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#$Date: 2019-11-24 12:59:58 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/90/4089071.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_4089071
loop_
_publ_author_name
'Adler, Christian'
'Frerichs, Nils'
'Schmidtmann, Marc'
'Beckhaus, Rüdiger'
_publ_section_title
;
 Zwitterionic d0Metal Complexes [(Cy2N)3M]+[(μ-Me)B(C6F5)3]−(M =
 Ti, Zr, Hf) Derived from Tris(dicyclohexylamido)methyl Metal Precursors
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3728
_journal_paper_doi               10.1021/acs.organomet.6b00688
_journal_volume                  35
_journal_year                    2016
_chemical_formula_structural     '[Hf(N(C6H11)2)3] [B(CH3)(C6F5)3] *1.5C6H14'
_chemical_formula_sum            'C64 H90 B F15 Hf N3'
_chemical_formula_weight         1375.68
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.1878(6)
_cell_length_b                   19.1878(6)
_cell_length_c                   29.1550(12)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      2.55
_cell_volume                     9296.0(6)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            140003
_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         33.722
_diffrn_reflns_theta_min         1.410
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             4242
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.834
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         8241
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0356
_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)+(0.0300P)²+30.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6567
_reflns_number_total             8241
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00688_si_002.cif
_cod_data_source_block           '[(Cy2N)3Hf][MeB(C6F5)3_(3-Hf)'
_cod_original_cell_volume        9296.0(7)
_cod_database_code               4089071
_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   0.765
_shelx_estimated_absorpt_t_max   0.790
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.3333 0.6667 0.41522(2) 0.01583(4) Uani 1 3 d S T P . .
F1 F 0.39109(9) 0.58338(9) 0.62722(5) 0.0277(3) Uani 1 1 d . . . . .
F2 F 0.53946(9) 0.63711(10) 0.65392(5) 0.0299(3) Uani 1 1 d . . . . .
F3 F 0.66203(9) 0.77899(10) 0.62182(6) 0.0337(3) Uani 1 1 d . . . . .
F4 F 0.62923(9) 0.86428(9) 0.55908(6) 0.0360(4) Uani 1 1 d . . . . .
F5 F 0.47913(8) 0.81287(8) 0.53178(5) 0.0258(3) Uani 1 1 d . . . . .
N1 N 0.44583(11) 0.70141(11) 0.39406(6) 0.0211(3) Uani 1 1 d . . . . .
C1 C 0.47280(12) 0.65190(13) 0.41933(7) 0.0201(4) Uani 1 1 d . . . . .
H1 H 0.4235 0.6082 0.4344 0.024 Uiso 1 1 calc R U . . .
C2 C 0.50587(15) 0.60878(15) 0.38955(8) 0.0271(5) Uani 1 1 d . . . . .
H2A H 0.4672 0.5788 0.3647 0.033 Uiso 1 1 calc R U . . .
H2B H 0.5572 0.6491 0.3753 0.033 Uiso 1 1 calc R U . . .
C3 C 0.51987(18) 0.55010(17) 0.41870(10) 0.0352(6) Uani 1 1 d . . . . .
H3A H 0.4675 0.5065 0.4301 0.042 Uiso 1 1 calc R U . . .
H3B H 0.5441 0.5254 0.3993 0.042 Uiso 1 1 calc R U . . .
C4 C 0.57493(18) 0.59201(19) 0.45925(10) 0.0362(6) Uani 1 1 d . . . . .
H4A H 0.6297 0.6301 0.4479 0.043 Uiso 1 1 calc R U . . .
H4B H 0.5783 0.5515 0.4787 0.043 Uiso 1 1 calc R U . . .
C5 C 0.54440(17) 0.63767(18) 0.48802(9) 0.0330(5) Uani 1 1 d . . . . .
H5A H 0.5837 0.6677 0.5126 0.040 Uiso 1 1 calc R U . . .
