#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322202.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_4322202
loop_
_publ_author_name
'Joseph L. Thorman'
'Ilia A. Guzei'
'Victor G. Young'
'L. Keith Woo'
_publ_contact_author_address
;
   Department of Chemistry
   Iowa State University of Science and Technology
   Ames, Iowa, 50011
   USA
;
_publ_contact_author_email       iguzei@iastate.edu
_publ_contact_author_fax         +515-294-5717
_publ_contact_author_name
;
Ilia A. Guzei
;
_publ_contact_author_phone       +515-294-6419
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Zirconium and Hafnium Imido
 Metalloporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3814
_journal_page_last               3824
_journal_paper_doi               10.1021/ic981399j
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'J. Thorman / Prof. K. Woo - ISU'
_chemical_formula_sum            'C70.5 H69 Hf N5'
_chemical_formula_weight         1164.80
_chemical_name_common            98063
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.029(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6081(2)
_cell_length_b                   18.6360(3)
_cell_length_c                   19.3910(1)
_cell_measurement_temperature    173(2)
_cell_volume                     5822.67(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32323
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996) '
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       Block
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.444
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_obs          0.0263
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0208P)²+6.0854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0602
_refine_ls_wR_factor_obs         0.0573
_reflns_number_observed          9002
_reflns_number_total             10215
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981399j_2.cif
_cod_data_source_block           98063
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+6.0854P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+6.0854P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1'
_cod_original_formula_sum        'C70.50 H69 Hf N5'
_cod_database_code               4322202
loop_
_symmetry_equiv_pos_as_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Hf1 Hf -0.087843(7) 0.852927(6) 0.366437(6) 0.01930(4) Uani 1 d . .
N1 N -0.05394(14) 0.89105(12) 0.27095(12) 0.0225(5) Uani 1 d . .
N2 N -0.21251(14) 0.88714(12) 0.31219(12) 0.0220(5) Uani 1 d . .
N3 N -0.12337(14) 0.89067(12) 0.46204(12) 0.0223(5) Uani 1 d . .
N4 N 0.03442(14) 0.89506(12) 0.42062(12) 0.0219(5) Uani 1 d . .
C1 C 0.0252(2) 0.9030(2) 0.2622(2) 0.0255(6) Uani 1 d . .
C2 C 0.0209(2) 0.9055(2) 0.1872(2) 0.0324(7) Uani 1 d . .
H2A H 0.0662(2) 0.9129(2) 0.1662(2) 0.039 Uiso 1 calc R .
C3 C -0.0589(2) 0.8953(2) 0.1522(2) 0.0317(7) Uani 1 d . .
H3A H -0.0796(2) 0.8939(2) 0.1020(2) 0.038 Uiso 1 calc R .
C4 C -0.1068(2) 0.8870(2) 0.20389(15) 0.0254(6) Uani 1 d . .
C5 C -0.1935(2) 0.8796(2) 0.18916(15) 0.0254(6) Uani 1 d . .
C6 C -0.2423(2) 0.88091(15) 0.23918(15) 0.0234(6) Uani 1 d . .
C7 C -0.3309(2) 0.8750(2) 0.2235(2) 0.0285(7) Uani 1 d . .
H7A H -0.3669(2) 0.8707(2) 0.1775(2) 0.034 Uiso 1 calc R .
C8 C -0.3544(2) 0.8767(2) 0.2856(2) 0.0293(7) Uani 1 d . .
H8A H -0.4095(2) 0.8732(2) 0.2911(2) 0.035 Uiso 1 calc R .
C9 C -0.2801(2) 0.88477(15) 0.3420(2) 0.0237(6) Uani 1 d . .
C10 C -0.2768(2) 0.8870(2) 0.4152(2) 0.0253(6) Uani 1 d . .
C11 C -0.2040(2) 0.8919(2) 0.4706(2) 0.0244(6) Uani 1 d . .
C12 C -0.2011(2) 0.8966(2) 0.5448(2) 0.0281(7) Uani 1 d . .
H12A H -0.2476(2) 0.8994(2) 0.5653(2) 0.034 Uiso 1 calc R .
C13 C -0.1204(2) 0.8962(2) 0.5806(2) 0.0268(7) Uani 1 d . .
H13A H -0.0999(2) 0.8978(2) 0.6307(2) 0.032 Uiso 1 calc R .
C14 C -0.0710(2) 0.89306(14) 0.52940(15) 0.0226(6) Uani 1 d . .
C15 C 0.0166(2) 0.89329(14) 0.54436(15) 0.0240(6) Uani 1 d . .
C16 C 0.0642(2) 0.89888(14) 0.49349(15) 0.0231(6) Uani 1 d . .
C17 C 0.1513(2) 0.9152(2) 0.5093(2) 0.0278(7) Uani 1 d . .
H17A H 0.1870(2) 0.9203(2) 0.5554(2) 0.033 Uiso 1 calc R .
C18 C 0.1734(2) 0.9218(2) 0.4470(2) 0.0273(7) Uani 1 d . .
H18A H 0.2272(2) 0.9331(2) 0.4413(2) 0.033 Uiso 1 calc R .
C19 C 0.1004(2) 0.90850(15) 0.39064(15) 0.0233(6) Uani 1 d . .
C20 C 0.0969(2) 0.91180(15) 0.3176(2) 0.0243(6) Uani 1 d . .
C21 C -0.2378(2) 0.8682(2) 0.11271(15) 0.0275(7) Uani 1 d . .
