# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lby56-1
_database_code_depnum_ccdc_archive 'CCDC 1033751'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Cl2 N4 Zr'
_chemical_formula_weight         438.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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   'P2(1)/c  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4242(3)
_cell_length_b                   27.2768(9)
_cell_length_c                   9.1772(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.536(2)
_cell_angle_gamma                90.00
_cell_volume                     1974.78(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7844
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      26.49

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7885
_exptl_absorpt_correction_T_max  0.8854
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13841
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4076
_reflns_number_gt                3697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1000P)²+0.3010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4076
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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 0.30293(3) 0.583920(10) 0.60561(3) 0.02285(14) Uani 1 1 d . . .
Cl1 Cl 0.56341(10) 0.56051(3) 0.82395(10) 0.0439(2) Uani 1 1 d . . .
Cl2 Cl 0.23059(9) 0.49929(3) 0.48650(9) 0.0332(2) Uani 1 1 d . . .
H3N H 0.543(5) 0.5685(15) 0.485(5) 0.035(11) Uiso 1 1 d . . .
H4N H 0.063(5) 0.5439(15) 0.687(5) 0.040(11) Uiso 1 1 d . . .
N1 N 0.3167(3) 0.65761(9) 0.6712(3) 0.0264(5) Uani 1 1 d . . .
N2 N 0.0981(3) 0.61632(9) 0.4316(3) 0.0252(5) Uani 1 1 d . . .
N3 N 0.4869(4) 0.58984(11) 0.4644(4) 0.0337(6) Uani 1 1 d . . .
N4 N 0.1295(4) 0.55897(11) 0.7454(3) 0.0327(6) Uani 1 1 d . . .
C1 C 0.4285(5) 0.68082(13) 0.8153(4) 0.0451(9) Uani 1 1 d . . .
H1A H 0.5303 0.6601 0.8617 0.054 Uiso 1 1 calc R . .
H1B H 0.3685 0.6827 0.8905 0.054 Uiso 1 1 calc R . .
C2 C 0.4832(5) 0.73145(14) 0.7889(5) 0.0505(10) Uani 1 1 d . . .
H2A H 0.5609 0.7449 0.8885 0.061 Uiso 1 1 calc R . .
H2B H 0.5454 0.7298 0.7153 0.061 Uiso 1 1 calc R . .
C3 C 0.3325(4) 0.76463(12) 0.7243(4) 0.0376(7) Uani 1 1 d . . .
H3A H 0.2859 0.7725 0.8067 0.045 Uiso 1 1 calc R . .
H3B H 0.3678 0.7957 0.6888 0.045 Uiso 1 1 calc R . .
C4 C 0.1986(4) 0.74035(11) 0.5905(4) 0.0289(6) Uani 1 1 d . . .
C5 C 0.1984(3) 0.68983(10) 0.5702(3) 0.0224(6) Uani 1 1 d . . .
C6 C 0.0734(4) 0.76754(12) 0.4796(4) 0.0386(8) Uani 1 1 d . . .
H6 H 0.0702 0.8021 0.4919 0.046 Uiso 1 1 calc R . .
C7 C -0.0454(4) 0.74582(12) 0.3533(4) 0.0381(8) Uani 1 1 d . . .
H7 H -0.1286 0.7656 0.2802 0.046 Uiso 1 1 calc R . .
C8 C -0.0464(3) 0.69538(12) 0.3303(3) 0.0288(6) Uani 1 1 d . . .
C9 C 0.0778(3) 0.66733(11) 0.4402(3) 0.0235(6) Uani 1 1 d . . .
C10 C -0.1687(4) 0.67141(13) 0.1888(4) 0.0359(7) Uani 1 1 d . . .
H10A H -0.1919 0.6935 0.0980 0.043 Uiso 1 1 calc R . .
H10B H -0.2771 0.6650 0.2049 0.043 Uiso 1 1 calc R . .
C11 C -0.0945(5) 0.62348(14) 0.1578(4) 0.0477(9) Uani 1 1 d . . .
H11A H -0.1818 0.6054 0.0739 0.057 Uiso 1 1 calc R . .
H11B H 0.0015 0.6305 0.1224 0.057 Uiso 1 1 calc R . .
C12 C -0.0342(5) 0.59249(13) 0.3018(4) 0.0410(8) Uani 1 1 d . . .
H12A H -0.1317 0.5847 0.3342 0.049 Uiso 1 1 calc R . .
H12B H 0.0106 0.5612 0.2774 0.049 Uiso 1 1 calc R . .
C13 C 0.4099(6) 0.58441(15) 0.2936(5) 0.0494(10) Uani 1 1 d . . .
H13A H 0.3274 0.6108 0.2512 0.074 Uiso 1 1 calc R . .
H13B H 0.3525 0.5526 0.2686 0.074 Uiso 1 1 calc R . .
H13C H 0.4986 0.5863 0.2476 0.074 Uiso 1 1 calc R . .
C14 C 0.5936(5) 0.63413(15) 0.5044(5) 0.0494(9) Uani 1 1 d . . .
H14A H 0.6815 0.6321 0.4575 0.074 Uiso 1 1 calc R . .
H14B H 0.6471 0.6366 0.6178 0.074 Uiso 1 1 calc R . .
H14C H 0.5232 0.6632 0.4647 0.074 Uiso 1 1 calc R . .
C15 C 0.0434(6) 0.60017(17) 0.7906(6) 0.0602(12) Uani 1 1 d . . .
H15A H -0.0473 0.5875 0.8239 0.090 Uiso 1 1 calc R . .
H15B H -0.0050 0.6221 0.7015 0.090 Uiso 1 1 calc R . .
H15C H 0.1254 0.6183 0.8766 0.090 Uiso 1 1 calc R . .
C16 C 0.2027(5) 0.52491(17) 0.8770(4) 0.0535(11) Uani 1 1 d . . .
H16A H 0.2928 0.5416 0.9603 0.080 Uiso 1 1 calc R . .
H16B H 0.2499 0.4963 0.8418 0.080 Uiso 1 1 calc R . .
H16C H 0.1140 0.5142 0.9161 0.080 Uiso 1 1 calc R . .


_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 N1 2.090(2) . ?
Zr1 N2 2.092(2) . ?
Zr1 N3 2.349(3) . ?
Zr1 N4 2.358(3) . ?
Zr1 Cl1 2.4806(8) . ?
Zr1 Cl2 2.5353(8) . ?
N1 C5 1.406(4) . ?
N1 C1 1.471(4) . ?
N2 C9 1.408(4) . ?
N2 C12 1.467(4) . ?
N3 C14 1.473(5) . ?
N3 C13 1.479(5) . ?
N4 C15 1.474(5) . ?
N4 C16 1.476(5) . ?
C1 C2 1.502(5) . ?
C2 C3 1.502(5) . ?
C3 C4 1.499(4) . ?
C4 C5 1.390(4) . ?
C4 C6 1.395(5) . ?
C5 C9 1.408(4) . ?
C6 C7 1.372(5) . ?
C7 C8 1.391(5) . ?
C8 C9 1.399(4) . ?
C8 C10 1.495(4) . ?
C10 C11 1.518(5) . ?
C11 C12 1.499(5) . ?

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
N1 Zr1 N2 76.17(9) . . ?
N1 Zr1 N3 96.43(10) . . ?
N2 Zr1 N3 94.42(10) . . ?
N1 Zr1 N4 95.93(10) . . ?
N2 Zr1 N4 91.98(10) . . ?
N3 Zr1 N4 167.13(10) . . ?
N1 Zr1 Cl1 94.07(7) . . ?
N2 Zr1 Cl1 169.91(7) . . ?
N3 Zr1 Cl1 84.00(8) . . ?
N4 Zr1 Cl1 91.58(7) . . ?
N1 Zr1 Cl2 168.70(7) . . ?
N2 Zr1 Cl2 92.66(7) . . ?
N3 Zr1 Cl2 85.99(7) . . ?
N4 Zr1 Cl2 82.57(7) . . ?
Cl1 Zr1 Cl2 97.16(3) . . ?
C5 N1 C1 114.0(2) . . ?
C5 N1 Zr1 117.17(18) . . ?
C1 N1 Zr1 128.8(2) . . ?
C9 N2 C12 114.3(2) . . ?