H5B H 0.4927 0.5989 0.5026 0.040 Uiso 1 1 calc R U . . .
C6 C 0.53232(14) 0.69634(15) 0.45839(8) 0.0260(4) Uani 1 1 d . . . . .
H6A H 0.5847 0.7372 0.4453 0.031 Uiso 1 1 calc R U . . .
H6B H 0.5116 0.7246 0.4776 0.031 Uiso 1 1 calc R U . . .
C7 C 0.50862(18) 0.76465(17) 0.36484(10) 0.0367(6) Uani 1 1 d . . . . .
H7 H 0.5492 0.7477 0.3585 0.044 Uiso 1 1 calc R U . . .
C8 C 0.55334(17) 0.84610(17) 0.38784(13) 0.0443(8) Uani 1 1 d . . . . .
H8A H 0.5814 0.8420 0.4153 0.053 Uiso 1 1 calc R U . . .
H8B H 0.5141 0.8621 0.3981 0.053 Uiso 1 1 calc R U . . .
C9 C 0.6151(2) 0.9113(2) 0.35592(17) 0.0651(13) Uani 1 1 d . . . . .
H9A H 0.6387 0.9640 0.3716 0.078 Uiso 1 1 calc R U . . .
H9B H 0.6591 0.8998 0.3497 0.078 Uiso 1 1 calc R U . . .
C10 C 0.5799(2) 0.9163(2) 0.31204(16) 0.0665(13) Uani 1 1 d . . . . .
H10A H 0.6229 0.9562 0.2919 0.080 Uiso 1 1 calc R U . . .
H10B H 0.5408 0.9348 0.3177 0.080 Uiso 1 1 calc R U . . .
C11 C 0.5376(3) 0.8351(3) 0.28815(14) 0.0754(15) Uani 1 1 d . . . . .
H11A H 0.5780 0.8201 0.2788 0.090 Uiso 1 1 calc R U . . .
H11B H 0.5108 0.8391 0.2601 0.090 Uiso 1 1 calc R U . . .
C12 C 0.4748(2) 0.7692(2) 0.31949(11) 0.0508(8) Uani 1 1 d . . . . .
H12A H 0.4299 0.7798 0.3246 0.061 Uiso 1 1 calc R U . . .
H12B H 0.4526 0.7165 0.3038 0.061 Uiso 1 1 calc R U . . .
C13 C 0.42535(12) 0.69332(13) 0.57627(7) 0.0181(3) Uani 1 1 d . . . . .
C14 C 0.49136(13) 0.76499(13) 0.56118(7) 0.0206(4) Uani 1 1 d . . . . .
C15 C 0.56962(14) 0.79402(14) 0.57505(8) 0.0236(4) Uani 1 1 d . . . . .
C16 C 0.58665(13) 0.75092(15) 0.60671(8) 0.0241(4) Uani 1 1 d . . . . .
C17 C 0.52476(14) 0.67952(14) 0.62260(7) 0.0225(4) Uani 1 1 d . . . . .
C18 C 0.44697(13) 0.65263(13) 0.60758(7) 0.0196(4) Uani 1 1 d . . . . .
C19 C 0.3333 0.6667 0.50104(11) 0.0175(6) Uani 1 3 d S T P . .
H19 H 0.3536(19) 0.6335(19) 0.4913(10) 0.031(8) Uiso 1 1 d . . . . .
B1 B 0.3333 0.6667 0.55943(13) 0.0170(7) Uani 1 3 d S T P . .
