# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_ec75
_database_code_depnum_ccdc_archive 'CCDC 924151'
#TrackingRef 'Complex 4-Zr.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H67 B F15 N O2 Zr'
_chemical_formula_weight         1341.28
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.9985(4)
_cell_length_b                   15.8569(6)
_cell_length_c                   20.4970(8)
_cell_angle_alpha                86.967(2)
_cell_angle_beta                 75.119(2)
_cell_angle_gamma                73.850(2)
_cell_volume                     3317.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      30.47
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1380
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8873
_exptl_absorpt_correction_T_max  0.9598
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81935
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         30.55
_reflns_number_total             19831
_reflns_number_gt                14598
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2 (Bruker, 2009)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2009)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+3.8796P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         19831
_refine_ls_number_parameters     830
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1368
_refine_ls_wR_factor_gt          0.1282
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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 0.931815(19) 0.650897(16) 0.683668(11) 0.02322(6) Uani 1 1 d . A .
O1 O 0.91744(14) 0.53579(11) 0.71983(8) 0.0230(3) Uani 1 1 d . . .
N1 N 1.00392(16) 0.64850(13) 0.77984(10) 0.0218(4) Uani 1 1 d . . .
C1 C 0.89797(19) 0.49149(15) 0.77787(11) 0.0207(4) Uani 1 1 d . . .
C2 C 0.8529(2) 0.41571(15) 0.78350(11) 0.0220(4) Uani 1 1 d . . .
C3 C 0.8285(2) 0.38021(16) 0.84713(12) 0.0253(5) Uani 1 1 d . . .
H3A H 0.7938 0.3310 0.8522 0.030 Uiso 1 1 calc R . .
C4 C 0.8510(2) 0.41141(17) 0.90504(12) 0.0265(5) Uani 1 1 d . . .
C5 C 0.9005(2) 0.48290(16) 0.89667(11) 0.0249(5) Uani 1 1 d . . .
H5A H 0.9196 0.5050 0.9339 0.030 Uiso 1 1 calc R . .
C6 C 0.9233(2) 0.52400(15) 0.83390(11) 0.0214(4) Uani 1 1 d . . .
C7 C 0.8345(2) 0.37404(16) 0.72209(12) 0.0258(5) Uani 1 1 d . . .
C8 C 0.9673(2) 0.34704(18) 0.66927(13) 0.0331(6) Uani 1 1 d . . .
H8A H 0.9992 0.3989 0.6562 0.050 Uiso 1 1 calc R . .
H8B H 0.9565 0.3213 0.6294 0.050 Uiso 1 1 calc R . .
H8C H 1.0305 0.3037 0.6886 0.050 Uiso 1 1 calc R . .
C9 C 0.7881(3) 0.29128(18) 0.74089(14) 0.0364(6) Uani 1 1 d . . .
H9A H 0.7037 0.3066 0.7746 0.055 Uiso 1 1 calc R . .
H9B H 0.8526 0.2481 0.7596 0.055 Uiso 1 1 calc R . .
H9C H 0.7782 0.2662 0.7005 0.055 Uiso 1 1 calc R . .
C10 C 0.7305(2) 0.43874(18) 0.69230(13) 0.0309(5) Uani 1 1 d . . .
H10A H 0.6472 0.4549 0.7268 0.046 Uiso 1 1 calc R . .
H10B H 0.7192 0.4109 0.6535 0.046 Uiso 1 1 calc R . .
H10C H 0.7589 0.4916 0.6776 0.046 Uiso 1 1 calc R . .
C11 C 0.8211(3) 0.36542(19) 0.97210(13) 0.0339(6) Uani 1 1 d . . .
C12 C 0.8715(3) 0.3992(2) 1.02596(13) 0.0386(6) Uani 1 1 d . . .
H12A H 0.9667 0.3885 1.0105 0.058 Uiso 1 1 calc R . .
H12B H 0.8498 0.3683 1.0682 0.058 Uiso 1 1 calc R . .
H12C H 0.8303 0.4624 1.0336 0.058 Uiso 1 1 calc R . .
C13 C 0.6721(3) 0.3836(3) 0.99876(15) 0.0531(9) Uani 1 1 d . . .
H13A H 0.6368 0.3624 0.9656 0.080 Uiso 1 1 calc R . .
H13B H 0.6325 0.4469 1.0063 0.080 Uiso 1 1 calc R . .
H13C H 0.6521 0.3532 1.0414 0.080 Uiso 1 1 calc R . .
C14 C 0.8860(4) 0.2654(2) 0.96251(16) 0.0530(8) Uani 1 1 d . . .
H14A H 0.9808 0.2546 0.9451 0.080 Uiso 1 1 calc R . .
H14B H 0.8510 0.2417 0.9304 0.080 Uiso 1 1 calc R . .
H14C H 0.8672 0.2367 1.0060 0.080 Uiso 1 1 calc R . .
C15 C 0.9832(2) 0.59504(15) 0.82903(11) 0.0230(4) Uani 1 1 d . . .
H15A H 1.0116 0.6041 0.8675 0.028 Uiso 1 1 calc R . .
C16 C 1.0843(2) 0.70320(15) 0.79092(12) 0.0230(4) Uani 1 1 d . . .
C17 C 1.2210(2) 0.67174(17) 0.76577(13) 0.0283(5) Uani 1 1 d . . .
C18 C 1.2971(2) 0.72135(19) 0.78157(15) 0.0372(6) Uani 1 1 d . . .
H18A H 1.3896 0.7021 0.7656 0.045 Uiso 1 1 calc R . .
C19 C 1.2403(3) 0.7978(2) 0.81986(16) 0.0419(7) Uani 1 1 d . . .
H19A H 1.2941 0.8297 0.8307 0.050 Uiso 1 1 calc R . .
C20 C 1.1063(3) 0.82817(18) 0.84259(15) 0.0381(6) Uani 1 1 d . . .
H20A H 1.0688 0.8815 0.8682 0.046 Uiso 1 1 calc R . .
C21 C 1.0247(2) 0.78157(16) 0.82840(13) 0.0283(5) Uani 1 1 d . . .
C22 C 1.2852(2) 0.58670(18) 0.72475(14) 0.0351(6) Uani 1 1 d . . .
H22A H 1.2183 0.5739 0.7046 0.042 Uiso 1 1 calc R . .
C23 C 1.4012(3) 0.5946(2) 0.66629(16) 0.0471(7) Uani 1 1 d . . .
H23A H 1.3716 0.6436 0.6378 0.071 Uiso 1 1 calc R . .
H23B H 1.4360 0.5400 0.6392 0.071 Uiso 1 1 calc R . .
H23C H 1.4698 0.6051 0.6846 0.071 Uiso 1 1 calc R . .
C24 C 1.3269(3) 0.5102(2) 0.77041(18) 0.0515(8) Uani 1 1 d . . .
H24A H 1.2510 0.5062 0.8067 0.077 Uiso 1 1 calc R . .
H24B H 1.3943 0.5202 0.7900 0.077 Uiso 1 1 calc R . .
H24C H 1.3620 0.4553 0.7437 0.077 Uiso 1 1 calc R . .
C25 C 0.8775(2) 0.81557(17) 0.85581(15) 0.0334(6) Uani 1 1 d . . .
H25A H 0.8355 0.7841 0.8309 0.040 Uiso 1 1 calc R . .
C26 C 0.8281(3) 0.91401(18) 0.84401(17) 0.0429(7) Uani 1 1 d . . .
H26A H 0.8552 0.9256 0.7958 0.064 Uiso 1 1 calc R . .
H26B H 0.8650 0.9468 0.8694 0.064 Uiso 1 1 calc R . .
H26C H 0.7324 0.9327 0.8593 0.064 Uiso 1 1 calc R . .
C27 C 0.8362(3) 0.7955(2) 0.93057(16) 0.0444(7) Uani 1 1 d . . .
H27A H 0.8684 0.7323 0.9371 0.067 Uiso 1 1 calc R . .
H27B H 0.7406 0.8137 0.9462 0.067 Uiso 1 1 calc R . .
H27C H 0.8732 0.8275 0.9565 0.067 Uiso 1 1 calc R . .
C28 C 0.7141(2) 0.69772(17) 0.68830(11) 0.0254(5) Uani 1 1 d . . .
H28A H 0.6945 0.7495 0.6597 0.030 Uiso 1 1 calc R . .
H28B H 0.6833 0.6506 0.6737 0.030 Uiso 1 1 calc R . .
C29 C 0.65341(18) 0.72071(15) 0.76083(11) 0.0222(4) Uani 1 1 d . . .
C30 C 0.6104(2) 0.80808(17) 0.78508(13) 0.0287(5) Uani 1 1 d . . .
H30A H 0.6195 0.8543 0.7544 0.034 Uiso 1 1 calc R . .
C31 C 0.5550(2) 0.82749(19) 0.85330(14) 0.0368(6) Uani 1 1 d . . .
H31A H 0.5242 0.8870 0.8685 0.044 Uiso 1 1 calc R . .
C32 C 0.5441(2) 0.7617(2) 0.89932(13) 0.0396(7) Uani 1 1 d . . .
H32A H 0.5074 0.7756 0.9460 0.047 Uiso 1 1 calc R . .
C33 C 0.5871(2) 0.6750(2) 0.87672(13) 0.0371(6) Uani 1 1 d . . .
H33A H 0.5810 0.6291 0.9080 0.045 Uiso 1 1 calc R . .
C34 C 0.6390(2) 0.65541(17) 0.80850(12) 0.0277(5) Uani 1 1 d . . .
H34A H 0.6657 0.5958 0.7936 0.033 Uiso 1 1 calc R . .
C35 C 1.0913(2) 0.5979(2) 0.59027(13) 0.0432(7) Uani 1 1 d . . .
H35A H 1.1546 0.6331 0.5752 0.052 Uiso 1 1 calc R . .
H35B H 1.1358 0.5345 0.5912 0.052 Uiso 1 1 calc R . .
C36 C 0.9831(2) 0.6188(2) 0.55712(12) 0.0378(6) Uani 1 1 d . . .
C37 C 0.9038(3) 0.5618(2) 0.56160(13) 0.0401(7) Uani 1 1 d . . .
H37A H 0.9278 0.5056 0.5807 0.048 Uiso 1 1 calc R . .
C38 C 0.7901(3) 0.5864(2) 0.53843(13) 0.0434(7) Uani 1 1 d . . .
H38A H 0.7390 0.5464 0.5406 0.052 Uiso 1 1 calc R . .
C39 C 0.7520(3) 0.6690(2) 0.51231(14) 0.0468(8) Uani 1 1 d . . .
H39A H 0.6739 0.6862 0.4974 0.056 Uiso 1 1 calc R . .