C9 N2 Zr1 117.30(18) . . ?
C12 N2 Zr1 128.4(2) . . ?
C14 N3 C13 110.4(3) . . ?
C14 N3 Zr1 112.4(2) . . ?
C13 N3 Zr1 116.7(2) . . ?
C15 N4 C16 110.8(3) . . ?
C15 N4 Zr1 113.2(2) . . ?
C16 N4 Zr1 117.8(2) . . ?
N1 C1 C2 112.7(3) . . ?
C3 C2 C1 110.7(3) . . ?
C4 C3 C2 110.2(3) . . ?
C5 C4 C6 117.6(3) . . ?
C5 C4 C3 120.9(3) . . ?
C6 C4 C3 121.5(3) . . ?
C4 C5 N1 124.3(3) . . ?
C4 C5 C9 120.8(3) . . ?
N1 C5 C9 114.8(2) . . ?
C7 C6 C4 121.8(3) . . ?
C6 C7 C8 121.3(3) . . ?
C7 C8 C9 117.9(3) . . ?
C7 C8 C10 122.0(3) . . ?
C9 C8 C10 120.0(3) . . ?
C8 C9 N2 125.1(3) . . ?
C8 C9 C5 120.5(3) . . ?
N2 C9 C5 114.4(2) . . ?
C8 C10 C11 109.6(3) . . ?
C12 C11 C10 110.8(3) . . ?
N2 C12 C11 113.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.663
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.087
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lby57-3
_database_code_depnum_ccdc_archive 'CCDC 1033752'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H32 Cl2 N4 Zr'
_chemical_formula_weight         466.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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   'P2(1)   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.912(2)
_cell_length_b                   17.585(4)
_cell_length_c                   13.398(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.178(3)
_cell_angle_gamma                90.00
_cell_volume                     2191.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8373
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      26.26

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8638
_exptl_absorpt_correction_T_max  0.8953
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11133
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         26.26
_reflns_number_total             8465
_reflns_number_gt                8077
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0292P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_number_reflns         8465
_refine_ls_number_parameters     479
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.38633(2) 0.345577(13) 0.563598(17) 0.01900(6) Uani 1 1 d . . .
Cl1 Cl 0.61865(7) 0.34997(5) 0.53282(5) 0.03751(16) Uani 1 1 d . . .
Cl2 Cl 0.29935(8) 0.21168(4) 0.52250(6) 0.03408(16) Uani 1 1 d . . .
N1 N 0.3779(2) 0.46528(13) 0.57436(16) 0.0220(5) Uani 1 1 d . . .
N2 N 0.2243(2) 0.36780(11) 0.63011(16) 0.0187(5) Uani 1 1 d . . .
N3 N 0.2871(3) 0.36562(15) 0.37691(18) 0.0331(6) Uani 1 1 d . . .
N4 N 0.5322(3) 0.30166(15) 0.73370(19) 0.0296(5) Uani 1 1 d . . .
C1 C 0.6012(3) 0.5425(2) 0.6379(2) 0.0416(8) Uani 1 1 d . . .
H1A H 0.5708 0.5599 0.6964 0.062 Uiso 1 1 calc R . .
H1B H 0.6541 0.5833 0.6177 0.062 Uiso 1 1 calc R . .
H1C H 0.6634 0.4979 0.6609 0.062 Uiso 1 1 calc R . .
C2 C 0.4686(3) 0.52131(16) 0.5423(2) 0.0289(6) Uani 1 1 d . . .
H2 H 0.5028 0.4963 0.4883 0.035 Uiso 1 1 calc R . .
C3 C 0.3808(4) 0.59091(17) 0.4902(2) 0.0362(7) Uani 1 1 d . . .
H3A H 0.2996 0.5749 0.4266 0.043 Uiso 1 1 calc R . .
H3B H 0.4419 0.6262 0.4669 0.043 Uiso 1 1 calc R . .
C4 C 0.3225(4) 0.63201(17) 0.5671(3) 0.0387(7) Uani 1 1 d . . .
H4A H 0.4026 0.6562 0.6244 0.046 Uiso 1 1 calc R . .
H4B H 0.2547 0.6724 0.5289 0.046 Uiso 1 1 calc R . .
C5 C 0.2463(3) 0.57587(16) 0.6146(2) 0.0271(6) Uani 1 1 d . . .
C6 C 0.2745(3) 0.49757(15) 0.61141(19) 0.0206(6) Uani 1 1 d . . .
C7 C 0.1433(3) 0.59885(18) 0.6578(2) 0.0309(6) Uani 1 1 d . . .
H7 H 0.1221 0.6514 0.6597 0.037 Uiso 1 1 calc R . .
C8 C 0.0718(3) 0.54626(17) 0.6978(2) 0.0308(7) Uani 1 1 d . . .
H8 H 0.0052 0.5638 0.7294 0.037 Uiso 1 1 calc R . .
C9 C 0.0943(3) 0.46814(16) 0.6931(2) 0.0245(6) Uani 1 1 d . . .
C10 C 0.1939(3) 0.44330(15) 0.64650(19) 0.0194(5) Uani 1 1 d . . .
C11 C 0.0166(3) 0.41028(18) 0.7368(2) 0.0314(6) Uani 1 1 d . . .
H11A H -0.0822 0.4031 0.6859 0.038 Uiso 1 1 calc R . .
H11B H 0.0099 0.4291 0.8046 0.038 Uiso 1 1 calc R . .
C12 C 0.0961(3) 0.33456(17) 0.7555(2) 0.0304(6) Uani 1 1 d . . .
H12A H 0.0361 0.2950 0.7722 0.036 Uiso 1 1 calc R . .
H12B H 0.1865 0.3391 0.8171 0.036 Uiso 1 1 calc R . .
C13 C 0.1306(3) 0.31096(16) 0.6567(2) 0.0232(6) Uani 1 1 d . . .
H13 H 0.1841 0.2617 0.6729 0.028 Uiso 1 1 calc R . .
C14 C -0.0065(3) 0.29820(17) 0.5604(2) 0.0314(6) Uani 1 1 d . . .
H14A H -0.0535 0.3472 0.5360 0.047 Uiso 1 1 calc R . .
H14B H -0.0720 0.2649 0.5807 0.047 Uiso 1 1 calc R . .
H14C H 0.0184 0.2744 0.5029 0.047 Uiso 1 1 calc R . .
C15 C 0.1348(4) 0.3890(3) 0.3433(3) 0.0600(11) Uani 1 1 d . . .
H15A H 0.1028 0.4061 0.2692 0.090 Uiso 1 1 calc R . .
H15B H 0.1245 0.4307 0.3887 0.090 Uiso 1 1 calc R . .
H15C H 0.0761 0.3457 0.3498 0.090 Uiso 1 1 calc R . .
C16 C 0.3080(4) 0.3070(2) 0.3034(3) 0.0515(9) Uani 1 1 d . . .
H16A H 0.2483 0.2625 0.3031 0.077 Uiso 1 1 calc R . .
H16B H 0.4093 0.2918 0.3273 0.077 Uiso 1 1 calc R . .
H16C H 0.2803 0.3281 0.2314 0.077 Uiso 1 1 calc R . .
C17 C 0.5977(4) 0.3667(2) 0.8022(2) 0.0550(10) Uani 1 1 d . . .
H17A H 0.6425 0.3492 0.8758 0.083 Uiso 1 1 calc R . .
H17B H 0.5234 0.4044 0.7987 0.083 Uiso 1 1 calc R . .
H17C H 0.6709 0.3898 0.7780 0.083 Uiso 1 1 calc R . .
C18 C 0.6378(4) 0.2403(2) 0.7436(3) 0.0496(9) Uani 1 1 d . . .
H18A H 0.7114 0.2580 0.7155 0.074 Uiso 1 1 calc R . .
H18B H 0.5888 0.1958 0.7031 0.074 Uiso 1 1 calc R . .
H18C H 0.6831 0.2265 0.8186 0.074 Uiso 1 1 calc R . .
Zr2 Zr 0.64345(2) 0.533137(13) 0.163520(17) 0.01984(6) Uani 1 1 d . . .
Cl3 Cl 0.45643(8) 0.50765(5) 0.24721(6) 0.03784(18) Uani 1 1 d . . .