C22 C -0.2348(2) 0.8019(2) 0.0820(2) 0.0449(9) Uani 1 d . .
H22A H -0.2036(2) 0.7644(2) 0.1093(2) 0.054 Uiso 1 calc R .
C23 C -0.2764(2) 0.7890(2) 0.0120(2) 0.0514(10) Uani 1 d . .
H23A H -0.2733(2) 0.7427(2) -0.0077(2) 0.062 Uiso 1 calc R .
C24 C -0.3220(2) 0.8416(2) -0.0294(2) 0.0431(9) Uani 1 d . .
C25 C -0.3241(2) 0.9083(2) 0.0013(2) 0.0493(10) Uani 1 d . .
H25A H -0.3546(2) 0.9459(2) -0.0265(2) 0.059 Uiso 1 calc R .
C26 C -0.2828(2) 0.9223(2) 0.0715(2) 0.0402(8) Uani 1 d . .
H26A H -0.2855(2) 0.9687(2) 0.0912(2) 0.048 Uiso 1 calc R .
C27 C -0.3696(2) 0.8273(3) -0.1046(2) 0.0710(14) Uani 1 d . .
H27A H -0.3977(2) 0.7811(3) -0.1069(2) 0.106 Uiso 1 d R .
H27B H -0.3312(2) 0.8265(3) -0.1357(2) 0.106 Uiso 1 d R .
H27C H -0.4108(2) 0.8650(3) -0.1201(2) 0.106 Uiso 1 d R .
C28 C -0.3567(2) 0.8806(2) 0.4367(2) 0.0300(7) Uani 1 d . .
C29 C -0.3727(2) 0.8203(2) 0.4737(2) 0.0425(8) Uani 1 d . .
H29A H -0.3318(2) 0.7838(2) 0.4862(2) 0.051 Uiso 1 calc R .
C30 C -0.4478(2) 0.8131(2) 0.4926(2) 0.0518(10) Uani 1 d . .
H30A H -0.4575(2) 0.7716(2) 0.5178(2) 0.062 Uiso 1 calc R .
C31 C -0.5084(2) 0.8648(3) 0.4755(2) 0.0519(11) Uani 1 d . .
C32 C -0.4924(2) 0.9245(2) 0.4397(2) 0.0509(10) Uani 1 d . .
H32A H -0.5334(2) 0.9610(2) 0.4278(2) 0.061 Uiso 1 calc R .
C33 C -0.4178(2) 0.9330(2) 0.4204(2) 0.0421(8) Uani 1 d . .
H33A H -0.4084(2) 0.9751(2) 0.3957(2) 0.050 Uiso 1 calc R .
C34 C -0.5913(2) 0.8553(3) 0.4949(2) 0.081(2) Uani 1 d . .
H34A H -0.5854(2) 0.8201(3) 0.5330(2) 0.121 Uiso 1 d R .
H34B H -0.6329(2) 0.8387(3) 0.4532(2) 0.121 Uiso 1 d R .
H34C H -0.6090(2) 0.9010(3) 0.5108(2) 0.121 Uiso 1 d R .
C35 C 0.0636(2) 0.8870(2) 0.62033(15) 0.0252(6) Uani 1 d . .
C36 C 0.1159(2) 0.8281(2) 0.6417(2) 0.0288(7) Uani 1 d . .
H36A H 0.1219(2) 0.7932(2) 0.6076(2) 0.035 Uiso 1 calc R .
C37 C 0.1588(2) 0.8202(2) 0.7118(2) 0.0339(7) Uani 1 d . .
H37A H 0.1932(2) 0.7794(2) 0.7252(2) 0.041 Uiso 1 calc R .
C38 C 0.1528(2) 0.8705(2) 0.7630(2) 0.0329(7) Uani 1 d . .
C39 C 0.1017(2) 0.9296(2) 0.7415(2) 0.0352(7) Uani 1 d . .
H39A H 0.0968(2) 0.9649(2) 0.7756(2) 0.042 Uiso 1 calc R .
C40 C 0.0578(2) 0.9379(2) 0.6713(2) 0.0292(7) Uani 1 d . .
H40A H 0.0235(2) 0.9789(2) 0.6580(2) 0.035 Uiso 1 calc R .
C41 C 0.2001(2) 0.8615(2) 0.8399(2) 0.0497(10) Uani 1 d . .
H41A H 0.2143(2) 0.8111(2) 0.8494(2) 0.075 Uiso 1 d R .
H41B H 0.1655(2) 0.8776(2) 0.8712(2) 0.075 Uiso 1 d R .
H41C H 0.2509(2) 0.8900(2) 0.8488(2) 0.075 Uiso 1 d R .
C42 C 0.1766(2) 0.9273(2) 0.2970(2) 0.0264(6) Uani 1 d . .
C43 C 0.2417(2) 0.8789(2) 0.3113(2) 0.0353(7) Uani 1 d . .
H43A H 0.2356(2) 0.8349(2) 0.3342(2) 0.042 Uiso 1 calc R .
C44 C 0.3157(2) 0.8934(2) 0.2928(2) 0.0399(8) Uani 1 d . .
H44A H 0.3596(2) 0.8594(2) 0.3037(2) 0.048 Uiso 1 calc R .
C45 C 0.3265(2) 0.9563(2) 0.2589(2) 0.0422(8) Uani 1 d . .