C40 C 0.8279(3) 0.7264(2) 0.50793(14) 0.0460(7) Uani 1 1 d . . .
H40A H 0.8021 0.7829 0.4896 0.055 Uiso 1 1 calc R . .
C41 C 0.9409(3) 0.7020(2) 0.52997(13) 0.0408(7) Uani 1 1 d . . .
H41A H 0.9916 0.7425 0.5267 0.049 Uiso 1 1 calc R . .
O2 O 0.96062(17) 0.78612(13) 0.66469(10) 0.0365(4) Uani 1 1 d . . .
C42 C 1.1022(8) 0.7907(8) 0.6336(6) 0.029(2) Uani 0.404(17) 1 d P A 1
H42A H 1.1601 0.7667 0.6639 0.035 Uiso 0.404(17) 1 calc PR A 1
H42B H 1.1400 0.7603 0.5890 0.035 Uiso 0.404(17) 1 calc PR A 1
C43 C 1.0759(10) 0.8882(7) 0.6277(8) 0.041(3) Uani 0.404(17) 1 d P A 1
H43A H 1.1490 0.9043 0.5949 0.050 Uiso 0.404(17) 1 calc PR A 1
H43B H 1.0619 0.9164 0.6720 0.050 Uiso 0.404(17) 1 calc PR A 1
C42A C 1.0758(7) 0.8189(5) 0.6590(5) 0.0310(15) Uani 0.596(17) 1 d P A 2
H42C H 1.1564 0.7697 0.6536 0.037 Uiso 0.596(17) 1 calc PR A 2
H42D H 1.0651 0.8544 0.6995 0.037 Uiso 0.596(17) 1 calc PR A 2
C43A C 1.0812(6) 0.8745(5) 0.5971(4) 0.0357(15) Uani 0.596(17) 1 d P A 2
H43C H 1.1285 0.9188 0.5985 0.043 Uiso 0.596(17) 1 calc PR A 2
H43D H 1.1242 0.8379 0.5555 0.043 Uiso 0.596(17) 1 calc PR A 2
C44 C 0.9410(3) 0.9168(2) 0.60075(17) 0.0440(7) Uani 1 1 d . . .
H44A H 0.8991 0.9808 0.6052 0.053 Uiso 1 1 calc R A 1
H44B H 0.9566 0.8969 0.5536 0.053 Uiso 1 1 calc R A 1
C45 C 0.8637(3) 0.86561(19) 0.65079(15) 0.0396(6) Uani 1 1 d . A .
H45A H 0.8166 0.9007 0.6928 0.047 Uiso 1 1 calc R . .
H45B H 0.7992 0.8496 0.6315 0.047 Uiso 1 1 calc R . .
B1 B 0.4156(2) 0.15142(19) 0.72442(14) 0.0256(5) Uani 1 1 d . . .
C46 C 0.2738(2) 0.13946(16) 0.71949(13) 0.0287(5) Uani 1 1 d . . .
C47 C 0.2400(2) 0.13453(16) 0.65971(14) 0.0302(5) Uani 1 1 d . . .
C48 C 0.1307(3) 0.10882(17) 0.65521(17) 0.0423(7) Uani 1 1 d . . .
C49 C 0.0496(3) 0.0879(2) 0.7130(2) 0.0496(8) Uani 1 1 d . . .
C50 C 0.0782(3) 0.0904(2) 0.77358(19) 0.0494(8) Uani 1 1 d . . .
C51 C 0.1889(3) 0.11459(19) 0.77590(16) 0.0396(6) Uani 1 1 d . . .
C52 C 0.4018(2) 0.20827(16) 0.79307(12) 0.0266(5) Uani 1 1 d . . .
C53 C 0.2900(2) 0.27159(18) 0.82711(13) 0.0306(5) Uani 1 1 d . . .
C54 C 0.2832(3) 0.32133(19) 0.88212(13) 0.0347(6) Uani 1 1 d . . .
C55 C 0.3921(3) 0.31104(19) 0.90581(13) 0.0370(6) Uani 1 1 d . . .
C56 C 0.5054(3) 0.25169(19) 0.87374(14) 0.0356(6) Uani 1 1 d . . .
C57 C 0.5084(2) 0.20260(18) 0.81946(13) 0.0311(5) Uani 1 1 d . . .
C58 C 0.4797(2) 0.21168(16) 0.66329(12) 0.0252(5) Uani 1 1 d . . .
C59 C 0.6117(2) 0.19760(19) 0.63103(14) 0.0351(6) Uani 1 1 d . . .
C60 C 0.6612(3) 0.2546(2) 0.58453(15) 0.0460(8) Uani 1 1 d . . .
C61 C 0.5806(3) 0.3301(2) 0.56837(14) 0.0461(7) Uani 1 1 d . . .
C62 C 0.4494(3) 0.34905(19) 0.59947(14) 0.0379(6) Uani 1 1 d . . .
C63 C 0.4038(2) 0.29072(17) 0.64519(13) 0.0296(5) Uani 1 1 d . . .
C64 C 0.5031(2) 0.04740(17) 0.72675(13) 0.0308(5) Uani 1 1 d . . .
H64A H 0.5957 0.0463 0.7210 0.037 Uiso 1 1 calc R . .
H64B H 0.4723 0.0242 0.7719 0.037 Uiso 1 1 calc R . .
C65 C 0.4964(2) -0.01277(17) 0.67405(14) 0.0330(6) Uani 1 1 d . . .
C66 C 0.5692(3) -0.01507(19) 0.60768(15) 0.0448(7) Uani 1 1 d . . .
H66A H 0.6267 0.0213 0.5950 0.054 Uiso 1 1 calc R . .
C67 C 0.5597(4) -0.0695(2) 0.55933(18) 0.0597(10) Uani 1 1 d . . .
H67A H 0.6101 -0.0696 0.5141 0.072 Uiso 1 1 calc R . .
C68 C 0.4778(4) -0.1233(2) 0.5766(2) 0.0657(12) Uani 1 1 d . . .
H68A H 0.4712 -0.1603 0.5434 0.079 Uiso 1 1 calc R . .
C69 C 0.4054(3) -0.1232(2) 0.6423(2) 0.0548(9) Uani 1 1 d . . .
H69A H 0.3496 -0.1607 0.6547 0.066 Uiso 1 1 calc R . .
C70 C 0.4139(3) -0.06818(18) 0.69049(17) 0.0415(7) Uani 1 1 d . . .
H70A H 0.3627 -0.0681 0.7355 0.050 Uiso 1 1 calc R . .
F1 F -0.05756(18) 0.06431(14) 0.70903(14) 0.0737(7) Uani 1 1 d . . .
F2 F -0.00005(19) 0.06975(15) 0.83074(12) 0.0731(7) Uani 1 1 d . . .
F3 F 0.21286(18) 0.11126(13) 0.83736(9) 0.0535(5) Uani 1 1 d . . .
F4 F 0.62546(14) 0.14649(11) 0.79101(9) 0.0432(4) Uani 1 1 d . . .
F5 F 0.61395(17) 0.24087(13) 0.89610(9) 0.0519(5) Uani 1 1 d . . .
F6 F 0.17190(16) 0.38108(12) 0.91199(9) 0.0508(5) Uani 1 1 d . . .
F7 F 0.17729(14) 0.28828(11) 0.80766(8) 0.0419(4) Uani 1 1 d . . .
F8 F 0.70207(14) 0.12578(13) 0.64414(10) 0.0507(5) Uani 1 1 d . . .
F9 F 0.27407(14) 0.31579(10) 0.67381(8) 0.0379(4) Uani 1 1 d . . .
F10 F 0.79132(18) 0.23433(17) 0.55585(10) 0.0709(6) Uani 1 1 d . . .
F11 F 0.6284(2) 0.38527(16) 0.52408(10) 0.0720(6) Uani 1 1 d . . .
F12 F 0.3675(2) 0.42404(12) 0.58503(10) 0.0536(5) Uani 1 1 d . . .
F13 F 0.38668(18) 0.35979(13) 0.95896(9) 0.0524(5) Uani 1 1 d . . .
F14 F 0.10588(18) 0.10503(12) 0.59451(11) 0.0570(5) Uani 1 1 d . . .