Cl4 Cl 0.60906(9) 0.67462(4) 0.13690(6) 0.03742(18) Uani 1 1 d . . .
H3N H 0.341(4) 0.410(2) 0.366(3) 0.043(9) Uiso 1 1 d . . .
H4N H 0.474(3) 0.2829(15) 0.757(2) 0.011(7) Uiso 1 1 d . . .
H7N H 0.353(3) 0.5651(18) -0.003(2) 0.041(9) Uiso 1 1 d . . .
H8N H 0.740(3) 0.6034(19) 0.351(2) 0.028(8) Uiso 1 1 d . . .
N5 N 0.6887(2) 0.41775(12) 0.15043(16) 0.0209(5) Uani 1 1 d . . .
N6 N 0.8112(2) 0.53438(14) 0.10048(15) 0.0239(4) Uani 1 1 d . . .
N7 N 0.4393(2) 0.52751(15) 0.00374(16) 0.0294(5) Uani 1 1 d . . .
N8 N 0.7897(3) 0.56685(14) 0.33877(18) 0.0285(5) Uani 1 1 d . . .
C19 C 0.7176(4) 0.32413(18) 0.2949(2) 0.0441(8) Uani 1 1 d . . .
H19A H 0.8172 0.3185 0.2976 0.066 Uiso 1 1 calc R . .
H19B H 0.6825 0.2752 0.3111 0.066 Uiso 1 1 calc R . .
H19C H 0.7136 0.3620 0.3475 0.066 Uiso 1 1 calc R . .
C20 C 0.6237(3) 0.35009(17) 0.1840(2) 0.0320(6) Uani 1 1 d . . .
H20 H 0.5282 0.3655 0.1871 0.038 Uiso 1 1 calc R . .
C21 C 0.5989(4) 0.28474(17) 0.1026(3) 0.0447(8) Uani 1 1 d . . .
H21A H 0.5513 0.2416 0.1246 0.054 Uiso 1 1 calc R . .
H21B H 0.5351 0.3024 0.0319 0.054 Uiso 1 1 calc R . .
C22 C 0.7408(4) 0.25875(18) 0.0955(3) 0.0476(9) Uani 1 1 d . . .
H22A H 0.7228 0.2236 0.0346 0.057 Uiso 1 1 calc R . .
H22B H 0.7959 0.2309 0.1612 0.057 Uiso 1 1 calc R . .
C23 C 0.8278(3) 0.32598(17) 0.0815(2) 0.0332(7) Uani 1 1 d . . .
C24 C 0.7930(3) 0.39966(17) 0.10475(19) 0.0229(6) Uani 1 1 d . . .
C25 C 0.9403(4) 0.3176(2) 0.0419(2) 0.0426(9) Uani 1 1 d . . .
H25 H 0.9647 0.2682 0.0249 0.051 Uiso 1 1 calc R . .
C26 C 1.0158(4) 0.3789(2) 0.0270(3) 0.0441(9) Uani 1 1 d . . .
H26 H 1.0942 0.3708 0.0029 0.053 Uiso 1 1 calc R . .
C27 C 0.9810(3) 0.4529(2) 0.0464(2) 0.0348(7) Uani 1 1 d . . .
C28 C 0.8640(3) 0.46370(17) 0.0817(2) 0.0247(6) Uani 1 1 d . . .
C29 C 1.0702(3) 0.5201(2) 0.0371(3) 0.0488(9) Uani 1 1 d . . .
H29A H 1.0455 0.5340 -0.0387 0.059 Uiso 1 1 calc R . .
H29B H 1.1733 0.5063 0.0655 0.059 Uiso 1 1 calc R . .
C30 C 1.0431(3) 0.5880(2) 0.0988(3) 0.0463(9) Uani 1 1 d . . .
H30A H 1.0873 0.5784 0.1761 0.056 Uiso 1 1 calc R . .
H30B H 1.0881 0.6341 0.0815 0.056 Uiso 1 1 calc R . .
C31 C 0.8824(3) 0.60108(19) 0.0704(3) 0.0366(7) Uani 1 1 d . . .
H31 H 0.8696 0.6458 0.1123 0.044 Uiso 1 1 calc R . .
C32 C 0.8104(4) 0.6205(2) -0.0487(3) 0.0577(11) Uani 1 1 d . . .
H32A H 0.8050 0.5746 -0.0914 0.086 Uiso 1 1 calc R . .
H32B H 0.8672 0.6593 -0.0688 0.086 Uiso 1 1 calc R . .
H32C H 0.7132 0.6400 -0.0614 0.086 Uiso 1 1 calc R . .
C33 C 0.4563(4) 0.5619(2) -0.0926(2) 0.0527(10) Uani 1 1 d . . .
H33A H 0.5290 0.5335 -0.1117 0.079 Uiso 1 1 calc R . .
H33B H 0.4868 0.6150 -0.0781 0.079 Uiso 1 1 calc R . .
H33C H 0.3644 0.5598 -0.1517 0.079 Uiso 1 1 calc R . .
C34 C 0.3743(4) 0.45180(19) -0.0243(3) 0.0439(8) Uani 1 1 d . . .
H34A H 0.2823 0.4565 -0.0829 0.066 Uiso 1 1 calc R . .
H34B H 0.3583 0.4293 0.0376 0.066 Uiso 1 1 calc R . .
H34C H 0.4391 0.4191 -0.0464 0.066 Uiso 1 1 calc R . .
C35 C 0.9312(3) 0.5997(2) 0.3473(3) 0.0412(8) Uani 1 1 d . . .
H35A H 0.9773 0.6209 0.4187 0.062 Uiso 1 1 calc R . .
H35B H 0.9173 0.6401 0.2943 0.062 Uiso 1 1 calc R . .
H35C H 0.9924 0.5599 0.3346 0.062 Uiso 1 1 calc R . .
C36 C 0.8122(4) 0.5084(2) 0.4233(2) 0.0478(9) Uani 1 1 d . . .
H36A H 0.8722 0.4673 0.4122 0.072 Uiso 1 1 calc R . .
H36B H 0.7190 0.4878 0.4203 0.072 Uiso 1 1 calc R . .
H36C H 0.8600 0.5317 0.4931 0.072 Uiso 1 1 calc R . .


_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 N1 2.113(2) . ?
Zr1 N2 2.124(2) . ?
Zr1 N4 2.368(2) . ?
Zr1 N3 2.377(2) . ?
Zr1 Cl1 2.4767(9) . ?
Zr1 Cl2 2.5026(9) . ?
N1 C6 1.404(3) . ?
N1 C2 1.493(3) . ?
N2 C10 1.396(3) . ?
N2 C13 1.489(3) . ?
N3 C15 1.477(4) . ?
N3 C16 1.489(4) . ?
N4 C17 1.470(4) . ?
N4 C18 1.476(4) . ?
C1 C2 1.532(4) . ?
C2 C3 1.524(4) . ?
C3 C4 1.525(5) . ?
C4 C5 1.511(4) . ?
C5 C7 1.396(4) . ?
C5 C6 1.409(4) . ?
C6 C10 1.425(4) . ?
C7 C8 1.381(4) . ?
C8 C9 1.397(4) . ?
C9 C10 1.408(4) . ?
C9 C11 1.510(4) . ?
C11 C12 1.523(4) . ?
C12 C13 1.535(3) . ?
C13 C14 1.533(4) . ?
Zr2 N5 2.098(2) . ?
Zr2 N6 2.109(2) . ?
Zr2 N8 2.370(2) . ?
Zr2 N7 2.387(2) . ?
Zr2 Cl3 2.5156(9) . ?
Zr2 Cl4 2.5198(9) . ?
N5 C24 1.408(3) . ?
N5 C20 1.494(3) . ?
N6 C28 1.404(4) . ?
N6 C31 1.494(4) . ?
N7 C34 1.470(4) . ?
N7 C33 1.487(4) . ?
N8 C35 1.484(4) . ?
N8 C36 1.488(4) . ?
C19 C20 1.526(4) . ?
C20 C21 1.544(4) . ?
C21 C22 1.513(5) . ?
C22 C23 1.513(5) . ?
C23 C25 1.398(5) . ?
C23 C24 1.403(4) . ?
C24 C28 1.417(4) . ?
C25 C26 1.364(5) . ?
C26 C27 1.394(5) . ?
