#------------------------------------------------------------------------------
#$Date: 2025-10-30 01:13:42 +0200 (Thu, 30 Oct 2025) $
#$Revision: 303093 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/61/1576114.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_1576114
loop_
_publ_author_name
'Hansen, Hannah M.'
'Zgrabik, Joshua C.'
'Zacher, Peter A.'
'Schuely, Jacob J.'
'Amano, Emily M.'
'Yang, Mai Yer'
'Unruh, Daniel K.'
'Zuin, Lucia'
'Keith, Jason M.'
'Daly, Scott R.'
_publ_section_title
;
 Direct measurement of covalent three-center, two-electron M--H--B bonding
 in Zr and Hf borohydrides using B K-edge XAS
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC06254C
_journal_year                    2025
_chemical_formula_moiety         'C56 H48 B4 Hf, C7 H8'
_chemical_formula_sum            'C63 H56 B4 Hf'
_chemical_formula_weight         1034.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-06-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2025-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                111.6040(10)
_cell_angle_beta                 91.319(2)
_cell_angle_gamma                106.821(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4273(6)
_cell_length_b                   14.7865(6)
_cell_length_c                   16.3784(8)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.319
_cell_measurement_theta_min      2.151
_cell_volume                     2436.7(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87295
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         1.882
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0956 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.8705.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_preparation       'Salt metathesis'
_exptl_crystal_recrystallization_method
'Concentrated toluene solution, vapor diffused with pentane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.174
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         12158
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0263
_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)+(0.0189P)²+3.2540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11099
_reflns_number_total             12158
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc06254c3.cif
_cod_data_source_block           dal24_09
_cod_database_code               1576114
_shelx_shelxl_version_number     2019/3
_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_max   0.703
_shelx_estimated_absorpt_t_min   0.476
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 H3-H1C
 3 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36),
 C38(H38), C39(H39), C40(H40), C41(H41), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C59(H59), C60(H60),
 C61(H61), C62(H62), C63(H63)
3.b Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), C57(H57A,
 H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.59316(2) 0.69746(2) 0.33176(2) 0.01780(3) Uani 1 1 d . . . . .
C1 C 0.4635(3) 0.4643(2) 0.10696(17) 0.0256(5) Uani 1 1 d . . . . .
C2 C 0.3385(3) 0.4094(2) 0.06750(17) 0.0268(5) Uani 1 1 d . . . . .
C3 C 0.2385(3) 0.4395(2) 0.10643(18) 0.0299(6) Uani 1 1 d . . . . .
H3 H 0.255973 0.498893 0.159946 0.036 Uiso 1 1 calc DR U . . .
C4 C 0.1175(3) 0.3852(2) 0.0689(2) 0.0374(7) Uani 1 1 d . . . . .
H4 H 0.052968 0.407600 0.096249 0.045 Uiso 1 1 calc R U . . .
C5 C 0.0889(3) 0.2964(3) -0.0102(2) 0.0412(7) Uani 1 1 d . . . . .
H5 H 0.005102 0.258520 -0.035427 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1806(3) 0.2649(2) -0.0504(2) 0.0387(7) Uani 1 1 d . . . . .
H6 H 0.159899 0.204977 -0.103692 0.046 Uiso 1 1 calc R U . . .
C7 C 0.3082(3) 0.3201(2) -0.01419(18) 0.0312(6) Uani 1 1 d . . . . .
C8 C 0.4029(3) 0.2882(2) -0.05525(18) 0.0332(6) Uani 1 1 d . . . . .
H8 H 0.382412 0.228317 -0.108541 0.040 Uiso 1 1 calc R U . . .
C9 C 0.5265(3) 0.3418(2) -0.02027(18) 0.0306(6) Uani 1 1 d . . . . .
C10 C 0.6233(3) 0.3100(2) -0.0636(2) 0.0384(7) Uani 1 1 d . . . . .
H10 H 0.603072 0.250537 -0.117283 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7439(3) 0.3633(3) -0.0293(2) 0.0407(7) Uani 1 1 d . . . . .
H11 H 0.807018 0.341507 -0.059472 0.049 Uiso 1 1 calc R U . . .
C12 C 0.7759(3) 0.4513(3) 0.0512(2) 0.0367(7) Uani 1 1 d . . . . .
H12 H 0.860452 0.487758 0.074913 0.044 Uiso 1 1 calc R U . . .
C13 C 0.6868(3) 0.4840(2) 0.09476(18) 0.0303(6) Uani 1 1 d . . . . .
H13 H 0.710432 0.543458 0.148502 0.036 Uiso 1 1 calc R U . . .