F15 F 0.31563(15) 0.15309(10) 0.60073(8) 0.0362(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.01348(9) 0.03565(13) 0.02189(11) 0.00077(9) -0.00690(7) -0.00671(8)
O1 0.0182(7) 0.0308(9) 0.0217(7) -0.0029(6) -0.0072(6) -0.0068(6)
N1 0.0124(7) 0.0276(10) 0.0281(10) -0.0018(8) -0.0087(7) -0.0063(7)
C1 0.0136(9) 0.0271(11) 0.0222(10) -0.0024(9) -0.0060(8) -0.0050(8)
C2 0.0170(9) 0.0281(12) 0.0234(10) -0.0052(9) -0.0073(8) -0.0068(8)
C3 0.0223(10) 0.0290(12) 0.0311(12) -0.0017(10) -0.0098(9) -0.0142(9)
C4 0.0238(10) 0.0357(13) 0.0261(11) 0.0017(10) -0.0107(9) -0.0139(9)
C5 0.0238(10) 0.0331(13) 0.0238(11) -0.0025(9) -0.0101(9) -0.0131(9)
C6 0.0176(9) 0.0267(11) 0.0235(10) -0.0023(9) -0.0077(8) -0.0087(8)
C7 0.0237(10) 0.0297(12) 0.0269(11) -0.0083(9) -0.0089(9) -0.0080(9)
C8 0.0271(12) 0.0345(14) 0.0347(13) -0.0150(11) -0.0053(10) -0.0029(10)
C9 0.0401(14) 0.0387(15) 0.0385(14) -0.0098(12) -0.0145(11) -0.0177(12)
C10 0.0236(11) 0.0416(14) 0.0312(12) -0.0108(11) -0.0129(9) -0.0072(10)
C11 0.0400(14) 0.0462(16) 0.0279(12) 0.0043(11) -0.0147(11) -0.0268(12)
C12 0.0472(15) 0.0574(18) 0.0258(12) 0.0074(12) -0.0157(11) -0.0329(14)
C13 0.0454(17) 0.096(3) 0.0323(14) 0.0061(16) -0.0082(13) -0.0457(18)
C14 0.086(2) 0.0460(18) 0.0403(16) 0.0108(14) -0.0309(17) -0.0264(17)
C15 0.0178(9) 0.0292(12) 0.0259(11) -0.0027(9) -0.0091(8) -0.0085(8)
C16 0.0190(10) 0.0266(12) 0.0303(11) 0.0045(9) -0.0141(9) -0.0109(8)
C17 0.0185(10) 0.0369(14) 0.0341(13) 0.0037(10) -0.0125(9) -0.0104(9)
C18 0.0203(11) 0.0480(16) 0.0518(16) 0.0055(13) -0.0167(11) -0.0167(11)
C19 0.0331(13) 0.0477(17) 0.0598(19) 0.0038(14) -0.0230(13) -0.0249(12)
C20 0.0354(13) 0.0346(14) 0.0552(17) -0.0013(12) -0.0214(12) -0.0174(11)
C21 0.0220(10) 0.0293(12) 0.0396(13) 0.0024(10) -0.0151(10) -0.0102(9)
C22 0.0172(10) 0.0436(15) 0.0454(15) -0.0046(12) -0.0092(10) -0.0077(10)
C23 0.0244(12) 0.063(2) 0.0502(18) -0.0025(15) -0.0019(12) -0.0116(13)
C24 0.0370(15) 0.0409(17) 0.067(2) 0.0006(15) -0.0045(14) -0.0020(13)
C25 0.0225(11) 0.0283(13) 0.0519(16) -0.0042(11) -0.0130(11) -0.0071(9)
C26 0.0340(14) 0.0285(14) 0.067(2) -0.0049(13) -0.0188(13) -0.0039(11)
C27 0.0318(14) 0.0429(17) 0.0550(18) -0.0050(14) -0.0060(13) -0.0081(12)
C28 0.0153(9) 0.0377(13) 0.0240(11) -0.0016(10) -0.0079(8) -0.0057(9)
C29 0.0086(8) 0.0329(12) 0.0263(11) -0.0028(9) -0.0068(8) -0.0046(8)
C30 0.0177(10) 0.0303(13) 0.0365(13) -0.0021(10) -0.0042(9) -0.0059(9)
C31 0.0226(11) 0.0454(16) 0.0399(15) -0.0165(12) -0.0019(10) -0.0078(11)
C32 0.0225(11) 0.065(2) 0.0268(12) -0.0082(13) 0.0008(10) -0.0097(12)
C33 0.0210(11) 0.0523(17) 0.0313(13) 0.0091(12) -0.0004(10) -0.0065(11)
C34 0.0157(9) 0.0313(13) 0.0334(13) -0.0009(10) -0.0031(9) -0.0047(9)
C35 0.0189(11) 0.072(2) 0.0292(13) 0.0025(13) 0.0009(10) -0.0031(12)
C36 0.0260(12) 0.0596(18) 0.0189(11) -0.0033(12) 0.0009(9) -0.0026(12)
C37 0.0332(13) 0.0543(18) 0.0224(12) -0.0069(12) -0.0007(10) 0.0002(12)
C38 0.0399(15) 0.063(2) 0.0252(13) -0.0130(13) -0.0058(11) -0.0113(14)
C39 0.0400(15) 0.068(2) 0.0273(13) -0.0103(14) -0.0169(11) 0.0032(14)
C40 0.0532(18) 0.0575(19) 0.0236(13) -0.0009(13) -0.0165(12) -0.0026(15)
C41 0.0376(14) 0.0602(19) 0.0208(12) 0.0028(12) -0.0053(10) -0.0096(13)
O2 0.0292(9) 0.0471(11) 0.0428(11) 0.0166(9) -0.0195(8) -0.0194(8)
C42 0.018(3) 0.034(5) 0.034(5) 0.005(3) -0.006(3) -0.006(3)
C43 0.034(4) 0.033(5) 0.062(8) 0.003(5) -0.021(5) -0.011(3)
C42A 0.023(3) 0.031(3) 0.043(4) 0.003(2) -0.014(3) -0.010(2)
C43A 0.034(2) 0.034(3) 0.041(4) 0.003(3) -0.008(3) -0.014(2)
C44 0.0405(15) 0.0370(16) 0.0538(18) 0.0051(13) -0.0124(13) -0.0097(12)
C45 0.0303(13) 0.0459(17) 0.0446(16) 0.0059(13) -0.0161(12) -0.0087(12)
B1 0.0180(11) 0.0318(14) 0.0291(13) -0.0012(11) -0.0076(10) -0.0082(10)
C46 0.0200(10) 0.0246(12) 0.0433(14) -0.0049(10) -0.0107(10) -0.0055(9)
C47 0.0222(11) 0.0222(12) 0.0479(15) -0.0057(10) -0.0143(10) -0.0025(9)
C48 0.0384(14) 0.0250(13) 0.073(2) -0.0104(13) -0.0335(14) -0.0045(11)
C49 0.0253(13) 0.0366(16) 0.093(3) -0.0084(16) -0.0174(15) -0.0147(12)
C50 0.0334(14) 0.0430(17) 0.074(2) -0.0082(16) -0.0036(14) -0.0211(13)
C51 0.0281(12) 0.0381(15) 0.0538(18) -0.0050(13) -0.0030(12) -0.0165(11)
C52 0.0238(10) 0.0313(13) 0.0283(12) 0.0034(10) -0.0076(9) -0.0128(9)
C53 0.0248(11) 0.0390(14) 0.0297(12) -0.0019(11) -0.0065(9) -0.0113(10)
C54 0.0322(13) 0.0422(15) 0.0292(13) -0.0051(11) -0.0017(10) -0.0137(11)
C55 0.0432(15) 0.0477(16) 0.0263(12) -0.0042(12) -0.0087(11) -0.0214(13)
C56 0.0330(13) 0.0455(16) 0.0375(14) 0.0034(12) -0.0163(11) -0.0190(12)
C57 0.0236(11) 0.0382(14) 0.0343(13) -0.0001(11) -0.0082(10) -0.0122(10)
C58 0.0204(10) 0.0342(13) 0.0252(11) -0.0034(9) -0.0085(8) -0.0110(9)
C59 0.0231(11) 0.0486(16) 0.0373(14) -0.0009(12) -0.0101(10) -0.0131(11)
C60 0.0326(14) 0.075(2) 0.0365(15) -0.0015(15) -0.0016(12) -0.0309(15)
C61 0.0561(18) 0.064(2) 0.0318(14) 0.0130(14) -0.0138(13) -0.0386(16)
C62 0.0489(16) 0.0430(16) 0.0340(14) 0.0048(12) -0.0197(12) -0.0241(13)
C63 0.0288(12) 0.0354(14) 0.0304(12) -0.0006(10) -0.0111(10) -0.0145(10)
C64 0.0281(12) 0.0326(13) 0.0342(13) 0.0023(10) -0.0137(10) -0.0072(10)
C65 0.0294(12) 0.0260(13) 0.0424(15) -0.0018(11) -0.0185(11) 0.0035(10)
C66 0.0480(16) 0.0338(15) 0.0437(16) -0.0058(13) -0.0142(13) 0.0065(12)
C67 0.075(2) 0.0420(19) 0.0493(19) -0.0163(15) -0.0227(17) 0.0147(17)
C68 0.077(2) 0.0387(18) 0.083(3) -0.0293(18) -0.053(2) 0.0169(17)
C69 0.0490(18) 0.0321(16) 0.091(3) -0.0162(16) -0.0424(18) 0.0026(13)
C70 0.0352(14) 0.0329(15) 0.0590(19) -0.0046(13) -0.0226(13) -0.0026(11)
F1 0.0383(10) 0.0644(13) 0.136(2) -0.0101(13) -0.0325(12) -0.0300(9)
F2 0.0495(11) 0.0783(15) 0.0938(16) -0.0049(12) 0.0103(11) -0.0461(11)
F3 0.0530(10) 0.0713(13) 0.0444(10) 0.0029(9) -0.0020(8) -0.0398(10)
F4 0.0248(7) 0.0525(10) 0.0556(10) -0.0128(8) -0.0160(7) -0.0078(7)
F5 0.0444(9) 0.0689(12) 0.0549(11) -0.0084(9) -0.0280(8) -0.0195(9)
F6 0.0397(9) 0.0610(11) 0.0454(10) -0.0241(9) -0.0021(7) -0.0069(8)
F7 0.0248(7) 0.0527(10) 0.0465(9) -0.0175(8) -0.0109(6) -0.0029(7)
F8 0.0193(7) 0.0656(12) 0.0629(11) 0.0032(9) -0.0081(7) -0.0073(7)
F9 0.0274(7) 0.0322(8) 0.0520(10) 0.0018(7) -0.0110(7) -0.0039(6)
F10 0.0365(10) 0.1157(19) 0.0600(12) 0.0059(12) 0.0082(9) -0.0397(11)
F11 0.0868(15) 0.0992(17) 0.0489(11) 0.0285(11) -0.0128(11) -0.0644(14)
F12 0.0726(13) 0.0420(10) 0.0582(11) 0.0204(9) -0.0329(10) -0.0236(9)
F13 0.0561(11) 0.0710(13) 0.0370(9) -0.0172(9) -0.0135(8) -0.0236(9)
F14 0.0567(11) 0.0500(11) 0.0851(14) -0.0043(10) -0.0488(10) -0.0185(9)
F15 0.0377(8) 0.0363(8) 0.0408(9) -0.0046(7) -0.0228(7) -0.0073(6)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O1 1.9655(17) . ?
Zr1 C35 2.252(3) . ?
Zr1 O2 2.2529(19) . ?
Zr1 C28 2.280(2) . ?
Zr1 N1 2.3010(18) . ?
O1 C1 1.349(3) . ?
N1 C15 1.299(3) . ?
N1 C16 1.461(3) . ?
C1 C6 1.403(3) . ?
C1 C2 1.410(3) . ?
C2 C3 1.384(3) . ?
C2 C7 1.535(3) . ?
C3 C4 1.413(3) . ?
C4 C5 1.373(3) . ?
C4 C11 1.524(4) . ?
C5 C6 1.407(3) . ?
C6 C15 1.442(3) . ?
C7 C9 1.533(4) . ?
C7 C10 1.541(3) . ?
C7 C8 1.542(3) . ?
C11 C12 1.535(3) . ?
C11 C13 1.536(4) . ?
C11 C14 1.547(4) . ?
C16 C21 1.398(3) . ?
C16 C17 1.410(3) . ?
C17 C18 1.399(3) . ?
C17 C22 1.520(4) . ?
C18 C19 1.379(4) . ?
C19 C20 1.377(4) . ?
C20 C21 1.401(3) . ?
C21 C25 1.519(3) . ?
C22 C24 1.532(4) . ?
C22 C23 1.538(4) . ?
C25 C27 1.525(4) . ?
C25 C26 1.532(4) . ?
C28 C29 1.483(3) . ?
C29 C34 1.399(3) . ?
C29 C30 1.406(3) . ?
C30 C31 1.388(4) . ?
C31 C32 1.379(4) . ?
C32 C33 1.386(4) . ?
C33 C34 1.384(4) . ?
C35 C36 1.469(4) . ?