C27 C28 1.408(4) . ?
C27 C29 1.507(5) . ?
C29 C30 1.529(5) . ?
C30 C31 1.522(4) . ?
C31 C32 1.544(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
N1 Zr1 N2 74.63(8) . . ?
N1 Zr1 N4 106.53(9) . . ?
N2 Zr1 N4 87.44(8) . . ?
N1 Zr1 N3 84.97(8) . . ?
N2 Zr1 N3 108.41(8) . . ?
N4 Zr1 N3 162.68(8) . . ?
N1 Zr1 Cl1 92.35(6) . . ?
N2 Zr1 Cl1 160.89(6) . . ?
N4 Zr1 Cl1 82.89(7) . . ?
N3 Zr1 Cl1 83.76(6) . . ?
N1 Zr1 Cl2 158.97(6) . . ?
N2 Zr1 Cl2 90.71(6) . . ?
N4 Zr1 Cl2 87.40(7) . . ?
N3 Zr1 Cl2 85.52(7) . . ?
Cl1 Zr1 Cl2 105.21(3) . . ?
C6 N1 C2 114.8(2) . . ?
C6 N1 Zr1 118.54(17) . . ?
C2 N1 Zr1 126.57(17) . . ?
C10 N2 C13 114.5(2) . . ?
C10 N2 Zr1 118.45(16) . . ?
C13 N2 Zr1 126.95(16) . . ?
C15 N3 C16 110.6(3) . . ?
C15 N3 Zr1 111.7(2) . . ?
C16 N3 Zr1 119.5(2) . . ?
C17 N4 C18 111.5(3) . . ?
C17 N4 Zr1 109.80(18) . . ?
C18 N4 Zr1 120.20(19) . . ?
N1 C2 C3 110.9(2) . . ?
N1 C2 C1 110.3(2) . . ?
C3 C2 C1 112.1(3) . . ?
C2 C3 C4 111.2(2) . . ?
C5 C4 C3 109.6(2) . . ?
C7 C5 C6 118.5(3) . . ?
C7 C5 C4 121.9(3) . . ?
C6 C5 C4 119.5(3) . . ?
N1 C6 C5 125.7(3) . . ?
N1 C6 C10 114.0(2) . . ?
C5 C6 C10 120.3(3) . . ?
C8 C7 C5 120.9(3) . . ?
C7 C8 C9 122.0(3) . . ?
C8 C9 C10 118.2(3) . . ?
C8 C9 C11 122.3(3) . . ?
C10 C9 C11 119.5(2) . . ?
N2 C10 C9 126.0(2) . . ?
N2 C10 C6 114.2(2) . . ?
C9 C10 C6 119.9(2) . . ?
C9 C11 C12 110.4(2) . . ?
C11 C12 C13 110.5(2) . . ?
N2 C13 C14 110.0(2) . . ?
N2 C13 C12 111.6(2) . . ?
C14 C13 C12 111.7(2) . . ?
N5 Zr2 N6 75.87(9) . . ?
N5 Zr2 N8 104.44(8) . . ?
N6 Zr2 N8 95.55(9) . . ?
N5 Zr2 N7 91.40(8) . . ?
N6 Zr2 N7 100.54(8) . . ?
N8 Zr2 N7 159.77(9) . . ?
N5 Zr2 Cl3 94.39(6) . . ?
N6 Zr2 Cl3 169.86(7) . . ?
N8 Zr2 Cl3 84.04(7) . . ?
N7 Zr2 Cl3 82.25(6) . . ?
N5 Zr2 Cl4 164.86(6) . . ?
N6 Zr2 Cl4 91.14(7) . . ?
N8 Zr2 Cl4 84.25(6) . . ?
N7 Zr2 Cl4 83.26(7) . . ?
Cl3 Zr2 Cl4 98.89(3) . . ?
C24 N5 C20 114.1(2) . . ?
C24 N5 Zr2 117.71(17) . . ?
C20 N5 Zr2 128.18(18) . . ?
C28 N6 C31 114.0(2) . . ?
C28 N6 Zr2 117.15(18) . . ?
C31 N6 Zr2 128.9(2) . . ?
C34 N7 C33 108.5(2) . . ?
C34 N7 Zr2 115.32(18) . . ?
C33 N7 Zr2 116.53(19) . . ?
C35 N8 C36 108.7(2) . . ?
C35 N8 Zr2 114.36(19) . . ?
C36 N8 Zr2 117.46(19) . . ?
N5 C20 C19 110.5(2) . . ?
N5 C20 C21 111.1(2) . . ?
C19 C20 C21 111.1(3) . . ?
C22 C21 C20 110.1(3) . . ?
C21 C22 C23 110.7(3) . . ?
C25 C23 C24 118.1(3) . . ?
C25 C23 C22 121.9(3) . . ?
C24 C23 C22 120.0(3) . . ?
C23 C24 N5 125.4(3) . . ?
C23 C24 C28 120.5(3) . . ?
N5 C24 C28 114.2(2) . . ?
C26 C25 C23 121.5(3) . . ?
C25 C26 C27 121.8(3) . . ?
C26 C27 C28 118.3(3) . . ?
C26 C27 C29 121.8(3) . . ?
C28 C27 C29 119.8(3) . . ?
N6 C28 C27 125.5(3) . . ?
N6 C28 C24 114.9(2) . . ?
C27 C28 C24 119.6(3) . . ?
C27 C29 C30 110.5(3) . . ?
C31 C30 C29 110.3(3) . . ?
N6 C31 C30 111.4(3) . . ?
N6 C31 C32 111.0(2) . . ?
C30 C31 C32 111.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        26.26
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.053
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lby59-2
_database_code_depnum_ccdc_archive 'CCDC 1033753'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H28 Cl2 N2 O2 Zr'
_chemical_formula_weight         490.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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   'C2/c  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.9174(4)
_cell_length_b                   10.6760(3)
_cell_length_c                   14.1935(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.0420(10)
_cell_angle_gamma                90.00
_cell_volume                     2167.08(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9985
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      29.15

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_T_max  0.9269
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13771
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2017
_reflns_number_gt                1922
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0342P)²+5.3094P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2017
_refine_ls_number_parameters     123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.002
_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 0.0000 0.87681(3) 0.2500 0.02862(13) Uani 1 2 d S . .
Cl1 Cl -0.08781(6) 1.03060(7) 0.10937(6) 0.0501(2) Uani 1 1 d . . .
N1 N -0.04921(14) 0.72133(19) 0.15065(16) 0.0322(5) Uani 1 1 d . . .
C1 C -0.0943(2) 0.7225(3) 0.0342(2) 0.0507(7) Uani 1 1 d . . .
H1A H -0.0456 0.7144 0.0089 0.061 Uiso 1 1 calc R . .
H1B H -0.1264 0.8037 0.0090 0.061 Uiso 1 1 calc R . .
C2 C -0.1636(3) 0.6183(3) -0.0105(3) 0.0633(10) Uani 1 1 d . . .
H2A H -0.1938 0.6241 -0.0880 0.076 Uiso 1 1 calc R . .
H2B H -0.2128 0.6268 0.0139 0.076 Uiso 1 1 calc R . .
C3 C -0.1163(2) 0.4918(3) 0.0227(3) 0.0600(9) Uani 1 1 d . . .
H3A H -0.1645 0.4255 0.0042 0.072 Uiso 1 1 calc R . .
H3B H -0.0783 0.4746 -0.0154 0.072 Uiso 1 1 calc R . .
C4 C -0.05443(19) 0.4890(3) 0.1392(3) 0.0460(7) Uani 1 1 d . . .
C5 C -0.02692(17) 0.6017(2) 0.1947(2) 0.0331(6) Uani 1 1 d . . .
C6 C -0.0265(2) 0.3780(3) 0.1959(3) 0.0598(10) Uani 1 1 d . . .
H6 H -0.0440 0.3003 0.1598 0.072 Uiso 1 1 calc R . .
C7 C 0.1591(3) 1.0020(3) 0.1890(3) 0.0658(10) Uani 1 1 d . . .
H7A H 0.1743 1.0619 0.2474 0.079 Uiso 1 1 calc R . .
H7B H 0.1154 1.0428 0.1229 0.079 Uiso 1 1 calc R . .