C46 C 0.2614(2) 1.0055(2) 0.2449(2) 0.0450(9) Uani 1 d . .
H46A H 0.2678(2) 1.0495(2) 0.2220(2) 0.054 Uiso 1 calc R .
C47 C 0.1875(2) 0.9915(2) 0.2636(2) 0.0380(8) Uani 1 d . .
H47A H 0.1440(2) 1.0259(2) 0.2536(2) 0.046 Uiso 1 calc R .
C48 C 0.4070(2) 0.9713(3) 0.2373(2) 0.0649(12) Uani 1 d . .
H48A H 0.4017(2) 1.0165(3) 0.2114(2) 0.097 Uiso 1 d R .
H48B H 0.4183(2) 0.9328(3) 0.2068(2) 0.097 Uiso 1 d R .
H48C H 0.4526(2) 0.9745(3) 0.2798(2) 0.097 Uiso 1 d R .
N5 N -0.08781(14) 0.75321(12) 0.36357(12) 0.0240(5) Uani 1 d . .
C49 C -0.0823(2) 0.67981(15) 0.36943(15) 0.0224(6) Uani 1 d . .
C50 C -0.0890(2) 0.6357(2) 0.3082(2) 0.0262(6) Uani 1 d . .
C51 C -0.0794(2) 0.5620(2) 0.3169(2) 0.0319(7) Uani 1 d . .
H51A H -0.0840(2) 0.5324(2) 0.2762(2) 0.038 Uiso 1 calc R .
C52 C -0.0634(2) 0.5305(2) 0.3839(2) 0.0384(8) Uani 1 d . .
H52A H -0.0556(2) 0.4801(2) 0.3889(2) 0.046 Uiso 1 calc R .
C53 C -0.0589(2) 0.5730(2) 0.4431(2) 0.0338(7) Uani 1 d . .
H53A H -0.0494(2) 0.5512(2) 0.4887(2) 0.041 Uiso 1 calc R .
C54 C -0.0680(2) 0.6472(2) 0.4373(2) 0.0272(6) Uani 1 d . .
C55 C -0.1054(2) 0.6699(2) 0.2354(2) 0.0307(7) Uani 1 d . .
H55A H -0.1432(2) 0.7117(2) 0.2355(2) 0.037 Uiso 1 calc R .
C56 C -0.1493(2) 0.6192(2) 0.1756(2) 0.0422(8) Uani 1 d . .
H56A H -0.1972(2) 0.5972(2) 0.1883(2) 0.063 Uiso 1 d R .
H56B H -0.1107(2) 0.5819(2) 0.1686(2) 0.063 Uiso 1 d R .
H56C H -0.1680(2) 0.6465(2) 0.1317(2) 0.063 Uiso 1 d R .
C57 C -0.0250(2) 0.6992(2) 0.2207(2) 0.0435(8) Uani 1 d . .
H57A H 0.0007(2) 0.7326(2) 0.2584(2) 0.065 Uiso 1 d R .
H57B H -0.0379(2) 0.7240(2) 0.1750(2) 0.065 Uiso 1 d R .
H57C H 0.0132(2) 0.6598(2) 0.2193(2) 0.065 Uiso 1 d R .
C58 C -0.0670(2) 0.6937(2) 0.5015(2) 0.0296(7) Uani 1 d . .
H58A H -0.0414(2) 0.7405(2) 0.4934(2) 0.035 Uiso 1 calc R .
C59 C -0.1551(2) 0.7095(2) 0.5060(2) 0.0447(9) Uani 1 d . .
H59A H -0.1538(2) 0.7435(2) 0.5445(2) 0.067 Uiso 1 d R .
H59B H -0.1824(2) 0.6654(2) 0.5153(2) 0.067 Uiso 1 d R .
H59C H -0.1859(2) 0.7302(2) 0.4611(2) 0.067 Uiso 1 d R .
C60 C -0.0160(2) 0.6641(2) 0.5714(2) 0.0455(9) Uani 1 d . .
H60A H 0.0392(2) 0.6512(2) 0.5659(2) 0.068 Uiso 1 d R .
H60B H -0.0434(2) 0.6217(2) 0.5844(2) 0.068 Uiso 1 d R .
H60C H -0.0108(2) 0.7002(2) 0.6086(2) 0.068 Uiso 1 d R .
C61 C 0.3061(3) 0.7084(2) 0.2487(3) 0.0677(13) Uani 1 d . .
C62 C 0.3707(3) 0.7262(3) 0.2178(3) 0.0740(14) Uani 1 d . .
H62A H 0.3585(3) 0.7397(3) 0.1691(3) 0.089 Uiso 1 calc R .
C63 C 0.4509(3) 0.7246(3) 0.2559(3) 0.085(2) Uani 1 d . .
H63A H 0.4940(3) 0.7358(3) 0.2332(3) 0.102 Uiso 1 calc R .
C64 C 0.4702(3) 0.7074(3) 0.3249(3) 0.096(2) Uani 1 d . .
H64A H 0.5266(3) 0.7077(3) 0.3509(3) 0.115 Uiso 1 calc R .
C65 C 0.4101(3) 0.6895(3) 0.3581(3) 0.088(2) Uani 1 d . .
H65A H 0.4242(3) 0.6770(3) 0.4070(3) 0.106 Uiso 1 calc R .
C66 C 0.3290(3) 0.6895(3) 0.3208(3) 0.0728(13) Uani 1 d . .