C36 C37 1.406(4) . ?
C36 C41 1.408(4) . ?
C37 C38 1.398(4) . ?
C38 C39 1.383(5) . ?
C39 C40 1.381(5) . ?
C40 C41 1.379(4) . ?
O2 C42A 1.475(5) . ?
O2 C45 1.475(3) . ?
O2 C42 1.545(8) . ?
C42 C43 1.496(16) . ?
C43 C44 1.653(11) . ?
C42A C43A 1.504(11) . ?
C43A C44 1.484(7) . ?
C44 C45 1.510(4) . ?
B1 C46 1.651(3) . ?
B1 C52 1.663(4) . ?
B1 C58 1.666(4) . ?
B1 C64 1.668(4) . ?
C46 C47 1.380(4) . ?
C46 C51 1.403(4) . ?
C47 F15 1.350(3) . ?
C47 C48 1.398(3) . ?
C48 F14 1.348(3) . ?
C48 C49 1.374(5) . ?
C49 F1 1.353(3) . ?
C49 C50 1.363(5) . ?
C50 F2 1.348(4) . ?
C50 C51 1.387(4) . ?
C51 F3 1.347(4) . ?
C52 C57 1.392(3) . ?
C52 C53 1.398(3) . ?
C53 F7 1.351(3) . ?
C53 C54 1.385(4) . ?
C54 F6 1.343(3) . ?
C54 C55 1.370(4) . ?
C55 F13 1.348(3) . ?
C55 C56 1.364(4) . ?
C56 F5 1.351(3) . ?
C56 C57 1.380(4) . ?
C57 F4 1.350(3) . ?
C58 C63 1.391(4) . ?
C58 C59 1.392(3) . ?
C59 F8 1.354(3) . ?
C59 C60 1.392(4) . ?
C60 F10 1.352(3) . ?
C60 C61 1.360(5) . ?
C61 F11 1.339(3) . ?
C61 C62 1.372(4) . ?
C62 F12 1.348(3) . ?
C62 C63 1.382(4) . ?
C63 F9 1.348(3) . ?
C64 C65 1.507(4) . ?
C65 C66 1.387(4) . ?
C65 C70 1.402(4) . ?
C66 C67 1.389(4) . ?
C67 C68 1.378(6) . ?
C68 C69 1.377(6) . ?
C69 C70 1.388(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
O1 Zr1 C35 95.87(10) . . ?
O1 Zr1 O2 166.71(6) . . ?
C35 Zr1 O2 90.68(10) . . ?
O1 Zr1 C28 92.08(8) . . ?
C35 Zr1 C28 124.97(9) . . ?
O2 Zr1 C28 93.62(8) . . ?
O1 Zr1 N1 78.74(6) . . ?
C35 Zr1 N1 114.39(8) . . ?
O2 Zr1 N1 88.03(7) . . ?
C28 Zr1 N1 120.56(7) . . ?
C1 O1 Zr1 142.60(14) . . ?
C15 N1 C16 112.30(18) . . ?
C15 N1 Zr1 123.60(14) . . ?
C16 N1 Zr1 124.02(14) . . ?
O1 C1 C6 117.41(19) . . ?
O1 C1 C2 122.36(19) . . ?
C6 C1 C2 120.2(2) . . ?
C3 C2 C1 116.37(19) . . ?
C3 C2 C7 121.9(2) . . ?
C1 C2 C7 121.7(2) . . ?
C2 C3 C4 125.2(2) . . ?
C5 C4 C3 116.5(2) . . ?
C5 C4 C11 123.6(2) . . ?
C3 C4 C11 119.8(2) . . ?
C4 C5 C6 121.2(2) . . ?
C1 C6 C5 120.4(2) . . ?
C1 C6 C15 122.4(2) . . ?
C5 C6 C15 117.01(19) . . ?
C9 C7 C2 111.8(2) . . ?
C9 C7 C10 107.12(19) . . ?
C2 C7 C10 110.54(19) . . ?
C9 C7 C8 107.7(2) . . ?
C2 C7 C8 108.64(18) . . ?
C10 C7 C8 111.0(2) . . ?
C4 C11 C12 112.1(2) . . ?
C4 C11 C13 108.9(2) . . ?
C12 C11 C13 107.4(2) . . ?
C4 C11 C14 110.2(2) . . ?
C12 C11 C14 108.0(2) . . ?
C13 C11 C14 110.2(3) . . ?
N1 C15 C6 129.5(2) . . ?
C21 C16 C17 122.6(2) . . ?
C21 C16 N1 119.52(19) . . ?
C17 C16 N1 117.8(2) . . ?
C18 C17 C16 117.0(2) . . ?
C18 C17 C22 120.6(2) . . ?
C16 C17 C22 122.4(2) . . ?
C19 C18 C17 121.2(2) . . ?
C20 C19 C18 120.7(2) . . ?
C19 C20 C21 120.9(3) . . ?
C16 C21 C20 117.6(2) . . ?
C16 C21 C25 122.8(2) . . ?
C20 C21 C25 119.6(2) . . ?
C17 C22 C24 110.6(2) . . ?
C17 C22 C23 111.9(2) . . ?
C24 C22 C23 111.3(2) . . ?
C21 C25 C27 111.0(2) . . ?
C21 C25 C26 111.8(2) . . ?
C27 C25 C26 110.7(2) . . ?
C29 C28 Zr1 102.96(13) . . ?
C34 C29 C30 117.0(2) . . ?
C34 C29 C28 120.9(2) . . ?
C30 C29 C28 122.1(2) . . ?
C31 C30 C29 120.7(2) . . ?
C32 C31 C30 121.0(3) . . ?
C31 C32 C33 119.3(2) . . ?
C34 C33 C32 119.9(3) . . ?
C33 C34 C29 122.0(2) . . ?
C36 C35 Zr1 83.95(14) . . ?
C37 C36 C41 116.9(3) . . ?
C37 C36 C35 120.7(3) . . ?
C41 C36 C35 121.5(3) . . ?
C38 C37 C36 121.2(3) . . ?
C39 C38 C37 119.9(3) . . ?
C40 C39 C38 119.9(3) . . ?
C41 C40 C39 120.3(3) . . ?
C40 C41 C36 121.7(3) . . ?
C42A O2 C45 101.9(3) . . ?
C42A O2 C42 25.0(3) . . ?
C45 O2 C42 111.7(4) . . ?
C42A O2 Zr1 131.6(3) . . ?
C45 O2 Zr1 126.48(15) . . ?
C42 O2 Zr1 116.5(4) . . ?
C43 C42 O2 98.7(8) . . ?
C42 C43 C44 103.1(8) . . ?
O2 C42A C43A 104.2(5) . . ?
C44 C43A C42A 103.0(5) . . ?
C43A C44 C45 106.7(3) . . ?
C43A C44 C43 23.4(4) . . ?
C45 C44 C43 97.7(5) . . ?
O2 C45 C44 105.7(2) . . ?
C46 B1 C52 112.23(19) . . ?
C46 B1 C58 113.9(2) . . ?
C52 B1 C58 101.61(18) . . ?
C46 B1 C64 101.83(19) . . ?
C52 B1 C64 111.8(2) . . ?
C58 B1 C64 115.91(19) . . ?
C47 C46 C51 113.5(2) . . ?
C47 C46 B1 124.3(2) . . ?
C51 C46 B1 120.8(2) . . ?
F15 C47 C46 120.3(2) . . ?
F15 C47 C48 115.9(2) . . ?
C46 C47 C48 123.8(3) . . ?
F14 C48 C49 120.8(2) . . ?
F14 C48 C47 119.8(3) . . ?
C49 C48 C47 119.4(3) . . ?
F1 C49 C50 120.6(3) . . ?
F1 C49 C48 119.7(3) . . ?
C50 C49 C48 119.8(2) . . ?
F2 C50 C49 120.6(3) . . ?
F2 C50 C51 120.2(3) . . ?
C49 C50 C51 119.2(3) . . ?
F3 C51 C50 115.1(3) . . ?
F3 C51 C46 120.6(2) . . ?
C50 C51 C46 124.2(3) . . ?
C57 C52 C53 112.1(2) . . ?
C57 C52 B1 121.9(2) . . ?
C53 C52 B1 125.8(2) . . ?
F7 C53 C54 114.6(2) . . ?
F7 C53 C52 120.8(2) . . ?
C54 C53 C52 124.6(2) . . ?
F6 C54 C55 119.2(2) . . ?
F6 C54 C53 120.9(2) . . ?
C55 C54 C53 119.8(2) . . ?
F13 C55 C56 121.4(2) . . ?
F13 C55 C54 120.2(3) . . ?
C56 C55 C54 118.4(2) . . ?
F5 C56 C55 119.4(2) . . ?
F5 C56 C57 120.4(2) . . ?
C55 C56 C57 120.2(2) . . ?
F4 C57 C56 115.5(2) . . ?
F4 C57 C52 119.8(2) . . ?
C56 C57 C52 124.8(2) . . ?
C63 C58 C59 112.0(2) . . ?
C63 C58 B1 121.1(2) . . ?
C59 C58 B1 126.4(2) . . ?
F8 C59 C58 120.9(2) . . ?
F8 C59 C60 115.2(2) . . ?
C58 C59 C60 124.0(3) . . ?
F10 C60 C61 120.1(3) . . ?
F10 C60 C59 119.1(3) . . ?
C61 C60 C59 120.7(3) . . ?
F11 C61 C60 120.7(3) . . ?
F11 C61 C62 120.9(3) . . ?
C60 C61 C62 118.3(3) . . ?
F12 C62 C61 119.6(3) . . ?
F12 C62 C63 121.1(3) . . ?
C61 C62 C63 119.3(3) . . ?
F9 C63 C62 114.8(2) . . ?
F9 C63 C58 119.5(2) . . ?
C62 C63 C58 125.6(2) . . ?
C65 C64 B1 114.8(2) . . ?
C66 C65 C70 117.3(3) . . ?
C66 C65 C64 122.0(3) . . ?
C70 C65 C64 120.7(3) . . ?
C65 C66 C67 121.3(3) . . ?
C68 C67 C66 120.4(4) . . ?
C69 C68 C67 119.5(3) . . ?
C68 C69 C70 120.1(3) . . ?
C69 C70 C65 121.4(3) . . ?
