# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1044550'
_audit_update_record             
;
2015-06-26 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H33 Cl2 N Ti'
_chemical_formula_sum            'C22 H33 Cl2 N Ti'
_chemical_formula_weight         430.29

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.5530(4)
_cell_length_b                   15.4710(11)
_cell_length_c                   20.2441(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2365.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    14634
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.188
_exptl_absorpt_coefficient_mu    0.593
_shelx_estimated_absorpt_T_min   0.866
_shelx_estimated_absorpt_T_max   0.898
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.076
0 0 1 0.126
1 0 0 0.123
-1 0 0 0.117
0 -1 0 0.094
0 1 0 0.085
-1 0 -1 0.091


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            13779
_diffrn_reflns_sigmaI/netI       0.0357
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.078
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4602
_reflns_number_gt                3919
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_max     0.986
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 The reflections were merged according to the crystal class
 for structure refinement and the calculation of statistics.
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. These statistics refer to single and
 composite reflections containing twin component 1 only.

 All Cp* carbon and hydrogen atoms were split to two positions
 DFIX 1.520 0.020 instruction is used to correct the C-C distances 
 between the carbon atoms of Cp ring and appropriate methyls
 SADI 0.02, DELU 0.010  0.010 and SIMU 0.040 0.080 1.700 instructions 
 were used for the same pairs of carbon atoms.
 EADP instruction was used for neighbouring carbon atoms.
 ISOR 0.100 instruction was used for all the split carbon atoms

;

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0626P)²+1.9798P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4602
_refine_ls_number_parameters     263
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1398
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.104
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.59891(11) 0.07482(6) 0.60128(4) 0.0365(2) Uani 1 1 d . . . . .
Cl1 Cl 0.7684(2) 0.02146(13) 0.51809(8) 0.0707(5) Uani 1 1 d . . . . .
Cl2 Cl 0.7918(2) 0.16751(11) 0.64951(9) 0.0653(5) Uani 1 1 d . . . . .
N1 N 0.5689(5) -0.0169(3) 0.6626(2) 0.0397(10) Uani 1 1 d . . . . .
H1 H 0.4606 -0.0327 0.6732 0.048 Uiso 1 1 calc . U . . .
C1A C 0.336(2) 0.0561(6) 0.5428(5) 0.062(6) Uani 0.488(10) 1 d DG . P A 1
C2A C 0.4203(16) 0.1289(6) 0.5141(4) 0.052(4) Uani 0.488(10) 1 d DG . P A 1
C3A C 0.4294(18) 0.1950(6) 0.5626(5) 0.045(5) Uani 0.488(10) 1 d DG . P A 1
C4A C 0.3502(16) 0.1630(7) 0.6214(4) 0.040(4) Uani 0.488(10) 1 d DG . P A 1
C5A C 0.292(2) 0.0772(7) 0.6091(5) 0.047(5) Uani 0.488(10) 1 d DG . P A 1
C6A C 0.289(2) -0.0252(10) 0.5071(9) 0.122(5) Uani 0.488(10) 1 d D . P A 1
H6A1 H 0.2248 -0.0640 0.5370 0.183 Uiso 0.488(10) 1 calc R U P A 1
H6A2 H 0.3971 -0.0536 0.4917 0.183 Uiso 0.488(10) 1 calc R U P A 1
H6A3 H 0.2134 -0.0113 0.4691 0.183 Uiso 0.488(10) 1 calc R U P A 1
C7A C 0.476(3) 0.1372(11) 0.4438(8) 0.122(5) Uani 0.488(10) 1 d D . P A 1
H7A1 H 0.4515 0.0831 0.4204 0.183 Uiso 0.488(10) 1 calc R U P A 1
H7A2 H 0.6033 0.1496 0.4418 0.183 Uiso 0.488(10) 1 calc R U P A 1
H7A3 H 0.4104 0.1845 0.4229 0.183 Uiso 0.488(10) 1 calc R U P A 1
C8A C 0.509(2) 0.2814(10) 0.5530(9) 0.122(5) Uani 0.488(10) 1 d D . P A 1
H8A1 H 0.5031 0.3139 0.5945 0.183 Uiso 0.488(10) 1 calc R U P A 1
H8A2 H 0.4429 0.3126 0.5187 0.183 Uiso 0.488(10) 1 calc R U P A 1
H8A3 H 0.6325 0.2751 0.5393 0.183 Uiso 0.488(10) 1 calc R U P A 1
C9A C 0.329(3) 0.2112(11) 0.6839(8) 0.122(5) Uani 0.488(10) 1 d D . P A 1
H9A1 H 0.2685 0.1746 0.7163 0.183 Uiso 0.488(10) 1 calc R U P A 1
H9A2 H 0.2591 0.2634 0.6760 0.183 Uiso 0.488(10) 1 calc R U P A 1
H9A3 H 0.4461 0.2273 0.7009 0.183 Uiso 0.488(10) 1 calc R U P A 1
C10A C 0.178(2) 0.0241(11) 0.6527(9) 0.122(5) Uani 0.488(10) 1 d D . P A 1
H10A H 0.0545 0.0284 0.6378 0.183 Uiso 0.488(10) 1 calc R U P A 1
H10B H 0.1867 0.0453 0.6982 0.183 Uiso 0.488(10) 1 calc R U P A 1
H10C H 0.2160 -0.0363 0.6509 0.183 Uiso 0.488(10) 1 calc R U P A 1
C1B C 0.283(2) 0.0551(6) 0.5876(5) 0.041(4) Uani 0.512(10) 1 d DG . P A 2
C2B C 0.358(2) 0.0858(7) 0.5276(4) 0.046(4) Uani 0.512(10) 1 d DG . P A 2
C3B C 0.4295(16) 0.1691(6) 0.5395(5) 0.052(6) Uani 0.512(10) 1 d DG . P A 2
C4B C 0.3999(16) 0.1899(6) 0.6070(6) 0.051(4) Uani 0.512(10) 1 d DG . P A 2
C5B C 0.3095(11) 0.1194(7) 0.6366(4) 0.045(4) Uani 0.512(10) 1 d DG . P A 2
C6B C 0.191(2) -0.0281(10) 0.5987(8) 0.111(4) Uani 0.512(10) 1 d D . P A 2
H6B1 H 0.0633 -0.0195 0.5947 0.166 Uiso 0.512(10) 1 calc R U P A 2
H6B2 H 0.2191 -0.0495 0.6430 0.166 Uiso 0.512(10) 1 calc R U P A 2
H6B3 H 0.2307 -0.0703 0.5657 0.166 Uiso 0.512(10) 1 calc R U P A 2
C7B C 0.349(2) 0.0411(11) 0.4635(7) 0.111(4) Uani 0.512(10) 1 d D . P A 2
H7B1 H 0.4106 0.0754 0.4300 0.166 Uiso 0.512(10) 1 calc R U P A 2
H7B2 H 0.2245 0.0339 0.4505 0.166 Uiso 0.512(10) 1 calc R U P A 2
H7B3 H 0.4048 -0.0158 0.4673 0.166 Uiso 0.512(10) 1 calc R U P A 2
C8B C 0.515(2) 0.2272(11) 0.4912(8) 0.111(4) Uani 0.512(10) 1 d D . P A 2
H8B1 H 0.5226 0.1980 0.4483 0.166 Uiso 0.512(10) 1 calc R U P A 2
H8B2 H 0.6338 0.2422 0.5065 0.166 Uiso 0.512(10) 1 calc R U P A 2
H8B3 H 0.4440 0.2800 0.4866 0.166 Uiso 0.512(10) 1 calc R U P A 2
C9B C 0.432(2) 0.2753(9) 0.6394(8) 0.111(4) Uani 0.512(10) 1 d D . P A 2
H9B1 H 0.4939 0.3137 0.6085 0.166 Uiso 0.512(10) 1 calc R U P A 2
H9B2 H 0.5056 0.2670 0.6788 0.166 Uiso 0.512(10) 1 calc R U P A 2
H9B3 H 0.3190 0.3013 0.6521 0.166 Uiso 0.512(10) 1 calc R U P A 2
C10B C 0.248(2) 0.1153(11) 0.7063(7) 0.111(4) Uani 0.512(10) 1 d D . P A 2
H10D H 0.1918 0.0592 0.7145 0.166 Uiso 0.512(10) 1 calc R U P A 2
H10E H 0.1615 0.1616 0.7142 0.166 Uiso 0.512(10) 1 calc R U P A 2
H10F H 0.3489 0.1226 0.7361 0.166 Uiso 0.512(10) 1 calc R U P A 2
C11 C 0.7152(7) -0.0616(3) 0.6923(2) 0.0374(11) Uani 1 1 d . . . . .
C12 C 0.7857(8) -0.0313(3) 0.7517(3) 0.0442(12) Uani 1 1 d . . . . .
C13 C 0.9313(8) -0.0748(4) 0.7777(3) 0.0563(15) Uani 1 1 d . . . . .
H13 H 0.9820 -0.0556 0.8169 0.068 Uiso 1 1 d R U . . .
C14 C 1.0018(10) -0.1457(5) 0.7471(4) 0.0664(19) Uani 1 1 d . . . . .
H14 H 1.1008 -0.1730 0.7647 0.080 Uiso 1 1 d R U . . .
C15 C 0.9289(9) -0.1757(4) 0.6909(4) 0.0636(18) Uani 1 1 d . . . . .
H15 H 0.9763 -0.2248 0.6711 0.076 Uiso 1 1 d R U . . .
C16 C 0.7832(9) -0.1361(3) 0.6611(3) 0.0496(13) Uani 1 1 d . . . . .
C17 C 0.6982(9) 0.0415(4) 0.7896(3) 0.0537(15) Uani 1 1 d . . . . .
H17 H 0.6392 0.0789 0.7573 0.064 Uiso 1 1 d R U . . .
C18 C 0.5540(12) 0.0051(5) 0.8350(4) 0.078(2) Uani 1 1 d . . . . .
H18A H 0.6100 -0.0250 0.8708 0.093 Uiso 1 1 d R U . . .
H18B H 0.4828 0.0513 0.8522 0.093 Uiso 1 1 d R U . . .
H18C H 0.4802 -0.0344 0.8108 0.093 Uiso 1 1 d R U . . .
C19 C 0.8271(12) 0.0968(5) 0.8288(4) 0.079(2) Uani 1 1 d . . . . .
H19A H 0.9183 0.1184 0.8002 0.094 Uiso 1 1 d R U . . .
H19B H 0.7643 0.1445 0.8482 0.094 Uiso 1 1 d R U . . .
H19C H 0.8794 0.0624 0.8631 0.094 Uiso 1 1 d R U . . .
C20 C 0.6904(11) -0.1752(4) 0.6025(4) 0.0671(17) Uani 1 1 d . . . . .
H20 H 0.6301 -0.1280 0.5793 0.080 Uiso 1 1 d R U . . .
C21 C 0.5504(16) -0.2380(6) 0.6254(5) 0.112(4) Uani 1 1 d . . . . .
H21A H 0.4807 -0.2113 0.6594 0.134 Uiso 1 1 d R U . . .
H21B H 0.4752 -0.2537 0.5891 0.134 Uiso 1 1 d R U . . .
H21C H 0.6065 -0.2889 0.6427 0.134 Uiso 1 1 d R U . . .
C22 C 0.8191(16) -0.2177(7) 0.5523(5) 0.119(4) Uani 1 1 d . . . . .
H22A H 0.7600 -0.2297 0.5113 0.143 Uiso 1 1 d R U . . .
H22B H 0.9157 -0.1787 0.5445 0.143 Uiso 1 1 d R U . . .
H22C H 0.8635 -0.2706 0.5708 0.143 Uiso 1 1 d R U . . .


_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 N1 1.898(4) . ?
Ti1 Cl2 2.2657(18) . ?
Ti1 Cl1 2.2707(18) . ?
Ti1 C3B 2.308(12) . ?
Ti1 C5A 2.322(15) . ?
Ti1 C4B 2.333(12) . ?
Ti1 C1A 2.333(16) . ?
Ti1 C4A 2.357(12) . ?
Ti1 C2B 2.362(13) . ?
Ti1 C2A 2.374(10) . ?
Ti1 C3A 2.389(14) . ?
Ti1 C5B 2.401(9) . ?
N1 C11 1.436(7) . ?
N1 H1 0.8800 . ?
C1A C2A 1.4200 . ?
C1A C5A 1.4200 . ?
C1A C6A 1.493(14) . ?
C2A C3A 1.4200 . ?
C2A C7A 1.488(14) . ?
C3A C4A 1.4200 . ?
C3A C8A 1.478(14) . ?
C4A C5A 1.4200 . ?
C4A C9A 1.477(14) . ?
C5A C10A 1.484(14) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C1B C2B 1.4200 . ?
C1B C5B 1.4200 . ?
C1B C6B 1.479(13) . ?
C2B C3B 1.4200 . ?
C2B C7B 1.471(13) . ?
C3B C4B 1.4200 . ?
C3B C8B 1.476(16) . ?
C4B C5B 1.4200 . ?
C4B C9B 1.497(14) . ?
C5B C10B 1.487(13) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11 C12 1.397(7) . ?
C11 C16 1.410(8) . ?
C12 C13 1.392(8) . ?
C12 C17 1.514(8) . ?
C13 C14 1.368(10) . ?
C13 H13 0.9298 . ?
C14 C15 1.347(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.396(9) . ?
C15 H15 0.9300 . ?
C16 C20 1.506(9) . ?
C17 C19 1.521(10) . ?
C17 C18 1.533(9) . ?
C17 H17 0.9801 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9599 . ?
C20 C21 1.509(11) . ?
C20 C22 1.552(12) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9601 . ?
C21 H21B 0.9599 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9601 . ?
C22 H22B 0.9601 . ?
C22 H22C 0.9600 . ?