C8 C 0.2455(2) 0.9618(3) 0.1820(3) 0.0606(9) Uani 1 1 d . . .
H8A H 0.2527 1.0078 0.1254 0.073 Uiso 1 1 calc R . .
H8B H 0.3012 0.9777 0.2491 0.073 Uiso 1 1 calc R . .
C9 C 0.2341(3) 0.8258(4) 0.1588(4) 0.0714(11) Uani 1 1 d . . .
H9 H 0.2666 0.7772 0.1294 0.086 Uiso 1 1 calc R . .
C10 C 0.1636(3) 0.7812(3) 0.1898(4) 0.0700(11) Uani 1 1 d . . .
H10A H 0.1176 0.7279 0.1338 0.084 Uiso 1 1 calc R . .
H10B H 0.1933 0.7307 0.2547 0.084 Uiso 1 1 calc R . .
O1 O 0.11793(14) 0.88870(16) 0.20731(16) 0.0412(5) Uani 1 1 d . . .


_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 N1 2.095(2) . ?
Zr1 N1 2.095(2) 2 ?
Zr1 O1 2.2147(19) 2 ?
Zr1 O1 2.2148(19) . ?
Zr1 Cl1 2.4867(7) 2 ?
Zr1 Cl1 2.4867(7) . ?
N1 C5 1.397(3) . ?
N1 C1 1.485(3) . ?
C1 C2 1.497(4) . ?
C2 C3 1.517(5) . ?
C3 C4 1.508(5) . ?
C4 C6 1.392(5) . ?
C4 C5 1.399(4) . ?
C5 C5 1.421(6) 2 ?
C6 C6 1.391(8) 2 ?
C7 O1 1.453(3) . ?
C7 C8 1.484(5) . ?
C8 C9 1.482(5) . ?
C9 C10 1.453(5) . ?
C10 O1 1.438(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
N1 Zr1 N1 75.17(11) . 2 ?
N1 Zr1 O1 96.79(8) . 2 ?
N1 Zr1 O1 88.43(8) 2 2 ?
N1 Zr1 O1 88.43(7) . . ?
N1 Zr1 O1 96.79(8) 2 . ?
O1 Zr1 O1 173.43(9) 2 . ?
N1 Zr1 Cl1 167.39(6) . 2 ?
N1 Zr1 Cl1 94.05(6) 2 2 ?
O1 Zr1 Cl1 89.30(5) 2 2 ?
O1 Zr1 Cl1 86.36(5) . 2 ?
N1 Zr1 Cl1 94.05(6) . . ?
N1 Zr1 Cl1 167.39(6) 2 . ?
O1 Zr1 Cl1 86.36(5) 2 . ?
O1 Zr1 Cl1 89.30(5) . . ?
Cl1 Zr1 Cl1 97.36(4) 2 . ?
C5 N1 C1 114.1(2) . . ?
C5 N1 Zr1 118.48(17) . . ?
C1 N1 Zr1 126.71(18) . . ?
N1 C1 C2 111.8(3) . . ?
C1 C2 C3 110.9(3) . . ?
C4 C3 C2 110.7(2) . . ?
C6 C4 C5 117.7(3) . . ?
C6 C4 C3 122.7(3) . . ?
C5 C4 C3 119.5(3) . . ?
N1 C5 C4 125.4(3) . . ?
N1 C5 C5 113.93(14) . 2 ?
C4 C5 C5 120.67(19) . 2 ?
C4 C6 C6 121.59(19) . 2 ?
O1 C7 C8 106.0(3) . . ?
C9 C8 C7 105.7(3) . . ?
C10 C9 C8 106.8(3) . . ?
O1 C10 C9 107.9(3) . . ?
C10 O1 C7 109.3(2) . . ?
C10 O1 Zr1 123.75(17) . . ?
C7 O1 Zr1 126.88(18) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lby58-1
_database_code_depnum_ccdc_archive 'CCDC 1033754'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H27 Al Cl2 N2 Zr'
_chemical_formula_weight         448.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.11890(10)
_cell_length_b                   13.5588(2)
_cell_length_c                   14.7171(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2019.19(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7388
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      29.88

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8479
_exptl_absorpt_correction_T_max  0.8972
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12848
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3545
_reflns_number_gt                3398
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0300P)²+0.4559P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_number_reflns         3545
_refine_ls_number_parameters     213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0537
_refine_ls_wR_factor_gt          0.0527
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002

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 0.74355(2) 0.123545(16) 0.192094(15) 0.02352(7) Uani 1 1 d . . .
Al1 Al 0.68432(7) 0.24222(6) 0.37112(5) 0.02537(16) Uani 1 1 d . . .
Cl1 Cl 0.67576(8) -0.03590(5) 0.24004(6) 0.0496(2) Uani 1 1 d . . .
Cl2 Cl 0.97358(6) 0.08529(5) 0.17420(5) 0.04159(18) Uani 1 1 d . . .
N1 N 0.57067(17) 0.18788(14) 0.27670(13) 0.0219(4) Uani 1 1 d . . .
N2 N 0.78789(17) 0.27267(14) 0.26253(13) 0.0227(4) Uani 1 1 d . . .
C1 C 0.3620(3) 0.1930(2) 0.3642(2) 0.0451(7) Uani 1 1 d . . .
H1A H 0.4128 0.1965 0.4208 0.068 Uiso 1 1 calc R . .
H1B H 0.2783 0.1587 0.3754 0.068 Uiso 1 1 calc R . .
H1C H 0.3440 0.2598 0.3422 0.068 Uiso 1 1 calc R . .
C2 C 0.4413(2) 0.13677(19) 0.29298(17) 0.0288(6) Uani 1 1 d . . .
H2 H 0.4610 0.0698 0.3181 0.035 Uiso 1 1 calc R . .
C3 C 0.3659(2) 0.1228(2) 0.2045(2) 0.0403(7) Uani 1 1 d . . .
H3A H 0.2794 0.0920 0.2179 0.048 Uiso 1 1 calc R . .
H3B H 0.4159 0.0770 0.1650 0.048 Uiso 1 1 calc R . .
C4 C 0.3428(2) 0.2194(2) 0.15310(19) 0.0368(7) Uani 1 1 d . . .
H4A H 0.3040 0.2051 0.0928 0.044 Uiso 1 1 calc R . .
H4B H 0.2796 0.2611 0.1873 0.044 Uiso 1 1 calc R . .
C5 C 0.4708(2) 0.27388(18) 0.14135(17) 0.0280(6) Uani 1 1 d . . .
C6 C 0.5721(2) 0.25719(17) 0.20447(16) 0.0210(5) Uani 1 1 d . . .
C7 C 0.4981(3) 0.3391(2) 0.07184(18) 0.0361(7) Uani 1 1 d . . .
H7 H 0.4316 0.3526 0.0280 0.043 Uiso 1 1 calc R . .
C8 C 0.6205(3) 0.3857(2) 0.06389(18) 0.0371(6) Uani 1 1 d . . .
H8 H 0.6344 0.4300 0.0148 0.045 Uiso 1 1 calc R . .
C9 C 0.7213(2) 0.37011(18) 0.12429(16) 0.0281(5) Uani 1 1 d . . .
C10 C 0.6954(2) 0.30460(16) 0.19644(16) 0.0212(5) Uani 1 1 d . . .
C11 C 0.8566(3) 0.4179(2) 0.1181(2) 0.0378(7) Uani 1 1 d . . .
H11A H 0.8516 0.4860 0.1421 0.045 Uiso 1 1 calc R . .
H11B H 0.8840 0.4216 0.0537 0.045 Uiso 1 1 calc R . .
C12 C 0.9591(2) 0.3600(2) 0.17179(18) 0.0344(6) Uani 1 1 d . . .
H12A H 0.9798 0.2979 0.1394 0.041 Uiso 1 1 calc R . .
H12B H 1.0414 0.3990 0.1764 0.041 Uiso 1 1 calc R . .
C13 C 0.9086(2) 0.33615(19) 0.26666(19) 0.0307(6) Uani 1 1 d . . .
H13 H 0.8817 0.4000 0.2952 0.037 Uiso 1 1 calc R . .
C14 C 1.0122(3) 0.2902(2) 0.3279(2) 0.0455(8) Uani 1 1 d . . .
H14A H 0.9750 0.2803 0.3887 0.068 Uiso 1 1 calc R . .
