#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310016.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_4310016
loop_
_publ_author_name
'Stanislav Groysman'
'Ekaterina Sergeeva'
'Israel Goldberg'
'Moshe Kol'
_publ_section_title
;
Group IV Complexes of a Tetradentate Amine Mono(phenolate) Ligand: a
Second Side-Arm Donor Stabilizes Cationic Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8188
_journal_page_last               8190
_journal_paper_doi               10.1021/ic051400w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C53 H54 B F20 N O5 Zr'
_chemical_formula_weight         1267.00
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.905(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9790(5)
_cell_length_b                   10.9770(4)
_cell_length_c                   26.8330(7)
_cell_measurement_temperature    110(2)
_cell_volume                     5533.2(3)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B. V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg Phi and Omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            13315
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.313
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2576
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         13315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1026P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                7896
_reflns_number_total             13315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051400wsi20051010_112930_3.cif
_cod_data_source_block           mk155
_cod_database_code               4310016
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_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
Zr1 Zr 0.513229(17) 0.71124(3) 0.266189(12) 0.03119(12) Uani 1 1 d . . .
O2 O 0.61706(12) 0.7103(2) 0.28155(9) 0.0362(6) Uani 1 1 d . . .
O3 O 0.53866(12) 0.6529(2) 0.35630(8) 0.0364(6) Uani 1 1 d . . .
O4 O 0.41385(12) 0.7751(2) 0.28128(9) 0.0356(6) Uani 1 1 d . . .
O5 O 0.48492(12) 0.8011(2) 0.20142(9) 0.0382(6) Uani 1 1 d . . .
O6 O 0.48040(12) 0.5474(2) 0.24806(8) 0.0356(6) Uani 1 1 d . . .
N7 N 0.54547(14) 0.8853(3) 0.32440(10) 0.0335(6) Uani 1 1 d . . .
C8 C 0.67876(18) 0.7665(3) 0.31090(13) 0.0356(8) Uani 1 1 d . . .
C9 C 0.74442(19) 0.7059(4) 0.32380(14) 0.0389(8) Uani 1 1 d . . .
C10 C 0.80361(19) 0.7680(4) 0.35779(14) 0.0411(9) Uani 1 1 d . . .
H10 H 0.8488 0.7294 0.3670 0.049 Uiso 1 1 calc R . .
C11 C 0.80047(18) 0.8830(4) 0.37897(13) 0.0387(8) Uani 1 1 d . . .
C12 C 0.73463(19) 0.9397(4) 0.36378(13) 0.0397(9) Uani 1 1 d . . .
H12 H 0.7308 1.0188 0.3769 0.048 Uiso 1 1 calc R . .
C13 C 0.67405(17) 0.8831(3) 0.32959(13) 0.0353(8) Uani 1 1 d . . .
C14 C 0.60390(18) 0.9509(3) 0.31143(13) 0.0359(8) Uani 1 1 d . . .
H14A H 0.6110 1.0322 0.3284 0.043 Uiso 1 1 calc R . .
H14B H 0.5887 0.9632 0.2726 0.043 Uiso 1 1 calc R . .
C15 C 0.56793(18) 0.8579(3) 0.38275(12) 0.0348(8) Uani 1 1 d . . .
H15A H 0.5276 0.8746 0.3953 0.042 Uiso 1 1 calc R . .
H15B H 0.6077 0.9126 0.4022 0.042 Uiso 1 1 calc R . .
C16 C 0.59125(18) 0.7273(3) 0.39499(13) 0.0349(8) Uani 1 1 d . . .
H16A H 0.6389 0.7148 0.3922 0.042 Uiso 1 1 calc R . .
H16B H 0.5935 0.7057 0.4313 0.042 Uiso 1 1 calc R . .
C17 C 0.5430(2) 0.5282(4) 0.37380(15) 0.0486(10) Uani 1 1 d . . .
H17A H 0.5905 0.4960 0.3786 0.073 Uiso 1 1 calc R . .