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 Ti1 Cl2 105.57(14) . . ?
N1 Ti1 Cl1 106.27(15) . . ?
Cl2 Ti1 Cl1 100.79(9) . . ?
N1 Ti1 C3B 139.5(3) . . ?
Cl2 Ti1 C3B 100.9(3) . . ?
Cl1 Ti1 C3B 98.1(2) . . ?
N1 Ti1 C5A 81.3(3) . . ?
Cl2 Ti1 C5A 127.0(3) . . ?
Cl1 Ti1 C5A 128.2(3) . . ?
N1 Ti1 C4B 117.5(3) . . ?
Cl2 Ti1 C4B 84.9(2) . . ?
Cl1 Ti1 C4B 132.6(3) . . ?
C3B Ti1 C4B 35.63(18) . . ?
N1 Ti1 C1A 97.9(3) . . ?
Cl2 Ti1 C1A 147.7(3) . . ?
Cl1 Ti1 C1A 93.4(3) . . ?
C5A Ti1 C1A 35.5(2) . . ?
N1 Ti1 C4A 103.0(3) . . ?
Cl2 Ti1 C4A 94.1(2) . . ?
Cl1 Ti1 C4A 142.0(2) . . ?
C5A Ti1 C4A 35.32(16) . . ?
C1A Ti1 C4A 58.7(2) . . ?
N1 Ti1 C2B 112.0(3) . . ?
Cl2 Ti1 C2B 136.3(2) . . ?
Cl1 Ti1 C2B 89.6(3) . . ?
C3B Ti1 C2B 35.38(16) . . ?
C4B Ti1 C2B 58.59(19) . . ?
N1 Ti1 C2A 133.0(3) . . ?
Cl2 Ti1 C2A 117.6(3) . . ?
Cl1 Ti1 C2A 84.1(2) . . ?
C5A Ti1 C2A 58.6(2) . . ?
C1A Ti1 C2A 35.10(16) . . ?
C4A Ti1 C2A 58.10(19) . . ?
N1 Ti1 C3A 137.0(3) . . ?
Cl2 Ti1 C3A 89.6(3) . . ?
Cl1 Ti1 C3A 110.0(2) . . ?
C5A Ti1 C3A 58.35(19) . . ?
C1A Ti1 C3A 58.22(18) . . ?
C4A Ti1 C3A 34.81(17) . . ?
C2A Ti1 C3A 34.69(15) . . ?
N1 Ti1 C5B 84.9(3) . . ?
Cl2 Ti1 C5B 106.0(2) . . ?
Cl1 Ti1 C5B 147.0(2) . . ?
C3B Ti1 C5B 58.36(16) . . ?
C4B Ti1 C5B 34.87(12) . . ?
C2B Ti1 C5B 57.7(2) . . ?
C11 N1 Ti1 122.8(3) . . ?
C11 N1 H1 118.6 . . ?
Ti1 N1 H1 118.6 . . ?
C2A C1A C5A 108.0 . . ?
C2A C1A C6A 125.2(7) . . ?
C5A C1A C6A 126.6(7) . . ?
C2A C1A Ti1 74.0(6) . . ?
C5A C1A Ti1 71.8(4) . . ?
C6A C1A Ti1 123.5(12) . . ?
C3A C2A C1A 108.0 . . ?
C3A C2A C7A 125.8(7) . . ?
C1A C2A C7A 126.0(7) . . ?
C3A C2A Ti1 73.2(6) . . ?
C1A C2A Ti1 70.9(6) . . ?
C7A C2A Ti1 125.5(10) . . ?
C2A C3A C4A 108.0 . . ?
C2A C3A C8A 125.4(7) . . ?
C4A C3A C8A 126.6(7) . . ?
C2A C3A Ti1 72.1(5) . . ?
C4A C3A Ti1 71.4(4) . . ?
C8A C3A Ti1 122.0(11) . . ?
C5A C4A C3A 108.0 . . ?
C5A C4A C9A 126.0(7) . . ?
C3A C4A C9A 126.0(7) . . ?
C5A C4A Ti1 71.0(7) . . ?
C3A C4A Ti1 73.8(5) . . ?
C9A C4A Ti1 121.7(10) . . ?
C1A C5A C4A 108.0 . . ?
C1A C5A C10A 124.8(7) . . ?
C4A C5A C10A 126.4(7) . . ?
C1A C5A Ti1 72.7(4) . . ?
C4A C5A Ti1 73.7(6) . . ?
C10A C5A Ti1 127.8(11) . . ?
C1A C6A H6A1 109.5 . . ?
C1A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C1A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C2A C7A H7A1 109.5 . . ?
C2A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C2A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C3A C8A H8A1 109.5 . . ?
C3A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C3A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C4A C9A H9A1 109.5 . . ?
C4A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C4A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C5A C10A H10A 109.5 . . ?
C5A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C5A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C2B C1B C5B 108.0 . . ?
C2B C1B C6B 127.4(7) . . ?
C5B C1B C6B 124.6(7) . . ?
C2B C1B Ti1 70.6(4) . . ?
C5B C1B Ti1 72.2(5) . . ?
C6B C1B Ti1 123.7(11) . . ?
C1B C2B C3B 108.0 . . ?
C1B C2B C7B 125.3(7) . . ?
C3B C2B C7B 126.5(7) . . ?
C1B C2B Ti1 74.9(4) . . ?
C3B C2B Ti1 70.2(6) . . ?
C7B C2B Ti1 123.9(10) . . ?
C4B C3B C2B 108.0 . . ?
C4B C3B C8B 124.6(8) . . ?
C2B C3B C8B 127.3(8) . . ?
C4B C3B Ti1 73.1(4) . . ?
C2B C3B Ti1 74.4(6) . . ?
C8B C3B Ti1 120.2(10) . . ?
C3B C4B C5B 108.0 . . ?
C3B C4B C9B 126.6(7) . . ?
C5B C4B C9B 124.9(7) . . ?
C3B C4B Ti1 71.2(4) . . ?
C5B C4B Ti1 75.2(5) . . ?
C9B C4B Ti1 126.1(10) . . ?
C1B C5B C4B 108.0 . . ?
C1B C5B C10B 126.2(7) . . ?
C4B C5B C10B 125.8(7) . . ?
C1B C5B Ti1 73.6(5) . . ?
C4B C5B Ti1 69.9(6) . . ?
C10B C5B Ti1 123.8(8) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10D 109.5 . . ?
C5B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C5B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C12 C11 C16 121.3(5) . . ?
C12 C11 N1 119.5(5) . . ?
C16 C11 N1 119.1(5) . . ?
C13 C12 C11 117.6(5) . . ?
C13 C12 C17 120.9(5) . . ?
C11 C12 C17 121.3(5) . . ?
C14 C13 C12 121.6(6) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C13 120.0(6) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 122.3(6) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 118.5 . . ?
C15 C16 C11 117.0(6) . . ?
C15 C16 C20 122.0(6) . . ?
C11 C16 C20 120.7(6) . . ?
C12 C17 C19 113.8(6) . . ?
C12 C17 C18 109.9(5) . . ?
C19 C17 C18 110.4(6) . . ?
C12 C17 H17 107.5 . . ?
C19 C17 H17 107.8 . . ?
C18 C17 H17 107.1 . . ?
C17 C18 H18A 108.5 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.9 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.9 . . ?
C17 C19 H19B 109.3 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.2 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 C21 110.1(6) . . ?
C16 C20 C22 113.2(7) . . ?
C21 C20 C22 111.5(7) . . ?
C16 C20 H20 107.1 . . ?
C21 C20 H20 107.5 . . ?
C22 C20 H20 107.1 . . ?
C20 C21 H21A 109.1 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.3 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 110.9 . . ?
C20 C22 H22B 108.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.0 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_refine_diff_density_max         0.518
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.058

#
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1044551'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H33 Cl2 N Zr'
_chemical_formula_sum            'C22 H33 Cl2 N Zr'
_chemical_formula_weight         473.61

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.607(5)
_cell_length_b                   15.343(10)
_cell_length_c                   20.501(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2393(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18852
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.50

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.689
_shelx_estimated_absorpt_T_min   0.665
_shelx_estimated_absorpt_T_max   0.928
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.012
0 1 -1 0.067
0 1 1 0.030
0 -1 -1 0.057
1 0 0 0.304
-1 0 0 0.323


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            18057
_diffrn_reflns_sigmaI/netI       0.0587
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.107
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             4809
_reflns_number_gt                4139
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_max     0.976
_reflns_Friedel_fraction_full    0.989

_reflns_special_details          
;
 The reflections were merged according to the crystal class
 for structure refinement and the calculation of statistics.
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. These statistics refer to single and
 composite reflections containing twin component 1 only.


 All Cp* carbon and hydrogen atoms were split to two positions
 DFIX 1.520 0.020 instruction is used to correct the C-C distances 
 between the carbon atoms of Cp ring and appropriate methyls
 SADI 0.02, DELU 0.010  0.010 and SIMU 0.040 0.080 1.700 instructions 
 were used for the same pairs of carbon atoms.
 EADP instruction was used for neighbouring carbon atoms.
 ISOR 0.100 instruction was used for all the split carbon atoms
;

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'