_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        30.55
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.075
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.022 0.000 0.000 232 53 ' '
2 0.460 0.527 0.128 16 1 ' '
3 0.539 0.473 0.873 16 1 ' '
_platon_squeeze_details          
;
;


data_ec77
_database_code_depnum_ccdc_archive 'CCDC 924152'
#TrackingRef 'Complex 5-Ti.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C73 H74 B F15 N O2 Ti'
_chemical_formula_weight         1341.04
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.0260(4)
_cell_length_b                   15.5861(6)
_cell_length_c                   20.5604(8)
_cell_angle_alpha                84.504(2)
_cell_angle_beta                 74.448(2)
_cell_angle_gamma                73.522(2)
_cell_volume                     3263.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9806
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      30.38
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1394
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9505
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61033
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         24.71
_reflns_number_total             11052
_reflns_number_gt                7891
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2 (Bruker, 2009)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2009)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+2.2096P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11052
_refine_ls_number_parameters     849
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1047
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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
Ti1 Ti 0.55698(4) 0.85914(3) 0.31791(2) 0.01761(12) Uani 1 1 d . . .
O1 O 0.57435(15) 0.96873(10) 0.28251(7) 0.0179(4) Uani 1 1 d . . .
N1 N 0.48799(18) 0.85481(13) 0.22962(9) 0.0166(4) Uani 1 1 d . . .
C1 C 0.5905(2) 1.01586(16) 0.22395(11) 0.0175(5) Uani 1 1 d . . .
C2 C 0.6359(2) 1.09291(16) 0.21517(11) 0.0175(5) Uani 1 1 d . . .
C3 C 0.6550(2) 1.13066(17) 0.15067(12) 0.0213(6) Uani 1 1 d . . .
H3 H 0.6888 1.1815 0.1434 0.026 Uiso 1 1 calc R . .
C4 C 0.6285(2) 1.10013(17) 0.09517(11) 0.0214(6) Uani 1 1 d . . .
C5 C 0.5794(2) 1.02699(17) 0.10658(12) 0.0214(6) Uani 1 1 d . . .
H5 H 0.5571 1.0053 0.0709 0.026 Uiso 1 1 calc R . .
C6 C 0.5613(2) 0.98353(16) 0.17015(11) 0.0179(5) Uani 1 1 d . . .
C7 C 0.5050(2) 0.90977(16) 0.17851(12) 0.0188(6) Uani 1 1 d . . .
H7 H 0.4757 0.8995 0.1412 0.023 Uiso 1 1 calc R . .
C8 C 0.6600(2) 1.13430(16) 0.27389(11) 0.0199(6) Uani 1 1 d . . .
C9 C 0.7069(3) 1.21836(17) 0.25134(13) 0.0281(6) Uani 1 1 d . . .
H9A H 0.7924 1.2022 0.2187 0.042 Uiso 1 1 calc R . .
H9B H 0.7144 1.2455 0.2907 0.042 Uiso 1 1 calc R . .
H9C H 0.6439 1.2612 0.2302 0.042 Uiso 1 1 calc R . .
C10 C 0.5310(2) 1.16064(17) 0.32831(12) 0.0266(6) Uani 1 1 d . . .
H10A H 0.4660 1.2052 0.3095 0.040 Uiso 1 1 calc R . .
H10B H 0.5451 1.1860 0.3666 0.040 Uiso 1 1 calc R . .
H10C H 0.4995 1.1075 0.3436 0.040 Uiso 1 1 calc R . .
C11 C 0.7672(2) 1.06777(17) 0.30196(12) 0.0253(6) Uani 1 1 d . . .
H11A H 0.7412 1.0126 0.3170 0.038 Uiso 1 1 calc R . .
H11B H 0.7797 1.0942 0.3402 0.038 Uiso 1 1 calc R . .
H11C H 0.8492 1.0541 0.2665 0.038 Uiso 1 1 calc R . .
C12 C 0.6540(3) 1.14897(18) 0.02673(12) 0.0279(6) Uani 1 1 d . . .
C13 C 0.8009(3) 1.1360(2) -0.00038(14) 0.0505(9) Uani 1 1 d . . .
H13A H 0.8334 1.1622 0.0308 0.076 Uiso 1 1 calc R . .
H13B H 0.8185 1.1656 -0.0448 0.076 Uiso 1 1 calc R . .
H13C H 0.8452 1.0720 -0.0045 0.076 Uiso 1 1 calc R . .
C14 C 0.5832(4) 1.24830(19) 0.03409(14) 0.0478(9) Uani 1 1 d . . .
H14A H 0.4893 1.2555 0.0527 0.072 Uiso 1 1 calc R . .
H14B H 0.5980 1.2784 -0.0103 0.072 Uiso 1 1 calc R . .
H14C H 0.6167 1.2748 0.0646 0.072 Uiso 1 1 calc R . .
C15 C 0.6072(3) 1.11132(19) -0.02550(12) 0.0322(7) Uani 1 1 d . . .
H15A H 0.6543 1.0480 -0.0324 0.048 Uiso 1 1 calc R . .
H15B H 0.6243 1.1446 -0.0684 0.048 Uiso 1 1 calc R . .
H15C H 0.5132 1.1173 -0.0091 0.048 Uiso 1 1 calc R . .
C16 C 0.4141(2) 0.79428(16) 0.21923(11) 0.0180(5) Uani 1 1 d . . .
C17 C 0.2772(2) 0.82241(16) 0.24054(12) 0.0214(6) Uani 1 1 d . . .
C18 C 0.2083(2) 0.76891(18) 0.22392(13) 0.0272(6) Uani 1 1 d . . .
H18 H 0.1155 0.7859 0.2377 0.033 Uiso 1 1 calc R . .
C19 C 0.2721(3) 0.69196(18) 0.18803(13) 0.0284(6) Uani 1 1 d . . .
H19 H 0.2232 0.6572 0.1764 0.034 Uiso 1 1 calc R . .
C20 C 0.4064(3) 0.66509(17) 0.16892(12) 0.0260(6) Uani 1 1 d . . .
H20 H 0.4490 0.6111 0.1449 0.031 Uiso 1 1 calc R . .
C21 C 0.4813(2) 0.71545(16) 0.18401(12) 0.0205(6) Uani 1 1 d . . .
C22 C 0.2051(2) 0.90893(17) 0.27864(13) 0.0274(6) Uani 1 1 d . . .
H22 H 0.2667 0.9244 0.3005 0.033 Uiso 1 1 calc R . .
C23 C 0.0853(3) 0.8996(2) 0.33424(14) 0.0365(7) Uani 1 1 d . . .
H23A H 0.0204 0.8888 0.3138 0.055 Uiso 1 1 calc R . .
H23B H 0.0473 0.9548 0.3600 0.055 Uiso 1 1 calc R . .
H23C H 0.1115 0.8492 0.3645 0.055 Uiso 1 1 calc R . .
C24 C 0.1658(3) 0.98547(19) 0.22964(16) 0.0432(8) Uani 1 1 d . . .
H24A H 0.2444 0.9949 0.1973 0.065 Uiso 1 1 calc R . .
H24B H 0.1181 1.0403 0.2549 0.065 Uiso 1 1 calc R . .
H24C H 0.1097 0.9702 0.2053 0.065 Uiso 1 1 calc R . .
C25 C 0.6287(2) 0.68706(17) 0.15953(12) 0.0243(6) Uani 1 1 d . . .
H25 H 0.6648 0.7173 0.1877 0.029 Uiso 1 1 calc R . .
C26 C 0.6851(3) 0.58615(17) 0.16680(14) 0.0334(7) Uani 1 1 d . . .
H26A H 0.6629 0.5554 0.1341 0.050 Uiso 1 1 calc R . .
H26B H 0.6482 0.5662 0.2126 0.050 Uiso 1 1 calc R . .
H26C H 0.7804 0.5722 0.1584 0.050 Uiso 1 1 calc R . .
C27 C 0.6730(3) 0.7172(2) 0.08599(13) 0.0352(7) Uani 1 1 d . . .
H27A H 0.6324 0.6926 0.0578 0.053 Uiso 1 1 calc R . .
H27B H 0.7684 0.6954 0.0704 0.053 Uiso 1 1 calc R . .
H27C H 0.6467 0.7827 0.0827 0.053 Uiso 1 1 calc R . .
C28 C 0.4207(2) 0.91254(18) 0.40824(12) 0.0250(6) Uani 1 1 d . . .
H28A H 0.3801 0.9777 0.4055 0.030 Uiso 1 1 calc R . .
H28B H 0.3535 0.8797 0.4266 0.030 Uiso 1 1 calc R . .
C29 C 0.5279(2) 0.88891(17) 0.44160(11) 0.0230(6) Uani 1 1 d . . .
C30 C 0.6051(2) 0.94743(18) 0.43906(11) 0.0255(6) Uani 1 1 d . . .
H30 H 0.5813 1.0059 0.4202 0.031 Uiso 1 1 calc R . .
C31 C 0.7159(3) 0.92109(18) 0.46372(12) 0.0282(6) Uani 1 1 d . . .
H31 H 0.7673 0.9615 0.4616 0.034 Uiso 1 1 calc R . .
C32 C 0.7513(3) 0.83667(19) 0.49121(12) 0.0311(7) Uani 1 1 d . . .
H32 H 0.8289 0.8181 0.5065 0.037 Uiso 1 1 calc R . .
C33 C 0.6747(3) 0.77874(18) 0.49668(12) 0.0295(7) Uani 1 1 d . . .
H33 H 0.6978 0.7213 0.5173 0.035 Uiso 1 1 calc R . .
C34 C 0.5648(3) 0.80425(18) 0.47220(11) 0.0258(6) Uani 1 1 d . . .
H34 H 0.5129 0.7638 0.4761 0.031 Uiso 1 1 calc R . .
C35 C 0.7634(2) 0.81178(17) 0.31171(11) 0.0207(6) Uani 1 1 d . . .
H35A H 0.7928 0.8586 0.3275 0.025 Uiso 1 1 calc R . .
H35B H 0.7803 0.7581 0.3413 0.025 Uiso 1 1 calc R . .
C36 C 0.8372(2) 0.78936(16) 0.24148(11) 0.0183(6) Uani 1 1 d . . .
C37 C 0.8573(2) 0.85640(17) 0.19307(12) 0.0235(6) Uani 1 1 d . . .
H37 H 0.8250 0.9172 0.2061 0.028 Uiso 1 1 calc R . .
C38 C 0.9233(2) 0.83649(18) 0.12652(13) 0.0285(6) Uani 1 1 d . . .
H38 H 0.9335 0.8835 0.0943 0.034 Uiso 1 1 calc R . .
C39 C 0.9741(2) 0.74892(18) 0.10684(12) 0.0275(6) Uani 1 1 d . . .
H39 H 1.0192 0.7352 0.0612 0.033 Uiso 1 1 calc R . .
C40 C 0.9588(2) 0.68135(18) 0.15403(12) 0.0256(6) Uani 1 1 d . . .
H40 H 0.9958 0.6207 0.1411 0.031 Uiso 1 1 calc R . .
