#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:14:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179100 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/62/4306286.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_4306286
loop_
_publ_author_name
'Karen J. Blackmore'
'Michael B. Sly'
'Mason R. Haneline'
'Joseph W. Ziller'
'Alan F. Heyduk'
_publ_section_title
;
Group IV Imino-Semiquinone Complexes Obtained by Oxidative Addition of
Halogens
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10522
_journal_page_last               10532
_journal_paper_doi               10.1021/ic801127r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C48 H84 Hf N2 O5'
_chemical_formula_weight         947.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.407(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3201(14)
_cell_length_b                   19.716(2)
_cell_length_c                   19.218(2)
_cell_measurement_temperature    163(2)
_cell_volume                     4929.1(9)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50452
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.159
_exptl_absorpt_correction_T_max  0.8997
_exptl_absorpt_correction_T_min  0.5022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.274
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10887
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          2.687
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0278P)²+7.9805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                8870
_reflns_number_total             10887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801127r_si_002_4.cif
_cod_data_source_block           afh38
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4929.3(9)
_cod_database_code               4306286
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.340693(9) 0.704995(6) 0.654934(6) 0.01779(4) Uani 1 1 d . . .
O1 O 0.26020(15) 0.77983(10) 0.59315(11) 0.0197(4) Uani 1 1 d . . .
O2 O 0.42326(15) 0.65665(10) 0.74303(10) 0.0199(4) Uani 1 1 d . . .
O3 O 0.25012(16) 0.73256(12) 0.73733(11) 0.0252(5) Uani 1 1 d . . .
O4 O 0.43446(16) 0.79751(11) 0.69723(12) 0.0266(5) Uani 1 1 d . . .
N1 N 0.21120(19) 0.65280(12) 0.59591(13) 0.0194(5) Uani 1 1 d . . .
N2 N 0.46490(19) 0.66228(13) 0.61733(13) 0.0207(5) Uani 1 1 d . . .
C1 C 0.1704(2) 0.76321(15) 0.54759(15) 0.0184(6) Uani 1 1 d . . .
C2 C 0.1102(2) 0.81088(15) 0.50290(15) 0.0193(6) Uani 1 1 d . . .
C3 C 0.0178(2) 0.78785(15) 0.45890(15) 0.0205(6) Uani 1 1 d . . .
H3A H -0.0236 0.8192 0.4278 0.025 Uiso 1 1 calc R . .
C4 C -0.0146(2) 0.72133(16) 0.45936(16) 0.0215(6) Uani 1 1 d . . .
C5 C 0.0476(2) 0.67476(15) 0.50450(16) 0.0222(6) Uani 1 1 d . . .
H5A H 0.0255 0.6290 0.5051 0.027 Uiso 1 1 calc R . .
C6 C 0.1408(2) 0.69385(15) 0.54861(15) 0.0193(6) Uani 1 1 d . . .
C7 C 0.1423(2) 0.88577(15) 0.50207(16) 0.0216(6) Uani 1 1 d . . .
C8 C 0.0659(3) 0.92766(17) 0.44862(18) 0.0321(8) Uani 1 1 d . . .
H8A H -0.0027 0.9234 0.4590 0.048 Uiso 1 1 calc R . .
H8B H 0.0643 0.9111 0.4003 0.048 Uiso 1 1 calc R . .
H8C H 0.0870 0.9754 0.4522 0.048 Uiso 1 1 calc R . .
C9 C 0.1475(3) 0.91693(16) 0.57591(16) 0.0263(7) Uani 1 1 d . . .
H9A H 0.0797 0.9142 0.5878 0.040 Uiso 1 1 calc R . .
H9B H 0.1685 0.9645 0.5756 0.040 Uiso 1 1 calc R . .
H9C H 0.1976 0.8920 0.6115 0.040 Uiso 1 1 calc R . .
C10 C 0.2479(2) 0.89148(16) 0.48205(18) 0.0275(7) Uani 1 1 d . . .
H10A H 0.2671 0.9394 0.4809 0.041 Uiso 1 1 calc R . .
H10B H 0.2442 0.8712 0.4350 0.041 Uiso 1 1 calc R . .
H10C H 0.2995 0.8675 0.5175 0.041 Uiso 1 1 calc R . .
C11 C -0.1175(2) 0.69649(16) 0.41352(17) 0.0264(7) Uani 1 1 d . . .
C12 C -0.0981(3) 0.63745(18) 0.36620(19) 0.0342(8) Uani 1 1 d . . .