_refine_special_details          
;
 Refined as a 2-component racemic twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0242P)²+5.2021P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.06(11)
_refine_ls_number_reflns         4809
_refine_ls_number_parameters     224
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1142
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.89196(8) 0.93352(4) 0.59761(3) 0.02611(17) Uani 1 1 d D . .
Cl1 Cl 0.7202(3) 0.99207(16) 0.50945(11) 0.0543(6) Uani 1 1 d D A .
Cl2 Cl 0.7000(3) 0.83011(13) 0.64902(12) 0.0516(6) Uani 1 1 d D A .
N1 N 0.9357(7) 1.0326(4) 0.6610(3) 0.0320(13) Uani 1 1 d D A .
H1 H 1.0409 1.0482 0.6711 0.038 Uiso 1 1 d RD . .
C1A C 1.1718(12) 0.9471(4) 0.5365(3) 0.045(3) Uani 0.689(6) 1 d PGD A 1
C2A C 1.0829(12) 0.8735(5) 0.5106(3) 0.039(3) Uani 0.689(6) 1 d PGD A 1
C3A C 1.0749(14) 0.8088(4) 0.5600(4) 0.031(3) Uani 0.689(6) 1 d PGD A 1
C4A C 1.1588(12) 0.8425(5) 0.6165(3) 0.036(3) Uani 0.689(6) 1 d PGD A 1
C5A C 1.2188(10) 0.9280(4) 0.6020(3) 0.035(2) Uani 0.689(6) 1 d PGD A 1
C6A C 1.211(2) 1.0302(9) 0.5006(8) 0.079(4) Uiso 0.689(6) 1 d PD A 1
H6A1 H 1.2739 1.0703 0.5295 0.119 Uiso 0.689(6) 1 calc PRD A 1
H6A2 H 1.1007 1.0571 0.4863 0.119 Uiso 0.689(6) 1 calc PRD A 1
H6A3 H 1.2842 1.0173 0.4624 0.119 Uiso 0.689(6) 1 calc PRD A 1
C7A C 1.023(2) 0.8630(10) 0.4408(7) 0.079(4) Uiso 0.689(6) 1 d PD A 1
H7A1 H 0.9641 0.8067 0.4357 0.119 Uiso 0.689(6) 1 calc PRD A 1
H7A2 H 1.1252 0.8656 0.4117 0.119 Uiso 0.689(6) 1 calc PRD A 1
H7A3 H 0.9411 0.9100 0.4297 0.119 Uiso 0.689(6) 1 calc PRD A 1
C8A C 1.001(2) 0.7186(8) 0.5514(7) 0.067(4) Uiso 0.689(6) 1 d PD A 1
H8A1 H 1.0105 0.6865 0.5926 0.100 Uiso 0.689(6) 1 calc PRD A 1
H8A2 H 1.0676 0.6879 0.5175 0.100 Uiso 0.689(6) 1 calc PRD A 1
H8A3 H 0.8774 0.7225 0.5385 0.100 Uiso 0.689(6) 1 calc PRD A 1
C9A C 1.183(2) 0.7942(10) 0.6783(7) 0.078(4) Uiso 0.689(6) 1 d PD A 1
H9A1 H 1.1274 0.7367 0.6747 0.117 Uiso 0.689(6) 1 calc PRD A 1
H9A2 H 1.1280 0.8267 0.7141 0.117 Uiso 0.689(6) 1 calc PRD A 1
H9A3 H 1.3085 0.7871 0.6872 0.117 Uiso 0.689(6) 1 calc PRD A 1
C10A C 1.324(2) 0.9835(10) 0.6466(8) 0.079(4) Uiso 0.689(6) 1 d PD A 1
H10A H 1.3497 1.0393 0.6252 0.119 Uiso 0.689(6) 1 calc PRD A 1
H10B H 1.4347 0.9539 0.6571 0.119 Uiso 0.689(6) 1 calc PRD A 1
H10C H 1.2577 0.9941 0.6867 0.119 Uiso 0.689(6) 1 calc PRD A 1
C1B C 1.221(3) 0.9535(10) 0.5804(8) 0.045(3) Uani 0.311(6) 1 d PGD A 2
C2B C 1.149(3) 0.9140(11) 0.5238(6) 0.039(3) Uani 0.311(6) 1 d PGD A 2
C3B C 1.082(4) 0.8310(12) 0.5419(8) 0.031(3) Uani 0.311(6) 1 d PGD A 2
C4B C 1.113(3) 0.8192(12) 0.6096(8) 0.036(3) Uani 0.311(6) 1 d PGD A 2
C5B C 1.200(2) 0.8950(11) 0.6334(6) 0.035(2) Uani 0.311(6) 1 d PGD A 2
C6B C 1.304(5) 1.0419(15) 0.5858(15) 0.079(4) Uiso 0.311(6) 1 d PD A 2
H6B1 H 1.3045 1.0701 0.5429 0.119 Uiso 0.311(6) 1 calc PRD A 2
H6B2 H 1.4254 1.0358 0.6014 0.119 Uiso 0.311(6) 1 calc PRD A 2
H6B3 H 1.2370 1.0776 0.6166 0.119 Uiso 0.311(6) 1 calc PRD A 2
C7B C 1.152(5) 0.9532(19) 0.4567(10) 0.079(4) Uiso 0.311(6) 1 d PD A 2
H7B1 H 1.0955 0.9133 0.4258 0.119 Uiso 0.311(6) 1 calc PRD A 2
H7B2 H 1.2745 0.9629 0.4433 0.119 Uiso 0.311(6) 1 calc PRD A 2
H7B3 H 1.0894 1.0089 0.4570 0.119 Uiso 0.311(6) 1 calc PRD A 2
C8B C 1.000(4) 0.7642(16) 0.4977(13) 0.067(4) Uiso 0.311(6) 1 d PD A 2
H8B1 H 0.9924 0.7876 0.4533 0.100 Uiso 0.311(6) 1 calc PRD A 2
H8B2 H 0.8813 0.7503 0.5135 0.100 Uiso 0.311(6) 1 calc PRD A 2
H8B3 H 1.0716 0.7113 0.4977 0.100 Uiso 0.311(6) 1 calc PRD A 2
C9B C 1.090(5) 0.7372(15) 0.6472(13) 0.078(4) Uiso 0.311(6) 1 d PD A 2
H9B1 H 1.1197 0.7475 0.6931 0.117 Uiso 0.311(6) 1 calc PRD A 2
H9B2 H 1.1684 0.6922 0.6294 0.117 Uiso 0.311(6) 1 calc PRD A 2
H9B3 H 0.9681 0.7177 0.6437 0.117 Uiso 0.311(6) 1 calc PRD A 2
C10B C 1.273(5) 0.9086(19) 0.7002(11) 0.079(4) Uiso 0.311(6) 1 d PD A 2
H10D H 1.2398 0.8597 0.7283 0.119 Uiso 0.311(6) 1 calc PRD A 2
H10E H 1.2264 0.9629 0.7184 0.119 Uiso 0.311(6) 1 calc PRD A 2
H10F H 1.4016 0.9123 0.6977 0.119 Uiso 0.311(6) 1 calc PRD A 2
C11 C 0.7852(9) 1.0744(5) 0.6897(3) 0.0305(14) Uani 1 1 d D . .
C12 C 0.7142(10) 1.0410(4) 0.7486(3) 0.0314(16) Uani 1 1 d D A .
C13 C 0.5639(11) 1.0805(5) 0.7731(4) 0.0439(19) Uani 1 1 d D . .
H13 H 0.5115 1.0583 0.8105 0.053 Uiso 1 1 d RD A .
C14 C 0.4885(12) 1.1515(6) 0.7424(5) 0.051(2) Uani 1 1 d D A .
H14 H 0.3882 1.1771 0.7598 0.062 Uiso 1 1 d RD . .
C15 C 0.5633(11) 1.1853(5) 0.6870(5) 0.049(2) Uani 1 1 d D . .
H15 H 0.5133 1.2338 0.6673 0.059 Uiso 1 1 d RD A .
C16 C 0.7122(11) 1.1467(5) 0.6590(4) 0.0408(18) Uani 1 1 d D A .
C17 C 0.8033(11) 0.9686(5) 0.7857(4) 0.0395(18) Uani 1 1 d D . .
H17 H 0.8619 0.9311 0.7537 0.047 Uiso 1 1 d RD A .
C18 C 0.9470(13) 1.0062(6) 0.8294(5) 0.058(2) Uani 1 1 d D A .
H18A H 0.8944 1.0456 0.8601 0.070 Uiso 1 1 d RD . .
H18B H 1.0042 0.9597 0.8525 0.070 Uiso 1 1 d RD . .
H18C H 1.0317 1.0369 0.8035 0.070 Uiso 1 1 d RD . .
C19 C 0.6800(14) 0.9113(6) 0.8250(4) 0.057(2) Uani 1 1 d D A .
H19A H 0.5835 0.8930 0.7982 0.068 Uiso 1 1 d RD . .
H19B H 0.7430 0.8611 0.8403 0.068 Uiso 1 1 d RD . .
H19C H 0.6360 0.9436 0.8617 0.068 Uiso 1 1 d RD . .
C20 C 0.8019(13) 1.1896(5) 0.6009(5) 0.051(2) Uani 1 1 d D . .
H20 H 0.8677 1.1439 0.5780 0.062 Uiso 1 1 d RD A .
C21 C 0.9338(19) 1.2556(7) 0.6243(6) 0.094(5) Uani 1 1 d D A .
H21A H 1.0008 1.2313 0.6596 0.113 Uiso 1 1 d RD . .
H21B H 1.0115 1.2712 0.5893 0.113 Uiso 1 1 d RD . .
H21C H 0.8726 1.3065 0.6392 0.113 Uiso 1 1 d RD . .
C22 C 0.6713(18) 1.2303(8) 0.5520(6) 0.090(4) Uani 1 1 d D A .
H22A H 0.7329 1.2545 0.5154 0.108 Uiso 1 1 d RD . .
H22B H 0.5934 1.1852 0.5373 0.108 Uiso 1 1 d RD . .
H22C H 0.6044 1.2753 0.5731 0.108 Uiso 1 1 d RD . .


_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 2.027(6) . ?
Zr1 Cl2 2.400(3) . ?
Zr1 Cl1 2.404(2) . ?
Zr1 C3B 2.42(3) . ?
Zr1 C4B 2.44(3) . ?
Zr1 C2A 2.478(8) . ?
Zr1 C1A 2.479(9) . ?
Zr1 C3A 2.488(10) . ?
Zr1 C2B 2.49(2) . ?
Zr1 C5A 2.489(8) . ?
Zr1 C4A 2.495(10) . ?
Zr1 C5B 2.523(18) . ?
N1 C11 1.439(9) . ?
N1 H1 0.8600 . ?
C1A C2A 1.4200 . ?
C1A C5A 1.4200 . ?
C1A C6A 1.502(13) . ?
C2A C3A 1.4200 . ?
C2A C7A 1.509(14) . ?
C3A C4A 1.4200 . ?
C3A C8A 1.505(12) . ?
C4A C5A 1.4200 . ?
C4A C9A 1.479(14) . ?
C5A C10A 1.485(14) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C1B C5B 1.4200 . ?
C1B C2B 1.4200 . ?
C1B C6B 1.499(16) . ?
C2B C3B 1.4200 . ?
C2B C7B 1.503(17) . ?
C3B C4B 1.4200 . ?
C3B C8B 1.504(16) . ?
C4B C5B 1.4200 . ?
C4B C9B 1.486(17) . ?
C5B C10B 1.494(18) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11 C16 1.391(11) . ?
C11 C12 1.419(10) . ?
C12 C13 1.388(10) . ?
C12 C17 1.507(10) . ?
C13 C14 1.382(12) . ?
C13 H13 0.9301 . ?
C14 C15 1.372(13) . ?
C14 H14 0.9299 . ?
C15 C16 1.402(12) . ?
C15 H15 0.9301 . ?
C16 C20 1.523(12) . ?
C17 C19 1.517(11) . ?
C17 C18 1.526(12) . ?
C17 H17 0.9800 . ?
C18 H18A 0.9601 . ?
C18 H18B 0.9601 . ?
C18 H18C 0.9598 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9599 . ?
C20 C21 1.504(13) . ?
C20 C22 1.543(14) . ?
C20 H20 0.9801 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9601 . ?
C22 H22A 0.9599 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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 Cl2 108.32(18) . . ?
N1 Zr1 Cl1 106.91(18) . . ?
Cl2 Zr1 Cl1 104.27(11) . . ?
N1 Zr1 C3B 133.7(5) . . ?
Cl2 Zr1 C3B 98.1(4) . . ?
Cl1 Zr1 C3B 102.3(4) . . ?
N1 Zr1 C4B 111.1(4) . . ?
Cl2 Zr1 C4B 84.3(4) . . ?
Cl1 Zr1 C4B 135.9(4) . . ?
C3B Zr1 C4B 33.9(4) . . ?
N1 Zr1 C2A 130.1(2) . . ?
Cl2 Zr1 C2A 115.29(18) . . ?
Cl1 Zr1 C2A 85.18(16) . . ?
N1 Zr1 C1A 96.9(2) . . ?
Cl2 Zr1 C1A 143.14(16) . . ?
Cl1 Zr1 C1A 93.17(18) . . ?
C2A Zr1 C1A 33.29(10) . . ?
N1 Zr1 C3A 133.1(2) . . ?
Cl2 Zr1 C3A 88.17(19) . . ?
Cl1 Zr1 C3A 111.00(16) . . ?
C2A Zr1 C3A 33.23(12) . . ?
C1A Zr1 C3A 55.10(14) . . ?
N1 Zr1 C2B 110.5(4) . . ?
Cl2 Zr1 C2B 131.7(4) . . ?
Cl1 Zr1 C2B 90.8(4) . . ?
C3B Zr1 C2B 33.6(3) . . ?
C4B Zr1 C2B 55.5(4) . . ?
N1 Zr1 C5A 80.7(2) . . ?
Cl2 Zr1 C5A 124.69(18) . . ?
Cl1 Zr1 C5A 125.64(18) . . ?
C2A Zr1 C5A 55.10(13) . . ?
C1A Zr1 C5A 33.22(10) . . ?
C3A Zr1 C5A 54.98(15) . . ?
N1 Zr1 C4A 100.7(2) . . ?
Cl2 Zr1 C4A 93.26(17) . . ?
Cl1 Zr1 C4A 140.20(18) . . ?
C2A Zr1 C4A 55.03(15) . . ?
C1A Zr1 C4A 55.02(13) . . ?
C3A Zr1 C4A 33.12(13) . . ?
C5A Zr1 C4A 33.11(10) . . ?
N1 Zr1 C5B 80.6(4) . . ?
Cl2 Zr1 C5B 106.4(3) . . ?
Cl1 Zr1 C5B 144.1(3) . . ?
C3B Zr1 C5B 55.3(4) . . ?
C4B Zr1 C5B 33.2(3) . . ?
C2B Zr1 C5B 54.6(3) . . ?
C11 N1 Zr1 117.8(4) . . ?
C11 N1 H1 121.1 . . ?
Zr1 N1 H1 121.1 . . ?
C2A C1A C5A 108.0 . . ?
C2A C1A C6A 125.9(7) . . ?
C5A C1A C6A 126.1(7) . . ?
C2A C1A Zr1 73.3(3) . . ?
C5A C1A Zr1 73.8(3) . . ?
C6A C1A Zr1 119.4(8) . . ?
C1A C2A C3A 108.0 . . ?
C1A C2A C7A 125.7(7) . . ?
C3A C2A C7A 126.1(7) . . ?
C1A C2A Zr1 73.4(3) . . ?
C3A C2A Zr1 73.8(4) . . ?
C7A C2A Zr1 123.0(8) . . ?
C2A C3A C4A 108.0 . . ?
C2A C3A C8A 125.1(7) . . ?
C4A C3A C8A 126.7(7) . . ?
C2A C3A Zr1 73.0(3) . . ?
C4A C3A Zr1 73.7(3) . . ?
C8A C3A Zr1 122.4(9) . . ?
C5A C4A C3A 108.0 . . ?
C5A C4A C9A 127.1(7) . . ?
C3A C4A C9A 124.9(7) . . ?
C5A C4A Zr1 73.2(4) . . ?
C3A C4A Zr1 73.2(3) . . ?
C9A C4A Zr1 120.9(9) . . ?
C4A C5A C1A 108.0 . . ?
C4A C5A C10A 125.1(7) . . ?
C1A C5A C10A 126.8(7) . . ?
C4A C5A Zr1 73.7(4) . . ?
C1A C5A Zr1 73.0(3) . . ?
C10A C5A Zr1 122.8(8) . . ?
C1A C6A H6A1 109.5 . . ?
C1A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C1A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C2A C7A H7A1 109.5 . . ?
C2A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C2A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C3A C8A H8A1 109.5 . . ?
C3A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C3A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C4A C9A H9A1 109.5 . . ?
C4A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C4A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C5A C10A H10A 109.5 . . ?
C5A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C5A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C5B C1B C2B 108.0 . . ?
C5B C1B C6B 124.4(10) . . ?
C2B C1B C6B 127.6(10) . . ?
C5B C1B Zr1 72.7(9) . . ?
C2B C1B Zr1 71.3(9) . . ?
C6B C1B Zr1 120.8(19) . . ?
C3B C2B C1B 108.0 . . ?
C3B C2B C7B 127.2(10) . . ?
C1B C2B C7B 124.8(10) . . ?
C3B C2B Zr1 70.7(11) . . ?
C1B C2B Zr1 76.0(9) . . ?
C7B C2B Zr1 122(2) . . ?
C2B C3B C4B 108.0 . . ?
C2B C3B C8B 127.1(10) . . ?
C4B C3B C8B 124.9(10) . . ?
C2B C3B Zr1 75.8(11) . . ?
C4B C3B Zr1 73.9(8) . . ?
C8B C3B Zr1 118(2) . . ?
C5B C4B C3B 108.0 . . ?
C5B C4B C9B 124.7(10) . . ?
C3B C4B C9B 126.5(11) . . ?
C5B C4B Zr1 76.4(10) . . ?
C3B C4B Zr1 72.2(9) . . ?
C9B C4B Zr1 125(2) . . ?
C1B C5B C4B 108.0 . . ?
C1B C5B C10B 124.7(10) . . ?
C4B C5B C10B 127.0(10) . . ?
C1B C5B Zr1 74.8(10) . . ?
C4B C5B Zr1 70.4(11) . . ?
C10B C5B Zr1 125.5(18) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10D 109.5 . . ?
C5B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C5B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C16 C11 C12 121.5(7) . . ?
C16 C11 N1 119.2(7) . . ?
C12 C11 N1 119.3(6) . . ?
C13 C12 C11 117.5(7) . . ?
C13 C12 C17 120.7(7) . . ?
C11 C12 C17 121.7(7) . . ?
C14 C13 C12 121.5(8) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 120.1(8) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 121.0(8) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C15 118.2(8) . . ?
C11 C16 C20 121.4(7) . . ?
C15 C16 C20 120.1(7) . . ?
C12 C17 C19 114.7(7) . . ?
C12 C17 C18 109.9(6) . . ?
C19 C17 C18 110.5(7) . . ?
C12 C17 H17 107.4 . . ?
C19 C17 H17 107.3 . . ?
C18 C17 H17 106.8 . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 110.0 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.7 . . ?
C17 C19 H19B 109.2 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.4 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C16 109.9(8) . . ?
C21 C20 C22 111.4(9) . . ?
C16 C20 C22 113.2(8) . . ?
C21 C20 H20 107.0 . . ?
C16 C20 H20 107.1 . . ?
C22 C20 H20 108.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.9 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.0 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 110.4 . . ?
C20 C22 H22B 108.0 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.9 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_refine_diff_density_max         0.690
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.089
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1044552'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H33 Cl2 Hf N'
_chemical_formula_sum            'C22 H33 Cl2 Hf N'
_chemical_formula_weight         560.88