H66A H 0.2871(3) 0.6764(3) 0.3442(3) 0.087 Uiso 1 calc R .
C67 C 0.2172(4) 0.7097(4) 0.2071(3) 0.114(2) Uani 1 d . .
H67A H 0.2117(4) 0.7394(4) 0.1647(3) 0.171 Uiso 1 d R .
H67B H 0.1823(4) 0.7291(4) 0.2366(3) 0.171 Uiso 1 d R .
H67C H 0.1996(4) 0.6609(4) 0.1928(3) 0.171 Uiso 1 d R .
C68 C -0.0346(3) 1.0276(3) -0.0006(3) 0.0801(15) Uani 1 d . .
H68A H -0.0380(3) 1.0374(3) 0.0488(3) 0.096 Uiso 1 calc R .
H68B H -0.0200(3) 1.0731(3) -0.0209(3) 0.096 Uiso 1 calc R .
C69 C -0.1189(3) 1.0030(3) -0.0434(3) 0.085(2) Uani 1 d . .
H69A H -0.1342(3) 0.9583(3) -0.0220(3) 0.102 Uiso 1 calc R 1
H69B H -0.1148(3) 0.9915(3) -0.0923(3) 0.102 Uiso 1 calc R 1
C70 C -0.1876(4) 1.0581(4) -0.0474(3) 0.107(2) Uani 0.50 d P 1
H70A H -0.2187(4) 1.0476(4) -0.0117(3) 0.161 Uiso 0.50 d PR 1
H70B H -0.2252(4) 1.0569(4) -0.0947(3) 0.161 Uiso 0.50 d PR 1
H70C H -0.1625(4) 1.1055(4) -0.0385(3) 0.161 Uiso 0.50 d PR 1
C70' C -0.1876(4) 1.0581(4) -0.0474(3) 0.107(2) Uani 0.50 d P 2
H70D H -0.2411(7) 1.0339(6) -0.0680(6) 0.129 Uiso 0.50 calc PR 2
H70E H -0.1878(7) 1.0716(6) 0.0020(6) 0.129 Uiso 0.50 calc PR 2
C71' C -0.1859(7) 1.1241(6) -0.0872(6) 0.091(3) Uani 0.50 d P 2
H71A H -0.2354(7) 1.1519(6) -0.0862(6) 0.137 Uiso 0.50 d PR 2
H71B H -0.1855(7) 1.1134(6) -0.1365(6) 0.137 Uiso 0.50 d PR 2
H71C H -0.1363(7) 1.1517(6) -0.0652(6) 0.137 Uiso 0.50 d PR 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'
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
N5 Hf1 N2 106.57(9) . . ?
N5 Hf1 N1 107.35(9) . . ?
N2 Hf1 N1 84.58(8) . . ?
N5 Hf1 N4 111.42(9) . . ?
N2 Hf1 N4 142.00(8) . . ?
N1 Hf1 N4 83.71(8) . . ?
N5 Hf1 N3 110.36(9) . . ?
N2 Hf1 N3 83.99(8) . . ?
N1 Hf1 N3 142.27(8) . . ?
N4 Hf1 N3 83.56(8) . . ?
C4 N1 C1 107.4(2) . . ?
C4 N1 Hf1 123.0(2) . . ?
C1 N1 Hf1 127.2(2) . . ?
C9 N2 C6 107.4(2) . . ?
C9 N2 Hf1 124.2(2) . . ?
C6 N2 Hf1 122.0(2) . . ?
C14 N3 C11 106.9(2) . . ?
C14 N3 Hf1 124.9(2) . . ?
C11 N3 Hf1 124.8(2) . . ?
C16 N4 C19 107.3(2) . . ?
C16 N4 Hf1 124.7(2) . . ?
C19 N4 Hf1 126.8(2) . . ?
N1 C1 C20 125.3(3) . . ?
N1 C1 C2 108.2(2) . . ?
C20 C1 C2 126.4(3) . . ?
C3 C2 C1 107.9(3) . . ?
C2 C3 C4 107.9(3) . . ?
N1 C4 C5 125.6(3) . . ?
N1 C4 C3 108.5(2) . . ?
C5 C4 C3 125.8(3) . . ?
C4 C5 C6 126.2(3) . . ?
C4 C5 C21 116.6(3) . . ?
C6 C5 C21 117.2(2) . . ?
N2 C6 C5 125.7(2) . . ?
N2 C6 C7 108.5(2) . . ?
C5 C6 C7 125.9(3) . . ?
C8 C7 C6 108.2(3) . . ?
C7 C8 C9 107.4(3) . . ?
N2 C9 C10 125.7(2) . . ?
N2 C9 C8 108.5(2) . . ?
C10 C9 C8 125.7(3) . . ?
C9 C10 C11 125.9(3) . . ?
C9 C10 C28 117.4(2) . . ?
C11 C10 C28 116.6(3) . . ?
N3 C11 C10 125.4(3) . . ?
N3 C11 C12 108.9(2) . . ?
C10 C11 C12 125.6(3) . . ?
C13 C12 C11 107.6(3) . . ?
C12 C13 C14 107.9(3) . . ?
N3 C14 C15 125.1(3) . . ?
N3 C14 C13 108.7(2) . . ?
C15 C14 C13 126.2(3) . . ?
C16 C15 C14 125.5(3) . . ?
C16 C15 C35 116.6(2) . . ?
C14 C15 C35 117.9(3) . . ?