H12A H -0.0639 0.6004 0.3962 0.051 Uiso 1 1 calc R . .
H12B H -0.0541 0.6529 0.3345 0.051 Uiso 1 1 calc R . .
H12C H -0.1637 0.6214 0.3377 0.051 Uiso 1 1 calc R . .
C13 C -0.1733(3) 0.7526(2) 0.3648(2) 0.0407(9) Uani 1 1 d . . .
H13A H -0.2381 0.7348 0.3366 0.061 Uiso 1 1 calc R . .
H13B H -0.1298 0.7681 0.3329 0.061 Uiso 1 1 calc R . .
H13C H -0.1877 0.7907 0.3939 0.061 Uiso 1 1 calc R . .
C14 C -0.1871(3) 0.6720(2) 0.4619(2) 0.0399(9) Uani 1 1 d . . .
H14A H -0.1532 0.6350 0.4920 0.060 Uiso 1 1 calc R . .
H14B H -0.2522 0.6559 0.4328 0.060 Uiso 1 1 calc R . .
H14C H -0.2004 0.7096 0.4921 0.060 Uiso 1 1 calc R . .
C15 C 0.5125(2) 0.62482(14) 0.73802(15) 0.0183(6) Uani 1 1 d . . .
C16 C 0.5760(2) 0.59179(15) 0.79564(15) 0.0196(6) Uani 1 1 d . . .
C17 C 0.6670(2) 0.56312(15) 0.78445(16) 0.0219(6) Uani 1 1 d . . .
H17A H 0.7109 0.5405 0.8229 0.026 Uiso 1 1 calc R . .
C18 C 0.6961(2) 0.56638(15) 0.71888(16) 0.0212(6) Uani 1 1 d . . .
C19 C 0.6303(2) 0.59838(15) 0.66262(16) 0.0218(6) Uani 1 1 d . . .
H19A H 0.6489 0.6003 0.6176 0.026 Uiso 1 1 calc R . .
C20 C 0.5375(2) 0.62796(15) 0.66973(15) 0.0201(6) Uani 1 1 d . . .
C21 C 0.5456(2) 0.58769(16) 0.86862(16) 0.0247(7) Uani 1 1 d . . .
C22 C 0.6230(3) 0.5465(2) 0.92269(17) 0.0370(9) Uani 1 1 d . . .
H22A H 0.6907 0.5681 0.9301 0.056 Uiso 1 1 calc R . .
H22B H 0.6273 0.5003 0.9045 0.056 Uiso 1 1 calc R . .
H22C H 0.6006 0.5446 0.9680 0.056 Uiso 1 1 calc R . .
C23 C 0.4409(3) 0.55317(18) 0.86100(18) 0.0320(8) Uani 1 1 d . . .
H23A H 0.3889 0.5789 0.8275 0.048 Uiso 1 1 calc R . .
H23B H 0.4222 0.5515 0.9076 0.048 Uiso 1 1 calc R . .
H23C H 0.4447 0.5069 0.8431 0.048 Uiso 1 1 calc R . .
C24 C 0.5422(3) 0.65947(17) 0.89944(17) 0.0304(7) Uani 1 1 d . . .
H24A H 0.6113 0.6793 0.9087 0.046 Uiso 1 1 calc R . .
H24B H 0.5180 0.6570 0.9441 0.046 Uiso 1 1 calc R . .
H24C H 0.4953 0.6878 0.8652 0.046 Uiso 1 1 calc R . .
C25 C 0.7986(2) 0.53552(16) 0.71004(16) 0.0236(6) Uani 1 1 d . . .
C26 C 0.7996(3) 0.45942(18) 0.7247(2) 0.0419(9) Uani 1 1 d . . .
H26A H 0.7904 0.4516 0.7733 0.063 Uiso 1 1 calc R . .
H26B H 0.8655 0.4402 0.7196 0.063 Uiso 1 1 calc R . .
H26C H 0.7436 0.4376 0.6907 0.063 Uiso 1 1 calc R . .
C27 C 0.8173(3) 0.5454(2) 0.63499(19) 0.0398(9) Uani 1 1 d . . .
H27A H 0.8213 0.5940 0.6252 0.060 Uiso 1 1 calc R . .
H27B H 0.7605 0.5251 0.6002 0.060 Uiso 1 1 calc R . .
H27C H 0.8820 0.5234 0.6315 0.060 Uiso 1 1 calc R . .
C28 C 0.8871(3) 0.5686(2) 0.7625(2) 0.0415(9) Uani 1 1 d . . .