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'
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   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   7.5820(4)
_cell_length_b                   15.3669(10)
_cell_length_c                   20.4961(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2388.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    11106
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    4.598
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.040
0 -1 0 0.106
-1 0 0 0.123
1 0 0 0.168
0 0 -1 0.031
0 0 1 0.094


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10516
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.10
_diffrn_reflns_theta_max         25.80
_reflns_number_total             4629
_reflns_number_gt                4258
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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 > 2σ(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.


 All Cp* carbon and hydrogen atoms were split to two positions
 DFIX 1.520 0.020 instruction is used to correct the C-C distances 
 between the carbon atoms of Cp ring and appropriate methyls
 SADI 0.02, DELU 0.010  0.010 and SIMU 0.040 0.080 1.700 instructions 
 were used for the same pairs of carbon atoms.
 EADP instruction was used for neighbouring carbon atoms.
 ISOR 0.100 instruction was used for all the split carbon atoms
;

_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)+(0.0000P)²+4.3304P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(11)
_refine_ls_number_reflns         4629
_refine_ls_number_parameters     248
_refine_ls_number_restraints     213
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0569
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.113
_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 0.39623(3) 0.934050(15) 0.403233(11) 0.02512(6) Uani 1 1 d . . .
Cl2 Cl 0.1994(2) 0.83485(11) 0.35309(9) 0.0501(5) Uani 1 1 d . A .
Cl1 Cl 0.2262(2) 0.99148(13) 0.49018(9) 0.0540(5) Uani 1 1 d . A .
N1 N 0.4296(6) 1.0321(3) 0.3400(2) 0.0276(11) Uani 1 1 d . A .
H1 H 0.5349 1.0484 0.3302 0.033 Uiso 1 1 d R . .
C2 C 0.2128(8) 1.0428(3) 0.2512(3) 0.0322(14) Uani 1 1 d . A .
C1 C 0.2821(7) 1.0750(4) 0.3103(3) 0.0286(12) Uani 1 1 d . . .
C3 C 0.0618(8) 1.0827(4) 0.2257(3) 0.0412(16) Uani 1 1 d . . .
H3 H 0.0128 1.0612 0.1874 0.049 Uiso 1 1 d R A .
C10 C 0.2972(9) 1.1902(4) 0.3991(4) 0.0500(16) Uani 1 1 d . . .
H10 H 0.3617 1.1446 0.4225 0.060 Uiso 1 1 d R A .
C5 C 0.0605(9) 1.1864(4) 0.3118(4) 0.0479(18) Uani 1 1 d . . .
H5 H 0.0119 1.2360 0.3307 0.057 Uiso 1 1 d R A .
C7 C 0.3024(9) 0.9694(4) 0.2151(3) 0.0390(15) Uani 1 1 d . . .
H7 H 0.3610 0.9324 0.2474 0.047 Uiso 1 1 d R A .
C6 C 0.2092(9) 1.1485(4) 0.3403(3) 0.0359(14) Uani 1 1 d . A .
C9 C 0.1775(11) 0.9126(4) 0.1748(4) 0.058(2) Uani 1 1 d . A .
H9A H 0.2389 0.8609 0.1616 0.070 Uiso 1 1 d R . .
H9B H 0.0777 0.8969 0.2011 0.070 Uiso 1 1 d R . .
H9C H 0.1379 0.9435 0.1368 0.070 Uiso 1 1 d R . .
C13 C 0.7190(9) 0.9310(4) 0.3983(3) 0.039(2) Uani 0.650(5) 1 d PGDU A 1
C14 C 0.6611(10) 0.8459(4) 0.3820(2) 0.034(3) Uani 0.650(5) 1 d PGDU A 1
C15 C 0.5795(11) 0.8094(3) 0.4380(3) 0.031(2) Uani 0.650(5) 1 d PGDU A 1
C16 C 0.5870(10) 0.8720(4) 0.4889(2) 0.039(3) Uani 0.650(5) 1 d PGDU A 1
C17 C 0.6732(10) 0.9472(3) 0.4644(3) 0.045(3) Uani 0.650(5) 1 d PGDU A 1
C4 C -0.0142(9) 1.1535(4) 0.2558(4) 0.0497(19) Uani 1 1 d . A .
H4 H -0.1161 1.1785 0.2388 0.060 Uiso 1 1 d R . .
C8 C 0.4463(10) 1.0070(5) 0.1707(4) 0.059(2) Uani 1 1 d . A .
H8A H 0.3931 1.0439 0.1384 0.071 Uiso 1 1 d R . .
H8B H 0.5279 1.0404 0.1963 0.071 Uiso 1 1 d R . .
H8C H 0.5078 0.9603 0.1495 0.071 Uiso 1 1 d R . .
C12 C 0.4304(14) 1.2576(5) 0.3745(4) 0.092(4) Uani 1 1 d . A .
H12A H 0.3705 1.3012 0.3493 0.111 Uiso 1 1 d R . .
H12B H 0.4912 1.2848 0.4102 0.111 Uiso 1 1 d R . .
H12C H 0.5138 1.2277 0.3474 0.111 Uiso 1 1 d R . .
C11 C 0.1648(12) 1.2306(6) 0.4470(4) 0.081(3) Uani 1 1 d . A .
H11A H 0.0841 1.1862 0.4610 0.098 Uiso 1 1 d R . .
H11B H 0.2246 1.2542 0.4843 0.098 Uiso 1 1 d R . .
H11C H 0.1009 1.2760 0.4253 0.098 Uiso 1 1 d R . .
C14A C 0.6144(19) 0.8187(7) 0.3909(5) 0.034(3) Uani 0.350(5) 1 d PGDU A 2
C13A C 0.6978(16) 0.8943(8) 0.3658(4) 0.039(2) Uani 0.350(5) 1 d PGDU A 2
C17A C 0.7202(18) 0.9540(6) 0.4181(6) 0.045(3) Uani 0.350(5) 1 d PGDU A 2
C16A C 0.651(2) 0.9152(7) 0.4755(5) 0.039(3) Uani 0.350(5) 1 d PGDU A 2
C15A C 0.585(2) 0.8316(7) 0.4587(5) 0.031(2) Uani 0.350(5) 1 d PGDU A 2
C23 C 0.8250(15) 0.9902(9) 0.3552(7) 0.092(5) Uani 0.650(5) 1 d PDU A 1
H23A H 0.8471 1.0440 0.3776 0.138 Uiso 0.650(5) 1 calc PR A 1
H23B H 0.7605 1.0017 0.3158 0.138 Uiso 0.650(5) 1 calc PR A 1
H23C H 0.9351 0.9629 0.3446 0.138 Uiso 0.650(5) 1 calc PR A 1
C24 C 0.6855(18) 0.8007(9) 0.3181(5) 0.087(5) Uani 0.650(5) 1 d PDU A 1
H24A H 0.7437 0.8390 0.2881 0.131 Uiso 0.650(5) 1 calc PR A 1
H24B H 0.5725 0.7845 0.3008 0.131 Uiso 0.650(5) 1 calc PR A 1
H24C H 0.7559 0.7494 0.3243 0.131 Uiso 0.650(5) 1 calc PR A 1
C25 C 0.5055(17) 0.7193(6) 0.4458(7) 0.091(5) Uani 0.650(5) 1 d PDU A 1
H25A H 0.5142 0.6887 0.4051 0.137 Uiso 0.650(5) 1 calc PR A 1
H25B H 0.3840 0.7230 0.4587 0.137 Uiso 0.650(5) 1 calc PR A 1
H25C H 0.5710 0.6886 0.4786 0.137 Uiso 0.650(5) 1 calc PR A 1
C26 C 0.5289(18) 0.8603(9) 0.5590(4) 0.088(5) Uani 0.650(5) 1 d PDU A 1
H26A H 0.5493 0.9132 0.5827 0.132 Uiso 0.650(5) 1 calc PR A 1
H26B H 0.5950 0.8139 0.5786 0.132 Uiso 0.650(5) 1 calc PR A 1
H26C H 0.4055 0.8464 0.5601 0.132 Uiso 0.650(5) 1 calc PR A 1
C27 C 0.7133(16) 1.0289(7) 0.5013(7) 0.096(5) Uani 0.650(5) 1 d PDU A 1
H27A H 0.7722 1.0694 0.4730 0.145 Uiso 0.650(5) 1 calc PR A 1
H27B H 0.7881 1.0156 0.5377 0.145 Uiso 0.650(5) 1 calc PR A 1
H27C H 0.6053 1.0542 0.5168 0.145 Uiso 0.650(5) 1 calc PR A 1
C27A C 0.809(3) 1.0411(9) 0.4122(12) 0.096(5) Uani 0.350(5) 1 d PDU A 2
H27D H 0.8094 1.0695 0.4539 0.145 Uiso 0.350(5) 1 calc PR A 2
H27E H 0.7471 1.0763 0.3811 0.145 Uiso 0.350(5) 1 calc PR A 2
H27F H 0.9288 1.0329 0.3978 0.145 Uiso 0.350(5) 1 calc PR A 2
C23A C 0.761(2) 0.9083(14) 0.2967(8) 0.092(5) Uani 0.350(5) 1 d PDU A 2
H23D H 0.7300 0.8589 0.2704 0.138 Uiso 0.350(5) 1 calc PR A 2
H23E H 0.8873 0.9151 0.2966 0.138 Uiso 0.350(5) 1 calc PR A 2
H23F H 0.7074 0.9596 0.2790 0.138 Uiso 0.350(5) 1 calc PR A 2
C26A C 0.658(3) 0.9539(14) 0.5439(7) 0.088(5) Uani 0.350(5) 1 d PDU A 2
H26D H 0.7086 1.0111 0.5419 0.132 Uiso 0.350(5) 1 calc PR A 2
H26E H 0.7298 0.9176 0.5713 0.132 Uiso 0.350(5) 1 calc PR A 2
H26F H 0.5412 0.9573 0.5616 0.132 Uiso 0.350(5) 1 calc PR A 2
C24A C 0.581(3) 0.7368(12) 0.3514(10) 0.087(5) Uani 0.350(5) 1 d PDU A 2
H24D H 0.5235 0.6943 0.3783 0.131 Uiso 0.350(5) 1 calc PR A 2
H24E H 0.6914 0.7138 0.3361 0.131 Uiso 0.350(5) 1 calc PR A 2
H24F H 0.5073 0.7505 0.3147 0.131 Uiso 0.350(5) 1 calc PR A 2
C25A C 0.502(3) 0.7654(11) 0.5048(10) 0.091(5) Uani 0.350(5) 1 d PDU A 2
H25D H 0.4689 0.7144 0.4807 0.137 Uiso 0.350(5) 1 calc PR A 2
H25E H 0.3992 0.7903 0.5247 0.137 Uiso 0.350(5) 1 calc PR A 2
H25F H 0.5855 0.7498 0.5380 0.137 Uiso 0.350(5) 1 calc PR A 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 2.003(4) . ?
Hf1 Cl2 2.3680(16) . ?
Hf1 Cl1 2.3699(17) . ?
Hf1 C15A 2.414(16) . ?
Hf1 C14A 2.438(15) . ?
Hf1 C16A 2.449(14) . ?
Hf1 C13 2.450(7) . ?
Hf1 C17 2.454(7) . ?
Hf1 C14 2.461(8) . ?
Hf1 C16 2.467(7) . ?
Hf1 C15 2.472(8) . ?
Hf1 C13A 2.488(12) . ?
N1 C1 1.434(7) . ?
N1 H1 0.8600 . ?
C2 C3 1.399(8) . ?
C2 C1 1.411(8) . ?
C2 C7 1.510(8) . ?
C1 C6 1.401(9) . ?
C3 C4 1.377(9) . ?
C3 H3 0.9299 . ?
C10 C6 1.519(9) . ?
C10 C12 1.532(10) . ?
C10 C11 1.536(10) . ?
C10 H10 0.9800 . ?
C5 C4 1.377(10) . ?
C5 C6 1.398(9) . ?
C5 H5 0.9300 . ?
C7 C9 1.530(9) . ?
C7 C8 1.533(9) . ?
C7 H7 0.9800 . ?
C9 H9A 0.9599 . ?
C9 H9B 0.9601 . ?
C9 H9C 0.9601 . ?
C13 C14 1.4200 . ?
C13 C17 1.4200 . ?
C13 C23 1.501(10) . ?
C14 C15 1.4200 . ?
C14 C24 1.495(9) . ?
C15 C16 1.4200 . ?
C15 C25 1.502(8) . ?
C16 C17 1.4200 . ?
C16 C26 1.512(8) . ?
C17 C27 1.498(10) . ?
C4 H4 0.9301 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9599 . ?
C8 H8C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C11 H11A 0.9599 . ?
C11 H11B 0.9601 . ?
C11 H11C 0.9600 . ?
C14A C13A 1.4200 . ?
C14A C15A 1.4200 . ?
C14A C24A 1.518(10) . ?
C13A C17A 1.4200 . ?
C13A C23A 1.513(13) . ?
C17A C16A 1.4200 . ?
C17A C27A 1.504(10) . ?
C16A C15A 1.4200 . ?
C16A C26A 1.525(11) . ?
C15A C25A 1.525(10) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27A H27D 0.9600 . ?
C27A H27E 0.9600 . ?
C27A H27F 0.9600 . ?
C23A H23D 0.9600 . ?
C23A H23E 0.9600 . ?
C23A H23F 0.9600 . ?
C26A H26D 0.9600 . ?
C26A H26E 0.9600 . ?
C26A H26F 0.9600 . ?
C24A H24D 0.9600 . ?
C24A H24E 0.9600 . ?
C24A H24F 0.9600 . ?
C25A H25D 0.9600 . ?
C25A H25E 0.9600 . ?
C25A H25F 0.9600 . ?