C14 C 0.5579(3) 0.4311(2) 0.06179(17) 0.0277(5) Uani 1 1 d . . . . .
C15 C 0.5777(2) 0.64064(18) 0.54519(16) 0.0227(5) Uani 1 1 d . . . . .
C16 C 0.6938(2) 0.65679(19) 0.59024(17) 0.0242(5) Uani 1 1 d . . . . .
C17 C 0.8064(3) 0.6781(2) 0.55363(19) 0.0298(6) Uani 1 1 d . . . . .
H17 H 0.803478 0.681989 0.497057 0.036 Uiso 1 1 calc R U . . .
C18 C 0.9173(3) 0.6928(2) 0.5973(2) 0.0369(7) Uani 1 1 d . . . . .
H18 H 0.990069 0.706543 0.570860 0.044 Uiso 1 1 calc R U . . .
C19 C 0.9251(3) 0.6877(2) 0.6817(2) 0.0402(7) Uani 1 1 d . . . . .
H19 H 1.002834 0.697217 0.711438 0.048 Uiso 1 1 calc R U . . .
C20 C 0.8220(3) 0.6693(2) 0.7204(2) 0.0360(7) Uani 1 1 d . . . . .
H20 H 0.828495 0.666860 0.777402 0.043 Uiso 1 1 calc R U . . .
C21 C 0.7035(3) 0.6534(2) 0.67662(18) 0.0276(5) Uani 1 1 d . . . . .
C22 C 0.5971(3) 0.6375(2) 0.71662(18) 0.0304(6) Uani 1 1 d . . . . .
H22 H 0.603543 0.636722 0.774292 0.037 Uiso 1 1 calc R U . . .
C23 C 0.4817(3) 0.62256(19) 0.67457(18) 0.0279(6) Uani 1 1 d . . . . .
C24 C 0.3745(3) 0.6101(2) 0.7178(2) 0.0344(6) Uani 1 1 d . . . . .
H24 H 0.381857 0.610975 0.776013 0.041 Uiso 1 1 calc R U . . .
C25 C 0.2630(3) 0.5970(2) 0.6776(2) 0.0388(7) Uani 1 1 d . . . . .
H25 H 0.192928 0.588905 0.707573 0.047 Uiso 1 1 calc R U . . .
C26 C 0.2503(3) 0.5953(2) 0.5907(2) 0.0379(7) Uani 1 1 d . . . . .
H26 H 0.171383 0.585364 0.562551 0.046 Uiso 1 1 calc R U . . .
C27 C 0.3503(3) 0.6078(2) 0.54726(19) 0.0312(6) Uani 1 1 d . . . . .
H27 H 0.339471 0.606411 0.489065 0.037 Uiso 1 1 calc R U . . .
C28 C 0.4706(2) 0.62296(18) 0.58675(17) 0.0244(5) Uani 1 1 d . . . . .
C29 C 0.4468(2) 0.9120(2) 0.36827(17) 0.0261(5) Uani 1 1 d . . . . .
C30 C 0.3524(3) 0.9190(2) 0.42299(18) 0.0316(6) Uani 1 1 d . . . . .
C31 C 0.3182(3) 0.8578(3) 0.47402(19) 0.0382(7) Uani 1 1 d . . . . .
H31 H 0.364276 0.814121 0.475534 0.046 Uiso 1 1 calc R U . . .
C32 C 0.2207(3) 0.8604(3) 0.5208(2) 0.0518(9) Uani 1 1 d . . . . .
H32 H 0.200609 0.818796 0.554224 0.062 Uiso 1 1 calc R U . . .
C33 C 0.1504(3) 0.9231(3) 0.5201(2) 0.0582(11) Uani 1 1 d . . . . .
H33 H 0.080240 0.921196 0.550263 0.070 Uiso 1 1 calc R U . . .
C34 C 0.1819(3) 0.9867(3) 0.4766(2) 0.0544(11) Uani 1 1 d . . . . .
H34 H 0.134746 1.030510 0.477982 0.065 Uiso 1 1 calc R U . . .
C35 C 0.2859(3) 0.9893(2) 0.4280(2) 0.0399(7) Uani 1 1 d . . . . .
C36 C 0.3212(3) 1.0544(2) 0.3837(2) 0.0419(8) Uani 1 1 d . . . . .
H36 H 0.278052 1.101740 0.388085 0.050 Uiso 1 1 calc R U . . .
C37 C 0.4173(3) 1.0533(2) 0.3331(2) 0.0368(7) Uani 1 1 d . . . . .
C38 C 0.4529(4) 1.1204(2) 0.2883(2) 0.0459(8) Uani 1 1 d . . . . .