H17B H 0.5072 0.4794 0.3472 0.073 Uiso 1 1 calc R . .
H17C H 0.5341 0.5242 0.4075 0.073 Uiso 1 1 calc R . .
C18 C 0.47951(18) 0.9596(3) 0.30700(14) 0.0368(8) Uani 1 1 d . . .
H18A H 0.4702 0.9880 0.2702 0.044 Uiso 1 1 calc R . .
H18B H 0.4860 1.0322 0.3301 0.044 Uiso 1 1 calc R . .
C19 C 0.41637(17) 0.8867(3) 0.30943(13) 0.0340(8) Uani 1 1 d . . .
H19A H 0.4215 0.8695 0.3468 0.041 Uiso 1 1 calc R . .
H19B H 0.3718 0.9333 0.2931 0.041 Uiso 1 1 calc R . .
C20 C 0.35765(19) 0.6961(4) 0.28336(16) 0.0441(9) Uani 1 1 d . . .
H20A H 0.3633 0.6790 0.3204 0.066 Uiso 1 1 calc R . .
H20B H 0.3596 0.6196 0.2651 0.066 Uiso 1 1 calc R . .
H20C H 0.3116 0.7357 0.2660 0.066 Uiso 1 1 calc R . .
C21 C 0.45967(18) 0.4324(3) 0.22167(13) 0.0347(8) Uani 1 1 d . . .
C22 C 0.4279(2) 0.4580(4) 0.16236(13) 0.0454(10) Uani 1 1 d . . .
H22A H 0.3858 0.5101 0.1553 0.068 Uiso 1 1 calc R . .
H22B H 0.4140 0.3809 0.1431 0.068 Uiso 1 1 calc R . .
H22C H 0.4633 0.4993 0.1505 0.068 Uiso 1 1 calc R . .
C23 C 0.4052(2) 0.3729(4) 0.24180(14) 0.0455(9) Uani 1 1 d . . .
H23A H 0.4245 0.3674 0.2806 0.068 Uiso 1 1 calc R . .
H23B H 0.3944 0.2909 0.2267 0.068 Uiso 1 1 calc R . .
H23C H 0.3616 0.4218 0.2311 0.068 Uiso 1 1 calc R . .
C24 C 0.5268(2) 0.3545(4) 0.23412(15) 0.0472(10) Uani 1 1 d . . .
H24A H 0.5612 0.3956 0.2211 0.071 Uiso 1 1 calc R . .
H24B H 0.5144 0.2751 0.2167 0.071 Uiso 1 1 calc R . .
H24C H 0.5479 0.3428 0.2725 0.071 Uiso 1 1 calc R . .
C25 C 0.46608(19) 0.8494(4) 0.14838(13) 0.0404(9) Uani 1 1 d . . .
C26 C 0.4734(2) 0.9863(4) 0.15204(16) 0.0507(10) Uani 1 1 d . . .
H26A H 0.4381 1.0199 0.1662 0.076 Uiso 1 1 calc R . .
H26B H 0.4655 1.0201 0.1167 0.076 Uiso 1 1 calc R . .
H26C H 0.5213 1.0078 0.1756 0.076 Uiso 1 1 calc R . .
C27 C 0.5167(3) 0.7929(4) 0.12313(17) 0.0582(11) Uani 1 1 d . . .
H27A H 0.5660 0.8107 0.1451 0.087 Uiso 1 1 calc R . .
H27B H 0.5071 0.8272 0.0877 0.087 Uiso 1 1 calc R . .
H27C H 0.5096 0.7045 0.1204 0.087 Uiso 1 1 calc R . .
C28 C 0.3901(2) 0.8109(5) 0.11895(17) 0.0637(13) Uani 1 1 d . . .
H28A H 0.3871 0.7217 0.1182 0.096 Uiso 1 1 calc R . .
H28B H 0.3752 0.8422 0.0826 0.096 Uiso 1 1 calc R . .
H28C H 0.3589 0.8437 0.1370 0.096 Uiso 1 1 calc R . .