H28A H 0.8781 0.5612 0.8113 0.062 Uiso 1 1 calc R . .
H28B H 0.8879 0.6174 0.7530 0.062 Uiso 1 1 calc R . .
H28C H 0.9522 0.5484 0.7572 0.062 Uiso 1 1 calc R . .
C29 C 0.1891(3) 0.57898(15) 0.60155(17) 0.0259(7) Uani 1 1 d . . .
C30 C 0.1801(3) 0.54185(17) 0.53028(19) 0.0346(8) Uani 1 1 d . . .
H30A H 0.2433 0.5485 0.5128 0.052 Uiso 1 1 calc R . .
H30B H 0.1215 0.5600 0.4955 0.052 Uiso 1 1 calc R . .
H30C H 0.1697 0.4933 0.5371 0.052 Uiso 1 1 calc R . .
C31 C 0.0943(3) 0.56853(18) 0.6337(2) 0.0354(8) Uani 1 1 d . . .
H31A H 0.1064 0.5892 0.6811 0.053 Uiso 1 1 calc R . .
H31B H 0.0816 0.5199 0.6376 0.053 Uiso 1 1 calc R . .
H31C H 0.0344 0.5898 0.6029 0.053 Uiso 1 1 calc R . .
C32 C 0.2801(3) 0.54692(17) 0.65333(19) 0.0351(8) Uani 1 1 d . . .
H32A H 0.3429 0.5535 0.6354 0.053 Uiso 1 1 calc R . .
H32B H 0.2676 0.4983 0.6576 0.053 Uiso 1 1 calc R . .
H32C H 0.2882 0.5684 0.7002 0.053 Uiso 1 1 calc R . .
C33 C 0.4808(3) 0.66485(18) 0.54274(17) 0.0296(7) Uani 1 1 d . . .
C34 C 0.4829(3) 0.5939(2) 0.51061(18) 0.0402(9) Uani 1 1 d . . .
H34A H 0.5424 0.5688 0.5372 0.060 Uiso 1 1 calc R . .
H34B H 0.4879 0.5978 0.4606 0.060 Uiso 1 1 calc R . .
H34C H 0.4197 0.5696 0.5134 0.060 Uiso 1 1 calc R . .
C35 C 0.5753(3) 0.7070(2) 0.5375(2) 0.0414(9) Uani 1 1 d . . .
H35A H 0.5689 0.7525 0.5566 0.062 Uiso 1 1 calc R . .
H35B H 0.5804 0.7105 0.4875 0.062 Uiso 1 1 calc R . .
H35C H 0.6372 0.6850 0.5651 0.062 Uiso 1 1 calc R . .
C36 C 0.3881(3) 0.7019(2) 0.49706(18) 0.0410(10) Uani 1 1 d . . .
H36A H 0.3846 0.7481 0.5151 0.061 Uiso 1 1 calc R . .
H36B H 0.3248 0.6775 0.4995 0.061 Uiso 1 1 calc R . .
H36C H 0.3958 0.7036 0.4475 0.061 Uiso 1 1 calc R . .
C37 C 0.1414(2) 0.75187(19) 0.71729(18) 0.0301(7) Uani 1 1 d . . .
H37A H 0.1034 0.7221 0.6791 0.036 Uiso 1 1 calc R . .
H37B H 0.1337 0.7996 0.7009 0.036 Uiso 1 1 calc R . .
C38 C 0.1036(3) 0.7426(2) 0.78536(18) 0.0353(8) Uani 1 1 d . . .
H38A H 0.0866 0.6946 0.7924 0.042 Uiso 1 1 calc R . .
H38B H 0.0424 0.7710 0.7856 0.042 Uiso 1 1 calc R . .
C39 C 0.1947(3) 0.76569(18) 0.84149(17) 0.0291(7) Uani 1 1 d . . .
H39A H 0.1916 0.7475 0.8890 0.035 Uiso 1 1 calc R . .
H39B H 0.1987 0.8158 0.8441 0.035 Uiso 1 1 calc R . .
C40 C 0.2847(3) 0.73626(19) 0.81516(16) 0.0297(7) Uani 1 1 d . . .
H40A H 0.3459 0.7659 0.8285 0.036 Uiso 1 1 calc R . .
H40B H 0.3023 0.6906 0.8356 0.036 Uiso 1 1 calc R . .
C41 C 0.3961(3) 0.86555(17) 0.7059(2) 0.0345(8) Uani 1 1 d . . .
H41A H 0.3276 0.8636 0.7180 0.041 Uiso 1 1 calc R . .