C20 C 0.8029(12) 1.0149(11) 0.4582(6) 0.131(6) Uani 0.5 1 d . U P A -1
H20A H 0.8376 1.0649 0.4748 0.197 Uiso 0.5 1 calc R U P A -1
H20B H 0.7527 1.0132 0.4496 0.197 Uiso 0.5 1 calc R U P A -1
H20C H 0.8306 1.0128 0.4304 0.197 Uiso 0.5 1 calc R U P A -1
C21 C 0.7857(10) 0.9489(8) 0.4862(4) 0.107(4) Uani 0.5 1 d . U P A -1
H21A H 0.7626 0.9558 0.5150 0.128 Uiso 0.5 1 calc R U P A -1
H21B H 0.7425 0.9005 0.4708 0.128 Uiso 0.5 1 calc R U P A -1
C22 C 0.8458(9) 0.9314(9) 0.4984(5) 0.111(4) Uani 0.5 1 d . U P A -1
H22A H 0.8906 0.9810 0.5119 0.133 Uiso 0.5 1 calc R U P A -1
H22B H 0.8664 0.9208 0.4697 0.133 Uiso 0.5 1 calc R U P A -1
C23 C 0.8280(8) 0.8619(7) 0.5316(5) 0.098(4) Uani 0.5 1 d . U P A -1
H23A H 0.8784 0.8613 0.5379 0.117 Uiso 0.5 1 calc R U P A -1
H23B H 0.8080 0.8710 0.5610 0.117 Uiso 0.5 1 calc R U P A -1
C24 C 0.7660(6) 0.7814(6) 0.5120(3) 0.065(2) Uani 0.5 1 d . U P A -1
H24A H 0.7134 0.7792 0.5098 0.078 Uiso 0.5 1 calc R U P A -1
H24B H 0.7823 0.7757 0.4807 0.078 Uiso 0.5 1 calc R U P A -1
C25 C 0.7575(6) 0.7149(7) 0.5405(3) 0.074(2) Uani 0.5 1 d . U P A -1
H25A H 0.8104 0.7200 0.5451 0.111 Uiso 0.5 1 calc R U P A -1
H25B H 0.7217 0.6637 0.5252 0.111 Uiso 0.5 1 calc R U P A -1
H25C H 0.7346 0.7165 0.5703 0.111 Uiso 0.5 1 calc R U P A -1
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N1 Hf1 N1 111.03(5) 2_665 .
N1 Hf1 N1 111.03(5) 2_665 3_565
N1 Hf1 N1 111.03(5) . 3_565
N1 Hf1 C19 107.86(5) 2_665 .
N1 Hf1 C19 107.86(5) . .
N1 Hf1 C19 107.86(5) 3_565 .
C7 N1 C1 114.16(19) . .
C7 N1 Hf1 138.37(17) . .
C1 N1 Hf1 107.18(13) . .
N1 C1 C6 114.42(18) . .
N1 C1 C2 115.68(18) . .
C6 C1 C2 108.98(18) . .
N1 C1 H1 105.6 . .
C6 C1 H1 105.6 . .
C2 C1 H1 105.6 . .
C3 C2 C1 110.6(2) . .
C3 C2 H2A 109.5 . .
C1 C2 H2A 109.5 . .
C3 C2 H2B 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
C4 C3 C2 111.8(2) . .
C4 C3 H3A 109.2 . .
C2 C3 H3A 109.2 . .
C4 C3 H3B 109.2 . .
C2 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
C3 C4 C5 111.5(2) . .
C3 C4 H4A 109.3 . .
C5 C4 H4A 109.3 . .
C3 C4 H4B 109.3 . .
C5 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
C4 C5 C6 110.9(2) . .
C4 C5 H5A 109.5 . .
C6 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
C6 C5 H5B 109.5 . .
H5A C5 H5B 108.1 . .
C5 C6 C1 110.8(2) . .
C5 C6 H6A 109.5 . .
C1 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
C1 C6 H6B 109.5 . .
H6A C6 H6B 108.1 . .
N1 C7 C12 111.0(3) . .
N1 C7 C8 113.6(2) . .
C12 C7 C8 111.8(3) . .
N1 C7 H7 106.7 . .
C12 C7 H7 106.7 . .
C8 C7 H7 106.7 . .
C7 C8 C9 112.4(3) . .
C7 C8 H8A 109.1 . .