C29 C 0.7500(2) 0.5793(4) 0.30093(16) 0.0470(10) Uani 1 1 d . . .
C30 C 0.7198(2) 0.5837(5) 0.24031(16) 0.0633(13) Uani 1 1 d . . .
H30A H 0.6700 0.6099 0.2288 0.095 Uiso 1 1 calc R . .
H30B H 0.7228 0.5025 0.2260 0.095 Uiso 1 1 calc R . .
H30C H 0.7474 0.6415 0.2273 0.095 Uiso 1 1 calc R . .
C31 C 0.8284(2) 0.5371(5) 0.31667(19) 0.0681(14) Uani 1 1 d . . .
H31A H 0.8554 0.5960 0.3036 0.102 Uiso 1 1 calc R . .
H31B H 0.8302 0.4570 0.3010 0.102 Uiso 1 1 calc R . .
H31C H 0.8492 0.5314 0.3554 0.102 Uiso 1 1 calc R . .
C32 C 0.7098(2) 0.4840(4) 0.32250(17) 0.0557(11) Uani 1 1 d . . .
H32A H 0.7302 0.4816 0.3613 0.084 Uiso 1 1 calc R . .
H32B H 0.7142 0.4035 0.3081 0.084 Uiso 1 1 calc R . .
H32C H 0.6594 0.5065 0.3118 0.084 Uiso 1 1 calc R . .
C33 C 0.8683(2) 0.9409(4) 0.41764(14) 0.0459(10) Uani 1 1 d . . .
C34 C 0.8873(2) 0.8773(5) 0.47169(15) 0.0678(14) Uani 1 1 d . . .
H34A H 0.9327 0.9088 0.4956 0.102 Uiso 1 1 calc R . .
H34B H 0.8912 0.7893 0.4671 0.102 Uiso 1 1 calc R . .
H34C H 0.8499 0.8932 0.4869 0.102 Uiso 1 1 calc R . .
C35 C 0.9304(2) 0.9277(4) 0.39732(16) 0.0554(11) Uani 1 1 d . . .
H35A H 0.9186 0.9678 0.3627 0.083 Uiso 1 1 calc R . .
H35B H 0.9397 0.8411 0.3937 0.083 Uiso 1 1 calc R . .
H35C H 0.9729 0.9658 0.4225 0.083 Uiso 1 1 calc R . .
C36 C 0.8585(2) 1.0762(4) 0.42505(17) 0.0576(12) Uani 1 1 d . . .
H36A H 0.9032 1.1106 0.4490 0.086 Uiso 1 1 calc R . .
H36B H 0.8208 1.0879 0.4403 0.086 Uiso 1 1 calc R . .
H36C H 0.8453 1.1174 0.3906 0.086 Uiso 1 1 calc R . .
B37 B 0.2003(2) 0.2360(4) 0.04059(15) 0.0326(9) Uani 1 1 d . . .
C38 C 0.12009(17) 0.2548(3) -0.00431(12) 0.0304(7) Uani 1 1 d . . .
C39 C 0.06497(18) 0.2967(3) 0.01125(12) 0.0324(8) Uani 1 1 d . . .
C40 C -0.00091(17) 0.3320(3) -0.02261(13) 0.0350(8) Uani 1 1 d . . .
C41 C -0.01578(17) 0.3238(3) -0.07653(13) 0.0334(8) Uani 1 1 d . . .
C42 C 0.03663(18) 0.2798(3) -0.09412(12) 0.0317(8) Uani 1 1 d . . .
C43 C 0.10227(18) 0.2489(3) -0.05874(12) 0.0309(7) Uani 1 1 d . . .
F44 F 0.07490(10) 0.30741(19) 0.06395(7) 0.0373(5) Uani 1 1 d . . .
F45 F -0.05164(10) 0.3739(2) -0.00367(8) 0.0435(5) Uani 1 1 d . . .
F46 F -0.07924(9) 0.35898(19) -0.11072(7) 0.0403(5) Uani 1 1 d . . .