H41B H 0.3908 0.8923 0.6616 0.041 Uiso 1 1 calc R . .
C42 C 0.4745(3) 0.8965(2) 0.7663(2) 0.0421(9) Uani 1 1 d . . .
H42A H 0.4761 0.9465 0.7622 0.051 Uiso 1 1 calc R . .
H42B H 0.4604 0.8841 0.8132 0.051 Uiso 1 1 calc R . .
C43 C 0.5728(3) 0.8652(2) 0.7556(3) 0.0499(11) Uani 1 1 d . . .
H43A H 0.6255 0.8654 0.8006 0.060 Uiso 1 1 calc R . .
H43B H 0.5998 0.8901 0.7188 0.060 Uiso 1 1 calc R . .
C44 C 0.5439(2) 0.79377(18) 0.7319(2) 0.0348(8) Uani 1 1 d . . .
H44A H 0.5852 0.7778 0.6980 0.042 Uiso 1 1 calc R . .
H44B H 0.5548 0.7625 0.7732 0.042 Uiso 1 1 calc R . .
O5 O 0.8222(5) 0.6364(3) 1.0783(3) 0.0807(9) Uiso 0.725(5) 1 d PD A 1
C45 C 0.7640(6) 0.5950(4) 1.1225(4) 0.0807(9) Uiso 0.725(5) 1 d PD A 1
H45A H 0.7143 0.5662 1.0895 0.097 Uiso 0.725(5) 1 calc PR A 1
H45B H 0.7234 0.6267 1.1454 0.097 Uiso 0.725(5) 1 calc PR A 1
C46 C 0.8245(11) 0.5494(5) 1.1801(7) 0.0807(9) Uiso 0.725(5) 1 d PD A 1
H46A H 0.8665 0.5179 1.1589 0.121 Uiso 0.725(5) 1 calc PR A 1
H46B H 0.7768 0.5236 1.2023 0.121 Uiso 0.725(5) 1 calc PR A 1
H46C H 0.8692 0.5772 1.2162 0.121 Uiso 0.725(5) 1 calc PR A 1
C47 C 0.9001(6) 0.6874(4) 1.1240(5) 0.0807(9) Uiso 0.725(5) 1 d PD A 1
H47A H 0.9449 0.6617 1.1630 0.097 Uiso 0.725(5) 1 calc PR A 1
H47B H 0.9446 0.7061 1.0935 0.097 Uiso 0.725(5) 1 calc PR A 1
C48 C 0.8553(8) 0.7435(5) 1.1551(5) 0.0807(9) Uiso 0.725(5) 1 d PD A 1
H48A H 0.8066 0.7261 1.1825 0.121 Uiso 0.725(5) 1 calc PR A 1
H48B H 0.8192 0.7734 1.1172 0.121 Uiso 0.725(5) 1 calc PR A 1
H48C H 0.9098 0.7691 1.1868 0.121 Uiso 0.725(5) 1 calc PR A 1
O5B O 0.8765(12) 0.6231(7) 1.0984(8) 0.0807(9) Uiso 0.275(5) 1 d PD A 2
C45B C 0.9017(15) 0.5846(10) 1.1656(11) 0.0807(9) Uiso 0.275(5) 1 d PD A 2
H45C H 0.9232 0.6177 1.2047 0.097 Uiso 0.275(5) 1 calc PR A 2
H45D H 0.9625 0.5562 1.1640 0.097 Uiso 0.275(5) 1 calc PR A 2
C46B C 0.821(3) 0.5388(14) 1.186(2) 0.0807(9) Uiso 0.275(5) 1 d PD A 2
H46D H 0.7647 0.5665 1.1956 0.121 Uiso 0.275(5) 1 calc PR A 2
H46E H 0.8524 0.5131 1.2290 0.121 Uiso 0.275(5) 1 calc PR A 2
H46F H 0.7952 0.5073 1.1470 0.121 Uiso 0.275(5) 1 calc PR A 2
C47B C 0.7798(14) 0.6754(10) 1.1076(11) 0.0807(9) Uiso 0.275(5) 1 d PD A 2
H47C H 0.7484 0.6962 1.0611 0.097 Uiso 0.275(5) 1 calc PR A 2
H47D H 0.7260 0.6495 1.1246 0.097 Uiso 0.275(5) 1 calc PR A 2
C48B C 0.822(2) 0.7286(12) 1.1596(14) 0.0807(9) Uiso 0.275(5) 1 d PD A 2
H48D H 0.8536 0.7075 1.2053 0.121 Uiso 0.275(5) 1 calc PR A 2
H48E H 0.7671 0.7592 1.1660 0.121 Uiso 0.275(5) 1 calc PR A 2
H48F H 0.8747 0.7544 1.1420 0.121 Uiso 0.275(5) 1 calc PR A 2
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'
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
O2 Hf1 O1 159.64(8) . . ?