N4 C16 C15 126.2(3) . . ?
N4 C16 C17 108.8(2) . . ?
C15 C16 C17 124.9(3) . . ?
C18 C17 C16 107.8(3) . . ?
C17 C18 C19 107.5(3) . . ?
N4 C19 C20 126.1(2) . . ?
N4 C19 C18 108.6(2) . . ?
C20 C19 C18 125.3(3) . . ?
C19 C20 C1 125.8(3) . . ?
C19 C20 C42 117.0(2) . . ?
C1 C20 C42 117.2(3) . . ?
C22 C21 C26 118.4(3) . . ?
C22 C21 C5 119.5(3) . . ?
C26 C21 C5 122.1(3) . . ?
C21 C22 C23 121.1(3) . . ?
C24 C23 C22 121.5(4) . . ?
C23 C24 C25 117.3(3) . . ?
C23 C24 C27 121.8(4) . . ?
C25 C24 C27 120.9(4) . . ?
C24 C25 C26 122.1(3) . . ?
C21 C26 C25 119.7(3) . . ?
C33 C28 C29 117.7(3) . . ?
C33 C28 C10 122.1(3) . . ?
C29 C28 C10 120.2(3) . . ?
C30 C29 C28 120.6(3) . . ?
C31 C30 C29 121.4(4) . . ?
C32 C31 C30 118.0(3) . . ?
C32 C31 C34 121.1(4) . . ?
C30 C31 C34 120.8(4) . . ?
C31 C32 C33 121.6(3) . . ?
C28 C33 C32 120.6(3) . . ?
C40 C35 C36 118.0(3) . . ?
C40 C35 C15 122.5(3) . . ?
C36 C35 C15 119.4(3) . . ?
C37 C36 C35 120.7(3) . . ?
C36 C37 C38 121.6(3) . . ?
C37 C38 C39 117.8(3) . . ?
C37 C38 C41 121.3(3) . . ?
C39 C38 C41 120.9(3) . . ?
C40 C39 C38 121.2(3) . . ?
C39 C40 C35 120.7(3) . . ?
C43 C42 C47 118.0(3) . . ?
C43 C42 C20 121.3(3) . . ?
C47 C42 C20 120.8(3) . . ?
C42 C43 C44 121.3(3) . . ?
C45 C44 C43 121.0(3) . . ?
C44 C45 C46 118.0(3) . . ?
C44 C45 C48 120.8(3) . . ?
C46 C45 C48 121.2(3) . . ?
C47 C46 C45 121.2(3) . . ?
C46 C47 C42 120.5(3) . . ?
C49 N5 Hf1 173.4(2) . . ?
N5 C49 C54 119.8(3) . . ?
N5 C49 C50 121.0(3) . . ?
C54 C49 C50 119.2(3) . . ?
C51 C50 C49 119.1(3) . . ?
C51 C50 C55 121.3(3) . . ?
C49 C50 C55 119.6(3) . . ?
C50 C51 C52 121.4(3) . . ?
C53 C52 C51 119.6(3) . . ?
C52 C53 C54 121.2(3) . . ?
C53 C54 C49 119.5(3) . . ?
C53 C54 C58 121.4(3) . . ?
C49 C54 C58 119.0(3) . . ?
C50 C55 C57 110.8(3) . . ?
C50 C55 C56 113.0(3) . . ?
C57 C55 C56 110.7(3) . . ?
C54 C58 C60 114.9(3) . . ?
C54 C58 C59 109.8(3) . . ?
C60 C58 C59 110.9(3) . . ?
C62 C61 C66 116.0(4) . . ?
C62 C61 C67 121.7(5) . . ?
C66 C61 C67 122.3(5) . . ?
C63 C62 C61 121.2(5) . . ?
C64 C63 C62 121.0(5) . . ?
C63 C64 C65 120.6(5) . . ?
C64 C65 C66 119.6(5) . . ?
C65 C66 C61 121.5(5) . . ?
C69 C68 C68 113.1(6) . 3_575 ?
C68 C69 C70' 113.9(5) . . ?
C68 C69 C70 113.9(5) . . ?
C71' C70' C69 119.0(6) . . ?
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 N5 1.859(2) . ?
Hf1 N2 2.178(2) . ?
Hf1 N1 2.181(2) . ?
Hf1 N4 2.193(2) . ?
Hf1 N3 2.193(2) . ?
N1 C4 1.384(3) . ?
N1 C1 1.383(4) . ?
N2 C9 1.382(4) . ?
N2 C6 1.387(3) . ?
N3 C14 1.383(3) . ?
N3 C11 1.388(4) . ?
N4 C16 1.381(3) . ?
N4 C19 1.382(4) . ?
C1 C20 1.407(4) . ?
C1 C2 1.439(4) . ?
C2 C3 1.348(4) . ?
C3 C4 1.432(4) . ?
C4 C5 1.405(4) . ?
C5 C6 1.406(4) . ?
C5 C21 1.502(4) . ?
C6 C7 1.432(4) . ?
C7 C8 1.353(4) . ?
C8 C9 1.444(4) . ?
C9 C10 1.407(4) . ?
C10 C11 1.413(4) . ?
C10 C28 1.489(4) . ?
C11 C12 1.431(4) . ?
C12 C13 1.353(4) . ?
C13 C14 1.433(4) . ?
C14 C15 1.413(4) . ?
C15 C16 1.409(4) . ?