F47 F 0.02310(10) 0.26874(19) -0.14705(7) 0.0393(5) Uani 1 1 d . . .
F48 F 0.15049(10) 0.21342(18) -0.08149(7) 0.0360(5) Uani 1 1 d . . .
C49 C 0.21848(16) 0.3782(3) 0.06190(12) 0.0297(7) Uani 1 1 d . . .
C50 C 0.21934(17) 0.4691(3) 0.02589(13) 0.0350(8) Uani 1 1 d . . .
C51 C 0.22281(17) 0.5917(3) 0.03618(14) 0.0362(8) Uani 1 1 d . . .
C52 C 0.22580(17) 0.6315(3) 0.08523(15) 0.0386(9) Uani 1 1 d . . .
C53 C 0.22657(17) 0.5475(3) 0.12310(13) 0.0359(8) Uani 1 1 d . . .
C54 C 0.22208(17) 0.4245(3) 0.11102(13) 0.0331(8) Uani 1 1 d . . .
F55 F 0.21928(10) 0.35005(18) 0.15067(7) 0.0377(5) Uani 1 1 d . . .
F56 F 0.22880(11) 0.5844(2) 0.17175(8) 0.0468(5) Uani 1 1 d . . .
F57 F 0.22646(11) 0.7519(2) 0.09565(9) 0.0518(6) Uani 1 1 d . . .
F58 F 0.22023(11) 0.6731(2) -0.00207(9) 0.0489(5) Uani 1 1 d . . .
F59 F 0.21467(10) 0.43560(18) -0.02419(7) 0.0372(5) Uani 1 1 d . . .
C60 C 0.20109(17) 0.1375(3) 0.08712(12) 0.0298(7) Uani 1 1 d . . .
C61 C 0.14858(18) 0.0549(3) 0.08696(13) 0.0335(8) Uani 1 1 d . . .
C62 C 0.15655(19) -0.0316(3) 0.12639(14) 0.0371(8) Uani 1 1 d . . .
C63 C 0.21905(19) -0.0375(3) 0.16825(13) 0.0376(8) Uani 1 1 d . . .
C64 C 0.27251(18) 0.0407(3) 0.17001(13) 0.0373(8) Uani 1 1 d . . .
C65 C 0.26352(17) 0.1244(3) 0.13037(13) 0.0338(8) Uani 1 1 d . . .
F66 F 0.08512(10) 0.05275(19) 0.04682(7) 0.0412(5) Uani 1 1 d . . .
F67 F 0.10307(11) -0.1084(2) 0.12311(9) 0.0483(5) Uani 1 1 d . . .
F68 F 0.22729(12) -0.1211(2) 0.20691(8) 0.0528(6) Uani 1 1 d . . .
F69 F 0.33519(11) 0.0363(2) 0.21149(8) 0.0493(6) Uani 1 1 d . . .
F70 F 0.31972(9) 0.19750(18) 0.13447(7) 0.0361(5) Uani 1 1 d . . .
C71 C 0.25884(17) 0.1751(3) 0.01699(12) 0.0310(7) Uani 1 1 d . . .
C72 C 0.24633(17) 0.0595(3) -0.00616(12) 0.0323(8) Uani 1 1 d . . .
C73 C 0.32667(17) 0.2178(3) 0.02399(13) 0.0326(8) Uani 1 1 d . . .
C74 C 0.37688(19) 0.1547(4) 0.00899(14) 0.0408(9) Uani 1 1 d . . .
C75 C 0.3605(2) 0.0421(4) -0.01408(15) 0.0438(9) Uani 1 1 d . . .
C76 C 0.29388(19) -0.0073(3) -0.02183(13) 0.0389(8) Uani 1 1 d . . .
F77 F 0.34836(9) 0.32830(19) 0.04633(7) 0.0379(5) Uani 1 1 d . . .
F78 F 0.44258(11) 0.2023(2) 0.01785(9) 0.0496(6) Uani 1 1 d . . .