H14B H 1.0889 0.3341 0.3319 0.068 Uiso 1 1 calc R . .
H14C H 1.0396 0.2265 0.3028 0.068 Uiso 1 1 calc R . .
C15 C 0.6762(2) 0.1150(2) 0.04897(17) 0.0335(6) Uani 1 1 d . . .
H15A H 0.5851 0.0908 0.0471 0.050 Uiso 1 1 calc R . .
H15B H 0.7336 0.0698 0.0152 0.050 Uiso 1 1 calc R . .
H15C H 0.6803 0.1807 0.0214 0.050 Uiso 1 1 calc R . .
C16 C 0.6271(3) 0.3644(2) 0.42983(19) 0.0421(7) Uani 1 1 d . . .
H16A H 0.5604 0.3969 0.3919 0.063 Uiso 1 1 calc R . .
H16B H 0.7032 0.4084 0.4375 0.063 Uiso 1 1 calc R . .
H16C H 0.5890 0.3492 0.4894 0.063 Uiso 1 1 calc R . .
C17 C 0.7523(3) 0.1308(2) 0.44118(19) 0.0468(7) Uani 1 1 d . . .
H17A H 0.6785 0.0895 0.4613 0.070 Uiso 1 1 calc R . .
H17B H 0.8005 0.1554 0.4943 0.070 Uiso 1 1 calc R . .
H17C H 0.8120 0.0917 0.4031 0.070 Uiso 1 1 calc R . .


_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 C15 2.217(3) . ?
Zr1 N2 2.3161(19) . ?
Zr1 N1 2.3177(18) . ?
Zr1 Cl1 2.3753(7) . ?
Zr1 Cl2 2.3993(6) . ?
Zr1 C10 2.504(2) . ?
Zr1 C6 2.515(2) . ?
Zr1 Al1 3.1448(8) . ?
Al1 N1 1.948(2) . ?
Al1 C17 1.954(3) . ?
Al1 N2 1.955(2) . ?
Al1 C16 1.957(3) . ?
N1 C6 1.419(3) . ?
N1 C2 1.500(3) . ?
N2 C10 1.418(3) . ?
N2 C13 1.495(3) . ?
C1 C2 1.524(4) . ?
C2 C3 1.521(4) . ?
C3 C4 1.531(4) . ?
C4 C5 1.501(4) . ?
C5 C7 1.380(4) . ?
C5 C6 1.401(3) . ?
C6 C10 1.408(3) . ?
C7 C8 1.396(4) . ?
C8 C9 1.370(3) . ?
C9 C10 1.409(3) . ?
C9 C11 1.517(3) . ?
C11 C12 1.522(4) . ?
C12 C13 1.522(4) . ?
C13 C14 1.517(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
C15 Zr1 N2 122.03(9) . . ?
C15 Zr1 N1 107.35(8) . . ?
N2 Zr1 N1 64.99(6) . . ?
C15 Zr1 Cl1 98.40(8) . . ?
N2 Zr1 Cl1 135.85(5) . . ?
N1 Zr1 Cl1 87.99(5) . . ?
C15 Zr1 Cl2 100.52(7) . . ?
N2 Zr1 Cl2 92.86(5) . . ?
N1 Zr1 Cl2 150.76(5) . . ?
Cl1 Zr1 Cl2 96.66(3) . . ?
C15 Zr1 C10 90.89(9) . . ?
N2 Zr1 C10 33.93(7) . . ?
N1 Zr1 C10 58.01(7) . . ?
Cl1 Zr1 C10 145.95(6) . . ?
Cl2 Zr1 C10 113.81(5) . . ?
C15 Zr1 C6 83.94(8) . . ?
N2 Zr1 C6 58.15(7) . . ?
N1 Zr1 C6 33.83(7) . . ?
Cl1 Zr1 C6 115.78(5) . . ?
Cl2 Zr1 C6 146.40(5) . . ?
C10 Zr1 C6 32.59(7) . . ?
C15 Zr1 Al1 139.84(7) . . ?
N2 Zr1 Al1 38.31(5) . . ?
N1 Zr1 Al1 38.14(5) . . ?
Cl1 Zr1 Al1 99.31(3) . . ?
Cl2 Zr1 Al1 112.80(2) . . ?
C10 Zr1 Al1 55.93(6) . . ?
C6 Zr1 Al1 55.90(5) . . ?
N1 Al1 C17 106.97(11) . . ?
N1 Al1 N2 79.24(8) . . ?
C17 Al1 N2 113.94(11) . . ?
N1 Al1 C16 117.42(11) . . ?
C17 Al1 C16 121.73(13) . . ?
N2 Al1 C16 109.92(11) . . ?
N1 Al1 Zr1 47.27(6) . . ?
C17 Al1 Zr1 88.83(9) . . ?
N2 Al1 Zr1 47.24(6) . . ?
C16 Al1 Zr1 149.29(9) . . ?
C6 N1 C2 115.74(18) . . ?
C6 N1 Al1 106.14(14) . . ?
C2 N1 Al1 125.15(16) . . ?
C6 N1 Zr1 80.74(12) . . ?
C2 N1 Zr1 124.78(14) . . ?
Al1 N1 Zr1 94.59(7) . . ?
C10 N2 C13 113.04(18) . . ?
C10 N2 Al1 105.74(13) . . ?
C13 N2 Al1 121.74(16) . . ?
C10 N2 Zr1 80.30(12) . . ?
C13 N2 Zr1 132.77(15) . . ?
Al1 N2 Zr1 94.45(8) . . ?
N1 C2 C3 111.0(2) . . ?
N1 C2 C1 109.8(2) . . ?
C3 C2 C1 112.8(2) . . ?
C2 C3 C4 113.1(2) . . ?
C5 C4 C3 110.2(2) . . ?
C7 C5 C6 116.6(2) . . ?
C7 C5 C4 125.0(2) . . ?
C6 C5 C4 118.4(2) . . ?
C5 C6 C10 121.2(2) . . ?
C5 C6 N1 126.6(2) . . ?
C10 C6 N1 111.97(19) . . ?
C5 C6 Zr1 124.94(16) . . ?
C10 C6 Zr1 73.25(12) . . ?
N1 C6 Zr1 65.42(11) . . ?
C5 C7 C8 122.0(2) . . ?
C9 C8 C7 122.4(2) . . ?
C8 C9 C10 116.6(2) . . ?
C8 C9 C11 124.5(2) . . ?
C10 C9 C11 118.8(2) . . ?
C6 C10 C9 121.1(2) . . ?
C6 C10 N2 112.8(2) . . ?
C9 C10 N2 125.9(2) . . ?
C6 C10 Zr1 74.16(13) . . ?
C9 C10 Zr1 124.23(16) . . ?
N2 C10 Zr1 65.77(11) . . ?
C9 C11 C12 111.3(2) . . ?
C13 C12 C11 110.9(2) . . ?
N2 C13 C14 110.6(2) . . ?
N2 C13 C12 111.1(2) . . ?