C15 C35 1.495(4) . ?
C16 C17 1.437(4) . ?
C17 C18 1.351(4) . ?
C18 C19 1.444(4) . ?
C19 C20 1.404(4) . ?
C20 C42 1.499(4) . ?
C21 C22 1.377(4) . ?
C21 C26 1.387(4) . ?
C22 C23 1.388(5) . ?
C23 C24 1.372(5) . ?
C24 C25 1.383(5) . ?
C24 C27 1.504(5) . ?
C25 C26 1.393(5) . ?
C28 C33 1.388(4) . ?
C28 C29 1.393(5) . ?
C29 C30 1.389(5) . ?
C30 C31 1.374(5) . ?
C31 C32 1.372(6) . ?
C31 C34 1.523(5) . ?
C32 C33 1.388(5) . ?
C35 C40 1.390(4) . ?
C35 C36 1.398(4) . ?
C36 C37 1.381(4) . ?
C37 C38 1.385(5) . ?
C38 C39 1.391(4) . ?
C38 C41 1.518(4) . ?
C39 C40 1.389(4) . ?
C42 C43 1.384(4) . ?
C42 C47 1.393(4) . ?
C43 C44 1.388(4) . ?
C44 C45 1.377(5) . ?
C45 C46 1.392(5) . ?
C45 C48 1.522(5) . ?
C46 C47 1.388(5) . ?
N5 C49 1.374(4) . ?
C49 C54 1.416(4) . ?
C49 C50 1.426(4) . ?
C50 C51 1.388(4) . ?
C50 C55 1.513(4) . ?
C51 C52 1.391(4) . ?
C52 C53 1.382(4) . ?
C53 C54 1.393(4) . ?
C54 C58 1.514(4) . ?
C55 C57 1.532(5) . ?
C55 C56 1.537(4) . ?
C58 C60 1.516(4) . ?
C58 C59 1.517(5) . ?
C61 C62 1.389(7) . ?
C61 C66 1.402(7) . ?
C61 C67 1.501(7) . ?
C62 C63 1.358(7) . ?
C63 C64 1.337(7) . ?
C64 C65 1.354(7) . ?
C65 C66 1.366(7) . ?
C68 C69 1.515(7) . ?
C68 C68 1.539(9) 3_575 ?
C69 C70' 1.523(7) . ?
C69 C70 1.523(7) . ?
C70' C71' 1.458(12) . ?
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
N5 Hf1 N1 C4 72.6(2) . . . . ?
N2 Hf1 N1 C4 -33.1(2) . . . . ?
N4 Hf1 N1 C4 -176.9(2) . . . . ?
N3 Hf1 N1 C4 -106.0(2) . . . . ?
N5 Hf1 N1 C1 -87.7(2) . . . . ?
N2 Hf1 N1 C1 166.6(2) . . . . ?
N4 Hf1 N1 C1 22.8(2) . . . . ?
N3 Hf1 N1 C1 93.7(3) . . . . ?
N5 Hf1 N2 C9 77.4(2) . . . . ?
N1 Hf1 N2 C9 -176.1(2) . . . . ?
N4 Hf1 N2 C9 -103.6(2) . . . . ?
N3 Hf1 N2 C9 -32.1(2) . . . . ?
N5 Hf1 N2 C6 -71.1(2) . . . . ?
N1 Hf1 N2 C6 35.4(2) . . . . ?
N4 Hf1 N2 C6 107.9(2) . . . . ?
N3 Hf1 N2 C6 179.4(2) . . . . ?
N5 Hf1 N3 C14 79.3(2) . . . . ?
N2 Hf1 N3 C14 -175.3(2) . . . . ?
N1 Hf1 N3 C14 -102.2(2) . . . . ?
N4 Hf1 N3 C14 -31.2(2) . . . . ?
N5 Hf1 N3 C11 -77.1(2) . . . . ?
N2 Hf1 N3 C11 28.3(2) . . . . ?
N1 Hf1 N3 C11 101.4(2) . . . . ?
N4 Hf1 N3 C11 172.4(2) . . . . ?
N5 Hf1 N4 C16 -80.4(2) . . . . ?
N2 Hf1 N4 C16 100.6(2) . . . . ?
N1 Hf1 N4 C16 173.4(2) . . . . ?
N3 Hf1 N4 C16 29.0(2) . . . . ?
N5 Hf1 N4 C19 85.7(2) . . . . ?
N2 Hf1 N4 C19 -93.4(2) . . . . ?
N1 Hf1 N4 C19 -20.6(2) . . . . ?
N3 Hf1 N4 C19 -165.0(2) . . . . ?
C4 N1 C1 C20 178.7(3) . . . . ?
Hf1 N1 C1 C20 -18.6(4) . . . . ?
C4 N1 C1 C2 -0.8(3) . . . . ?
Hf1 N1 C1 C2 162.0(2) . . . . ?
N1 C1 C2 C3 0.1(4) . . . . ?
C20 C1 C2 C3 -179.4(3) . . . . ?
C1 C2 C3 C4 0.6(4) . . . . ?
C1 N1 C4 C5 -176.0(3) . . . . ?
Hf1 N1 C4 C5 20.4(4) . . . . ?
C1 N1 C4 C3 1.1(3) . . . . ?
Hf1 N1 C4 C3 -162.5(2) . . . . ?
C2 C3 C4 N1 -1.1(4) . . . . ?
C2 C3 C4 C5 176.0(3) . . . . ?