F79 F 0.40868(12) -0.0219(2) -0.02839(10) 0.0588(6) Uani 1 1 d . . .
F80 F 0.27675(12) -0.1170(2) -0.04409(9) 0.0501(5) Uani 1 1 d . . .
F81 F 0.18191(10) 0.00615(18) -0.01404(7) 0.0374(5) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
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'
Zr Zr -2.9673 0.5597 '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
O5 Zr1 O6 106.48(10) . . ?
O5 Zr1 O2 99.06(10) . . ?
O6 Zr1 O2 106.99(10) . . ?
O5 Zr1 O4 89.82(9) . . ?
O6 Zr1 O4 95.19(9) . . ?
O2 Zr1 O4 152.45(9) . . ?
O5 Zr1 O3 163.23(10) . . ?
O6 Zr1 O3 86.66(9) . . ?
O2 Zr1 O3 86.60(9) . . ?
O4 Zr1 O3 78.42(8) . . ?
O5 Zr1 N7 96.39(10) . . ?
O6 Zr1 N7 154.04(9) . . ?
O2 Zr1 N7 80.74(9) . . ?
O4 Zr1 N7 72.34(9) . . ?
O3 Zr1 N7 68.80(9) . . ?
C8 O2 Zr1 142.9(2) . . ?
C17 O3 C16 110.7(2) . . ?
C17 O3 Zr1 123.7(2) . . ?
C16 O3 Zr1 115.28(19) . . ?
C19 O4 C20 112.6(3) . . ?
C19 O4 Zr1 118.90(19) . . ?
C20 O4 Zr1 124.4(2) . . ?
C25 O5 Zr1 169.9(2) . . ?
C21 O6 Zr1 164.5(2) . . ?
C18 N7 C15 110.8(3) . . ?
C18 N7 C14 109.9(3) . . ?
C15 N7 C14 110.8(2) . . ?
C18 N7 Zr1 102.63(19) . . ?
C15 N7 Zr1 115.7(2) . . ?
C14 N7 Zr1 106.58(19) . . ?
O2 C8 C13 117.8(3) . . ?
O2 C8 C9 120.8(3) . . ?
C13 C8 C9 121.3(3) . . ?
C10 C9 C8 116.2(3) . . ?
C10 C9 C29 122.7(3) . . ?
C8 C9 C29 121.2(3) . . ?
C11 C10 C9 124.1(3) . . ?
C11 C10 H10 117.9 . . ?
C9 C10 H10 117.9 . . ?
C12 C11 C10 117.2(3) . . ?
C12 C11 C33 122.9(4) . . ?
C10 C11 C33 119.9(3) . . ?
C11 C12 C13 121.2(4) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C12 119.9(3) . . ?
C8 C13 C14 120.4(3) . . ?
C12 C13 C14 119.7(3) . . ?
N7 C14 C13 113.3(3) . . ?
N7 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
N7 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
N7 C15 C16 112.2(3) . . ?
N7 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
N7 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
O3 C16 C15 106.5(3) . . ?
O3 C16 H16A 110.4 . . ?
C15 C16 H16A 110.4 . . ?
O3 C16 H16B 110.4 . . ?
C15 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
O3 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N7 C18 C19 111.1(3) . . ?
N7 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
N7 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
O4 C19 C18 108.0(3) . . ?
O4 C19 H19A 110.1 . . ?
C18 C19 H19A 110.1 . . ?
O4 C19 H19B 110.1 . . ?
C18 C19 H19B 110.1 . . ?
H19A C19 H19B 108.4 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O6 C21 C23 108.9(3) . . ?
O6 C21 C22 107.5(3) . . ?
C23 C21 C22 110.9(3) . . ?
O6 C21 C24 107.4(3) . . ?
C23 C21 C24 111.3(3) . . ?
C22 C21 C24 110.7(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C25 C26 108.3(3) . . ?
O5 C25 C28 106.9(3) . . ?
C26 C25 C28 111.7(3) . . ?