C14 C13 C12 113.6(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.061
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lby34-3
_database_code_depnum_ccdc_archive 'CCDC 1033755'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Hf N2'
_chemical_formula_weight         791.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.362(2)
_cell_length_b                   13.598(3)
_cell_length_c                   28.407(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4002.4(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7447
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      21.56

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    2.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7426
_exptl_absorpt_correction_T_max  0.7785
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40930
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7053
_reflns_number_gt                5806
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0750P)²+0.5001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(16)
_refine_ls_number_reflns         7053
_refine_ls_number_parameters     431
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1241
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.044
_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
Hf1 Hf 0.50662(3) 0.06003(2) 0.152385(10) 0.04861(12) Uani 1 1 d . A 1
N1 N 0.4930(7) 0.1249(3) 0.23063(18) 0.0411(12) Uani 1 1 d . A 1
N2 N 0.3568(6) 0.1618(4) 0.1532(2) 0.0486(15) Uani 1 1 d . A 1
C1 C 0.5674(8) 0.1106(5) 0.2676(3) 0.0463(18) Uani 1 1 d . A 1
C2 C 0.5257(10) 0.1359(6) 0.3134(3) 0.062(2) Uani 1 1 d . A 1
H2 H 0.5808 0.1278 0.3390 0.075 Uiso 1 1 calc R A 1
C3 C 0.4049(9) 0.1721(6) 0.3200(3) 0.061(2) Uani 1 1 d . A 1
H3 H 0.3765 0.1862 0.3503 0.073 Uiso 1 1 calc R A 1
C4 C 0.3237(8) 0.1881(6) 0.2821(3) 0.053(2) Uani 1 1 d . A 1
C5 C 0.3715(7) 0.1653(5) 0.2375(3) 0.0430(18) Uani 1 1 d . A 1
C6 C 0.1990(10) 0.2279(7) 0.2864(4) 0.069(3) Uani 1 1 d . A 1
H6 H 0.1657 0.2441 0.3158 0.083 Uiso 1 1 calc R A 1
C7 C 0.1292(9) 0.2420(6) 0.2473(4) 0.066(3) Uani 1 1 d . A 1
H7 H 0.0463 0.2674 0.2504 0.079 Uiso 1 1 calc R A 1
C8 C 0.1745(8) 0.2204(6) 0.2017(3) 0.056(2) Uani 1 1 d . A 1
C9 C 0.2965(7) 0.1831(5) 0.1957(3) 0.0453(19) Uani 1 1 d . A 1
C10 C 0.0905(8) 0.2328(8) 0.1592(4) 0.074(3) Uani 1 1 d . A 1
H10A H 0.0818 0.3022 0.1522 0.089 Uiso 1 1 calc R A 1
H10B H 0.0051 0.2071 0.1660 0.089 Uiso 1 1 calc R A 1
C11 C 0.1448(9) 0.1803(8) 0.1167(4) 0.078(3) Uani 1 1 d . A 1
H11A H 0.0994 0.2013 0.0886 0.094 Uiso 1 1 calc R A 1
H11B H 0.1330 0.1098 0.1201 0.094 Uiso 1 1 calc R A 1
C12 C 0.2909(9) 0.2043(6) 0.1119(3) 0.063(2) Uani 1 1 d . A 1
H12 H 0.3231 0.1703 0.0839 0.075 Uiso 1 1 calc R A 1
C13 C 0.7054(8) 0.0719(6) 0.2596(3) 0.054(2) Uani 1 1 d . A 1
H13 H 0.7120 0.0482 0.2271 0.065 Uiso 1 1 calc R A 1
C14 C 0.7389(11) -0.0118(7) 0.2923(4) 0.079(3) Uani 1 1 d . A 1
H14A H 0.8257 -0.0330 0.2863 0.118 Uiso 1 1 calc R A 1
H14B H 0.6805 -0.0655 0.2870 0.118 Uiso 1 1 calc R A 1
H14C H 0.7318 0.0100 0.3243 0.118 Uiso 1 1 calc R A 1
C15 C 0.7997(10) 0.1543(7) 0.2661(4) 0.083(3) Uani 1 1 d . A 1
H15A H 0.7869 0.2025 0.2418 0.124 Uiso 1 1 calc R A 1
H15B H 0.8861 0.1290 0.2642 0.124 Uiso 1 1 calc R A 1
H15C H 0.7866 0.1841 0.2963 0.124 Uiso 1 1 calc R A 1
C16 C 0.3195(10) 0.3159(7) 0.1058(3) 0.067(3) Uani 1 1 d . A 1
H16 H 0.2838 0.3498 0.1333 0.081 Uiso 1 1 calc R A 1
C17 C 0.4633(10) 0.3364(7) 0.1050(4) 0.090(3) Uani 1 1 d . A 1
H17A H 0.5037 0.3041 0.1311 0.134 Uiso 1 1 calc R A 1
H17B H 0.4777 0.4060 0.1071 0.134 Uiso 1 1 calc R A 1
H17C H 0.4995 0.3121 0.0761 0.134 Uiso 1 1 calc R A 1
C18 C 0.2528(14) 0.3591(10) 0.0618(5) 0.117(5) Uani 1 1 d . A 1
H18A H 0.2570 0.4295 0.0629 0.176 Uiso 1 1 calc R A 1
H18B H 0.1641 0.3386 0.0612 0.176 Uiso 1 1 calc R A 1
H18C H 0.2957 0.3359 0.0340 0.176 Uiso 1 1 calc R A 1
C19 C 0.4489(11) -0.0069(8) 0.0820(3) 0.077(3) Uani 1 1 d . A 1
H19A H 0.3562 0.0015 0.0793 0.093 Uiso 1 1 calc R A 1
H19B H 0.4876 0.0339 0.0579 0.093 Uiso 1 1 calc R A 1
C20 C 0.4767(13) -0.1101(7) 0.0690(3) 0.076(3) Uani 1 1 d . A 1
C21 C 0.5980(13) -0.1403(10) 0.0570(4) 0.093(4) Uani 1 1 d . A 1
H21 H 0.6643 -0.0942 0.0561 0.111 Uiso 1 1 calc R A 1
C22 C 0.6251(16) -0.2361(13) 0.0463(5) 0.114(5) Uani 1 1 d . A 1
H22 H 0.7085 -0.2539 0.0377 0.137 Uiso 1 1 calc R A 1
C23 C 0.530(2) -0.3061(10) 0.0483(5) 0.128(7) Uani 1 1 d . A 1
H23 H 0.5467 -0.3719 0.0415 0.154 Uiso 1 1 calc R A 1
C24 C 0.4150(19) -0.2754(11) 0.0603(5) 0.114(5) Uani 1 1 d . A 1
H24 H 0.3498 -0.3223 0.0617 0.137 Uiso 1 1 calc R A 1
C25 C 0.3821(14) -0.1818(11) 0.0707(4) 0.103(4) Uani 1 1 d . A 1
H25 H 0.2977 -0.1660 0.0790 0.124 Uiso 1 1 calc R A 1
C26 C 0.6996(8) 0.1280(7) 0.1346(3) 0.066(3) Uani 1 1 d . A 1
H26A H 0.6851 0.1826 0.1132 0.080 Uiso 1 1 calc R A 1
H26B H 0.7368 0.1547 0.1632 0.080 Uiso 1 1 calc R A 1
C27 C 0.7962(8) 0.0592(7) 0.1125(3) 0.056(2) Uani 1 1 d . A 1
C28 C 0.8510(9) -0.0180(7) 0.1364(3) 0.065(2) Uani 1 1 d . A 1
H28 H 0.8285 -0.0283 0.1677 0.078 Uiso 1 1 calc R A 1
C29 C 0.9383(10) -0.0807(8) 0.1155(4) 0.084(3) Uani 1 1 d . A 1
H29 H 0.9729 -0.1314 0.1334 0.101 Uiso 1 1 calc R A 1
C30 C 0.9752(13) -0.0721(9) 0.0711(4) 0.101(4) Uani 1 1 d . A 1
H30 H 1.0354 -0.1144 0.0577 0.121 Uiso 1 1 calc R A 1
C31 C 0.9198(11) 0.0023(11) 0.0463(4) 0.100(4) Uani 1 1 d . A 1
H31 H 0.9409 0.0091 0.0146 0.120 Uiso 1 1 calc R A 1
C32 C 0.8345(10) 0.0676(9) 0.0657(4) 0.081(3) Uani 1 1 d . A 1
H32 H 0.8017 0.1183 0.0473 0.098 Uiso 1 1 calc R A 1
C33 C 0.4960(11) -0.0841(5) 0.1905(3) 0.064(2) Uani 1 1 d . A 1
H33A H 0.4939 -0.1380 0.1682 0.077 Uiso 1 1 calc R A 1
H33B H 0.5710 -0.0923 0.2106 0.077 Uiso 1 1 calc R A 1
C34 C 0.3745(8) -0.0838(5) 0.2198(3) 0.052(2) Uani 1 1 d . A 1
C35 C 0.2537(11) -0.0670(7) 0.2000(4) 0.079(3) Uani 1 1 d . A 1
H35 H 0.2464 -0.0635 0.1674 0.094 Uiso 1 1 calc R A 1
C36 C 0.1440(11) -0.0553(8) 0.2274(5) 0.094(4) Uani 1 1 d . A 1
H36 H 0.0650 -0.0417 0.2133 0.113 Uiso 1 1 calc R A 1
C37 C 0.1524(11) -0.0640(9) 0.2754(5) 0.098(4) Uani 1 1 d . A 1
H37 H 0.0794 -0.0567 0.2941 0.118 Uiso 1 1 calc R A 1
C38 C 0.2697(12) -0.0834(8) 0.2952(4) 0.088(3) Uani 1 1 d . A 1
H38 H 0.2762 -0.0887 0.3277 0.105 Uiso 1 1 calc R A 1
C39 C 0.3799(10) -0.0954(7) 0.2676(4) 0.068(3) Uani 1 1 d . A 1
H39 H 0.4579 -0.1115 0.2819 0.081 Uiso 1 1 calc R A 1
C42 C 0.421(2) 0.9745(18) 0.9300(11) 0.288(12) Uani 1 1 d DU . .