N1 C4 C5 C6 5.7(5) . . . . ?
C3 C4 C5 C6 -171.0(3) . . . . ?
N1 C4 C5 C21 -173.5(3) . . . . ?
C3 C4 C5 C21 9.8(4) . . . . ?
C9 N2 C6 C5 -178.8(3) . . . . ?
Hf1 N2 C6 C5 -25.7(4) . . . . ?
C9 N2 C6 C7 0.4(3) . . . . ?
Hf1 N2 C6 C7 153.4(2) . . . . ?
C4 C5 C6 N2 -2.6(5) . . . . ?
C21 C5 C6 N2 176.5(3) . . . . ?
C4 C5 C6 C7 178.4(3) . . . . ?
C21 C5 C6 C7 -2.4(4) . . . . ?
N2 C6 C7 C8 -0.7(3) . . . . ?
C5 C6 C7 C8 178.4(3) . . . . ?
C6 C7 C8 C9 0.8(3) . . . . ?
C6 N2 C9 C10 177.8(3) . . . . ?
Hf1 N2 C9 C10 25.5(4) . . . . ?
C6 N2 C9 C8 0.1(3) . . . . ?
Hf1 N2 C9 C8 -152.2(2) . . . . ?
C7 C8 C9 N2 -0.6(3) . . . . ?
C7 C8 C9 C10 -178.3(3) . . . . ?
N2 C9 C10 C11 -0.2(5) . . . . ?
C8 C9 C10 C11 177.2(3) . . . . ?
N2 C9 C10 C28 -177.4(3) . . . . ?
C8 C9 C10 C28 -0.1(4) . . . . ?
C14 N3 C11 C10 -177.0(3) . . . . ?
Hf1 N3 C11 C10 -17.1(4) . . . . ?
C14 N3 C11 C12 1.1(3) . . . . ?
Hf1 N3 C11 C12 161.1(2) . . . . ?
C9 C10 C11 N3 -4.4(5) . . . . ?
C28 C10 C11 N3 172.9(3) . . . . ?
C9 C10 C11 C12 177.8(3) . . . . ?
C28 C10 C11 C12 -4.9(4) . . . . ?
N3 C11 C12 C13 -1.6(3) . . . . ?
C10 C11 C12 C13 176.5(3) . . . . ?
C11 C12 C13 C14 1.4(3) . . . . ?
C11 N3 C14 C15 -179.5(3) . . . . ?
Hf1 N3 C14 C15 20.6(4) . . . . ?
C11 N3 C14 C13 -0.3(3) . . . . ?
Hf1 N3 C14 C13 -160.2(2) . . . . ?
C12 C13 C14 N3 -0.7(3) . . . . ?
C12 C13 C14 C15 178.5(3) . . . . ?
N3 C14 C15 C16 7.2(4) . . . . ?
C13 C14 C15 C16 -171.9(3) . . . . ?
N3 C14 C15 C35 -172.7(3) . . . . ?
C13 C14 C15 C35 8.2(4) . . . . ?
C19 N4 C16 C15 175.5(3) . . . . ?
Hf1 N4 C16 C15 -16.2(4) . . . . ?
C19 N4 C16 C17 0.0(3) . . . . ?
Hf1 N4 C16 C17 168.3(2) . . . . ?
C14 C15 C16 N4 -9.6(5) . . . . ?
C35 C15 C16 N4 170.3(3) . . . . ?
C14 C15 C16 C17 165.3(3) . . . . ?
C35 C15 C16 C17 -14.8(4) . . . . ?
N4 C16 C17 C18 0.7(3) . . . . ?
C15 C16 C17 C18 -175.0(3) . . . . ?
C16 C17 C18 C19 -1.0(3) . . . . ?
C16 N4 C19 C20 -178.1(3) . . . . ?
Hf1 N4 C19 C20 13.9(4) . . . . ?
C16 N4 C19 C18 -0.6(3) . . . . ?
Hf1 N4 C19 C18 -168.5(2) . . . . ?
C17 C18 C19 N4 1.0(3) . . . . ?
C17 C18 C19 C20 178.5(3) . . . . ?
N4 C19 C20 C1 1.0(5) . . . . ?
C18 C19 C20 C1 -176.1(3) . . . . ?
N4 C19 C20 C42 179.9(3) . . . . ?
C18 C19 C20 C42 2.8(4) . . . . ?
N1 C1 C20 C19 1.4(5) . . . . ?
C2 C1 C20 C19 -179.3(3) . . . . ?
N1 C1 C20 C42 -177.6(3) . . . . ?
C2 C1 C20 C42 1.8(4) . . . . ?
C4 C5 C21 C22 76.1(4) . . . . ?
C6 C5 C21 C22 -103.2(4) . . . . ?
C4 C5 C21 C26 -104.5(4) . . . . ?
C6 C5 C21 C26 76.3(4) . . . . ?
C26 C21 C22 C23 -0.9(5) . . . . ?
C5 C21 C22 C23 178.6(3) . . . . ?
C21 C22 C23 C24 0.1(6) . . . . ?
C22 C23 C24 C25 0.7(6) . . . . ?
C22 C23 C24 C27 -178.0(4) . . . . ?
C23 C24 C25 C26 -0.9(6) . . . . ?
C27 C24 C25 C26 177.9(4) . . . . ?
C22 C21 C26 C25 0.7(5) . . . . ?