O5 C25 C27 107.4(3) . . ?
C26 C25 C27 111.6(3) . . ?
C28 C25 C27 110.7(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C9 109.8(4) . . ?
C30 C29 C32 110.6(3) . . ?
C9 C29 C32 110.1(3) . . ?
C30 C29 C31 107.2(4) . . ?
C9 C29 C31 111.4(3) . . ?
C32 C29 C31 107.6(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C36 C33 C35 107.2(3) . . ?
C36 C33 C34 108.8(4) . . ?
C35 C33 C34 109.0(4) . . ?
C36 C33 C11 111.7(3) . . ?
C35 C33 C11 111.0(3) . . ?
C34 C33 C11 109.1(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C60 B37 C71 101.5(3) . . ?
C60 B37 C38 112.9(3) . . ?
C71 B37 C38 114.1(3) . . ?
C60 B37 C49 114.3(3) . . ?
C71 B37 C49 114.4(3) . . ?
C38 B37 C49 100.2(3) . . ?
C43 C38 C39 112.9(3) . . ?
C43 C38 B37 126.8(3) . . ?
C39 C38 B37 119.6(3) . . ?
F44 C39 C40 115.4(3) . . ?
F44 C39 C38 119.5(3) . . ?
C40 C39 C38 125.1(3) . . ?
F45 C40 C39 121.1(3) . . ?
F45 C40 C41 119.6(3) . . ?
C39 C40 C41 119.4(3) . . ?
F46 C41 C42 121.2(3) . . ?
F46 C41 C40 120.9(3) . . ?
C42 C41 C40 117.8(3) . . ?
F47 C42 C41 119.2(3) . . ?
F47 C42 C43 120.3(3) . . ?
C41 C42 C43 120.6(3) . . ?
F48 C43 C42 114.5(3) . . ?
F48 C43 C38 121.4(3) . . ?
C42 C43 C38 124.1(3) . . ?
C54 C49 C50 112.7(3) . . ?
C54 C49 B37 127.2(3) . . ?
C50 C49 B37 119.2(3) . . ?
F59 C50 C51 116.4(3) . . ?
F59 C50 C49 118.5(3) . . ?
C51 C50 C49 125.1(3) . . ?
F58 C51 C52 119.9(3) . . ?
F58 C51 C50 120.7(3) . . ?
C52 C51 C50 119.3(3) . . ?
F57 C52 C53 120.6(3) . . ?
F57 C52 C51 120.4(3) . . ?
C53 C52 C51 119.0(3) . . ?
F56 C53 C52 120.2(3) . . ?
F56 C53 C54 119.8(3) . . ?
C52 C53 C54 120.0(3) . . ?
F55 C54 C53 114.9(3) . . ?
F55 C54 C49 121.3(3) . . ?
C53 C54 C49 123.8(3) . . ?
C61 C60 C65 113.4(3) . . ?
C61 C60 B37 128.0(3) . . ?
C65 C60 B37 118.3(3) . . ?
F66 C61 C60 121.1(3) . . ?
F66 C61 C62 115.3(3) . . ?
C60 C61 C62 123.7(3) . . ?
F67 C62 C63 120.6(3) . . ?
F67 C62 C61 119.8(3) . . ?
C63 C62 C61 119.6(3) . . ?
F68 C63 C64 120.9(3) . . ?
F68 C63 C62 120.1(3) . . ?
C64 C63 C62 119.1(3) . . ?
C63 C64 F69 119.9(3) . . ?
C63 C64 C65 120.2(3) . . ?
F69 C64 C65 119.9(3) . . ?
F70 C65 C64 116.7(3) . . ?
F70 C65 C60 119.3(3) . . ?
C64 C65 C60 124.1(3) . . ?
C73 C71 C72 112.7(3) . . ?
C73 C71 B37 126.8(3) . . ?
C72 C71 B37 119.7(3) . . ?
F81 C72 C76 115.9(3) . . ?
F81 C72 C71 118.4(3) . . ?