H42A H 0.4881 0.9916 0.9525 0.346 Uiso 1 1 calc R . .
H42B H 0.4354 1.0149 0.9023 0.346 Uiso 1 1 calc R . .
C43 C 0.441(2) 0.8743(18) 0.9166(11) 0.282(13) Uani 1 1 d DU . .
H43A H 0.4138 0.8321 0.9423 0.339 Uiso 1 1 calc R . .
H43B H 0.3865 0.8596 0.8897 0.339 Uiso 1 1 calc R . .
C44 C 0.568(2) 0.8532(17) 0.9053(9) 0.259(12) Uani 1 1 d DU . .
H44A H 0.6103 0.9122 0.8953 0.389 Uiso 1 1 calc R . .
H44B H 0.5697 0.8056 0.8803 0.389 Uiso 1 1 calc R . .
H44C H 0.6107 0.8270 0.9325 0.389 Uiso 1 1 calc R . .
C40 C 0.292(2) 1.1065(15) 0.9594(9) 0.236(11) Uani 1 1 d DU . .
H40A H 0.3603 1.1263 0.9802 0.353 Uiso 1 1 calc R . .
H40B H 0.2102 1.1191 0.9740 0.353 Uiso 1 1 calc R . .
H40C H 0.2979 1.1431 0.9305 0.353 Uiso 1 1 calc R . .
C41 C 0.304(3) 1.0010(18) 0.9492(13) 0.350(15) Uani 1 1 d DU . .
H41A H 0.2911 0.9645 0.9782 0.420 Uiso 1 1 calc R . .
H41B H 0.2358 0.9822 0.9275 0.420 Uiso 1 1 calc R . .


_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
Hf1 N2 2.080(6) . ?
Hf1 C33 2.242(7) . ?
Hf1 C26 2.260(9) . ?
Hf1 C19 2.276(9) . ?
Hf1 N1 2.395(5) . ?
N1 C1 1.317(10) . ?
N1 C5 1.388(10) . ?
N2 C9 1.389(10) . ?
N2 C12 1.475(10) . ?
C1 C2 1.414(11) . ?
C1 C13 1.540(11) . ?
C2 C3 1.357(13) . ?
C3 C4 1.383(12) . ?
C4 C5 1.395(11) . ?
C4 C6 1.405(13) . ?
C5 C9 1.440(11) . ?
C6 C7 1.341(13) . ?
C7 C8 1.408(13) . ?
C8 C9 1.373(11) . ?
C8 C10 1.497(12) . ?
C10 C11 1.512(13) . ?
C11 C12 1.554(13) . ?
C12 C16 1.556(12) . ?
C13 C15 1.498(12) . ?
C13 C14 1.507(11) . ?
C16 C17 1.516(14) . ?
C16 C18 1.545(14) . ?
C19 C20 1.480(13) . ?
C20 C21 1.365(16) . ?
C20 C25 1.384(16) . ?
C21 C22 1.367(18) . ?
C22 C23 1.37(2) . ?
C23 C24 1.31(2) . ?
C24 C25 1.35(2) . ?
C26 C27 1.507(11) . ?
C27 C28 1.374(12) . ?
C27 C32 1.392(12) . ?
C28 C29 1.377(13) . ?
C29 C30 1.322(14) . ?
C30 C31 1.361(15) . ?
C31 C32 1.369(14) . ?
C33 C34 1.509(12) . ?
C34 C39 1.368(13) . ?
C34 C35 1.391(13) . ?
C35 C36 1.387(16) . ?
C36 C37 1.370(17) . ?
C37 C38 1.365(16) . ?
C38 C39 1.394(15) . ?
C42 C41 1.383(18) . ?
C42 C43 1.429(18) . ?
C43 C44 1.383(17) . ?
C40 C41 1.469(19) . ?

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
N2 Hf1 C33 122.6(3) . . ?
N2 Hf1 C26 113.0(3) . . ?
C33 Hf1 C26 120.6(4) . . ?
N2 Hf1 C19 94.6(3) . . ?
C33 Hf1 C19 93.6(3) . . ?
C26 Hf1 C19 101.5(4) . . ?
N2 Hf1 N1 72.6(2) . . ?
C33 Hf1 N1 82.5(2) . . ?
C26 Hf1 N1 96.3(3) . . ?
C19 Hf1 N1 161.2(3) . . ?
C1 N1 C5 118.5(6) . . ?
C1 N1 Hf1 130.7(5) . . ?
C5 N1 Hf1 109.3(5) . . ?
C9 N2 C12 113.6(6) . . ?
C9 N2 Hf1 119.0(5) . . ?
C12 N2 Hf1 126.7(5) . . ?
N1 C1 C2 121.3(8) . . ?
N1 C1 C13 118.5(7) . . ?
C2 C1 C13 120.2(8) . . ?
C3 C2 C1 119.8(8) . . ?
C2 C3 C4 120.7(8) . . ?
C3 C4 C5 117.1(8) . . ?
C3 C4 C6 123.5(8) . . ?
C5 C4 C6 119.4(8) . . ?
N1 C5 C4 122.6(7) . . ?
N1 C5 C9 116.0(7) . . ?
C4 C5 C9 121.4(7) . . ?
C7 C6 C4 118.6(9) . . ?
C6 C7 C8 123.6(9) . . ?
C9 C8 C7 119.9(8) . . ?
C9 C8 C10 118.5(8) . . ?
C7 C8 C10 121.5(8) . . ?
C8 C9 N2 126.8(8) . . ?
C8 C9 C5 117.2(8) . . ?
N2 C9 C5 116.1(7) . . ?
C8 C10 C11 112.0(7) . . ?
C10 C11 C12 109.4(8) . . ?
N2 C12 C11 107.5(8) . . ?
N2 C12 C16 112.5(7) . . ?
C11 C12 C16 113.6(8) . . ?
C15 C13 C14 109.8(7) . . ?
C15 C13 C1 109.4(7) . . ?
C14 C13 C1 112.4(7) . . ?
C17 C16 C18 111.0(9) . . ?
C17 C16 C12 111.6(7) . . ?
C18 C16 C12 112.1(9) . . ?
C20 C19 Hf1 123.3(7) . . ?
C21 C20 C25 116.7(11) . . ?
C21 C20 C19 121.8(11) . . ?
C25 C20 C19 121.4(12) . . ?
C20 C21 C22 122.0(14) . . ?
C21 C22 C23 120.4(15) . . ?
C24 C23 C22 116.3(14) . . ?
C23 C24 C25 126.0(16) . . ?
C24 C25 C20 118.5(14) . . ?
C27 C26 Hf1 115.3(6) . . ?
C28 C27 C32 114.6(8) . . ?
C28 C27 C26 122.9(8) . . ?
C32 C27 C26 122.5(8) . . ?
C27 C28 C29 122.1(9) . . ?
C30 C29 C28 123.1(10) . . ?
C29 C30 C31 116.0(10) . . ?
C30 C31 C32 123.0(10) . . ?
C31 C32 C27 121.1(10) . . ?
C34 C33 Hf1 107.7(5) . . ?
C39 C34 C35 117.2(9) . . ?
C39 C34 C33 120.8(8) . . ?
C35 C34 C33 121.9(9) . . ?
C36 C35 C34 122.0(10) . . ?
C37 C36 C35 119.7(10) . . ?
C38 C37 C36 118.9(12) . . ?
C37 C38 C39 121.3(11) . . ?
C34 C39 C38 120.7(10) . . ?
C41 C42 C43 118(3) . . ?
C44 C43 C42 113.1(19) . . ?
C42 C41 C40 114(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.199