O2 Hf1 N1 116.63(9) . . ?
O1 Hf1 N1 76.97(9) . . ?
O2 Hf1 N2 77.09(8) . . ?
O1 Hf1 N2 116.04(9) . . ?
N1 Hf1 N2 103.31(10) . . ?
O2 Hf1 O3 78.73(8) . . ?
O1 Hf1 O3 86.62(8) . . ?
N1 Hf1 O3 89.78(9) . . ?
N2 Hf1 O3 155.68(8) . . ?
O2 Hf1 O4 85.48(8) . . ?
O1 Hf1 O4 78.88(8) . . ?
N1 Hf1 O4 155.31(9) . . ?
N2 Hf1 O4 91.82(9) . . ?
O3 Hf1 O4 83.72(8) . . ?
C1 O1 Hf1 118.54(17) . . ?
C15 O2 Hf1 118.50(17) . . ?
C37 O3 C40 109.3(2) . . ?
C37 O3 Hf1 121.71(17) . . ?
C40 O3 Hf1 128.98(18) . . ?
C41 O4 C44 109.4(2) . . ?
C41 O4 Hf1 127.12(18) . . ?
C44 O4 Hf1 122.71(19) . . ?
C6 N1 C29 119.4(2) . . ?
C6 N1 Hf1 114.71(18) . . ?
C29 N1 Hf1 125.84(19) . . ?
C20 N2 C33 119.0(2) . . ?
C20 N2 Hf1 114.42(18) . . ?
C33 N2 Hf1 126.59(19) . . ?
O1 C1 C2 122.7(3) . . ?
O1 C1 C6 115.4(2) . . ?
C2 C1 C6 121.9(3) . . ?
C1 C2 C3 117.5(3) . . ?
C1 C2 C7 121.8(3) . . ?
C3 C2 C7 120.7(3) . . ?
C4 C3 C2 122.4(3) . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 C11 122.6(3) . . ?
C5 C4 C11 118.6(3) . . ?
C6 C5 C4 121.9(3) . . ?
C5 C6 N1 128.1(3) . . ?
C5 C6 C1 117.6(3) . . ?
N1 C6 C1 114.3(3) . . ?
C8 C7 C9 107.3(3) . . ?
C8 C7 C2 112.4(2) . . ?
C9 C7 C2 109.4(2) . . ?
C8 C7 C10 107.8(3) . . ?
C9 C7 C10 109.9(3) . . ?
C2 C7 C10 110.1(2) . . ?
C14 C11 C12 108.9(3) . . ?
C14 C11 C13 108.8(3) . . ?
C12 C11 C13 107.9(3) . . ?
C14 C11 C4 109.5(3) . . ?
C12 C11 C4 109.7(3) . . ?
C13 C11 C4 112.0(3) . . ?
O2 C15 C16 123.0(3) . . ?
O2 C15 C20 115.1(2) . . ?
C16 C15 C20 121.9(3) . . ?
C17 C16 C15 117.6(3) . . ?
C17 C16 C21 121.7(3) . . ?
C15 C16 C21 120.7(3) . . ?
C16 C17 C18 122.6(3) . . ?
C19 C18 C17 118.2(3) . . ?
C19 C18 C25 121.4(3) . . ?
C17 C18 C25 120.4(3) . . ?
C18 C19 C20 122.4(3) . . ?
C19 C20 N2 127.9(3) . . ?
C19 C20 C15 117.3(3) . . ?
N2 C20 C15 114.8(2) . . ?
C23 C21 C22 107.2(3) . . ?
C23 C21 C24 110.2(3) . . ?
C22 C21 C24 107.3(3) . . ?
C23 C21 C16 110.4(3) . . ?
C22 C21 C16 112.0(3) . . ?
C24 C21 C16 109.7(3) . . ?
C28 C25 C26 108.8(3) . . ?
C28 C25 C27 108.1(3) . . ?
C26 C25 C27 107.6(3) . . ?
C28 C25 C18 109.7(3) . . ?
C26 C25 C18 110.0(3) . . ?
C27 C25 C18 112.5(3) . . ?
