# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Aaron Sadow'
'Arkady Ellern'
'Kuntal Manna'

_publ_contact_author_name        'Aaron Sadow'
_publ_contact_author_email       SADOW@IASTATE.EDU

_publ_section_title              
;
A zwitterionic zirconium complex
that catalyzes hydroamination of aminoalkenes at room temperature
;

# Attachment 'PhBCpOx2ZrNMe2THF.cif'

data_sad63
_database_code_depnum_ccdc_archive 'CCDC 748394'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            {PhB(Cp)(OxMe2)2}Zr(NMe2)2THF
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H45 B N4 O3 Zr'
_chemical_properties_physical    'air-sensitive, , moisture-sensitive'
_exptl_crystal_recrystallization_method 'THF and pentane'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless

_diffrn_ambient_temperature      123(2)
_chemical_formula_weight         599.72

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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'

_cell_length_a                   12.7494(5)
_cell_length_b                   17.2023(7)
_cell_length_c                   13.5397(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.9520(10)
_cell_angle_gamma                90.00
_cell_volume                     2962.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.51
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31553
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         27.53
_reflns_number_total             6824
_reflns_number_gt                5833
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0343P)^2^+1.6045P] 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         6824
_refine_ls_number_parameters     351
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0681
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 0.626126(11) 0.148484(9) 0.774351(11) 0.01298(5) Uani 1 1 d . . .
B1 B 0.42776(14) 0.27556(11) 0.84554(13) 0.0161(3) Uani 1 1 d . . .
C2 C 0.32394(18) 0.53334(14) 0.72424(17) 0.0421(6) Uani 1 1 d . . .
H2A H 0.2731 0.5211 0.6688 0.063 Uiso 1 1 calc R . .
H2B H 0.3493 0.5867 0.7174 0.063 Uiso 1 1 calc R . .
H2C H 0.2900 0.5282 0.7867 0.063 Uiso 1 1 calc R . .
C3 C 0.46643(17) 0.48256(13) 0.62578(15) 0.0339(5) Uani 1 1 d . . .
H3A H 0.5265 0.4470 0.6267 0.051 Uiso 1 1 calc R . .
H3B H 0.4906 0.5358 0.6155 0.051 Uiso 1 1 calc R . .
H3C H 0.4149 0.4680 0.5719 0.051 Uiso 1 1 calc R . .
C4 C 0.49592(18) 0.48839(11) 0.81228(15) 0.0325(4) Uani 1 1 d . . .
H4A H 0.5630 0.5093 0.7906 0.039 Uiso 1 1 calc R . .
H4B H 0.4687 0.5244 0.8615 0.039 Uiso 1 1 calc R . .
C5 C 0.43483(12) 0.36468(10) 0.80698(12) 0.0172(3) Uani 1 1 d . . .
C6 C 0.66260(13) 0.20927(10) 1.01867(12) 0.0188(3) Uani 1 1 d . . .
C7 C 0.62946(15) 0.13563(10) 1.07103(13) 0.0234(4) Uani 1 1 d . . .
H7A H 0.5558 0.1403 1.0868 0.035 Uiso 1 1 calc R . .
H7B H 0.6740 0.1286 1.1323 0.035 Uiso 1 1 calc R . .
H7C H 0.6373 0.0907 1.0276 0.035 Uiso 1 1 calc R . .
C8 C 0.78086(14) 0.21157(12) 1.01037(14) 0.0261(4) Uani 1 1 d . . .
H8A H 0.8027 0.1657 0.9742 0.039 Uiso 1 1 calc R . .
H8B H 0.8166 0.2119 1.0768 0.039 Uiso 1 1 calc R . .
H8C H 0.7995 0.2587 0.9748 0.039 Uiso 1 1 calc R . .
C9 C 0.62283(14) 0.28159(10) 1.06984(13) 0.0224(4) Uani 1 1 d . . .
H9A H 0.6158 0.2717 1.1411 0.027 Uiso 1 1 calc R . .
H9B H 0.6711 0.3260 1.0628 0.027 Uiso 1 1 calc R . .