H38 H 0.410397 1.168251 0.293162 0.055 Uiso 1 1 calc R U . . .
C39 C 0.5460(4) 1.1182(2) 0.2389(2) 0.0490(9) Uani 1 1 d . . . . .
H39 H 0.568729 1.164986 0.210493 0.059 Uiso 1 1 calc R U . . .
C40 C 0.6102(3) 1.0462(2) 0.2291(2) 0.0403(7) Uani 1 1 d . . . . .
H40 H 0.674971 1.044637 0.193848 0.048 Uiso 1 1 calc R U . . .
C41 C 0.5786(3) 0.9793(2) 0.27056(19) 0.0315(6) Uani 1 1 d . . . . .
H41 H 0.621854 0.931516 0.263525 0.038 Uiso 1 1 calc R U . . .
C42 C 0.4817(3) 0.9797(2) 0.32428(18) 0.0286(6) Uani 1 1 d . . . . .
C43 C 0.9346(2) 0.7810(2) 0.29724(17) 0.0255(5) Uani 1 1 d . . . . .
C44 C 0.9791(2) 0.8613(2) 0.26703(17) 0.0254(5) Uani 1 1 d . . . . .
C45 C 0.9162(3) 0.9338(2) 0.27401(19) 0.0308(6) Uani 1 1 d . . . . .
H45 H 0.842173 0.928445 0.299773 0.037 Uiso 1 1 calc R U . . .
C46 C 0.9602(3) 1.0106(2) 0.2444(2) 0.0360(6) Uani 1 1 d . . . . .
H46 H 0.917932 1.059019 0.251318 0.043 Uiso 1 1 calc R U . . .
C47 C 1.0688(3) 1.0185(2) 0.2034(2) 0.0373(7) Uani 1 1 d . . . . .
H47 H 1.097110 1.070811 0.181229 0.045 Uiso 1 1 calc R U . . .
C48 C 1.1323(3) 0.9518(2) 0.19580(19) 0.0322(6) Uani 1 1 d . . . . .
H48 H 1.204843 0.957863 0.168286 0.039 Uiso 1 1 calc R U . . .
C49 C 1.0913(2) 0.8724(2) 0.22865(17) 0.0261(5) Uani 1 1 d . . . . .
C50 C 1.1593(2) 0.8073(2) 0.22572(17) 0.0269(5) Uani 1 1 d . . . . .
H50 H 1.232190 0.813383 0.198577 0.032 Uiso 1 1 calc R U . . .
C51 C 1.1227(2) 0.7330(2) 0.26189(17) 0.0259(5) Uani 1 1 d . . . . .
C52 C 1.1966(2) 0.6715(2) 0.26482(18) 0.0297(6) Uani 1 1 d . . . . .
H52 H 1.270436 0.678170 0.238790 0.036 Uiso 1 1 calc R U . . .
C53 C 1.1634(3) 0.6026(2) 0.3045(2) 0.0336(6) Uani 1 1 d . . . . .
H53 H 1.215187 0.563489 0.307315 0.040 Uiso 1 1 calc R U . . .
C54 C 1.0523(3) 0.5898(2) 0.3411(2) 0.0341(6) Uani 1 1 d . . . . .
H54 H 1.029699 0.542058 0.368555 0.041 Uiso 1 1 calc R U . . .
C55 C 0.9775(3) 0.6449(2) 0.33745(19) 0.0308(6) Uani 1 1 d . . . . .
H55 H 0.902186 0.633677 0.361417 0.037 Uiso 1 1 calc R U . . .
C56 C 1.0085(2) 0.7197(2) 0.29849(17) 0.0256(5) Uani 1 1 d . . . . .
B1 B 0.4976(3) 0.5587(2) 0.19954(17) 0.0200(5) Uani 1 1 d . . . . .
H1A H 0.406682 0.581414 0.220283 0.030 Uiso 1 1 calc R U . . .
H1B H 0.574058 0.630521 0.193793 0.030 Uiso 1 1 calc R U . . .
H1C H 0.537763 0.535935 0.254826 0.030 Uiso 1 1 calc DR U . . .
B2 B 0.5738(3) 0.6534(2) 0.45351(18) 0.0226(5) Uani 1 1 d . . . . .
H2A H 0.614513 0.742766 0.466499 0.034 Uiso 1 1 calc R U . . .
H2B H 0.468959 0.619508 0.417211 0.034 Uiso 1 1 calc R U . . .
H2C H 0.634933 0.607648 0.407279 0.034 Uiso 1 1 calc R U . . .
B3 B 0.5083(3) 0.8262(2) 0.35284(18) 0.0215(5) Uani 1 1 d . . . . .