N1 C29 C32 108.0(3) . . ?
N1 C29 C31 110.6(3) . . ?
C32 C29 C31 106.7(3) . . ?
N1 C29 C30 112.3(3) . . ?
C32 C29 C30 106.4(3) . . ?
C31 C29 C30 112.5(3) . . ?
N2 C33 C35 111.7(3) . . ?
N2 C33 C34 112.0(3) . . ?
C35 C33 C34 112.5(3) . . ?
N2 C33 C36 107.6(2) . . ?
C35 C33 C36 106.0(3) . . ?
C34 C33 C36 106.6(3) . . ?
O3 C37 C38 103.6(3) . . ?
C37 C38 C39 102.5(3) . . ?
C38 C39 C40 102.6(3) . . ?
O3 C40 C39 105.2(3) . . ?
O4 C41 C42 105.0(3) . . ?
C43 C42 C41 102.0(3) . . ?
C42 C43 C44 104.6(3) . . ?
O4 C44 C43 104.8(3) . . ?
C45 O5 C47 113.0(6) . . ?
O5 C45 C46 118.4(7) . . ?
C48 C47 O5 116.0(7) . . ?
C45B O5B C47B 105.0(13) . . ?
O5B C45B C46B 120(2) . . ?
C48B C47B O5B 108.3(16) . . ?
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 2.0456(19) . ?
Hf1 O1 2.047(2) . ?
Hf1 N1 2.117(2) . ?
Hf1 N2 2.117(2) . ?
Hf1 O3 2.254(2) . ?
Hf1 O4 2.261(2) . ?
O1 C1 1.362(3) . ?
O2 C15 1.366(3) . ?
O3 C37 1.467(4) . ?
O3 C40 1.469(4) . ?
O4 C41 1.458(4) . ?
O4 C44 1.468(4) . ?
N1 C6 1.412(4) . ?
N1 C29 1.493(4) . ?
N2 C20 1.410(4) . ?
N2 C33 1.494(4) . ?
C1 C2 1.403(4) . ?
C1 C6 1.424(4) . ?
C2 C3 1.410(4) . ?
C2 C7 1.538(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.404(4) . ?
C4 C11 1.542(4) . ?
C5 C6 1.397(4) . ?
C7 C8 1.525(4) . ?
C7 C9 1.534(4) . ?
C7 C10 1.540(4) . ?
C11 C14 1.525(5) . ?
C11 C12 1.533(5) . ?
C11 C13 1.534(5) . ?
C15 C16 1.401(4) . ?
C15 C20 1.423(4) . ?
C16 C17 1.395(4) . ?
C16 C21 1.544(4) . ?
C17 C18 1.397(4) . ?
C18 C19 1.389(4) . ?
C18 C25 1.537(4) . ?
C19 C20 1.399(4) . ?
C21 C23 1.529(5) . ?
C21 C22 1.531(4) . ?
C21 C24 1.539(4) . ?
C25 C28 1.524(5) . ?
C25 C26 1.526(5) . ?
C25 C27 1.528(4) . ?
C29 C32 1.530(5) . ?
C29 C31 1.535(5) . ?
C29 C30 1.535(5) . ?
C33 C35 1.530(5) . ?
C33 C34 1.532(5) . ?
C33 C36 1.537(4) . ?
C37 C38 1.510(5) . ?
C38 C39 1.511(5) . ?
C39 C40 1.513(4) . ?
C41 C42 1.513(5) . ?
C42 C43 1.501(6) . ?
C43 C44 1.505(5) . ?
O5 C45 1.507(9) . ?
O5 C47 1.572(9) . ?
C45 C46 1.517(14) . ?
C47 C48 1.446(11) . ?
O5B C45B 1.473(16) . ?
O5B C47B 1.689(16) . ?
C45B C46B 1.52(2) . ?
C47B C48B 1.475(18) . ?
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
O2 Hf1 O1 C1 -134.4(2) . . . . ?
N1 Hf1 O1 C1 -0.04(19) . . . . ?
N2 Hf1 O1 C1 98.6(2) . . . . ?
O3 Hf1 O1 C1 -90.6(2) . . . . ?
O4 Hf1 O1 C1 -174.9(2) . . . . ?
O1 Hf1 O2 C15 -130.5(2) . . . . ?
N1 Hf1 O2 C15 100.7(2) . . . . ?
N2 Hf1 O2 C15 2.1(2) . . . . ?
O3 Hf1 O2 C15 -175.2(2) . . . . ?
O4 Hf1 O2 C15 -90.8(2) . . . . ?