C10 C 0.52119(13) 0.26047(9) 0.92991(12) 0.0168(3) Uani 1 1 d . . .
C11 C 0.44956(12) 0.21454(10) 0.75815(12) 0.0169(3) Uani 1 1 d . . .
C12 C 0.49827(13) 0.22637(10) 0.66778(12) 0.0192(3) Uani 1 1 d . . .
H12 H 0.5133 0.2783 0.6387 0.023 Uiso 1 1 calc R . .
C13 C 0.50566(14) 0.15472(11) 0.61822(13) 0.0240(4) Uani 1 1 d . . .
H13 H 0.5274 0.1476 0.5492 0.029 Uiso 1 1 calc R . .
C14 C 0.46081(13) 0.09700(11) 0.67640(14) 0.0250(4) Uani 1 1 d . . .
H14 H 0.4471 0.0417 0.6566 0.030 Uiso 1 1 calc R . .
C15 C 0.42687(13) 0.13381(10) 0.76152(13) 0.0208(4) Uani 1 1 d . . .
H15 H 0.3851 0.1082 0.8123 0.025 Uiso 1 1 calc R . .
C16 C 0.57135(16) -0.01900(11) 0.86892(15) 0.0278(4) Uani 1 1 d . . .
H16A H 0.5888 -0.0663 0.8332 0.042 Uiso 1 1 calc R . .
H16B H 0.4987 -0.0039 0.8499 0.042 Uiso 1 1 calc R . .
H16C H 0.5790 -0.0288 0.9404 0.042 Uiso 1 1 calc R . .
C17 C 0.75028(15) 0.02222(11) 0.87384(14) 0.0270(4) Uani 1 1 d . . .
H17A H 0.7581 0.0154 0.9458 0.041 Uiso 1 1 calc R . .
H17B H 0.7975 0.0635 0.8543 0.041 Uiso 1 1 calc R . .
H17C H 0.7681 -0.0265 0.8413 0.041 Uiso 1 1 calc R . .
C18 C 0.69280(17) -0.00494(10) 0.63143(15) 0.0299(4) Uani 1 1 d . . .
H18A H 0.6160 -0.0142 0.6272 0.036 Uiso 1 1 calc R . .
H18B H 0.7259 -0.0381 0.6847 0.036 Uiso 1 1 calc R . .
C19 C 0.73739(16) -0.02344(11) 0.53419(14) 0.0286(4) Uani 1 1 d . . .
H19A H 0.6959 -0.0642 0.4978 0.034 Uiso 1 1 calc R . .
H19B H 0.8116 -0.0404 0.5437 0.034 Uiso 1 1 calc R . .
C20 C 0.72784(19) 0.05435(12) 0.48084(15) 0.0358(5) Uani 1 1 d . . .
H20A H 0.7776 0.0579 0.4280 0.043 Uiso 1 1 calc R . .
H20B H 0.6554 0.0629 0.4516 0.043 Uiso 1 1 calc R . .
C21 C 0.75555(15) 0.11168(10) 0.56272(13) 0.0228(4) Uani 1 1 d . . .
H21A H 0.8326 0.1193 0.5715 0.027 Uiso 1 1 calc R . .
H21B H 0.7217 0.1626 0.5481 0.027 Uiso 1 1 calc R . .
C22 C 0.86555(14) 0.19910(12) 0.75198(15) 0.0284(4) Uani 1 1 d . . .
H22A H 0.8907 0.2254 0.6939 0.043 Uiso 1 1 calc R . .
H22B H 0.8725 0.1427 0.7442 0.043 Uiso 1 1 calc R . .
H22C H 0.9074 0.2160 0.8115 0.043 Uiso 1 1 calc R . .
C23 C 0.74532(16) 0.30275(10) 0.76941(14) 0.0264(4) Uani 1 1 d . . .
H23A H 0.7891 0.3212 0.8270 0.040 Uiso 1 1 calc R . .
H23B H 0.6717 0.3162 0.7774 0.040 Uiso 1 1 calc R . .
H23C H 0.7683 0.3274 0.7093 0.040 Uiso 1 1 calc R . .