H3A H 0.529757 0.796449 0.277863 0.032 Uiso 1 1 calc R U . . .
H3B H 0.439260 0.755885 0.365634 0.032 Uiso 1 1 calc R U . . .
H3C H 0.602911 0.860482 0.403185 0.032 Uiso 1 1 calc R U . . .
B4 B 0.8003(2) 0.7545(2) 0.31976(18) 0.0191(5) Uani 1 1 d . . . . .
H4A H 0.761450 0.664893 0.306135 0.029 Uiso 1 1 calc R U . . .
H4B H 0.735576 0.773641 0.274032 0.029 Uiso 1 1 calc R U . . .
H4C H 0.800553 0.804593 0.396454 0.029 Uiso 1 1 calc R U . . .
C57 C 0.3143(4) 0.1330(3) 0.0770(3) 0.0547(9) Uani 1 1 d . . . . .
H57A H 0.256867 0.166302 0.065379 0.082 Uiso 1 1 calc R U . . .
H57B H 0.396540 0.165309 0.065586 0.082 Uiso 1 1 calc R U . . .
H57C H 0.318696 0.140317 0.139028 0.082 Uiso 1 1 calc R U . . .
C58 C 0.2695(3) 0.0208(3) 0.0170(2) 0.0434(8) Uani 1 1 d . . . . .
C59 C 0.3393(3) -0.0431(3) 0.0152(2) 0.0492(8) Uani 1 1 d . . . . .
H59 H 0.417317 -0.014983 0.051678 0.059 Uiso 1 1 calc R U . . .
C60 C 0.2969(4) -0.1470(3) -0.0388(3) 0.0564(10) Uani 1 1 d . . . . .
H60 H 0.346277 -0.189009 -0.039522 0.068 Uiso 1 1 calc R U . . .
C61 C 0.1837(4) -0.1893(3) -0.0914(3) 0.0565(10) Uani 1 1 d . . . . .
H61 H 0.154522 -0.260337 -0.128502 0.068 Uiso 1 1 calc R U . . .
C62 C 0.1129(4) -0.1272(3) -0.0895(3) 0.0554(9) Uani 1 1 d . . . . .
H62 H 0.034101 -0.155909 -0.125042 0.066 Uiso 1 1 calc R U . . .
C63 C 0.1562(3) -0.0230(3) -0.0359(2) 0.0476(8) Uani 1 1 d . . . . .
H63 H 0.106713 0.018723 -0.035678 0.057 Uiso 1 1 calc R U . . .
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'
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
_geom_angle_publ_flag
B2 Hf1 B1 112.43(9) . . ?
B3 Hf1 B1 109.98(10) . . ?
B3 Hf1 B2 108.27(10) . . ?
B3 Hf1 B4 110.01(10) . . ?
B4 Hf1 B1 107.11(10) . . ?
B4 Hf1 B2 109.02(10) . . ?
C2 C1 C14 118.3(2) . . ?
C2 C1 B1 121.1(2) . . ?
C14 C1 B1 120.6(2) . . ?
C1 C2 C3 122.1(2) . . ?
C1 C2 C7 120.7(3) . . ?
C3 C2 C7 117.3(3) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 121.9(3) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.4(3) . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C2 118.9(3) . . ?
C8 C7 C2 119.4(3) . . ?
C8 C7 C6 121.7(3) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C10 121.5(3) . . ?
C8 C9 C14 119.3(3) . . ?
C10 C9 C14 119.2(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.3(3) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 119.1 . . ?
C12 C13 C14 121.7(3) . . ?
C14 C13 H13 119.1 . . ?
C1 C14 C9 120.5(3) . . ?
C1 C14 C13 122.3(2) . . ?
C13 C14 C9 117.1(2) . . ?
C16 C15 C28 119.5(2) . . ?
C16 C15 B2 118.4(2) . . ?
C28 C15 B2 121.9(2) . . ?
C15 C16 C17 122.6(2) . . ?
C15 C16 C21 120.6(2) . . ?
C17 C16 C21 116.8(2) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 C16 122.1(3) . . ?
C18 C17 H17 118.9 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.1(3) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C16 119.4(3) . . ?
C22 C21 C16 118.8(2) . . ?
C22 C21 C20 121.8(3) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 C21 122.0(2) . . ?
C23 C22 H22 119.0 . . ?
C22 C23 C24 121.2(3) . . ?
C22 C23 C28 119.5(2) . . ?
C24 C23 C28 119.2(3) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.1(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(3) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.1 . . ?
C26 C27 C28 121.8(3) . . ?