O2 Hf1 O3 C37 -156.6(2) . . . . ?
O1 Hf1 O3 C37 37.6(2) . . . . ?
N1 Hf1 O3 C37 -39.4(2) . . . . ?
N2 Hf1 O3 C37 -162.8(2) . . . . ?
O4 Hf1 O3 C37 116.7(2) . . . . ?
O2 Hf1 O3 C40 24.8(3) . . . . ?
O1 Hf1 O3 C40 -140.9(3) . . . . ?
N1 Hf1 O3 C40 142.1(3) . . . . ?
N2 Hf1 O3 C40 18.7(4) . . . . ?
O4 Hf1 O3 C40 -61.8(3) . . . . ?
O2 Hf1 O4 C41 -131.0(3) . . . . ?
O1 Hf1 O4 C41 35.9(3) . . . . ?
N1 Hf1 O4 C41 23.8(4) . . . . ?
N2 Hf1 O4 C41 152.1(3) . . . . ?
O3 Hf1 O4 C41 -51.8(3) . . . . ?
O2 Hf1 O4 C44 38.0(2) . . . . ?
O1 Hf1 O4 C44 -155.1(3) . . . . ?
N1 Hf1 O4 C44 -167.3(3) . . . . ?
N2 Hf1 O4 C44 -38.9(2) . . . . ?
O3 Hf1 O4 C44 117.1(2) . . . . ?
O2 Hf1 N1 C6 163.12(18) . . . . ?
O1 Hf1 N1 C6 -0.73(19) . . . . ?
N2 Hf1 N1 C6 -114.8(2) . . . . ?
O3 Hf1 N1 C6 85.9(2) . . . . ?
O4 Hf1 N1 C6 11.5(3) . . . . ?
O2 Hf1 N1 C29 -15.8(3) . . . . ?
O1 Hf1 N1 C29 -179.6(2) . . . . ?
N2 Hf1 N1 C29 66.3(2) . . . . ?
O3 Hf1 N1 C29 -93.0(2) . . . . ?
O4 Hf1 N1 C29 -167.3(2) . . . . ?
O2 Hf1 N2 C20 -2.8(2) . . . . ?
O1 Hf1 N2 C20 160.68(19) . . . . ?
N1 Hf1 N2 C20 -117.5(2) . . . . ?
O3 Hf1 N2 C20 3.5(4) . . . . ?
O4 Hf1 N2 C20 82.2(2) . . . . ?
O2 Hf1 N2 C33 176.6(3) . . . . ?
O1 Hf1 N2 C33 -19.9(3) . . . . ?
N1 Hf1 N2 C33 61.9(3) . . . . ?
O3 Hf1 N2 C33 -177.1(2) . . . . ?
O4 Hf1 N2 C33 -98.4(3) . . . . ?
Hf1 O1 C1 C2 -179.7(2) . . . . ?
Hf1 O1 C1 C6 0.8(3) . . . . ?
O1 C1 C2 C3 -178.9(3) . . . . ?
C6 C1 C2 C3 0.6(4) . . . . ?
O1 C1 C2 C7 0.3(4) . . . . ?
C6 C1 C2 C7 179.9(3) . . . . ?
C1 C2 C3 C4 0.7(4) . . . . ?
C7 C2 C3 C4 -178.5(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C2 C3 C4 C11 177.6(3) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C11 C4 C5 C6 -178.7(3) . . . . ?
C4 C5 C6 N1 -179.4(3) . . . . ?
C4 C5 C6 C1 1.4(4) . . . . ?
C29 N1 C6 C5 1.1(4) . . . . ?
Hf1 N1 C6 C5 -177.9(2) . . . . ?
C29 N1 C6 C1 -179.7(3) . . . . ?
Hf1 N1 C6 C1 1.4(3) . . . . ?
O1 C1 C6 C5 177.9(3) . . . . ?
C2 C1 C6 C5 -1.6(4) . . . . ?
O1 C1 C6 N1 -1.4(4) . . . . ?
C2 C1 C6 N1 179.0(3) . . . . ?
C1 C2 C7 C8 179.2(3) . . . . ?
C3 C2 C7 C8 -1.6(4) . . . . ?
C1 C2 C7 C9 -61.8(4) . . . . ?
C3 C2 C7 C9 117.4(3) . . . . ?
C1 C2 C7 C10 59.0(4) . . . . ?
C3 C2 C7 C10 -121.7(3) . . . . ?
C3 C4 C11 C14 -116.6(3) . . . . ?