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 Hf1 Cl2 106.43(13) . . ?
N1 Hf1 Cl1 105.98(14) . . ?
Cl2 Hf1 Cl1 102.90(7) . . ?
N1 Hf1 C15A 136.1(3) . . ?
Cl2 Hf1 C15A 99.1(3) . . ?
Cl1 Hf1 C15A 102.2(3) . . ?
N1 Hf1 C14A 113.2(3) . . ?
Cl2 Hf1 C14A 85.1(2) . . ?
Cl1 Hf1 C14A 135.9(3) . . ?
C15A Hf1 C14A 34.0(2) . . ?
N1 Hf1 C16A 112.4(3) . . ?
Cl2 Hf1 C16A 133.1(3) . . ?
Cl1 Hf1 C16A 91.0(3) . . ?
C15A Hf1 C16A 33.95(19) . . ?
C14A Hf1 C16A 56.1(3) . . ?
N1 Hf1 C13 82.02(19) . . ?
Cl2 Hf1 C13 126.83(16) . . ?
Cl1 Hf1 C13 125.56(16) . . ?
C15A Hf1 C13 54.1(3) . . ?
C14A Hf1 C13 45.9(3) . . ?
C16A Hf1 C13 40.2(3) . . ?
N1 Hf1 C17 99.24(19) . . ?
Cl2 Hf1 C17 144.48(13) . . ?
Cl1 Hf1 C17 92.92(15) . . ?
C15A Hf1 C17 46.0(3) . . ?
C14A Hf1 C17 62.1(3) . . ?
C16A Hf1 C17 13.3(3) . . ?
C13 Hf1 C17 33.67(9) . . ?
N1 Hf1 C14 101.33(19) . . ?
Cl2 Hf1 C14 94.77(15) . . ?
Cl1 Hf1 C14 141.41(14) . . ?
C15A Hf1 C14 40.5(3) . . ?
C14A Hf1 C14 13.5(3) . . ?
C16A Hf1 C14 53.1(3) . . ?
C13 Hf1 C14 33.61(9) . . ?
C17 Hf1 C14 55.74(11) . . ?
N1 Hf1 C16 132.6(2) . . ?
Cl2 Hf1 C16 115.43(15) . . ?
Cl1 Hf1 C16 85.84(13) . . ?
C15A Hf1 C16 20.7(3) . . ?
C14A Hf1 C16 52.8(3) . . ?
C16A Hf1 C16 20.3(3) . . ?
C13 Hf1 C16 55.71(11) . . ?
C17 Hf1 C16 33.54(9) . . ?
C14 Hf1 C16 55.57(12) . . ?
N1 Hf1 C15 134.30(19) . . ?
Cl2 Hf1 C15 88.89(15) . . ?
Cl1 Hf1 C15 112.17(14) . . ?
C15A Hf1 C15 12.7(3) . . ?
C14A Hf1 C15 23.8(3) . . ?
C16A Hf1 C15 44.9(2) . . ?
C13 Hf1 C15 55.66(12) . . ?
C17 Hf1 C15 55.61(11) . . ?
C14 Hf1 C15 33.46(10) . . ?
C16 Hf1 C15 33.42(9) . . ?
N1 Hf1 C13A 82.5(3) . . ?
Cl2 Hf1 C13A 106.7(3) . . ?
Cl1 Hf1 C13A 145.4(2) . . ?
C15A Hf1 C13A 55.9(2) . . ?
C14A Hf1 C13A 33.49(16) . . ?
C16A Hf1 C13A 55.5(2) . . ?
C13 Hf1 C13A 20.7(3) . . ?
C17 Hf1 C13A 52.5(3) . . ?
C14 Hf1 C13A 20.0(3) . . ?
C16 Hf1 C13A 65.5(3) . . ?
C15 Hf1 C13A 51.8(3) . . ?
C1 N1 Hf1 121.4(3) . . ?
C1 N1 H1 119.4 . . ?
Hf1 N1 H1 119.1 . . ?
C3 C2 C1 118.1(5) . . ?
C3 C2 C7 120.8(6) . . ?
C1 C2 C7 121.0(5) . . ?
C6 C1 C2 120.9(6) . . ?
C6 C1 N1 119.5(5) . . ?
C2 C1 N1 119.6(5) . . ?
C4 C3 C2 121.5(6) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.1 . . ?
C6 C10 C12 108.3(6) . . ?
C6 C10 C11 113.0(6) . . ?
C12 C10 C11 111.6(7) . . ?
C6 C10 H10 107.8 . . ?
C12 C10 H10 108.4 . . ?
C11 C10 H10 107.6 . . ?
C4 C5 C6 121.8(6) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C2 C7 C9 114.3(6) . . ?
C2 C7 C8 109.2(5) . . ?
C9 C7 C8 109.6(6) . . ?
C2 C7 H7 107.9 . . ?
C9 C7 H7 108.2 . . ?
C8 C7 H7 107.3 . . ?
C5 C6 C1 118.1(6) . . ?
C5 C6 C10 120.7(6) . . ?
C1 C6 C10 121.0(6) . . ?
C7 C9 H9A 108.9 . . ?
C7 C9 H9B 109.1 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 110.4 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C14 C13 C17 108.0 . . ?
C14 C13 C23 125.9(6) . . ?
C17 C13 C23 125.9(6) . . ?
C14 C13 Hf1 73.6(3) . . ?
C17 C13 Hf1 73.3(3) . . ?
C23 C13 Hf1 123.2(6) . . ?
C13 C14 C15 108.0 . . ?
C13 C14 C24 126.6(6) . . ?
C15 C14 C24 125.4(6) . . ?
C13 C14 Hf1 72.8(3) . . ?
C15 C14 Hf1 73.7(3) . . ?
C24 C14 Hf1 120.8(6) . . ?
C14 C15 C16 108.0 . . ?
C14 C15 C25 127.8(6) . . ?
C16 C15 C25 124.1(6) . . ?
C14 C15 Hf1 72.9(3) . . ?
C16 C15 Hf1 73.1(3) . . ?
C25 C15 Hf1 122.3(7) . . ?
C17 C16 C15 108.0 . . ?
C17 C16 C26 124.5(6) . . ?
C15 C16 C26 127.3(6) . . ?
C17 C16 Hf1 72.7(3) . . ?
C15 C16 Hf1 73.5(3) . . ?
C26 C16 Hf1 123.4(6) . . ?
C16 C17 C13 108.0 . . ?
C16 C17 C27 126.6(6) . . ?
C13 C17 C27 125.3(6) . . ?
C16 C17 Hf1 73.8(3) . . ?
C13 C17 Hf1 73.0(3) . . ?
C27 C17 Hf1 120.0(6) . . ?
C3 C4 C5 119.5(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.1 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.4 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C12 H12A 109.7 . . ?
C10 C12 H12B 111.1 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 107.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C11 H11A 108.7 . . ?
C10 C11 H11B 110.7 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.1 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13A C14A C15A 108.0 . . ?
C13A C14A C24A 124.0(8) . . ?
C15A C14A C24A 127.7(8) . . ?
C13A C14A Hf1 75.2(5) . . ?
C15A C14A Hf1 72.0(5) . . ?
C24A C14A Hf1 123.0(10) . . ?
C17A C13A C14A 108.0 . . ?
C17A C13A C23A 125.3(7) . . ?
C14A C13A C23A 126.7(7) . . ?
C17A C13A Hf1 73.7(5) . . ?
C14A C13A Hf1 71.3(5) . . ?
C23A C13A Hf1 123.2(9) . . ?
C16A C17A C13A 108.0 . . ?
C16A C17A C27A 127.4(9) . . ?
C13A C17A C27A 124.6(9) . . ?
C16A C17A Hf1 71.6(5) . . ?
C13A C17A Hf1 73.2(5) . . ?
C27A C17A Hf1 122.9(10) . . ?
C15A C16A C17A 108.0 . . ?
C15A C16A C26A 126.1(8) . . ?
C17A C16A C26A 125.7(8) . . ?
C15A C16A Hf1 71.7(6) . . ?
C17A C16A Hf1 75.1(5) . . ?
C26A C16A Hf1 122.7(10) . . ?
C16A C15A C14A 108.0 . . ?
C16A C15A C25A 126.7(7) . . ?
C14A C15A C25A 125.3(7) . . ?
C16A C15A Hf1 74.4(5) . . ?
C14A C15A Hf1 73.9(5) . . ?
C25A C15A Hf1 118.8(11) . . ?
C13 C23 H23A 109.5 . . ?
C13 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C13 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 C24 H24A 109.5 . . ?
C14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C15 C25 H25A 109.5 . . ?
C15 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C15 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C26 H26A 109.5 . . ?
C16 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C16 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C17 C27 H27A 109.5 . . ?
C17 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C17 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C17A C27A H27D 109.5 . . ?
C17A C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C17A C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C13A C23A H23D 109.5 . . ?
C13A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C13A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C16A C26A H26D 109.5 . . ?
C16A C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
C16A C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C14A C24A H24D 109.5 . . ?
C14A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C14A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C15A C25A H25D 109.5 . . ?
C15A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
C15A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.80
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.108
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1044553'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H28 Cl2 N2 Ti'
_chemical_formula_sum            'C19 H28 Cl2 N2 Ti'
_chemical_formula_weight         403.23