C76 C72 C71 125.6(3) . . ?
F77 C73 C71 120.9(3) . . ?
F77 C73 C74 114.9(3) . . ?
C71 C73 C74 124.2(3) . . ?
F78 C74 C75 119.7(3) . . ?
F78 C74 C73 120.6(3) . . ?
C75 C74 C73 119.7(3) . . ?
F79 C75 C74 120.9(4) . . ?
F79 C75 C76 119.7(4) . . ?
C74 C75 C76 119.4(3) . . ?
F80 C76 C72 121.3(3) . . ?
F80 C76 C75 120.4(3) . . ?
C72 C76 C75 118.3(3) . . ?
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
Zr1 O5 1.909(2) . ?
Zr1 O6 1.919(2) . ?
Zr1 O2 1.973(2) . ?
Zr1 O4 2.268(2) . ?
Zr1 O3 2.383(2) . ?
Zr1 N7 2.413(3) . ?
O2 C8 1.364(4) . ?
O3 C17 1.440(4) . ?
O3 C16 1.451(4) . ?
O4 C19 1.431(4) . ?
O4 C20 1.435(4) . ?
O5 C25 1.443(4) . ?
O6 C21 1.437(4) . ?
N7 C18 1.483(4) . ?
N7 C15 1.505(4) . ?
N7 C14 1.509(4) . ?
C8 C13 1.389(5) . ?
C8 C9 1.405(5) . ?
C9 C10 1.400(5) . ?
C9 C29 1.539(5) . ?
C10 C11 1.394(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(5) . ?
C11 C33 1.536(5) . ?
C12 C13 1.392(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.513(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.509(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.514(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.518(5) . ?
C21 C22 1.525(5) . ?
C21 C24 1.529(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.510(6) . ?
C25 C28 1.513(5) . ?
C25 C27 1.528(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.531(6) . ?
C29 C32 1.546(6) . ?
C29 C31 1.548(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C36 1.520(6) . ?
C33 C35 1.522(6) . ?
C33 C34 1.536(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
B37 C60 1.648(5) . ?
B37 C71 1.649(5) . ?
B37 C38 1.658(5) . ?
B37 C49 1.659(5) . ?
C38 C43 1.382(4) . ?
C38 C39 1.383(5) . ?
C39 F44 1.365(4) . ?
C39 C40 1.376(5) . ?
C40 F45 1.359(4) . ?
C40 C41 1.377(5) . ?
C41 F46 1.344(4) . ?
C41 C42 1.374(5) . ?
C42 F47 1.358(4) . ?
C42 C43 1.374(5) . ?
C43 F48 1.361(4) . ?
C49 C54 1.392(5) . ?
C49 C50 1.393(5) . ?
C50 F59 1.365(4) . ?
C50 C51 1.371(5) . ?
C51 F58 1.348(4) . ?
C51 C52 1.368(5) . ?
C52 F57 1.350(4) . ?
C52 C53 1.368(5) . ?
C53 F56 1.353(4) . ?
C53 C54 1.383(5) . ?
C54 F55 1.358(4) . ?
C60 C61 1.386(5) . ?
C60 C65 1.392(5) . ?
C61 F66 1.356(4) . ?
C61 C62 1.390(5) . ?
C62 F67 1.340(4) . ?
C62 C63 1.367(5) . ?
C63 F68 1.352(4) . ?
C63 C64 1.358(5) . ?
C64 F69 1.364(4) . ?
C64 C65 1.370(5) . ?
C65 F70 1.354(4) . ?
C71 C73 1.385(5) . ?
C71 C72 1.397(5) . ?
C72 F81 1.363(4) . ?
C72 C76 1.374(5) . ?
C73 F77 1.357(4) . ?
C73 C74 1.387(5) . ?
C74 F78 1.357(4) . ?
C74 C75 1.371(6) . ?
C75 F79 1.349(4) . ?
C75 C76 1.386(5) . ?
C76 F80 1.336(4) . ?