C5 C4 C11 C14 62.0(4) . . . . ?
C3 C4 C11 C12 123.9(3) . . . . ?
C5 C4 C11 C12 -57.5(4) . . . . ?
C3 C4 C11 C13 4.2(4) . . . . ?
C5 C4 C11 C13 -177.3(3) . . . . ?
Hf1 O2 C15 C16 178.3(2) . . . . ?
Hf1 O2 C15 C20 -1.2(3) . . . . ?
O2 C15 C16 C17 -177.9(3) . . . . ?
C20 C15 C16 C17 1.6(4) . . . . ?
O2 C15 C16 C21 2.1(4) . . . . ?
C20 C15 C16 C21 -178.5(3) . . . . ?
C15 C16 C17 C18 0.1(5) . . . . ?
C21 C16 C17 C18 -179.9(3) . . . . ?
C16 C17 C18 C19 -1.3(5) . . . . ?
C16 C17 C18 C25 178.4(3) . . . . ?
C17 C18 C19 C20 0.9(5) . . . . ?
C25 C18 C19 C20 -178.8(3) . . . . ?
C18 C19 C20 N2 179.3(3) . . . . ?
C18 C19 C20 C15 0.6(5) . . . . ?
C33 N2 C20 C19 4.9(5) . . . . ?
Hf1 N2 C20 C19 -175.7(3) . . . . ?
C33 N2 C20 C15 -176.4(3) . . . . ?
Hf1 N2 C20 C15 3.0(3) . . . . ?
O2 C15 C20 C19 177.6(3) . . . . ?
C16 C15 C20 C19 -1.9(4) . . . . ?
O2 C15 C20 N2 -1.3(4) . . . . ?
C16 C15 C20 N2 179.2(3) . . . . ?
C17 C16 C21 C23 -122.3(3) . . . . ?
C15 C16 C21 C23 57.8(4) . . . . ?
C17 C16 C21 C22 -2.9(4) . . . . ?
C15 C16 C21 C22 177.1(3) . . . . ?
C17 C16 C21 C24 116.1(3) . . . . ?
C15 C16 C21 C24 -63.8(4) . . . . ?
C19 C18 C25 C28 121.1(3) . . . . ?
C17 C18 C25 C28 -58.6(4) . . . . ?
C19 C18 C25 C26 -119.2(3) . . . . ?
C17 C18 C25 C26 61.1(4) . . . . ?
C19 C18 C25 C27 0.7(4) . . . . ?
C17 C18 C25 C27 -179.0(3) . . . . ?
C6 N1 C29 C32 177.1(3) . . . . ?
Hf1 N1 C29 C32 -4.0(4) . . . . ?
C6 N1 C29 C31 -66.4(4) . . . . ?
Hf1 N1 C29 C31 112.4(3) . . . . ?
C6 N1 C29 C30 60.1(4) . . . . ?
Hf1 N1 C29 C30 -121.0(3) . . . . ?
C20 N2 C33 C35 -66.9(4) . . . . ?
Hf1 N2 C33 C35 113.8(3) . . . . ?
C20 N2 C33 C34 60.4(4) . . . . ?
Hf1 N2 C33 C34 -119.0(3) . . . . ?
C20 N2 C33 C36 177.2(3) . . . . ?
Hf1 N2 C33 C36 -2.2(4) . . . . ?
C40 O3 C37 C38 -19.7(4) . . . . ?
Hf1 O3 C37 C38 161.5(2) . . . . ?
O3 C37 C38 C39 37.1(4) . . . . ?
C37 C38 C39 C40 -40.4(4) . . . . ?
C37 O3 C40 C39 -5.6(4) . . . . ?
Hf1 O3 C40 C39 173.1(2) . . . . ?
C38 C39 C40 O3 28.6(4) . . . . ?
C44 O4 C41 C42 -17.8(4) . . . . ?
Hf1 O4 C41 C42 152.4(2) . . . . ?
O4 C41 C42 C43 33.8(4) . . . . ?
C41 C42 C43 C44 -37.4(4) . . . . ?
C41 O4 C44 C43 -5.6(4) . . . . ?
Hf1 O4 C44 C43 -176.3(3) . . . . ?
C42 C43 C44 O4 27.1(4) . . . . ?
C47 O5 C45 C46 -60.6(10) . . . . ?
C45 O5 C47 C48 -69.0(10) . . . . ?
C47B O5B C45B C46B 62(2) . . . . ?
C45B O5B C47B C48B 72(2) . . . . ?