C24 C 0.41572(14) 0.47766(10) 0.72384(14) 0.0234(4) Uani 1 1 d . . .
C25 C 0.31353(13) 0.25534(9) 0.88590(12) 0.0173(3) Uani 1 1 d . . .
C26 C 0.30032(14) 0.20098(10) 0.96124(13) 0.0216(3) Uani 1 1 d . . .
H26 H 0.3609 0.1786 0.9948 0.026 Uiso 1 1 calc R . .
C27 C 0.20117(15) 0.17876(11) 0.98838(13) 0.0250(4) Uani 1 1 d . . .
H27 H 0.1952 0.1414 1.0394 0.030 Uiso 1 1 calc R . .
C28 C 0.11168(14) 0.21067(11) 0.94165(13) 0.0251(4) Uani 1 1 d . . .
H28 H 0.0440 0.1958 0.9602 0.030 Uiso 1 1 calc R . .
C29 C 0.12234(14) 0.26488(11) 0.86705(13) 0.0248(4) Uani 1 1 d . . .
H29 H 0.0615 0.2876 0.8344 0.030 Uiso 1 1 calc R . .
C30 C 0.22149(13) 0.28615(10) 0.83991(12) 0.0209(3) Uani 1 1 d . . .
H30 H 0.2268 0.3230 0.7882 0.025 Uiso 1 1 calc R . .
N1 N 0.37938(12) 0.39661(9) 0.73703(12) 0.0281(4) Uani 1 1 d . . .
N2 N 0.59990(10) 0.21383(8) 0.92055(10) 0.0153(3) Uani 1 1 d . . .
N3 N 0.64202(11) 0.04333(8) 0.84419(11) 0.0201(3) Uani 1 1 d . . .
N4 N 0.75547(11) 0.21877(8) 0.76130(11) 0.0186(3) Uani 1 1 d . . .
O1 O 0.51063(12) 0.41149(8) 0.85348(11) 0.0373(4) Uani 1 1 d . . .
O2 O 0.52110(10) 0.29666(7) 1.01875(9) 0.0220(3) Uani 1 1 d . . .
O3 O 0.71533(9) 0.07663(7) 0.65190(9) 0.0190(2) 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 0.01191(8) 0.01358(8) 0.01350(8) 0.00066(6) 0.00113(5) -0.00035(6)
B1 0.0151(8) 0.0191(9) 0.0142(8) 0.0000(7) 0.0013(7) 0.0017(7)
C2 0.0424(13) 0.0446(13) 0.0414(12) 0.0191(10) 0.0172(10) 0.0164(10)
C3 0.0323(11) 0.0407(12) 0.0293(10) 0.0062(9) 0.0076(8) -0.0005(9)
C4 0.0447(12) 0.0210(9) 0.0309(10) 0.0049(8) -0.0047(9) -0.0075(8)
C5 0.0130(7) 0.0227(8) 0.0164(8) -0.0016(6) 0.0037(6) 0.0016(6)
C6 0.0200(8) 0.0222(8) 0.0134(7) 0.0021(6) -0.0030(6) -0.0029(7)
C7 0.0300(9) 0.0230(9) 0.0166(8) 0.0031(7) -0.0012(7) -0.0041(7)
C8 0.0204(9) 0.0356(10) 0.0214(9) 0.0025(8) -0.0053(7) -0.0038(8)
C9 0.0274(9) 0.0232(9) 0.0159(8) -0.0008(7) -0.0029(7) -0.0037(7)
C10 0.0205(8) 0.0171(8) 0.0131(7) 0.0000(6) 0.0028(6) -0.0027(6)
C11 0.0113(7) 0.0240(8) 0.0151(8) -0.0004(6) -0.0012(6) 0.0032(6)
C12 0.0174(8) 0.0269(9) 0.0130(7) 0.0013(6) -0.0013(6) 0.0077(7)
C13 0.0195(8) 0.0379(10) 0.0140(8) -0.0053(7) -0.0039(6) 0.0080(7)
C14 0.0168(8) 0.0297(10) 0.0277(9) -0.0120(8) -0.0043(7) -0.0007(7)
C15 0.0119(7) 0.0264(9) 0.0241(9) -0.0054(7) 0.0013(6) -0.0021(6)