C41 C 0.8902(2) 0.70110(17) 0.22012(12) 0.0214(6) Uani 1 1 d . . .
H41 H 0.8789 0.6536 0.2517 0.026 Uiso 1 1 calc R . .
O2 O 0.52392(15) 0.73226(11) 0.34629(8) 0.0233(4) Uani 1 1 d . . .
C42 C 0.6244(3) 0.64724(17) 0.35128(13) 0.0293(6) Uani 1 1 d . . .
H42A H 0.6834 0.6553 0.3776 0.035 Uiso 1 1 calc R . .
H42B H 0.6773 0.6262 0.3058 0.035 Uiso 1 1 calc R . .
C43 C 0.5504(3) 0.58117(19) 0.38650(16) 0.0377(7) Uani 1 1 d . . .
H43A H 0.5406 0.5797 0.4359 0.045 Uiso 1 1 calc R . .
H43B H 0.5946 0.5202 0.3688 0.045 Uiso 1 1 calc R . .
C44 C 0.4183(3) 0.61808(19) 0.36948(16) 0.0407(8) Uani 1 1 d . . .
H44A H 0.4229 0.6022 0.3232 0.049 Uiso 1 1 calc R . .
H44B H 0.3494 0.5957 0.4021 0.049 Uiso 1 1 calc R . .
C45 C 0.3946(2) 0.71560(18) 0.37510(13) 0.0299(6) Uani 1 1 d . . .
H45A H 0.3313 0.7491 0.3493 0.036 Uiso 1 1 calc R . .
H45B H 0.3602 0.7336 0.4229 0.036 Uiso 1 1 calc R . .
B1 B 0.0728(3) 0.3504(2) 0.27269(14) 0.0219(7) Uani 1 1 d . . .
C46 C 0.0808(2) 0.29950(17) 0.20309(12) 0.0220(6) Uani 1 1 d . . .
C47 C 0.1874(2) 0.23231(18) 0.17157(12) 0.0252(6) Uani 1 1 d . . .
C48 C 0.1923(3) 0.18566(18) 0.11646(12) 0.0296(6) Uani 1 1 d . . .
C49 C 0.0859(3) 0.20532(19) 0.08954(12) 0.0319(7) Uani 1 1 d . . .
C50 C -0.0218(3) 0.27084(19) 0.11805(13) 0.0299(7) Uani 1 1 d . . .
C51 C -0.0235(3) 0.31534(18) 0.17355(12) 0.0270(6) Uani 1 1 d . . .
C52 C 0.2156(2) 0.36177(16) 0.27527(12) 0.0211(6) Uani 1 1 d . . .
C53 C 0.3016(2) 0.38585(17) 0.21828(12) 0.0257(6) Uani 1 1 d . . .
C54 C 0.4120(3) 0.41032(17) 0.21932(13) 0.0280(6) Uani 1 1 d . . .
C55 C 0.4397(2) 0.41421(17) 0.27965(14) 0.0270(6) Uani 1 1 d . . .
C56 C 0.3580(2) 0.39297(16) 0.33793(13) 0.0243(6) Uani 1 1 d . . .
C57 C 0.2500(2) 0.36734(16) 0.33451(12) 0.0206(6) Uani 1 1 d . . .
C58 C 0.0143(2) 0.28331(16) 0.33397(11) 0.0199(6) Uani 1 1 d . . .
C59 C 0.0926(2) 0.20408(17) 0.35442(12) 0.0220(6) Uani 1 1 d . . .
C60 C 0.0483(3) 0.14278(17) 0.40039(13) 0.0257(6) Uani 1 1 d . . .
C61 C -0.0828(3) 0.15892(19) 0.43058(12) 0.0306(7) Uani 1 1 d . . .
C62 C -0.1653(3) 0.23491(19) 0.41255(13) 0.0286(7) Uani 1 1 d . . .
C63 C -0.1169(2) 0.29393(17) 0.36501(12) 0.0247(6) Uani 1 1 d . . .
C64 C -0.0165(2) 0.45576(17) 0.27478(12) 0.0255(6) Uani 1 1 d . . .
H64A H 0.0139 0.4852 0.2310 0.031 Uiso 1 1 calc R . .
H64B H -0.1083 0.4561 0.2791 0.031 Uiso 1 1 calc R . .
C65 C -0.0141(2) 0.51129(17) 0.33077(12) 0.0246(6) Uani 1 1 d . . .
C66 C 0.0695(3) 0.56618(18) 0.31960(14) 0.0324(7) Uani 1 1 d . . .
H66 H 0.1261 0.5687 0.2760 0.039 Uiso 1 1 calc R . .
C67 C 0.0724(3) 0.61748(19) 0.37056(16) 0.0405(8) Uani 1 1 d . . .
H67 H 0.1301 0.6548 0.3613 0.049 Uiso 1 1 calc R . .
C68 C -0.0077(3) 0.6145(2) 0.43429(16) 0.0431(8) Uani 1 1 d . . .
H68 H -0.0057 0.6492 0.4693 0.052 Uiso 1 1 calc R . .
C69 C -0.0909(3) 0.56027(19) 0.44658(14) 0.0387(7) Uani 1 1 d . . .
H69 H -0.1464 0.5574 0.4905 0.046 Uiso 1 1 calc R . .
C70 C -0.0946(3) 0.50994(18) 0.39563(13) 0.0302(6) Uani 1 1 d . . .
H70 H -0.1535 0.4735 0.4052 0.036 Uiso 1 1 calc R . .
F1 F 0.29784(14) 0.20749(10) 0.19370(7) 0.0349(4) Uani 1 1 d . . .
F2 F 0.30031(16) 0.12130(11) 0.08881(8) 0.0429(4) Uani 1 1 d . . .
F3 F 0.08919(16) 0.15982(12) 0.03640(7) 0.0462(4) Uani 1 1 d . . .
F4 F -0.12888(15) 0.29095(11) 0.09311(8) 0.0430(4) Uani 1 1 d . . .
F5 F -0.13707(14) 0.37709(10) 0.19877(7) 0.0372(4) Uani 1 1 d . . .
F6 F 0.27804(14) 0.38841(10) 0.15674(7) 0.0360(4) Uani 1 1 d . . .
F7 F 0.49175(15) 0.43067(11) 0.16127(8) 0.0411(4) Uani 1 1 d . . .
F8 F 0.54795(14) 0.43678(10) 0.28190(8) 0.0394(4) Uani 1 1 d . . .
F9 F 0.38325(14) 0.39771(10) 0.39807(7) 0.0345(4) Uani 1 1 d . . .
F10 F 0.17324(13) 0.34899(9) 0.39479(6) 0.0256(3) Uani 1 1 d . . .
F11 F 0.22329(13) 0.18249(9) 0.32817(7) 0.0308(4) Uani 1 1 d . . .
F12 F 0.13194(15) 0.06712(10) 0.41637(8) 0.0378(4) Uani 1 1 d . . .
F13 F -0.12840(17) 0.10009(12) 0.47597(8) 0.0471(4) Uani 1 1 d . . .
F14 F -0.29547(15) 0.25166(12) 0.44054(8) 0.0460(4) Uani 1 1 d . . .
F15 F -0.21002(13) 0.36464(10) 0.34931(7) 0.0346(4) Uani 1 1 d . . .
C71 C 0.1529(3) 0.4849(2) 0.03405(16) 0.0510(9) Uani 1 1 d . . .
H71A H 0.1942 0.4219 0.0206 0.061 Uiso 1 1 calc R . .
H71B H 0.1086 0.4847 0.0828 0.061 Uiso 1 1 calc R . .
C73 C 0.0520(3) 0.5254(2) -0.00447(15) 0.0482(8) Uani 1 1 d . . .
H73A H 0.0964 0.5277 -0.0531 0.058 Uiso 1 1 calc R . .
H73B H 0.0080 0.5877 0.0102 0.058 Uiso 1 1 calc R . .
C72 C 0.2603(3) 0.5330(2) 0.02351(17) 0.0612(10) Uani 1 1 d . . .
H72A H 0.3012 0.5371 -0.0249 0.092 Uiso 1 1 calc R . .
H72B H 0.3264 0.4993 0.0469 0.092 Uiso 1 1 calc R . .