C28 C27 H27 119.1 . . ?
C15 C28 C23 119.5(2) . . ?
C15 C28 C27 123.4(2) . . ?
C27 C28 C23 117.0(2) . . ?
C30 C29 B3 120.4(2) . . ?
C42 C29 C30 119.9(2) . . ?
C42 C29 B3 119.7(2) . . ?
C29 C30 C31 122.9(3) . . ?
C29 C30 C35 120.0(3) . . ?
C31 C30 C35 117.1(3) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 C30 121.7(3) . . ?
C32 C31 H31 119.2 . . ?
C31 C32 H32 119.5 . . ?
C31 C32 C33 121.0(4) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.1(3) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 119.3 . . ?
C33 C34 C35 121.3(3) . . ?
C35 C34 H34 119.3 . . ?
C30 C35 C34 118.5(3) . . ?
C36 C35 C30 118.9(3) . . ?
C36 C35 C34 122.6(3) . . ?
C35 C36 H36 118.7 . . ?
C35 C36 C37 122.7(3) . . ?
C37 C36 H36 118.7 . . ?
C36 C37 C38 122.2(3) . . ?
C36 C37 C42 119.1(3) . . ?
C38 C37 C42 118.7(3) . . ?
C37 C38 H38 119.2 . . ?
C39 C38 C37 121.7(3) . . ?
C39 C38 H38 119.2 . . ?
C38 C39 H39 119.7 . . ?
C38 C39 C40 120.5(3) . . ?
C40 C39 H39 119.7 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 C39 120.0(3) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.3 . . ?
C40 C41 C42 121.4(3) . . ?
C42 C41 H41 119.3 . . ?
C29 C42 C37 119.4(3) . . ?
C29 C42 C41 122.9(2) . . ?
C41 C42 C37 117.7(3) . . ?
C44 C43 B4 119.8(2) . . ?
C56 C43 C44 119.3(2) . . ?
C56 C43 B4 120.6(2) . . ?
C43 C44 C45 122.1(2) . . ?
C43 C44 C49 120.1(2) . . ?
C45 C44 C49 117.8(2) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 C44 121.4(3) . . ?
C46 C45 H45 119.3 . . ?
C45 C46 H46 119.8 . . ?
C45 C46 C47 120.4(3) . . ?
C47 C46 H46 119.8 . . ?
C46 C47 H47 119.8 . . ?
C48 C47 C46 120.3(3) . . ?
C48 C47 H47 119.8 . . ?
C47 C48 H48 119.6 . . ?
C47 C48 C49 120.8(3) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 C44 119.2(2) . . ?
C50 C49 C44 119.5(2) . . ?
C50 C49 C48 121.3(2) . . ?
C49 C50 H50 119.3 . . ?
C49 C50 C51 121.4(2) . . ?
C51 C50 H50 119.3 . . ?
C50 C51 C52 121.6(2) . . ?
C50 C51 C56 119.4(2) . . ?
C52 C51 C56 119.1(2) . . ?
C51 C52 H52 119.4 . . ?
C53 C52 C51 121.3(3) . . ?
C53 C52 H52 119.4 . . ?
C52 C53 H53 120.1 . . ?
C52 C53 C54 119.9(3) . . ?
C54 C53 H53 120.1 . . ?
C53 C54 H54 119.6 . . ?
C55 C54 C53 120.8(3) . . ?
C55 C54 H54 119.6 . . ?
C54 C55 H55 119.0 . . ?
C54 C55 C56 121.9(3) . . ?
C56 C55 H55 119.0 . . ?
C43 C56 C51 119.9(2) . . ?
C43 C56 C55 123.0(2) . . ?
C55 C56 C51 117.1(2) . . ?
Hf1 B1 H1A 83.4 . . ?
Hf1 B1 H1B 63.2 . . ?
Hf1 B1 H1C 65.8 . . ?
C1 B1 Hf1 167.0(2) . . ?
C1 B1 H1A 109.5 . . ?
C1 B1 H1B 109.5 . . ?
C1 B1 H1C 109.5 . . ?
H1A B1 H1B 109.5 . . ?
H1A B1 H1C 109.5 . . ?
H1B B1 H1C 109.5 . . ?
Hf1 B2 H2A 61.9 . . ?
Hf1 B2 H2B 78.1 . . ?
Hf1 B2 H2C 72.0 . . ?
C15 B2 Hf1 170.6(2) . . ?
C15 B2 H2A 109.5 . . ?
C15 B2 H2B 109.5 . . ?
C15 B2 H2C 109.5 . . ?
H2A B2 H2B 109.5 . . ?
H2A B2 H2C 109.5 . . ?