C9 C8 H8A 109.1 . .
C7 C8 H8B 109.1 . .
C9 C8 H8B 109.1 . .
H8A C8 H8B 107.9 . .
C10 C9 C8 112.8(3) . .
C10 C9 H9A 109.0 . .
C8 C9 H9A 109.0 . .
C10 C9 H9B 109.0 . .
C8 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
C9 C10 C11 111.0(3) . .
C9 C10 H10A 109.4 . .
C11 C10 H10A 109.4 . .
C9 C10 H10B 109.4 . .
C11 C10 H10B 109.4 . .
H10A C10 H10B 108.0 . .
C10 C11 C12 111.6(3) . .
C10 C11 H11A 109.3 . .
C12 C11 H11A 109.3 . .
C10 C11 H11B 109.3 . .
C12 C11 H11B 109.3 . .
H11A C11 H11B 108.0 . .
C7 C12 C11 112.8(3) . .
C7 C12 H12A 109.0 . .
C11 C12 H12A 109.0 . .
C7 C12 H12B 109.0 . .
C11 C12 H12B 109.0 . .
H12A C12 H12B 107.8 . .
C18 C13 C14 112.40(19) . .
C18 C13 B1 126.47(19) . .
C14 C13 B1 121.04(18) . .
F5 C14 C15 115.71(19) . .
F5 C14 C13 119.09(19) . .
C15 C14 C13 125.2(2) . .
F4 C15 C14 121.0(2) . .
F4 C15 C16 119.7(2) . .
C14 C15 C16 119.4(2) . .
F3 C16 C17 120.8(2) . .
F3 C16 C15 120.6(2) . .
C17 C16 C15 118.6(2) . .
F2 C17 C16 119.8(2) . .
F2 C17 C18 120.2(2) . .
C16 C17 C18 120.0(2) . .
F1 C18 C17 114.26(18) . .
F1 C18 C13 121.19(19) . .
C17 C18 C13 124.5(2) . .
B1 C19 Hf1 180.0 . .
B1 C19 H19 107.5(18) . .
Hf1 C19 H19 72.5(18) . .
C13 B1 C13 111.53(13) 2_665 .
C13 B1 C13 111.53(13) 2_665 3_565
C13 B1 C13 111.53(13) . 3_565
C13 B1 C19 107.33(14) 2_665 .
C13 B1 C19 107.33(14) . .
C13 B1 C19 107.33(14) 3_565 .
C21 C20 H20A 109.5 . .
C21 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C21 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C22 C21 C20 121.0(16) . .
C22 C21 H21A 107.1 . .
C20 C21 H21A 107.1 . .
C22 C21 H21B 107.1 . .
C20 C21 H21B 107.1 . .
H21A C21 H21B 106.8 . .
C21 C22 C23 120.9(14) . .
C21 C22 H22A 107.1 . .
C23 C22 H22A 107.1 . .
C21 C22 H22B 107.1 . .
C23 C22 H22B 107.1 . .
H22A C22 H22B 106.8 . .
C24 C23 C22 111.6(11) . .
C24 C23 H23A 109.3 . .
C22 C23 H23A 109.3 . .
C24 C23 H23B 109.3 . .
C22 C23 H23B 109.3 . .
H23A C23 H23B 108.0 . .
C25 C24 C23 111.4(9) . .
C25 C24 H24A 109.4 . .
C23 C24 H24A 109.4 . .
C25 C24 H24B 109.4 . .
C23 C24 H24B 109.4 . .
H24A C24 H24B 108.0 . .
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 N1 2.0114(18) 2_665
Hf1 N1 2.0114(18) .
Hf1 N1 2.0114(19) 3_565
Hf1 C19 2.502(3) .
F1 C18 1.349(3) .
F2 C17 1.343(3) .
F3 C16 1.341(3) .
F4 C15 1.342(3) .
F5 C14 1.360(2) .
N1 C7 1.479(3) .