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'
Cl Cl 0.1484 0.1585 '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'
Ti Ti 0.2776 0.4457 '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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   24.5850(16)
_cell_length_b                   9.2920(7)
_cell_length_c                   17.769(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.609(7)
_cell_angle_gamma                90
_cell_volume                     4046.1(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    32497
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    0.690
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.048
0 0 1 0.093
0 1 0 0.113
0 -1 0 0.129
1 0 0 0.067
-1 0 0 0.074
-1 -1 0 0.103
0 -1 -1 0.101


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32411
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9102
_reflns_number_gt                5985
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0247P)²+4.9316P] where P=(Fo²+2Fc²)/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         9102
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1152
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_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 0.10487(2) -0.23264(6) 0.12694(3) 0.02044(13) Uani 1 1 d . . .
Ti2 Ti 0.39010(2) 0.25097(6) 0.37615(3) 0.01893(13) Uani 1 1 d . . .
Cl4 Cl 0.38609(3) 0.46140(9) 0.44128(5) 0.0334(2) Uani 1 1 d . . .
Cl3 Cl 0.38951(3) 0.33456(10) 0.25664(5) 0.0344(2) Uani 1 1 d . . .
Cl1 Cl 0.10421(3) -0.26784(10) 0.25371(5) 0.0347(2) Uani 1 1 d . . .
Cl2 Cl 0.11229(4) -0.46122(9) 0.08471(6) 0.0379(2) Uani 1 1 d . . .
N2 N 0.32095(10) 0.1579(3) 0.37889(14) 0.0201(5) Uani 1 1 d . . .
H2 H 0.3183 0.0590 0.3912 0.024 Uiso 1 1 d R . .
N1 N 0.17418(10) -0.1459(3) 0.11713(14) 0.0219(6) Uani 1 1 d . . .
H1 H 0.1802 -0.0455 0.1041 0.026 Uiso 1 1 d R . .
C20 C 0.26836(12) 0.2061(3) 0.35344(16) 0.0175(6) Uani 1 1 d . . .
N3 N 0.23558(11) 0.1247(3) 0.09372(15) 0.0254(6) Uani 1 1 d . . .
C21 C 0.22674(13) 0.1040(3) 0.33435(18) 0.0232(7) Uani 1 1 d . . .
C1 C 0.22706(12) -0.1988(3) 0.13442(17) 0.0193(6) Uani 1 1 d . . .
C34 C 0.38882(15) -0.0254(4) 0.5067(2) 0.0452(10) Uani 1 1 d . . .
H34A H 0.3631 -0.0869 0.4788 0.054 Uiso 1 1 d R . .
H34B H 0.3696 0.0420 0.5358 0.054 Uiso 1 1 d R . .
H34C H 0.4127 -0.0826 0.5401 0.054 Uiso 1 1 d R . .
N4 N 0.26343(11) -0.1108(3) 0.40435(15) 0.0258(6) Uani 1 1 d . . .
C9 C 0.26719(19) 0.1782(4) 0.1602(2) 0.0482(11) Uani 1 1 d . . .
H9A H 0.3014 0.2149 0.1460 0.058 Uiso 1 1 d R . .
H9B H 0.2737 0.1015 0.1960 0.058 Uiso 1 1 d R . .
H9C H 0.2474 0.2540 0.1826 0.058 Uiso 1 1 d R . .
C25 C 0.25617(12) 0.3519(3) 0.34702(17) 0.0198(6) Uani 1 1 d . . .
H25 H 0.2832 0.4193 0.3600 0.024 Uiso 1 1 d R . .
C13 C 0.06734(13) -0.0023(3) 0.0988(2) 0.0267(8) Uani 1 1 d . . .
C7 C 0.26458(13) 0.0076(3) 0.05904(18) 0.0241(7) Uani 1 1 d . . .
H7A H 0.3001 0.0419 0.0471 0.029 Uiso 1 1 d R . .
H7B H 0.2443 -0.0192 0.0120 0.029 Uiso 1 1 d R . .
C11 C 0.01220(13) -0.2017(3) 0.08741(19) 0.0259(7) Uani 1 1 d . . .
C26 C 0.23797(13) -0.0551(3) 0.33302(18) 0.0256(7) Uani 1 1 d . . .
H26A H 0.2038 -0.1054 0.3211 0.031 Uiso 1 1 d R . .
H26B H 0.2616 -0.0755 0.2931 0.031 Uiso 1 1 d R . .
C2 C 0.27200(12) -0.1244(3) 0.10874(17) 0.0213(7) Uani 1 1 d . . .
C4 C 0.33248(14) -0.3054(4) 0.1674(2) 0.0322(8) Uani 1 1 d . . .
H4 H 0.3676 -0.3404 0.1786 0.039 Uiso 1 1 d R . .
C32 C 0.46747(13) 0.1170(4) 0.3503(2) 0.0303(8) Uani 1 1 d . . .
C14 C 0.07536(13) -0.0698(3) 0.02949(19) 0.0260(7) Uani 1 1 d . . .
C10 C 0.04121(13) -0.1928(3) 0.02219(19) 0.0257(7) Uani 1 1 d . . .
C8 C 0.22684(14) 0.2432(3) 0.04054(19) 0.0317(8) Uani 1 1 d . . .
H8A H 0.2072 0.3191 0.0631 0.038 Uiso 1 1 d R . .
H8B H 0.2061 0.2095 -0.0041 0.038 Uiso 1 1 d R . .
H8C H 0.2615 0.2789 0.0273 0.038 Uiso 1 1 d R . .
C15 C 0.03540(16) -0.2877(4) -0.0461(2) 0.0409(9) Uani 1 1 d . . .
H15A H 0.0105 -0.3647 -0.0377 0.049 Uiso 1 1 d R . .
H15B H 0.0704 -0.3269 -0.0553 0.049 Uiso 1 1 d R . .
H15C H 0.0215 -0.2322 -0.0890 0.049 Uiso 1 1 d R . .
C3 C 0.32397(13) -0.1792(4) 0.12642(19) 0.0295(8) Uani 1 1 d . . .
H3 H 0.3539 -0.1300 0.1105 0.035 Uiso 1 1 d R . .
C12 C 0.02819(13) -0.0842(4) 0.13510(19) 0.0281(8) Uani 1 1 d . . .
C22 C 0.17493(14) 0.1547(4) 0.3108(2) 0.0344(8) Uani 1 1 d . . .
H22 H 0.1471 0.0886 0.2990 0.041 Uiso 1 1 d R . .
C24 C 0.20442(13) 0.3983(3) 0.32181(18) 0.0240(7) Uani 1 1 d . . .
H24 H 0.1972 0.4962 0.3167 0.029 Uiso 1 1 d R . .
C19 C 0.10991(15) -0.0167(4) -0.0304(2) 0.0394(9) Uani 1 1 d . . .
H19A H 0.1268 -0.0968 -0.0535 0.047 Uiso 1 1 d R . .
H19B H 0.1376 0.0464 -0.0082 0.047 Uiso 1 1 d R . .
H19C H 0.0874 0.0348 -0.0681 0.047 Uiso 1 1 d R . .
C23 C 0.16348(14) 0.2998(4) 0.3045(2) 0.0335(8) Uani 1 1 d . . .
H23 H 0.1285 0.3306 0.2883 0.040 Uiso 1 1 d R . .
C38 C 0.40424(15) -0.1051(4) 0.3336(2) 0.0439(10) Uani 1 1 d . . .
H38A H 0.4314 -0.1782 0.3290 0.053 Uiso 1 1 d R . .
H38B H 0.3906 -0.0735 0.2842 0.053 Uiso 1 1 d R . .
H38C H 0.3748 -0.1437 0.3597 0.053 Uiso 1 1 d R . .
C6 C 0.23621(13) -0.3261(3) 0.17504(18) 0.0236(7) Uani 1 1 d . . .
H6 H 0.2066 -0.3758 0.1917 0.028 Uiso 1 1 d R . .
C29 C 0.42212(13) 0.0548(3) 0.4528(2) 0.0283(8) Uani 1 1 d . . .
C33 C 0.42925(13) 0.0194(3) 0.3771(2) 0.0291(8) Uani 1 1 d . . .
C30 C 0.45560(14) 0.1750(4) 0.4731(2) 0.0306(8) Uani 1 1 d . . .
C31 C 0.48297(13) 0.2140(3) 0.4095(2) 0.0296(8) Uani 1 1 d . . .
C18 C 0.09311(15) 0.1366(4) 0.1267(2) 0.0423(10) Uani 1 1 d . . .
H18A H 0.1316 0.1228 0.1377 0.051 Uiso 1 1 d R . .
H18B H 0.0771 0.1666 0.1717 0.051 Uiso 1 1 d R . .
H18C H 0.0870 0.2092 0.0885 0.051 Uiso 1 1 d R . .
C16 C -0.02818(14) -0.3163(4) 0.1036(2) 0.0388(9) Uani 1 1 d . . .
H16A H -0.0513 -0.3367 0.0587 0.047 Uiso 1 1 d R . .
H16B H -0.0501 -0.2832 0.1425 0.047 Uiso 1 1 d R . .
H16C H -0.0091 -0.4021 0.1203 0.047 Uiso 1 1 d R . .
C5 C 0.28827(14) -0.3793(4) 0.19112(19) 0.0289(8) Uani 1 1 d . . .
H5 H 0.2935 -0.4646 0.2181 0.035 Uiso 1 1 d R . .
C28 C 0.27681(15) -0.2627(3) 0.3967(2) 0.0325(8) Uani 1 1 d . . .
H28A H 0.2973 -0.2954 0.4418 0.039 Uiso 1 1 d R . .
H28B H 0.2981 -0.2754 0.3542 0.039 Uiso 1 1 d R . .
H28C H 0.2437 -0.3173 0.3891 0.039 Uiso 1 1 d R . .
C27 C 0.22725(19) -0.0946(4) 0.4647(2) 0.0472(11) Uani 1 1 d . . .
H27A H 0.1948 -0.1506 0.4535 0.057 Uiso 1 1 d R . .
H27B H 0.2176 0.0049 0.4695 0.057 Uiso 1 1 d R . .
H27C H 0.2457 -0.1275 0.5112 0.057 Uiso 1 1 d R . .
C17 C 0.00443(16) -0.0471(4) 0.2076(2) 0.0449(10) Uani 1 1 d . . .
H17A H 0.0320 -0.0021 0.2411 0.054 Uiso 1 1 d R . .
H17B H -0.0082 -0.1331 0.2307 0.054 Uiso 1 1 d R . .
H17C H -0.0256 0.0180 0.1977 0.054 Uiso 1 1 d R . .
C35 C 0.46283(18) 0.2405(5) 0.5504(2) 0.0511(11) Uani 1 1 d . . .
H35A H 0.4279 0.2669 0.5666 0.061 Uiso 1 1 d R . .
H35B H 0.4853 0.3247 0.5488 0.061 Uiso 1 1 d R . .
H35C H 0.4800 0.1723 0.5853 0.061 Uiso 1 1 d R . .
C36 C 0.52207(14) 0.3384(4) 0.4047(3) 0.0470(11) Uani 1 1 d . . .
H36A H 0.5488 0.3149 0.3702 0.056 Uiso 1 1 d R . .
H36B H 0.5400 0.3570 0.4537 0.056 Uiso 1 1 d R . .
H36C H 0.5022 0.4225 0.3871 0.056 Uiso 1 1 d R . .
C37 C 0.49023(17) 0.1110(5) 0.2749(2) 0.0500(11) Uani 1 1 d . . .
H37A H 0.5012 0.2058 0.2609 0.060 Uiso 1 1 d R . .
H37B H 0.4629 0.0755 0.2379 0.060 Uiso 1 1 d R . .
H37C H 0.5213 0.0480 0.2774 0.060 Uiso 1 1 d 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
Ti1 N1 1.906(3) . ?
Ti1 Cl2 2.2648(10) . ?
Ti1 Cl1 2.2775(10) . ?
Ti1 C11 2.347(3) . ?
Ti1 C12 2.349(3) . ?
Ti1 C10 2.363(3) . ?
Ti1 C13 2.368(3) . ?
Ti1 C14 2.369(3) . ?
Ti2 N2 1.912(2) . ?
Ti2 Cl3 2.2601(10) . ?
Ti2 Cl4 2.2783(10) . ?
Ti2 C31 2.338(3) . ?
Ti2 C32 2.349(3) . ?
Ti2 C33 2.357(3) . ?
Ti2 C30 2.370(3) . ?
Ti2 C29 2.372(3) . ?
N2 C20 1.408(4) . ?
N2 H2 0.9481 . ?
N1 C1 1.401(4) . ?
N1 H1 0.9750 . ?
C20 C25 1.390(4) . ?
C20 C21 1.417(4) . ?
N3 C9 1.449(4) . ?
N3 C8 1.456(4) . ?
N3 C7 1.463(4) . ?
C21 C22 1.391(5) . ?
C21 C26 1.505(4) . ?
C1 C6 1.394(4) . ?
C1 C2 1.410(4) . ?
C34 C29 1.507(5) . ?
C34 H34A 0.9602 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9598 . ?
N4 C27 1.455(4) . ?
N4 C28 1.458(4) . ?
N4 C26 1.462(4) . ?
C9 H9A 0.9602 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C25 C24 1.383(4) . ?
C25 H25 0.9297 . ?
C13 C14 1.409(5) . ?
C13 C12 1.423(5) . ?
C13 C18 1.504(4) . ?
C7 C2 1.514(4) . ?
C7 H7A 0.9699 . ?
C7 H7B 0.9699 . ?
C11 C10 1.411(5) . ?
C11 C12 1.418(5) . ?
C11 C16 1.499(5) . ?
C26 H26A 0.9694 . ?
C26 H26B 0.9700 . ?
C2 C3 1.388(4) . ?
C4 C5 1.380(5) . ?
C4 C3 1.388(5) . ?
C4 H4 0.9300 . ?
C32 C31 1.414(5) . ?
C32 C33 1.416(5) . ?
C32 C37 1.494(5) . ?
C14 C10 1.418(4) . ?
C14 C19 1.498(5) . ?
C10 C15 1.497(5) . ?
C8 H8A 0.9601 . ?
C8 H8B 0.9601 . ?
C8 H8C 0.9600 . ?
C15 H15A 0.9603 . ?
C15 H15B 0.9599 . ?
C15 H15C 0.9601 . ?
C3 H3 0.9300 . ?
C12 C17 1.497(5) . ?
C22 C23 1.380(5) . ?
C22 H22 0.9300 . ?
C24 C23 1.377(4) . ?
C24 H24 0.9300 . ?
C19 H19A 0.9602 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9601 . ?
C23 H23 0.9301 . ?
C38 C33 1.495(5) . ?
C38 H38A 0.9601 . ?
C38 H38B 0.9601 . ?
C38 H38C 0.9598 . ?
C6 C5 1.380(4) . ?
C6 H6 0.9299 . ?
C29 C33 1.409(5) . ?
C29 C30 1.418(5) . ?
C30 C31 1.409(5) . ?
C30 C35 1.499(5) . ?
C31 C36 1.510(5) . ?
C18 H18A 0.9598 . ?
C18 H18B 0.9599 . ?
C18 H18C 0.9600 . ?
C16 H16A 0.9599 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C5 H5 0.9299 . ?
C28 H28A 0.9599 . ?
C28 H28B 0.9601 . ?
C28 H28C 0.9602 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9601 . ?
C27 H27C 0.9600 . ?
C17 H17A 0.9601 . ?
C17 H17B 0.9601 . ?
C17 H17C 0.9603 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9601 . ?
C36 H36A 0.9601 . ?
C36 H36B 0.9599 . ?
C36 H36C 0.9601 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?