H2B B2 H2C 109.5 . . ?
Hf1 B3 H3A 71.6 . . ?
Hf1 B3 H3B 68.7 . . ?
Hf1 B3 H3C 71.3 . . ?
C29 B3 Hf1 178.2(2) . . ?
C29 B3 H3A 109.5 . . ?
C29 B3 H3B 109.5 . . ?
C29 B3 H3C 109.5 . . ?
H3A B3 H3B 109.5 . . ?
H3A B3 H3C 109.5 . . ?
H3B B3 H3C 109.5 . . ?
Hf1 B4 H4A 66.1 . . ?
Hf1 B4 H4B 66.9 . . ?
Hf1 B4 H4C 79.0 . . ?
C43 B4 Hf1 171.51(19) . . ?
C43 B4 H4A 109.5 . . ?
C43 B4 H4B 109.5 . . ?
C43 B4 H4C 109.5 . . ?
H4A B4 H4B 109.5 . . ?
H4A B4 H4C 109.5 . . ?
H4B B4 H4C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
C58 C57 H57C 109.5 . . ?
C59 C58 C57 121.2(3) . . ?
C63 C58 C57 121.1(3) . . ?
C63 C58 C59 117.7(3) . . ?
C58 C59 H59 119.4 . . ?
C60 C59 C58 121.2(4) . . ?
C60 C59 H59 119.4 . . ?
C59 C60 H60 119.9 . . ?
C61 C60 C59 120.2(4) . . ?
C61 C60 H60 119.9 . . ?
C60 C61 H61 120.4 . . ?
C60 C61 C62 119.2(4) . . ?
C62 C61 H61 120.4 . . ?
C61 C62 H62 119.8 . . ?
C61 C62 C63 120.4(4) . . ?
C63 C62 H62 119.8 . . ?
C58 C63 C62 121.3(4) . . ?
C58 C63 H63 119.4 . . ?
C62 C63 H63 119.4 . . ?
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 B1 2.327(3) . ?
Hf1 B2 2.311(3) . ?
Hf1 B3 2.298(3) . ?
Hf1 B4 2.311(3) . ?
C1 C2 1.420(4) . ?
C1 C14 1.424(4) . ?
C1 B1 1.581(4) . ?
C2 C3 1.424(4) . ?
C2 C7 1.438(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.375(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.410(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.354(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.435(4) . ?
C7 C8 1.393(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.390(4) . ?
C9 C10 1.429(4) . ?
C9 C14 1.441(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.358(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.415(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.358(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.435(4) . ?
C15 C16 1.415(4) . ?
C15 C28 1.420(4) . ?
C15 B2 1.582(4) . ?
C16 C17 1.434(4) . ?
C16 C21 1.437(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.360(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.415(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.356(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.432(4) . ?
C21 C22 1.396(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(4) . ?
C23 C24 1.429(4) . ?
C23 C28 1.443(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.348(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.417(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.363(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.426(4) . ?
C29 C30 1.421(4) . ?
C29 C42 1.412(4) . ?
C29 B3 1.567(4) . ?
C30 C31 1.428(4) . ?
C30 C35 1.436(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.368(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.395(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.354(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.444(5) . ?
C35 C36 1.385(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.391(5) . ?
C37 C38 1.415(5) . ?
C37 C42 1.448(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.351(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.425(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.366(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.430(4) . ?
C43 C44 1.417(4) . ?
C43 C56 1.411(4) . ?
C43 B4 1.558(3) . ?
C44 C45 1.428(4) . ?
C44 C49 1.434(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.365(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.419(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.359(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.430(4) . ?
C49 C50 1.391(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.398(4) . ?
C51 C52 1.421(4) . ?
C51 C56 1.441(3) . ?
C52 H52 0.9500 . ?
C52 C53 1.371(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.409(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.355(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.435(4) . ?
B1 H1A 1.2000 . ?
B1 H1B 1.2000 . ?
B1 H1C 1.2000 . ?
B2 H2A 1.2000 . ?
B2 H2B 1.2000 . ?
B2 H2C 1.2000 . ?
B3 H3A 1.2000 . ?
B3 H3B 1.2000 . ?
B3 H3C 1.2000 . ?
B4 H4A 1.2000 . ?
B4 H4B 1.2000 . ?
B4 H4C 1.2000 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C57 C58 1.505(5) . ?
C58 C59 1.396(5) . ?
C58 C63 1.376(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.388(6) . ?
C60 H60 0.9500 . ?
C60 C61 1.374(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.381(6) . ?
C62 H62 0.9500 . ?
C62 C63 1.390(5) . ?
C63 H63 0.9500 . ?