C16 0.0335(10) 0.0204(9) 0.0307(10) 0.0049(7) 0.0116(8) -0.0015(8)
C17 0.0283(10) 0.0239(9) 0.0288(10) 0.0051(7) 0.0016(8) 0.0026(7)
C18 0.0439(12) 0.0154(8) 0.0317(10) -0.0042(7) 0.0132(9) -0.0031(8)
C19 0.0367(11) 0.0228(9) 0.0266(10) -0.0056(7) 0.0049(8) 0.0028(8)
C20 0.0554(14) 0.0277(10) 0.0254(10) -0.0030(8) 0.0109(9) 0.0012(10)
C21 0.0269(9) 0.0222(9) 0.0205(8) 0.0024(7) 0.0102(7) -0.0003(7)
C22 0.0184(9) 0.0325(10) 0.0345(10) -0.0005(8) 0.0030(8) -0.0064(7)
C23 0.0365(10) 0.0198(9) 0.0233(9) 0.0009(7) 0.0045(8) -0.0061(8)
C24 0.0238(9) 0.0215(9) 0.0254(9) 0.0059(7) 0.0042(7) -0.0001(7)
C25 0.0195(8) 0.0180(8) 0.0148(7) -0.0032(6) 0.0039(6) 0.0013(6)
C26 0.0235(9) 0.0219(8) 0.0196(8) -0.0015(7) 0.0031(7) 0.0011(7)
C27 0.0341(10) 0.0222(9) 0.0197(9) 0.0006(7) 0.0080(7) -0.0045(8)
C28 0.0233(9) 0.0305(10) 0.0226(9) -0.0067(7) 0.0085(7) -0.0084(7)
C29 0.0195(8) 0.0325(10) 0.0223(9) -0.0032(7) -0.0002(7) -0.0025(7)
C30 0.0211(8) 0.0263(9) 0.0152(8) -0.0005(7) 0.0009(6) -0.0015(7)
N1 0.0264(8) 0.0255(8) 0.0314(9) 0.0095(7) -0.0053(7) -0.0044(6)
N2 0.0150(6) 0.0176(7) 0.0131(6) 0.0018(5) -0.0014(5) -0.0023(5)
N3 0.0233(7) 0.0168(7) 0.0208(7) 0.0026(6) 0.0051(6) 0.0007(6)
N4 0.0179(7) 0.0176(7) 0.0206(7) -0.0001(5) 0.0032(6) -0.0035(5)
O1 0.0463(9) 0.0242(7) 0.0380(8) 0.0098(6) -0.0212(7) -0.0125(6)
O2 0.0273(6) 0.0250(6) 0.0134(6) -0.0036(5) -0.0005(5) 0.0027(5)
O3 0.0233(6) 0.0154(6) 0.0192(6) 0.0001(4) 0.0073(5) -0.0005(5)

_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 N3 2.0448(14) . ?
Zr1 N4 2.0622(14) . ?
Zr1 N2 2.3205(14) . ?
Zr1 O3 2.4145(11) . ?
Zr1 C12 2.4920(16) . ?
Zr1 C11 2.5177(16) . ?
Zr1 C13 2.5283(17) . ?
Zr1 C15 2.5469(16) . ?
Zr1 C14 2.5690(17) . ?
B1 C10 1.614(2) . ?
B1 C11 1.620(2) . ?
B1 C5 1.624(2) . ?
B1 C25 1.628(2) . ?
C2 C24 1.512(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C24 1.519(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 O1 1.443(2) . ?
C4 C24 1.531(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N1 1.267(2) . ?
C5 O1 1.377(2) . ?
C6 N2 1.505(2) . ?
C6 C8 1.520(2) . ?
C6 C7 1.525(2) . ?
C6 C9 1.527(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O2 1.451(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.298(2) . ?
C10 O2 1.3545(19) . ?
C11 C15 1.420(2) . ?
C11 C12 1.424(2) . ?
C12 C13 1.410(2) . ?
C12 H12 1.0000 . ?