N1 C1 1.485(3) .
C1 C6 1.534(3) .
C1 C2 1.538(3) .
C1 H1 1.0000 .
C2 C3 1.538(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.520(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.526(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.526(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C12 1.495(5) .
C7 C8 1.512(4) .
C7 H7 1.0000 .
C8 C9 1.534(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.472(6) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.518(7) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.538(5) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C18 1.393(3) .
C13 C14 1.395(3) .
C13 B1 1.648(2) .
C14 C15 1.375(3) .
C15 C16 1.383(3) .
C16 C17 1.369(3) .
C17 C18 1.384(3) .
C19 B1 1.702(5) .
C19 H19 0.94(3) .
B1 C13 1.648(2) 2_665
B1 C13 1.648(2) 3_565
C20 C21 1.401(18) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 C22 1.400(18) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C23 1.540(19) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.514(14) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C25 1.462(14) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
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_4
C7 N1 C1 C6 70.9(2) .
Hf1 N1 C1 C6 -104.08(17) .
C7 N1 C1 C2 -57.1(3) .
Hf1 N1 C1 C2 127.98(17) .
N1 C1 C2 C3 -171.6(2) .
C6 C1 C2 C3 57.8(3) .
C1 C2 C3 C4 -55.7(3) .
C2 C3 C4 C5 53.7(3) .
C3 C4 C5 C6 -54.7(3) .
C4 C5 C6 C1 58.1(3) .
N1 C1 C6 C5 169.24(19) .
C2 C1 C6 C5 -59.5(3) .
C1 N1 C7 C12 137.7(2) .
Hf1 N1 C7 C12 -49.6(4) .
C1 N1 C7 C8 -95.3(3) .
Hf1 N1 C7 C8 77.4(3) .
N1 C7 C8 C9 -177.1(2) .
C12 C7 C8 C9 -50.6(4) .
C7 C8 C9 C10 53.4(4) .
C8 C9 C10 C11 -54.8(4) .
C9 C10 C11 C12 54.4(5) .
N1 C7 C12 C11 179.1(3) .
C8 C7 C12 C11 51.1(4) .
C10 C11 C12 C7 -53.2(5) .
C18 C13 C14 F5 -177.50(18) .
B1 C13 C14 F5 -0.6(3) .
C18 C13 C14 C15 -0.2(3) .
B1 C13 C14 C15 176.7(2) .
F5 C14 C15 F4 -1.7(3) .
C13 C14 C15 F4 -179.1(2) .
F5 C14 C15 C16 176.8(2) .
C13 C14 C15 C16 -0.6(4) .
F4 C15 C16 F3 0.5(3) .
C14 C15 C16 F3 -178.1(2) .
F4 C15 C16 C17 179.8(2) .
C14 C15 C16 C17 1.3(3) .
F3 C16 C17 F2 0.4(3) .
C15 C16 C17 F2 -178.9(2) .
F3 C16 C17 C18 178.2(2) .
C15 C16 C17 C18 -1.1(3) .
F2 C17 C18 F1 0.5(3) .
C16 C17 C18 F1 -177.3(2) .
F2 C17 C18 C13 178.14(19) .
C16 C17 C18 C13 0.4(3) .
C14 C13 C18 F1 177.79(19) .
B1 C13 C18 F1 1.1(3) .
C14 C13 C18 C17 0.3(3) .
B1 C13 C18 C17 -176.4(2) .
C18 C13 B1 C13 114.15(16) 2_665
C14 C13 B1 C13 -62.3(3) 2_665
C18 C13 B1 C13 -11.3(3) 3_565
C14 C13 B1 C13 172.32(18) 3_565
C18 C13 B1 C19 -128.57(19) .
C14 C13 B1 C19 55.03(19) .
C20 C21 C22 C23 176.2(14) .
C21 C22 C23 C24 63.0(17) .
C22 C23 C24 C25 172.1(11) .