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
C1 C2 C3 C4 -178.9(3) . . . . ?
C1 C2 C7 C6 178.1(2) . . . . ?
C1 C2 C7 C8 -0.8(4) . . . . ?
C2 C1 C14 C9 -2.2(4) . . . . ?
C2 C1 C14 C13 177.6(2) . . . . ?
C2 C1 B1 Hf1 176.7(6) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C2 C7 C8 C9 -1.3(4) . . . . ?
C3 C2 C7 C6 -1.7(4) . . . . ?
C3 C2 C7 C8 179.4(2) . . . . ?
C3 C4 C5 C6 -1.0(5) . . . . ?
C4 C5 C6 C7 0.1(5) . . . . ?
C5 C6 C7 C2 1.3(4) . . . . ?
C5 C6 C7 C8 -179.9(3) . . . . ?
C6 C7 C8 C9 179.9(3) . . . . ?
C7 C2 C3 C4 0.9(4) . . . . ?
C7 C8 C9 C10 -178.7(3) . . . . ?
C7 C8 C9 C14 1.6(4) . . . . ?
C8 C9 C10 C11 179.4(3) . . . . ?
C8 C9 C14 C1 0.2(4) . . . . ?
C8 C9 C14 C13 -179.6(2) . . . . ?
C9 C10 C11 C12 0.8(5) . . . . ?
C10 C9 C14 C1 -179.5(2) . . . . ?
C10 C9 C14 C13 0.7(4) . . . . ?
C10 C11 C12 C13 -0.5(5) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C12 C13 C14 C1 179.8(3) . . . . ?
C12 C13 C14 C9 -0.4(4) . . . . ?
C14 C1 C2 C3 -177.7(2) . . . . ?
C14 C1 C2 C7 2.5(4) . . . . ?
C14 C1 B1 Hf1 -2.2(9) . . . . ?
C14 C9 C10 C11 -0.9(4) . . . . ?
C15 C16 C17 C18 -179.6(3) . . . . ?
C15 C16 C21 C20 179.5(2) . . . . ?
C15 C16 C21 C22 -2.2(4) . . . . ?
C16 C15 C28 C23 0.5(4) . . . . ?
C16 C15 C28 C27 178.8(2) . . . . ?
C16 C17 C18 C19 -0.2(5) . . . . ?
C16 C21 C22 C23 1.4(4) . . . . ?
C17 C16 C21 C20 -1.1(4) . . . . ?
C17 C16 C21 C22 177.2(2) . . . . ?
C17 C18 C19 C20 -0.8(5) . . . . ?
C18 C19 C20 C21 0.8(5) . . . . ?
C19 C20 C21 C16 0.2(4) . . . . ?
C19 C20 C21 C22 -178.0(3) . . . . ?
C20 C21 C22 C23 179.6(3) . . . . ?
C21 C16 C17 C18 1.1(4) . . . . ?
C21 C22 C23 C24 -177.7(2) . . . . ?
C21 C22 C23 C28 0.3(4) . . . . ?
C22 C23 C24 C25 179.1(3) . . . . ?
C22 C23 C28 C15 -1.3(4) . . . . ?
C22 C23 C28 C27 -179.7(2) . . . . ?
C23 C24 C25 C26 0.1(4) . . . . ?
C24 C23 C28 C15 176.8(2) . . . . ?
C24 C23 C28 C27 -1.7(4) . . . . ?
C24 C25 C26 C27 -0.6(5) . . . . ?
C25 C26 C27 C28 0.0(4) . . . . ?
C26 C27 C28 C15 -177.2(3) . . . . ?
C26 C27 C28 C23 1.1(4) . . . . ?
C28 C15 C16 C17 -178.1(2) . . . . ?
C28 C15 C16 C21 1.2(4) . . . . ?
C28 C23 C24 C25 1.1(4) . . . . ?
C29 C30 C31 C32 -174.9(3) . . . . ?
C29 C30 C35 C34 173.5(3) . . . . ?
C29 C30 C35 C36 -4.4(4) . . . . ?
C30 C29 C42 C37 -2.2(4) . . . . ?
C30 C29 C42 C41 177.9(2) . . . . ?
C30 C31 C32 C33 0.2(5) . . . . ?
C30 C35 C36 C37 1.2(4) . . . . ?
C31 C30 C35 C34 -6.0(4) . . . . ?
C31 C30 C35 C36 176.2(3) . . . . ?
C31 C32 C33 C34 -3.5(5) . . . . ?
C32 C33 C34 C35 1.8(5) . . . . ?
C33 C34 C35 C30 3.0(5) . . . . ?