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 Ti1 Cl2 105.67(8) . . ?
N1 Ti1 Cl1 103.22(8) . . ?
Cl2 Ti1 Cl1 101.54(4) . . ?
N1 Ti1 C11 140.74(11) . . ?
Cl2 Ti1 C11 96.76(8) . . ?
Cl1 Ti1 C11 103.28(9) . . ?
N1 Ti1 C12 119.02(11) . . ?
Cl2 Ti1 C12 131.09(9) . . ?
Cl1 Ti1 C12 87.35(9) . . ?
C11 Ti1 C12 35.14(11) . . ?
N1 Ti1 C10 113.72(11) . . ?
Cl2 Ti1 C10 87.23(8) . . ?
Cl1 Ti1 C10 138.13(9) . . ?
C11 Ti1 C10 34.87(11) . . ?
C12 Ti1 C10 58.18(11) . . ?
N1 Ti1 C13 86.23(11) . . ?
Cl2 Ti1 C13 144.87(9) . . ?
Cl1 Ti1 C13 107.78(9) . . ?
C11 Ti1 C13 58.25(11) . . ?
C12 Ti1 C13 35.09(11) . . ?
C10 Ti1 C13 57.98(11) . . ?
N1 Ti1 C14 83.48(11) . . ?
Cl2 Ti1 C14 112.64(9) . . ?
Cl1 Ti1 C14 142.05(9) . . ?
C11 Ti1 C14 58.00(11) . . ?
C12 Ti1 C14 58.00(12) . . ?
C10 Ti1 C14 34.87(11) . . ?
C13 Ti1 C14 34.61(11) . . ?
N2 Ti2 Cl3 103.94(8) . . ?
N2 Ti2 Cl4 107.48(8) . . ?
Cl3 Ti2 Cl4 100.67(4) . . ?
N2 Ti2 C31 141.22(11) . . ?
Cl3 Ti2 C31 102.78(9) . . ?
Cl4 Ti2 C31 94.51(9) . . ?
N2 Ti2 C32 120.06(11) . . ?
Cl3 Ti2 C32 86.71(9) . . ?
Cl4 Ti2 C32 128.53(9) . . ?
C31 Ti2 C32 35.12(12) . . ?
N2 Ti2 C33 87.14(11) . . ?
Cl3 Ti2 C33 106.99(9) . . ?
Cl4 Ti2 C33 144.52(9) . . ?
C31 Ti2 C33 58.27(11) . . ?
C32 Ti2 C33 35.02(12) . . ?
N2 Ti2 C30 113.61(12) . . ?
Cl3 Ti2 C30 137.59(9) . . ?
Cl4 Ti2 C30 86.60(9) . . ?
C31 Ti2 C30 34.82(12) . . ?
C32 Ti2 C30 58.04(12) . . ?
C33 Ti2 C30 57.98(12) . . ?
N2 Ti2 C29 83.82(11) . . ?
Cl3 Ti2 C29 141.28(9) . . ?
Cl4 Ti2 C29 113.21(9) . . ?
C31 Ti2 C29 57.94(11) . . ?
C32 Ti2 C29 57.87(12) . . ?
C33 Ti2 C29 34.66(12) . . ?
C30 Ti2 C29 34.80(11) . . ?
C20 N2 Ti2 130.0(2) . . ?
C20 N2 H2 107.8 . . ?
Ti2 N2 H2 121.4 . . ?
C1 N1 Ti1 130.7(2) . . ?
C1 N1 H1 103.4 . . ?
Ti1 N1 H1 125.5 . . ?
C25 C20 N2 121.5(3) . . ?
C25 C20 C21 119.1(3) . . ?
N2 C20 C21 119.4(3) . . ?
C9 N3 C8 108.1(3) . . ?
C9 N3 C7 110.6(3) . . ?
C8 N3 C7 109.9(2) . . ?
C22 C21 C20 118.1(3) . . ?
C22 C21 C26 119.5(3) . . ?
C20 C21 C26 122.2(3) . . ?
C6 C1 N1 121.3(3) . . ?
C6 C1 C2 119.1(3) . . ?
N1 C1 C2 119.6(3) . . ?
C29 C34 H34A 109.5 . . ?
C29 C34 H34B 109.6 . . ?
H34A C34 H34B 109.5 . . ?
C29 C34 H34C 109.3 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C27 N4 C28 108.9(3) . . ?
C27 N4 C26 111.0(3) . . ?
C28 N4 C26 110.3(3) . . ?
N3 C9 H9A 109.4 . . ?
N3 C9 H9B 109.6 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C24 C25 C20 121.1(3) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.4 . . ?
C14 C13 C12 107.8(3) . . ?
C14 C13 C18 125.8(3) . . ?
C12 C13 C18 126.3(3) . . ?
C14 C13 Ti1 72.71(17) . . ?
C12 C13 Ti1 71.72(18) . . ?
C18 C13 Ti1 124.0(2) . . ?
N3 C7 C2 113.4(3) . . ?
N3 C7 H7A 109.1 . . ?
C2 C7 H7A 109.0 . . ?
N3 C7 H7B 108.6 . . ?
C2 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
C10 C11 C12 108.2(3) . . ?
C10 C11 C16 125.8(3) . . ?
C12 C11 C16 126.0(3) . . ?
C10 C11 Ti1 73.17(18) . . ?
C12 C11 Ti1 72.51(18) . . ?
C16 C11 Ti1 119.8(2) . . ?
N4 C26 C21 113.6(3) . . ?
N4 C26 H26A 108.8 . . ?
C21 C26 H26A 108.7 . . ?
N4 C26 H26B 109.0 . . ?
C21 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C3 C2 C1 118.5(3) . . ?
C3 C2 C7 119.7(3) . . ?
C1 C2 C7 121.7(3) . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.4 . . ?
C31 C32 C33 107.8(3) . . ?
C31 C32 C37 126.4(3) . . ?
C33 C32 C37 125.7(3) . . ?
C31 C32 Ti2 72.00(18) . . ?
C33 C32 Ti2 72.80(18) . . ?
C37 C32 Ti2 124.2(2) . . ?
C13 C14 C10 108.4(3) . . ?
C13 C14 C19 126.9(3) . . ?
C10 C14 C19 124.5(3) . . ?
C13 C14 Ti1 72.68(18) . . ?
C10 C14 Ti1 72.32(18) . . ?
C19 C14 Ti1 124.9(2) . . ?
C11 C10 C14 107.9(3) . . ?
C11 C10 C15 127.5(3) . . ?
C14 C10 C15 124.5(3) . . ?
C11 C10 Ti1 71.97(19) . . ?
C14 C10 Ti1 72.80(18) . . ?
C15 C10 Ti1 124.0(2) . . ?
N3 C8 H8A 109.7 . . ?
N3 C8 H8B 109.3 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.4 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.4 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C3 C2 121.7(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.2 . . ?
C11 C12 C13 107.8(3) . . ?
C11 C12 C17 125.7(3) . . ?
C13 C12 C17 126.3(3) . . ?
C11 C12 Ti1 72.35(18) . . ?
C13 C12 Ti1 73.18(18) . . ?
C17 C12 Ti1 124.0(2) . . ?
C23 C22 C21 122.1(3) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 H22 118.9 . . ?
C23 C24 C25 120.1(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 120.0 . . ?
C14 C19 H19A 109.7 . . ?
C14 C19 H19B 109.4 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.4 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C33 C38 H38A 109.4 . . ?
C33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C5 C6 C1 121.3(3) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.3 . . ?
C33 C29 C30 108.3(3) . . ?
C33 C29 C34 127.4(3) . . ?
C30 C29 C34 124.1(3) . . ?
C33 C29 Ti2 72.10(18) . . ?
C30 C29 Ti2 72.52(18) . . ?
C34 C29 Ti2 125.0(2) . . ?
C29 C33 C32 107.9(3) . . ?
C29 C33 C38 126.6(3) . . ?
C32 C33 C38 125.3(3) . . ?
C29 C33 Ti2 73.23(18) . . ?
C32 C33 Ti2 72.18(18) . . ?
C38 C33 Ti2 123.5(2) . . ?
C31 C30 C29 107.6(3) . . ?
C31 C30 C35 127.0(3) . . ?
C29 C30 C35 125.3(3) . . ?
C31 C30 Ti2 71.35(19) . . ?
C29 C30 Ti2 72.68(18) . . ?
C35 C30 Ti2 124.7(2) . . ?
C30 C31 C32 108.4(3) . . ?
C30 C31 C36 126.1(3) . . ?
C32 C31 C36 125.5(4) . . ?
C30 C31 Ti2 73.83(19) . . ?
C32 C31 Ti2 72.88(18) . . ?
C36 C31 Ti2 119.1(2) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.4 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C16 H16A 109.7 . . ?
C11 C16 H16B 109.2 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N4 C28 H28A 109.7 . . ?
N4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N4 C28 H28C 109.3 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C27 H27A 109.8 . . ?
N4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N4 C27 H27C 109.1 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C12 C17 H17A 109.2 . . ?
C12 C17 H17B 109.7 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C30 C35 H35A 109.6 . . ?
C30 C35 H35B 109.2 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 109.7 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C31 C36 H36C 109.4 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C37 H37A 109.3 . . ?
C32 C37 H37B 109.6 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.6 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 N4 0.95 2.10 2.922(3) 144.0 .
N1 H1 N3 0.98 2.10 2.978(4) 148.4 .