C13 C14 1.413(3) . ?
C13 H13 1.0000 . ?
C14 C15 1.409(2) . ?
C14 H14 1.0000 . ?
C15 H15 1.0000 . ?
C16 N3 1.454(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N3 1.457(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O3 1.455(2) . ?
C18 C19 1.504(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.522(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.508(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 O3 1.473(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N4 1.458(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 N4 1.455(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N1 1.484(2) . ?
C25 C30 1.395(2) . ?
C25 C26 1.403(2) . ?
C26 C27 1.394(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.380(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(2) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

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
N3 Zr1 N4 120.26(6) . . ?
N3 Zr1 N2 92.84(5) . . ?
N4 Zr1 N2 87.26(5) . . ?
N3 Zr1 O3 80.11(5) . . ?
N4 Zr1 O3 79.87(5) . . ?
N2 Zr1 O3 159.40(4) . . ?
N3 Zr1 C12 141.58(6) . . ?
N4 Zr1 C12 97.48(6) . . ?
N2 Zr1 C12 96.11(5) . . ?
O3 Zr1 C12 101.42(5) . . ?
N3 Zr1 C11 119.94(6) . . ?
N4 Zr1 C11 116.32(6) . . ?
N2 Zr1 C11 71.04(5) . . ?
O3 Zr1 C11 129.19(5) . . ?
C12 Zr1 C11 33.03(5) . . ?
N3 Zr1 C13 117.35(6) . . ?
N4 Zr1 C13 110.29(6) . . ?
N2 Zr1 C13 125.29(5) . . ?
O3 Zr1 C13 74.65(5) . . ?
C12 Zr1 C13 32.61(6) . . ?
C11 Zr1 C13 54.55(5) . . ?
N3 Zr1 C15 90.60(6) . . ?
N4 Zr1 C15 148.43(6) . . ?
N2 Zr1 C15 84.52(5) . . ?
O3 Zr1 C15 114.66(5) . . ?
C12 Zr1 C15 53.43(6) . . ?
C11 Zr1 C15 32.56(5) . . ?
C13 Zr1 C15 53.24(6) . . ?
N3 Zr1 C14 89.16(6) . . ?
N4 Zr1 C14 142.21(6) . . ?
N2 Zr1 C14 116.49(5) . . ?
O3 Zr1 C14 82.97(5) . . ?
C12 Zr1 C14 53.55(6) . . ?
C11 Zr1 C14 54.12(6) . . ?
C13 Zr1 C14 32.17(6) . . ?
C15 Zr1 C14 31.97(6) . . ?
C10 B1 C11 104.92(13) . . ?
C10 B1 C5 108.96(13) . . ?
C11 B1 C5 111.15(13) . . ?
C10 B1 C25 111.21(13) . . ?
C11 B1 C25 108.01(13) . . ?
C5 B1 C25 112.36(13) . . ?
C24 C2 H2A 109.5 . . ?
C24 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C24 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C24 C3 H3A 109.5 . . ?
C24 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C24 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 C24 104.70(15) . . ?
O1 C4 H4A 110.8 . . ?
C24 C4 H4A 110.8 . . ?
O1 C4 H4B 110.8 . . ?
C24 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
N1 C5 O1 115.22(15) . . ?
N1 C5 B1 127.51(15) . . ?
O1 C5 B1 117.25(14) . . ?
N2 C6 C8 113.75(14) . . ?
N2 C6 C7 107.83(13) . . ?
C8 C6 C7 111.34(15) . . ?
N2 C6 C9 100.68(13) . . ?
C8 C6 C9 111.98(15) . . ?
C7 C6 C9 110.75(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C6 104.07(13) . . ?
O2 C9 H9A 110.9 . . ?
C6 C9 H9A 110.9 . . ?
O2 C9 H9B 110.9 . . ?
C6 C9 H9B 110.9 . . ?
H9A C9 H9B 109.0 . . ?
N2 C10 O2 114.77(14) . . ?
N2 C10 B1 124.63(14) . . ?
O2 C10 B1 120.60(14) . . ?
C15 C11 C12 105.61(15) . . ?