C33 C34 C35 C36 -179.2(3) . . . . ?
C34 C35 C36 C37 -176.6(3) . . . . ?
C35 C30 C31 C32 4.5(4) . . . . ?
C35 C36 C37 C38 -179.8(3) . . . . ?
C35 C36 C37 C42 1.5(4) . . . . ?
C36 C37 C38 C39 -179.6(3) . . . . ?
C36 C37 C42 C29 -1.0(4) . . . . ?
C36 C37 C42 C41 178.9(3) . . . . ?
C37 C38 C39 C40 1.1(5) . . . . ?
C38 C37 C42 C29 -179.8(3) . . . . ?
C38 C37 C42 C41 0.2(4) . . . . ?
C38 C39 C40 C41 -0.6(5) . . . . ?
C39 C40 C41 C42 -0.1(4) . . . . ?
C40 C41 C42 C29 -179.8(3) . . . . ?
C40 C41 C42 C37 0.3(4) . . . . ?
C42 C29 C30 C31 -175.7(3) . . . . ?
C42 C29 C30 C35 4.9(4) . . . . ?
C42 C37 C38 C39 -0.9(5) . . . . ?
C43 C44 C45 C46 -179.9(3) . . . . ?
C43 C44 C49 C48 177.8(2) . . . . ?
C43 C44 C49 C50 -3.5(4) . . . . ?
C44 C43 C56 C51 -5.6(4) . . . . ?
C44 C43 C56 C55 172.5(3) . . . . ?
C44 C45 C46 C47 1.8(5) . . . . ?
C44 C49 C50 C51 -2.0(4) . . . . ?
C45 C44 C49 C48 -2.7(4) . . . . ?
C45 C44 C49 C50 176.0(2) . . . . ?
C45 C46 C47 C48 -2.1(5) . . . . ?
C46 C47 C48 C49 0.1(5) . . . . ?
C47 C48 C49 C44 2.4(4) . . . . ?
C47 C48 C49 C50 -176.3(3) . . . . ?
C48 C49 C50 C51 176.7(3) . . . . ?
C49 C44 C45 C46 0.7(4) . . . . ?
C49 C50 C51 C52 -175.3(2) . . . . ?
C49 C50 C51 C56 3.6(4) . . . . ?
C50 C51 C52 C53 176.6(3) . . . . ?
C50 C51 C56 C43 0.3(4) . . . . ?
C50 C51 C56 C55 -177.9(2) . . . . ?
C51 C52 C53 C54 1.8(4) . . . . ?
C52 C51 C56 C43 179.2(2) . . . . ?
C52 C51 C56 C55 1.0(4) . . . . ?
C52 C53 C54 C55 0.1(5) . . . . ?
C53 C54 C55 C56 -1.4(5) . . . . ?
C54 C55 C56 C43 -177.3(3) . . . . ?
C54 C55 C56 C51 0.9(4) . . . . ?
C56 C43 C44 C45 -172.3(2) . . . . ?
C56 C43 C44 C49 7.2(4) . . . . ?
C56 C51 C52 C53 -2.3(4) . . . . ?
B1 C1 C2 C3 3.4(4) . . . . ?
B1 C1 C2 C7 -176.4(2) . . . . ?
B1 C1 C14 C9 176.7(2) . . . . ?
B1 C1 C14 C13 -3.5(4) . . . . ?
B2 C15 C16 C17 -3.9(4) . . . . ?
B2 C15 C16 C21 175.5(2) . . . . ?
B2 C15 C28 C23 -173.6(2) . . . . ?
B2 C15 C28 C27 4.7(4) . . . . ?
B3 C29 C30 C31 7.2(4) . . . . ?
B3 C29 C30 C35 -172.2(2) . . . . ?
B3 C29 C42 C37 174.9(2) . . . . ?
B3 C29 C42 C41 -5.0(4) . . . . ?
B4 C43 C44 C45 13.7(4) . . . . ?
B4 C43 C44 C49 -166.9(2) . . . . ?
B4 C43 C56 C51 168.4(2) . . . . ?
B4 C43 C56 C55 -13.5(4) . . . . ?
C57 C58 C59 C60 178.7(3) . . . . ?
C57 C58 C63 C62 -178.1(3) . . . . ?
C58 C59 C60 C61 -0.7(5) . . . . ?
C59 C58 C63 C62 -0.3(5) . . . . ?
C59 C60 C61 C62 -0.1(6) . . . . ?
C60 C61 C62 C63 0.7(6) . . . . ?
C61 C62 C63 C58 -0.5(6) . . . . ?
C63 C58 C59 C60 0.9(5) . . . . ?