H72C H 0.2220 0.5933 0.0418 0.092 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0128(2) 0.0202(3) 0.0194(2) -0.00207(18) -0.00381(18) -0.0035(2)
O1 0.0155(9) 0.0210(10) 0.0186(8) -0.0025(7) -0.0053(7) -0.0054(8)
N1 0.0109(11) 0.0175(12) 0.0213(10) -0.0036(9) -0.0030(9) -0.0035(9)
C1 0.0090(13) 0.0192(14) 0.0211(12) -0.0028(11) -0.0013(10) -0.0002(11)
C2 0.0100(13) 0.0177(14) 0.0233(13) -0.0062(10) -0.0036(10) -0.0002(11)
C3 0.0160(14) 0.0228(15) 0.0273(13) -0.0027(11) -0.0038(11) -0.0093(12)
C4 0.0185(14) 0.0275(16) 0.0201(12) -0.0030(11) -0.0032(11) -0.0098(12)
C5 0.0174(14) 0.0275(16) 0.0217(12) -0.0066(11) -0.0050(11) -0.0077(12)
C6 0.0110(13) 0.0213(15) 0.0215(12) -0.0037(10) -0.0034(10) -0.0041(11)
C7 0.0144(14) 0.0210(15) 0.0219(13) -0.0057(11) -0.0059(11) -0.0030(12)
C8 0.0171(14) 0.0203(15) 0.0222(12) -0.0072(11) -0.0039(11) -0.0037(11)
C9 0.0336(17) 0.0261(16) 0.0301(14) -0.0066(12) -0.0113(13) -0.0116(13)
C10 0.0249(16) 0.0254(16) 0.0277(13) -0.0080(12) -0.0047(12) -0.0033(13)
C11 0.0225(15) 0.0279(16) 0.0284(13) -0.0061(11) -0.0103(12) -0.0058(12)
C12 0.0353(17) 0.0354(18) 0.0212(13) 0.0009(12) -0.0083(12) -0.0215(14)
C13 0.046(2) 0.091(3) 0.0271(15) 0.0043(16) -0.0051(14) -0.045(2)
C14 0.089(3) 0.037(2) 0.0297(15) 0.0086(13) -0.0228(17) -0.0315(19)
C15 0.0419(18) 0.0416(18) 0.0221(13) 0.0028(12) -0.0096(13) -0.0250(15)
C16 0.0160(14) 0.0192(14) 0.0218(12) 0.0003(10) -0.0071(11) -0.0075(12)
C17 0.0155(14) 0.0232(15) 0.0269(13) -0.0009(11) -0.0080(11) -0.0051(12)
C18 0.0142(14) 0.0333(17) 0.0355(15) -0.0005(13) -0.0062(12) -0.0086(13)
C19 0.0256(17) 0.0291(17) 0.0383(15) -0.0024(13) -0.0111(13) -0.0161(13)
C20 0.0261(17) 0.0222(15) 0.0322(14) -0.0038(12) -0.0093(12) -0.0074(13)
C21 0.0183(14) 0.0200(15) 0.0240(13) -0.0006(11) -0.0059(11) -0.0058(12)
C22 0.0148(15) 0.0283(16) 0.0391(15) -0.0087(12) -0.0046(12) -0.0051(12)
C23 0.0229(16) 0.0391(19) 0.0435(17) -0.0089(14) -0.0030(13) -0.0045(14)
C24 0.0287(18) 0.0297(18) 0.060(2) -0.0003(15) -0.0018(15) -0.0003(14)
C25 0.0180(15) 0.0224(16) 0.0324(14) -0.0052(11) -0.0063(12) -0.0035(12)
C26 0.0243(16) 0.0264(17) 0.0478(17) -0.0098(13) -0.0092(13) -0.0010(13)
C27 0.0224(16) 0.0419(19) 0.0357(15) -0.0051(13) 0.0000(13) -0.0056(14)
C28 0.0175(14) 0.0274(16) 0.0260(13) -0.0042(11) -0.0008(11) -0.0029(12)
C29 0.0202(15) 0.0267(16) 0.0146(12) -0.0061(11) 0.0038(11) -0.0003(12)
C30 0.0286(16) 0.0248(16) 0.0187(12) -0.0048(11) -0.0013(11) -0.0031(13)
C31 0.0299(16) 0.0327(18) 0.0234(13) -0.0074(12) -0.0042(12) -0.0109(14)
C32 0.0294(17) 0.0381(19) 0.0258(14) -0.0071(13) -0.0117(12) -0.0026(14)
C33 0.0365(17) 0.0290(16) 0.0193(13) -0.0003(11) -0.0086(12) -0.0017(14)
C34 0.0282(16) 0.0297(17) 0.0183(12) -0.0032(11) -0.0005(12) -0.0099(13)
C35 0.0158(14) 0.0233(15) 0.0237(13) -0.0007(11) -0.0062(11) -0.0051(12)
C36 0.0097(13) 0.0221(15) 0.0236(12) -0.0011(11) -0.0060(10) -0.0032(11)
C37 0.0120(14) 0.0229(15) 0.0313(14) -0.0044(12) -0.0014(11) -0.0003(12)
C38 0.0188(15) 0.0304(18) 0.0299(14) 0.0062(12) 0.0010(12) -0.0056(13)
C39 0.0187(15) 0.0364(18) 0.0232(13) -0.0055(13) 0.0004(11) -0.0048(13)
C40 0.0203(15) 0.0230(16) 0.0305(14) -0.0070(12) -0.0010(12) -0.0042(12)
C41 0.0127(14) 0.0226(16) 0.0272(13) 0.0018(11) -0.0034(11) -0.0043(12)
O2 0.0151(10) 0.0258(11) 0.0288(9) 0.0009(8) -0.0062(8) -0.0053(8)
C42 0.0249(16) 0.0243(16) 0.0364(15) -0.0018(12) -0.0100(13) -0.0006(13)
C43 0.0321(18) 0.0241(17) 0.0584(19) 0.0037(14) -0.0138(15) -0.0094(14)
C44 0.0350(18) 0.0343(19) 0.0581(19) 0.0015(15) -0.0167(15) -0.0140(15)
C45 0.0199(16) 0.0336(18) 0.0368(15) 0.0073(13) -0.0065(12) -0.0116(13)
B1 0.0178(16) 0.0259(18) 0.0221(14) -0.0010(12) -0.0067(13) -0.0044(14)
C46 0.0203(15) 0.0239(15) 0.0222(13) 0.0022(11) -0.0049(11) -0.0077(13)
C47 0.0233(16) 0.0307(16) 0.0243(13) 0.0031(12) -0.0089(12) -0.0101(13)
C48 0.0265(16) 0.0329(17) 0.0256(14) -0.0072(12) 0.0000(12) -0.0061(14)
C49 0.0346(18) 0.0439(19) 0.0226(13) -0.0070(13) -0.0051(13) -0.0193(16)
C50 0.0262(17) 0.0421(18) 0.0278(14) 0.0023(13) -0.0113(13) -0.0161(15)
C51 0.0220(16) 0.0302(17) 0.0291(14) -0.0004(12) -0.0057(12) -0.0083(14)
C52 0.0202(15) 0.0147(14) 0.0271(13) -0.0006(11) -0.0078(12) -0.0010(12)
C53 0.0234(16) 0.0257(16) 0.0279(14) 0.0012(12) -0.0063(12) -0.0069(13)
C54 0.0224(16) 0.0227(16) 0.0352(15) 0.0000(12) 0.0017(13) -0.0089(13)
C55 0.0158(15) 0.0186(15) 0.0480(17) -0.0046(12) -0.0071(13) -0.0066(12)
C56 0.0247(15) 0.0176(15) 0.0340(15) -0.0048(11) -0.0133(13) -0.0039(12)
C57 0.0188(14) 0.0166(14) 0.0239(13) -0.0004(11) -0.0026(11) -0.0034(12)
C58 0.0168(15) 0.0232(15) 0.0221(12) -0.0039(11) -0.0067(11) -0.0065(12)
C59 0.0156(15) 0.0268(16) 0.0251(13) -0.0034(12) -0.0041(11) -0.0083(13)
C60 0.0280(17) 0.0245(17) 0.0294(14) 0.0015(12) -0.0126(13) -0.0104(14)
C61 0.0379(19) 0.0384(19) 0.0241(14) 0.0078(13) -0.0079(13) -0.0264(16)
C62 0.0176(16) 0.0443(19) 0.0261(14) -0.0055(13) 0.0002(12) -0.0155(14)
C63 0.0179(16) 0.0282(16) 0.0277(14) -0.0035(12) -0.0083(12) -0.0027(13)
C64 0.0220(15) 0.0282(16) 0.0279(14) 0.0012(11) -0.0098(12) -0.0063(13)
C65 0.0189(15) 0.0196(15) 0.0330(15) -0.0002(11) -0.0129(12) 0.0042(12)
C66 0.0252(16) 0.0265(17) 0.0443(16) -0.0018(13) -0.0126(13) -0.0012(14)
C67 0.0342(18) 0.0271(18) 0.065(2) -0.0071(15) -0.0238(17) -0.0037(14)
C68 0.043(2) 0.0335(19) 0.052(2) -0.0175(15) -0.0222(17) 0.0055(16)
C69 0.0375(19) 0.0327(18) 0.0371(16) -0.0103(13) -0.0087(14) 0.0068(15)
C70 0.0248(16) 0.0244(16) 0.0365(16) -0.0039(12) -0.0075(13) 0.0020(13)
F1 0.0253(9) 0.0405(10) 0.0370(8) -0.0123(7) -0.0123(7) 0.0019(7)
F2 0.0362(10) 0.0496(11) 0.0385(9) -0.0206(8) -0.0040(8) -0.0034(9)
F3 0.0492(11) 0.0654(12) 0.0306(8) -0.0173(8) -0.0095(8) -0.0207(9)
F4 0.0358(10) 0.0624(12) 0.0410(9) -0.0051(8) -0.0204(8) -0.0176(9)
F5 0.0234(9) 0.0447(10) 0.0451(9) -0.0116(8) -0.0147(7) -0.0027(8)
F6 0.0372(10) 0.0514(11) 0.0246(8) 0.0061(7) -0.0070(7) -0.0230(8)
F7 0.0350(10) 0.0446(11) 0.0437(10) -0.0006(8) 0.0049(8) -0.0246(8)
F8 0.0252(9) 0.0370(10) 0.0632(11) -0.0070(8) -0.0112(8) -0.0177(8)
F9 0.0357(9) 0.0364(10) 0.0410(9) -0.0021(7) -0.0205(7) -0.0145(8)
F10 0.0243(8) 0.0295(9) 0.0252(8) 0.0005(6) -0.0085(7) -0.0091(7)
F11 0.0188(9) 0.0261(9) 0.0430(9) 0.0028(7) -0.0043(7) -0.0034(7)
F12 0.0451(10) 0.0259(9) 0.0478(9) 0.0108(7) -0.0205(8) -0.0133(8)
F13 0.0516(11) 0.0579(12) 0.0393(9) 0.0158(8) -0.0082(8) -0.0353(10)
F14 0.0249(10) 0.0694(13) 0.0427(9) 0.0002(9) 0.0030(8) -0.0224(9)
F15 0.0170(8) 0.0408(10) 0.0441(9) -0.0009(7) -0.0077(7) -0.0048(8)
C71 0.060(2) 0.041(2) 0.0454(18) -0.0161(15) -0.0103(17) -0.0005(18)
C73 0.057(2) 0.038(2) 0.0411(17) -0.0148(15) -0.0022(16) -0.0058(16)
C72 0.062(2) 0.063(3) 0.055(2) -0.0068(18) -0.0115(19) -0.013(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ti1 O1 1.8320(16) . ?
Ti1 O2 2.1114(17) . ?
Ti1 C28 2.119(2) . ?
Ti1 C35 2.156(2) . ?
Ti1 N1 2.1613(18) . ?
Ti1 C29 2.548(2) . ?
O1 C1 1.346(3) . ?
N1 C7 1.299(3) . ?
N1 C16 1.472(3) . ?
C1 C6 1.404(3) . ?
C1 C2 1.406(3) . ?
C2 C3 1.386(3) . ?
C2 C8 1.537(3) . ?
C3 C4 1.405(3) . ?
C4 C5 1.371(3) . ?
C4 C12 1.531(3) . ?
C5 C6 1.405(3) . ?
C6 C7 1.431(3) . ?
C8 C9 1.529(3) . ?
C8 C10 1.532(3) . ?
C8 C11 1.537(3) . ?
C12 C14 1.525(4) . ?
C12 C13 1.525(4) . ?
C12 C15 1.534(3) . ?
C16 C21 1.396(3) . ?
C16 C17 1.403(3) . ?
C17 C18 1.394(3) . ?
C17 C22 1.525(3) . ?
C18 C19 1.375(4) . ?
C19 C20 1.374(4) . ?
C20 C21 1.395(3) . ?
C21 C25 1.512(3) . ?
C22 C24 1.529(4) . ?
C22 C23 1.530(4) . ?
C25 C26 1.527(4) . ?
C25 C27 1.531(4) . ?
C28 C29 1.464(3) . ?
C29 C30 1.403(4) . ?