C15 C11 B1 124.38(15) . . ?
C12 C11 B1 129.92(15) . . ?
C15 C11 Zr1 74.85(9) . . ?
C12 C11 Zr1 72.49(9) . . ?
B1 C11 Zr1 115.23(10) . . ?
C13 C12 C11 109.36(16) . . ?
C13 C12 Zr1 75.11(10) . . ?
C11 C12 Zr1 74.48(9) . . ?
C13 C12 H12 124.9 . . ?
C11 C12 H12 124.9 . . ?
Zr1 C12 H12 124.9 . . ?
C12 C13 C14 107.83(15) . . ?
C12 C13 Zr1 72.28(9) . . ?
C14 C13 Zr1 75.51(10) . . ?
C12 C13 H13 125.7 . . ?
C14 C13 H13 125.7 . . ?
Zr1 C13 H13 125.7 . . ?
C15 C14 C13 107.41(16) . . ?
C15 C14 Zr1 73.15(9) . . ?
C13 C14 Zr1 72.33(10) . . ?
C15 C14 H14 126.1 . . ?
C13 C14 H14 126.1 . . ?
Zr1 C14 H14 126.1 . . ?
C14 C15 C11 109.79(16) . . ?
C14 C15 Zr1 74.88(10) . . ?
C11 C15 Zr1 72.59(9) . . ?
C14 C15 H15 124.9 . . ?
C11 C15 H15 124.9 . . ?
Zr1 C15 H15 124.9 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C18 C19 106.82(15) . . ?
O3 C18 H18A 110.4 . . ?
C19 C18 H18A 110.4 . . ?
O3 C18 H18B 110.4 . . ?
C19 C18 H18B 110.4 . . ?
H18A C18 H18B 108.6 . . ?
C18 C19 C20 101.93(15) . . ?
C18 C19 H19A 111.4 . . ?
C20 C19 H19A 111.4 . . ?
C18 C19 H19B 111.4 . . ?
C20 C19 H19B 111.4 . . ?
H19A C19 H19B 109.2 . . ?
C21 C20 C19 102.66(16) . . ?
C21 C20 H20A 111.2 . . ?
C19 C20 H20A 111.2 . . ?
C21 C20 H20B 111.2 . . ?
C19 C20 H20B 111.2 . . ?
H20A C20 H20B 109.1 . . ?
O3 C21 C20 104.94(14) . . ?
O3 C21 H21A 110.8 . . ?
C20 C21 H21A 110.8 . . ?
O3 C21 H21B 110.8 . . ?
C20 C21 H21B 110.8 . . ?
H21A C21 H21B 108.8 . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C24 C2 110.27(16) . . ?
N1 C24 C3 108.22(16) . . ?
C2 C24 C3 110.12(16) . . ?
N1 C24 C4 102.50(14) . . ?
C2 C24 C4 113.33(18) . . ?
C3 C24 C4 112.05(17) . . ?
C30 C25 C26 116.02(16) . . ?
C30 C25 B1 120.90(15) . . ?
C26 C25 B1 122.80(15) . . ?
C27 C26 C25 122.08(17) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C28 C27 C26 120.42(17) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 118.78(17) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C28 C29 C30 120.38(17) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 122.32(17) . . ?
C29 C30 H30 118.8 . . ?
C25 C30 H30 118.8 . . ?
C5 N1 C24 109.54(15) . . ?
C10 N2 C6 108.26(13) . . ?
C10 N2 Zr1 122.73(11) . . ?
C6 N2 Zr1 128.97(10) . . ?
C16 N3 C17 110.06(14) . . ?
C16 N3 Zr1 135.68(12) . . ?
C17 N3 Zr1 114.20(11) . . ?
C23 N4 C22 109.15(14) . . ?
C23 N4 Zr1 119.99(12) . . ?
C22 N4 Zr1 130.68(12) . . ?
C5 O1 C4 106.92(14) . . ?
C10 O2 C9 106.61(13) . . ?
C18 O3 C21 108.29(13) . . ?
C18 O3 Zr1 121.90(10) . . ?
C21 O3 Zr1 124.08(9) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.062