 1.543(19) .
C16 Hf1 2.819(14) 3_666
C16 H16 1.0000 .
C16 H16' 1.0000 .
C17A C18A 1.527(19) .
C17A H17C 0.9900 .
C17A H17D 0.9900 .
C18A C19 1.518(18) .
C18A H18C 0.9900 .
C18A H18D 0.9900 .
C17B C18B 1.546(19) .
C17B H17A 0.9900 .
C17B H17B 0.9900 .
C18B C19 1.531(18) .
C18B H18A 0.9900 .
C18B H18B 0.9900 .
C19 O9 1.452(13) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C19 H19C 0.9900 .
C19 H19D 0.9900 .
O1 Hf1 2.044(8) .
O1 Hf2 2.067(7) .
O1 Hf1 2.084(8) 3_666
O2 Hf1 2.114(8) .
O3 Hf2 2.077(8) .
O4 Hf2 2.202(8) .
O5 Hf2 2.194(9) .
O6 Hf2 2.110(9) .
O7 Hf1 2.099(9) 3_666
O8 Hf2 2.129(8) .
O8 Hf1 2.160(8) 3_666
O9 Hf1 2.334(9) 3_666
Cl1 Hf1 2.430(3) .
Cl2 Hf2 2.446(3) .
Hf1 O1 2.084(8) 3_666
Hf1 O7 2.099(9) 3_666
Hf1 O8 2.160(8) 3_666
Hf1 O9 2.334(9) 3_666
Hf1 C16 2.819(14) 3_666
Hf1 Hf1 3.2782(10) 3_666
Hf1 Hf2 3.4018(8) 3_666
Hf2 Hf1 3.4019(8) 3_666
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_4
O8 C16 C17A C18A 105(3) . .
O9 C16 C17A C18A -19(3) . .
Hf1 C16 C17A C18A 42(5) 3_666 .
C16 C17A C18A C19 26(4) . .
O8 C16 C17B C18B 150(2) . .
O9 C16 C17B C18B 40(3) . .
Hf1 C16 C17B C18B 98(2) 3_666 .
C16 C17B C18B C19 -46(3) . .
C17A C18A C19 O9 -24(3) . .
C17B C18B C19 O9 39(3) . .
O3 C1 N1 C4 1(2) . .
O2 C1 N1 C4 177.9(13) . .
O3 C1 N1 C2 171.3(16) . .
O2 C1 N1 C2 -12(2) . .
C5 C4 N1 C1 -105.3(17) . .
C5 C4 N1 C2 84(2) . .
C3 C2 N1 C1 82(2) . .
C3 C2 N1 C4 -107.7(18) . .
O5 C6 N2 C7 -5(2) . .
O4 C6 N2 C7 -180.0(16) . .
O5 C6 N2 C9 178.0(15) . .
O4 C6 N2 C9 3(2) . .
C8 C7 N2 C6 -75(2) . .
C8 C7 N2 C9 103(2) . .
C10 C9 N2 C6 85(2) . .
C10 C9 N2 C7 -92(2) . .
O7 C11 N3 C12 -174.1(13) . .
O6 C11 N3 C12 4(2) . .
O7 C11 N3 C14 14(2) . .
O6 C11 N3 C14 -167.4(15) . .
C13 C12 N3 C11 -93.1(18) . .
C13 C12 N3 C14 79.2(18) . .
C15 C14 N3 C11 -91(2) . .
C15 C14 N3 C12 97(2) . .
O3 C1 O2 Hf1 -3(2) . .
N1 C1 O2 Hf1 180.0(10) . .
O2 C1 O3 Hf2 -48(2) . .
N1 C1 O3 Hf2 128.7(13) . .
O5 C6 O4 Hf2 4.0(12) . .
N2 C6 O4 Hf2 179.7(12) . .
O4 C6 O5 Hf2 -4.1(12) . .
N2 C6 O5 Hf2 -179.5(13) . .
O7 C11 O6 Hf2 -12(2) . .
N3 C11 O6 Hf2 169.5(10) . .
O6 C11 O7 Hf1 12(2) . 3_666
N3 C11 O7 Hf1 -169.3(10) . 3_666
O9 C16 O8 Hf2 -135.7(9) . .
C17A C16 O8 Hf2 97(2) . .
C17B C16 O8 Hf2 115.1(19) . .
Hf1 C16 O8 Hf2 -130.4(13) 3_666 .
O9 C16 O8 Hf1 -5.3(12) . 3_666
C17A C16 O8 Hf1 -132.7(18) . 3_666
C17B C16 O8 Hf1 -114.5(17) . 3_666
O8 C16 O9 C19 -129.9(13) . .
C17A C16 O9 C19 5(2) . .
C17B C16 O9 C19 -15(2) . .
Hf1 C16 O9 C19 -134.6(12) 3_666 .
O8 C16 O9 Hf1 4.8(11) . 3_666
C17A C16 O9 Hf1 139(2) . 3_666
C17B C16 O9 Hf1 120.1(16) . 3_666
C18A C19 O9 C16 12(2) . .
C18B C19 O9 C16 -17(2) . .
C18A C19 O9 Hf1 -98(2) . 3_666
C18B C19 O9 Hf1 -127.2(19) . 3_666