C5 C21 C26 C25 -178.7(3) . . . . ?
C24 C25 C26 C21 0.2(6) . . . . ?
C9 C10 C28 C33 -66.4(4) . . . . ?
C11 C10 C28 C33 116.1(3) . . . . ?
C9 C10 C28 C29 112.9(3) . . . . ?
C11 C10 C28 C29 -64.6(4) . . . . ?
C33 C28 C29 C30 0.8(5) . . . . ?
C10 C28 C29 C30 -178.5(3) . . . . ?
C28 C29 C30 C31 0.0(6) . . . . ?
C29 C30 C31 C32 -0.7(6) . . . . ?
C29 C30 C31 C34 178.4(4) . . . . ?
C30 C31 C32 C33 0.5(6) . . . . ?
C34 C31 C32 C33 -178.5(4) . . . . ?
C29 C28 C33 C32 -0.9(5) . . . . ?
C10 C28 C33 C32 178.4(3) . . . . ?
C31 C32 C33 C28 0.3(6) . . . . ?
C16 C15 C35 C40 118.0(3) . . . . ?
C14 C15 C35 C40 -62.1(4) . . . . ?
C16 C15 C35 C36 -61.8(4) . . . . ?
C14 C15 C35 C36 118.1(3) . . . . ?
C40 C35 C36 C37 1.4(5) . . . . ?
C15 C35 C36 C37 -178.7(3) . . . . ?
C35 C36 C37 C38 -1.0(5) . . . . ?
C36 C37 C38 C39 0.1(5) . . . . ?
C36 C37 C38 C41 180.0(3) . . . . ?
C37 C38 C39 C40 0.3(5) . . . . ?
C41 C38 C39 C40 -179.5(3) . . . . ?
C38 C39 C40 C35 0.2(5) . . . . ?
C36 C35 C40 C39 -1.0(5) . . . . ?
C15 C35 C40 C39 179.1(3) . . . . ?
C19 C20 C42 C43 66.4(4) . . . . ?
C1 C20 C42 C43 -114.5(3) . . . . ?
C19 C20 C42 C47 -112.7(3) . . . . ?
C1 C20 C42 C47 66.3(4) . . . . ?
C47 C42 C43 C44 -0.3(5) . . . . ?
C20 C42 C43 C44 -179.5(3) . . . . ?
C42 C43 C44 C45 -0.6(5) . . . . ?
C43 C44 C45 C46 1.0(5) . . . . ?
C43 C44 C45 C48 -178.6(3) . . . . ?
C44 C45 C46 C47 -0.6(6) . . . . ?
C48 C45 C46 C47 179.0(4) . . . . ?
C45 C46 C47 C42 -0.2(5) . . . . ?
C43 C42 C47 C46 0.7(5) . . . . ?
C20 C42 C47 C46 179.9(3) . . . . ?
N2 Hf1 N5 C49 -139.3(18) . . . . ?
N1 Hf1 N5 C49 131.3(18) . . . . ?
N4 Hf1 N5 C49 41.3(18) . . . . ?
N3 Hf1 N5 C49 -49.7(18) . . . . ?
Hf1 N5 C49 C54 24.6(20) . . . . ?
Hf1 N5 C49 C50 -153.9(17) . . . . ?
N5 C49 C50 C51 177.2(3) . . . . ?
C54 C49 C50 C51 -1.4(4) . . . . ?
N5 C49 C50 C55 -2.2(4) . . . . ?
C54 C49 C50 C55 179.2(3) . . . . ?
C49 C50 C51 C52 -0.1(5) . . . . ?
C55 C50 C51 C52 179.3(3) . . . . ?
C50 C51 C52 C53 1.7(5) . . . . ?
C51 C52 C53 C54 -1.7(5) . . . . ?
C52 C53 C54 C49 0.1(5) . . . . ?
C52 C53 C54 C58 177.3(3) . . . . ?
N5 C49 C54 C53 -177.2(3) . . . . ?
C50 C49 C54 C53 1.4(4) . . . . ?
N5 C49 C54 C58 5.6(4) . . . . ?
C50 C49 C54 C58 -175.8(3) . . . . ?
C51 C50 C55 C57 -98.0(3) . . . . ?
C49 C50 C55 C57 81.4(3) . . . . ?
C51 C50 C55 C56 26.9(4) . . . . ?
C49 C50 C55 C56 -153.7(3) . . . . ?
C53 C54 C58 C60 28.7(4) . . . . ?
C49 C54 C58 C60 -154.1(3) . . . . ?
C53 C54 C58 C59 -97.1(3) . . . . ?
C49 C54 C58 C59 80.1(3) . . . . ?
C66 C61 C62 C63 0.4(7) . . . . ?
C67 C61 C62 C63 -179.7(5) . . . . ?
C61 C62 C63 C64 -1.5(8) . . . . ?
C62 C63 C64 C65 1.6(9) . . . . ?
C63 C64 C65 C66 -0.5(10) . . . . ?
C64 C65 C66 C61 -0.7(9) . . . . ?
C62 C61 C66 C65 0.7(7) . . . . ?
C67 C61 C66 C65 -179.2(5) . . . . ?
C68 C68 C69 C70' -178.0(5) 3_575 . . . ?
C68 C68 C69 C70 -178.0(5) 3_575 . . . ?
C68 C69 C70' C71' 68.3(8) . . . . ?
C70 C69 C70' C71' 0.0(1000) . . . . ?