C29 C34 1.406(4) . ?
C30 C31 1.387(3) . ?
C31 C32 1.374(4) . ?
C32 C33 1.379(4) . ?
C33 C34 1.377(3) . ?
C35 C36 1.475(3) . ?
C36 C37 1.395(3) . ?
C36 C41 1.396(3) . ?
C37 C38 1.385(3) . ?
C38 C39 1.375(4) . ?
C39 C40 1.377(4) . ?
C40 C41 1.382(3) . ?
O2 C45 1.476(3) . ?
O2 C42 1.482(3) . ?
C42 C43 1.505(4) . ?
C43 C44 1.528(4) . ?
C44 C45 1.478(4) . ?
B1 C52 1.649(4) . ?
B1 C64 1.656(4) . ?
B1 C58 1.671(4) . ?
B1 C46 1.672(3) . ?
C46 C47 1.386(4) . ?
C46 C51 1.392(3) . ?
C47 F1 1.355(3) . ?
C47 C48 1.385(3) . ?
C48 F2 1.348(3) . ?
C48 C49 1.374(4) . ?
C49 F3 1.345(3) . ?
C49 C50 1.360(4) . ?
C50 F4 1.356(3) . ?
C50 C51 1.384(3) . ?
C51 F5 1.352(3) . ?
C52 C57 1.386(3) . ?
C52 C53 1.391(4) . ?
C53 F6 1.353(3) . ?
C53 C54 1.381(4) . ?
C54 F7 1.350(3) . ?
C54 C55 1.365(4) . ?
C55 F8 1.349(3) . ?
C55 C56 1.368(4) . ?
C56 F9 1.351(3) . ?
C56 C57 1.380(3) . ?
C57 F10 1.357(3) . ?
C58 C63 1.384(3) . ?
C58 C59 1.392(3) . ?
C59 F11 1.351(3) . ?
C59 C60 1.374(4) . ?
C60 F12 1.349(3) . ?
C60 C61 1.371(4) . ?
C61 F13 1.346(3) . ?
C61 C62 1.362(4) . ?
C62 F14 1.353(3) . ?
C62 C63 1.384(4) . ?
C63 F15 1.357(3) . ?
C64 C65 1.515(3) . ?
C65 C66 1.390(4) . ?
C65 C70 1.391(4) . ?
C66 C67 1.390(4) . ?
C67 C68 1.375(4) . ?
C68 C69 1.376(4) . ?
C69 C70 1.383(4) . ?
C71 C73 1.497(4) . ?
C71 C72 1.531(5) . ?
C73 C73 1.532(6) 2_565 ?
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
O1 Ti1 O2 171.13(6) . . ?
O1 Ti1 C28 93.93(9) . . ?
O2 Ti1 C28 89.73(9) . . ?
O1 Ti1 C35 91.30(8) . . ?
O2 Ti1 C35 93.69(8) . . ?
C28 Ti1 C35 121.33(9) . . ?
O1 Ti1 N1 83.47(7) . . ?
O2 Ti1 N1 87.69(7) . . ?
C28 Ti1 N1 119.27(8) . . ?
C35 Ti1 N1 119.38(8) . . ?
O1 Ti1 C29 98.29(7) . . ?
O2 Ti1 C29 89.35(7) . . ?
C28 Ti1 C29 35.06(8) . . ?
C35 Ti1 C29 86.37(8) . . ?
N1 Ti1 C29 154.20(8) . . ?
C1 O1 Ti1 142.14(14) . . ?
C7 N1 C16 111.09(18) . . ?
C7 N1 Ti1 122.31(15) . . ?
C16 N1 Ti1 126.57(14) . . ?
O1 C1 C6 116.5(2) . . ?
O1 C1 C2 123.07(19) . . ?
C6 C1 C2 120.4(2) . . ?
C3 C2 C1 116.0(2) . . ?
C3 C2 C8 121.8(2) . . ?
C1 C2 C8 122.1(2) . . ?
C2 C3 C4 125.5(2) . . ?
C5 C4 C3 116.6(2) . . ?
C5 C4 C12 123.7(2) . . ?
C3 C4 C12 119.7(2) . . ?
C4 C5 C6 121.1(2) . . ?
C1 C6 C5 120.3(2) . . ?
C1 C6 C7 122.1(2) . . ?
C5 C6 C7 117.5(2) . . ?
N1 C7 C6 129.4(2) . . ?
C9 C8 C10 108.2(2) . . ?
C9 C8 C2 111.81(19) . . ?
C10 C8 C2 108.46(19) . . ?
C9 C8 C11 106.72(19) . . ?
C10 C8 C11 111.4(2) . . ?
C2 C8 C11 110.29(19) . . ?
C14 C12 C13 110.4(2) . . ?
C14 C12 C4 110.3(2) . . ?
C13 C12 C4 108.8(2) . . ?
C14 C12 C15 108.1(2) . . ?
C13 C12 C15 107.3(2) . . ?
C4 C12 C15 111.9(2) . . ?
C21 C16 C17 122.7(2) . . ?
C21 C16 N1 119.2(2) . . ?
C17 C16 N1 117.9(2) . . ?
C18 C17 C16 117.2(2) . . ?
C18 C17 C22 120.7(2) . . ?
C16 C17 C22 122.1(2) . . ?
C19 C18 C17 121.3(2) . . ?
C20 C19 C18 120.3(2) . . ?
C19 C20 C21 121.4(2) . . ?
C20 C21 C16 117.2(2) . . ?
C20 C21 C25 120.5(2) . . ?
C16 C21 C25 122.3(2) . . ?
C17 C22 C24 110.4(2) . . ?
C17 C22 C23 112.5(2) . . ?
C24 C22 C23 110.4(2) . . ?
C21 C25 C26 112.4(2) . . ?
C21 C25 C27 110.7(2) . . ?
C26 C25 C27 109.8(2) . . ?
C29 C28 Ti1 88.68(15) . . ?
C30 C29 C34 117.3(2) . . ?
C30 C29 C28 120.9(2) . . ?
C34 C29 C28 121.6(2) . . ?
C30 C29 Ti1 103.78(15) . . ?
C34 C29 Ti1 105.56(15) . . ?
C28 C29 Ti1 56.26(12) . . ?
C31 C30 C29 120.9(2) . . ?
C32 C31 C30 120.0(2) . . ?
C31 C32 C33 120.4(2) . . ?
C34 C33 C32 119.9(3) . . ?
C33 C34 C29 121.3(2) . . ?
C36 C35 Ti1 110.14(14) . . ?
C37 C36 C41 116.8(2) . . ?
C37 C36 C35 120.9(2) . . ?
C41 C36 C35 122.2(2) . . ?
C38 C37 C36 121.6(2) . . ?
C39 C38 C37 120.3(2) . . ?
C38 C39 C40 119.3(2) . . ?
C39 C40 C41 120.5(2) . . ?
C40 C41 C36 121.4(2) . . ?
C45 O2 C42 107.59(18) . . ?
C45 O2 Ti1 125.23(14) . . ?
C42 O2 Ti1 126.53(14) . . ?
O2 C42 C43 105.9(2) . . ?
C42 C43 C44 102.6(2) . . ?
C45 C44 C43 102.3(2) . . ?
O2 C45 C44 104.6(2) . . ?
C52 B1 C64 101.8(2) . . ?
C52 B1 C58 113.43(19) . . ?
C64 B1 C58 115.3(2) . . ?
C52 B1 C46 112.6(2) . . ?
C64 B1 C46 112.01(19) . . ?
C58 B1 C46 102.12(19) . . ?
C47 C46 C51 112.5(2) . . ?
C47 C46 B1 124.0(2) . . ?
C51 C46 B1 123.3(2) . . ?
F1 C47 C48 114.5(2) . . ?
F1 C47 C46 120.8(2) . . ?
C48 C47 C46 124.7(2) . . ?
F2 C48 C49 119.6(2) . . ?
F2 C48 C47 120.8(2) . . ?
C49 C48 C47 119.7(2) . . ?
F3 C49 C50 121.3(2) . . ?
F3 C49 C48 120.1(3) . . ?
C50 C49 C48 118.5(2) . . ?
F4 C50 C49 119.9(2) . . ?
F4 C50 C51 120.0(2) . . ?
C49 C50 C51 120.1(2) . . ?
F5 C51 C50 114.8(2) . . ?
F5 C51 C46 120.7(2) . . ?
C50 C51 C46 124.5(2) . . ?
C57 C52 C53 112.8(2) . . ?
C57 C52 B1 123.9(2) . . ?
C53 C52 B1 121.9(2) . . ?
F6 C53 C54 115.5(2) . . ?
F6 C53 C52 120.1(2) . . ?
C54 C53 C52 124.4(2) . . ?
F7 C54 C55 120.1(2) . . ?
F7 C54 C53 120.4(2) . . ?
C55 C54 C53 119.5(2) . . ?
F8 C55 C54 120.6(2) . . ?
F8 C55 C56 120.1(2) . . ?
C54 C55 C56 119.3(2) . . ?
F9 C56 C55 119.9(2) . . ?
F9 C56 C57 120.7(2) . . ?
C55 C56 C57 119.4(2) . . ?
F10 C57 C56 115.4(2) . . ?
F10 C57 C52 120.0(2) . . ?
C56 C57 C52 124.6(2) . . ?
C63 C58 C59 112.0(2) . . ?
C63 C58 B1 124.8(2) . . ?
C59 C58 B1 122.9(2) . . ?
F11 C59 C60 114.9(2) . . ?
F11 C59 C58 119.8(2) . . ?
C60 C59 C58 125.3(2) . . ?
F12 C60 C61 119.5(2) . . ?
F12 C60 C59 121.0(2) . . ?
C61 C60 C59 119.5(2) . . ?
F13 C61 C62 121.1(3) . . ?
F13 C61 C60 120.6(3) . . ?
C62 C61 C60 118.4(2) . . ?
F14 C62 C61 119.6(2) . . ?
F14 C62 C63 120.1(2) . . ?
C61 C62 C63 120.2(2) . . ?
F15 C63 C62 114.2(2) . . ?
F15 C63 C58 121.2(2) . . ?
C62 C63 C58 124.5(2) . . ?
C65 C64 B1 115.91(19) . . ?
C66 C65 C70 116.7(2) . . ?
C66 C65 C64 121.2(2) . . ?
C70 C65 C64 122.1(2) . . ?
C65 C66 C67 121.7(3) . . ?
C68 C67 C66 120.3(3) . . ?
C67 C68 C69 119.0(3) . . ?
C68 C69 C70 120.6(3) . . ?
C69 C70 C65 121.7(3) . . ?
C73 C71 C72 114.6(3) . . ?
C71 C73 C73 114.0(3) . 2_565 ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.056