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.078
####################################################################### 
# 
# 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_8prime
_database_code_depnum_ccdc_archive 'CCDC 1044554'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H28 Cl2 N2 Zr'
_chemical_formula_sum            'C19 H28 Cl2 N2 Zr'
_chemical_formula_weight         446.55

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1900(4)
_cell_length_b                   9.7300(5)
_cell_length_c                   14.4511(9)
_cell_angle_alpha                88.286(4)
_cell_angle_beta                 88.435(5)
_cell_angle_gamma                63.754(4)
_cell_volume                     1158.32(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    22110
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             460
_exptl_absorpt_coefficient_mu    0.708
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.067
0 -1 0 0.135
1 0 0 0.158
-1 0 0 0.172
0 0 -1 0.086
0 0 1 0.119
-1 0 1 0.131
-1 -1 0 0.211
1 1 0 0.193


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21916
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5233
_reflns_number_gt                4750
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences 


 All Cp* carbon and hydrogen atoms were split to two positions
 DFIX 1.520 0.020 instruction is used to correct the C-C distances 
 between the carbon atoms of Cp ring and appropriate methyls
 SADI 0.02, DELU 0.010  0.010 and SIMU 0.040 0.080 1.700 instructions 
 were used for the same pairs of carbon atoms.
 EADP instruction was used for neighbouring carbon atoms.
 ISOR 0.100 instruction was used for all the split carbon atoms
;


_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)+(0.0351P)²+2.1314P] where P=(Fo²+2Fc²)/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         5233
_refine_ls_number_parameters     232
_refine_ls_number_restraints     197
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.472
_refine_ls_shift/su_max          0.005
_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_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.64743(3) 0.26777(2) 0.29669(2) 0.01607(7) Uani 1 1 d . . . . .
Cl2 Cl 0.43537(8) 0.22009(8) 0.37717(5) 0.03282(16) Uani 1 1 d . . . . .
Cl1 Cl 0.74419(8) 0.12858(8) 0.15293(4) 0.03175(15) Uani 1 1 d . . . . .
N2 N 0.4055(2) 0.4101(2) 0.19622(13) 0.0180(4) Uani 1 1 d . . . . .
N1 N 0.6221(3) 0.4911(2) 0.28765(15) 0.0250(4) Uani 1 1 d . . . . .
H1 H 0.6711 0.5076 0.3346 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4694(3) 0.6295(3) 0.15182(17) 0.0218(5) Uani 1 1 d . . . . .
C8 C 0.2627(3) 0.5238(3) 0.24743(17) 0.0249(5) Uani 1 1 d . . . . .
H8A H 0.1782 0.5857 0.2034 0.037 Uiso 1 1 calc R U . . .
H8B H 0.2952 0.5907 0.2819 0.037 Uiso 1 1 calc R U . . .
H8C H 0.2206 0.4701 0.2907 0.037 Uiso 1 1 calc R U . . .
C7 C 0.4500(3) 0.4933(3) 0.12039(16) 0.0209(5) Uani 1 1 d . . . . .
H7A H 0.3650 0.5277 0.0728 0.025 Uiso 1 1 calc R U . . .
H7B H 0.5530 0.4209 0.0909 0.025 Uiso 1 1 calc R U . . .
C5 C 0.4071(3) 0.7638(3) 0.09771(19) 0.0296(5) Uani 1 1 d . . . . .
H5 H 0.3476 0.7686 0.0440 0.035 Uiso 1 1 calc R U . . .
C9 C 0.3504(3) 0.3063(3) 0.15027(18) 0.0260(5) Uani 1 1 d . . . . .
H9A H 0.3271 0.2439 0.1974 0.039 Uiso 1 1 calc R U . . .
H9B H 0.4359 0.2392 0.1080 0.039 Uiso 1 1 calc R U . . .
H9C H 0.2519 0.3678 0.1152 0.039 Uiso 1 1 calc R U . . .
C1 C 0.5536(3) 0.6236(3) 0.23214(18) 0.0237(5) Uani 1 1 d . . . . .
C2 C 0.5712(4) 0.7538(3) 0.2558(2) 0.0362(6) Uani 1 1 d . . . . .
H2 H 0.6251 0.7523 0.3112 0.043 Uiso 1 1 calc R U . . .
C4 C 0.4298(4) 0.8901(3) 0.1204(2) 0.0419(7) Uani 1 1 d . . . . .
H4 H 0.3896 0.9793 0.0816 0.050 Uiso 1 1 calc R U . . .
C3 C 0.5116(4) 0.8847(3) 0.2000(3) 0.0463(8) Uani 1 1 d . . . . .
H3 H 0.5271 0.9710 0.2166 0.056 Uiso 1 1 calc R U . . .
C13 C 0.7952(5) 0.2462(4) 0.4454(3) 0.0281(11) Uani 0.517(3) 1 d DG U P A 1
C14 C 0.7883(5) 0.1043(5) 0.4363(3) 0.0279(12) Uani 0.517(3) 1 d DG U P A 1
C15 C 0.8875(5) 0.0280(3) 0.3593(3) 0.0281(10) Uani 0.517(3) 1 d DG U P A 1
C16 C 0.9557(4) 0.1228(5) 0.3207(2) 0.0294(13) Uani 0.517(3) 1 d DG U P A 1
C17 C 0.8987(6) 0.2576(5) 0.3739(3) 0.0311(12) Uani 0.517(3) 1 d DG U P A 1
C23 C 0.7205(10) 0.3615(12) 0.5189(5) 0.088(3) Uani 0.517(3) 1 d D U P A 1
H23A H 0.7461 0.4481 0.5065 0.133 Uiso 0.517(3) 1 calc R U P A 1
H23B H 0.7635 0.3145 0.5792 0.133 Uiso 0.517(3) 1 calc R U P A 1
H23C H 0.6025 0.3981 0.5194 0.133 Uiso 0.517(3) 1 calc R U P A 1
C24 C 0.7186(10) 0.0303(11) 0.5057(7) 0.085(2) Uani 0.517(3) 1 d D U P A 1
H24A H 0.6544 0.1050 0.5524 0.127 Uiso 0.517(3) 1 calc R U P A 1
H24B H 0.8070 -0.0572 0.5358 0.127 Uiso 0.517(3) 1 calc R U P A 1
H24C H 0.6489 -0.0052 0.4740 0.127 Uiso 0.517(3) 1 calc R U P A 1
C25 C 0.9196(11) -0.1275(8) 0.3255(7) 0.088(3) Uani 0.517(3) 1 d D U P A 1
H25A H 0.8582 -0.1690 0.3639 0.132 Uiso 0.517(3) 1 calc R U P A 1
H25B H 1.0358 -0.1963 0.3296 0.132 Uiso 0.517(3) 1 calc R U P A 1
H25C H 0.8859 -0.1187 0.2610 0.132 Uiso 0.517(3) 1 calc R U P A 1
C26 C 1.0805(8) 0.0802(13) 0.2447(5) 0.091(3) Uani 0.517(3) 1 d D U P A 1
H26A H 1.1068 0.1660 0.2310 0.136 Uiso 0.517(3) 1 calc R U P A 1
H26B H 1.0378 0.0565 0.1891 0.136 Uiso 0.517(3) 1 calc R U P A 1
H26C H 1.1787 -0.0099 0.2640 0.136 Uiso 0.517(3) 1 calc R U P A 1
C27 C 0.9647(11) 0.3719(9) 0.3604(7) 0.083(2) Uani 0.517(3) 1 d D U P A 1
H27A H 0.9099 0.4562 0.4034 0.124 Uiso 0.517(3) 1 calc R U P A 1
H27B H 0.9462 0.4121 0.2966 0.124 Uiso 0.517(3) 1 calc R U P A 1
H27C H 1.0814 0.3225 0.3723 0.124 Uiso 0.517(3) 1 calc R U P A 1
C13A C 0.7643(4) 0.1793(5) 0.4603(2) 0.0281(11) Uani 0.483(3) 1 d DG U P A 2
C14A C 0.8300(6) 0.0475(4) 0.4041(3) 0.0279(12) Uani 0.483(3) 1 d DG U P A 2
C15A C 0.9316(5) 0.0693(5) 0.3353(3) 0.0281(10) Uani 0.483(3) 1 d DG U P A 2
C16A C 0.9287(6) 0.2144(5) 0.3489(3) 0.0309(17) Uani 0.483(3) 1 d DG U P A 2
C17A C 0.8252(6) 0.2824(4) 0.4262(3) 0.0311(12) Uani 0.483(3) 1 d DG U P A 2
C23A C 0.6669(10) 0.1941(13) 0.5472(5) 0.088(3) Uani 0.483(3) 1 d D U P A 2
H23D H 0.6354 0.2953 0.5734 0.133 Uiso 0.483(3) 1 calc R U P A 2
H23E H 0.7321 0.1144 0.5920 0.133 Uiso 0.483(3) 1 calc R U P A 2
H23F H 0.5693 0.1824 0.5332 0.133 Uiso 0.483(3) 1 calc R U P A 2
C24A C 0.8036(11) -0.0918(11) 0.4199(7) 0.085(2) Uani 0.483(3) 1 d D U P A 2
H24D H 0.8616 -0.1664 0.3719 0.127 Uiso 0.483(3) 1 calc R U P A 2
H24E H 0.6874 -0.0636 0.4174 0.127 Uiso 0.483(3) 1 calc R U P A 2
H24F H 0.8446 -0.1371 0.4809 0.127 Uiso 0.483(3) 1 calc R U P A 2
C25A C 1.0456(11) -0.0502(10) 0.2707(7) 0.088(3) Uani 0.483(3) 1 d D U P A 2
H25D H 1.1014 -0.0054 0.2304 0.132 Uiso 0.483(3) 1 calc R U P A 2
H25E H 0.9840 -0.0875 0.2329 0.132 Uiso 0.483(3) 1 calc R U P A 2
H25F H 1.1257 -0.1359 0.3068 0.132 Uiso 0.483(3) 1 calc R U P A 2
C26A C 1.0230(9) 0.2837(14) 0.2979(7) 0.091(3) Uani 0.483(3) 1 d D U P A 2
H26D H 1.0856 0.2164 0.2476 0.136 Uiso 0.483(3) 1 calc R U P A 2
H26E H 1.0971 0.2966 0.3404 0.136 Uiso 0.483(3) 1 calc R U P A 2
H26F H 0.9485 0.3839 0.2720 0.136 Uiso 0.483(3) 1 calc R U P A 2
C27A C 0.8035(12) 0.4225(9) 0.4748(7) 0.083(2) Uani 0.483(3) 1 d D U P A 2
H27D H 0.8448 0.3949 0.5378 0.124 Uiso 0.483(3) 1 calc R U P A 2
H27E H 0.6880 0.4943 0.4773 0.124 Uiso 0.483(3) 1 calc R U P A 2
H27F H 0.8635 0.4708 0.4412 0.124 Uiso 0.483(3) 1 calc R U P A 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
Zr1 N1 2.081(2) . ?
Zr1 Cl1 2.4379(7) . ?
Zr1 Cl2 2.4514(6) . ?
Zr1 N2 2.5104(19) . ?
Zr1 C13 2.527(4) . ?
Zr1 C14 2.532(4) . ?
Zr1 C15A 2.533(4) . ?
Zr1 C16A 2.533(5) . ?
Zr1 C17 2.553(5) . ?
Zr1 C15 2.561(4) . ?
Zr1 C14A 2.565(4) . ?
Zr1 C17A 2.565(5) . ?
N2 C8 1.485(3) . ?
N2 C9 1.492(3) . ?
N2 C7 1.496(3) . ?
N1 C1 1.396(3) . ?
N1 H1 0.8800 . ?
C6 C5 1.396(3) . ?
C6 C1 1.398(3) . ?
C6 C7 1.498(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C5 C4 1.384(4) . ?
C5 H5 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C1 C2 1.399(4) . ?
C2 C3 1.385(4) . ?
C2 H2 0.9500 . ?
C4 C3 1.379(5) . ?
C4 H4 0.9500 . ?
C3 H3 0.9500 . ?
C13 C17 1.4200 . ?
C13 C14 1.4200 . ?
C13 C23 1.487(7) . ?
C14 C15 1.4200 . ?
C14 C24 1.504(7) . ?
C15 C16 1.4200 . ?
C15 C25 1.502(7) . ?
C16 C17 1.4200 . ?
C16 C26 1.495(7) . ?
C17 C27 1.490(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C13A C14A 1.4200 . ?
C13A C17A 1.4200 . ?
C13A C23A 1.495(7) . ?
C14A C15A 1.4200 . ?
C14A C24A 1.489(8) . ?
C15A C16A 1.4200 . ?
C15A C25A 1.502(8) . ?
C16A C17A 1.4200 . ?
C16A C26A 1.484(8) . ?
C17A C27A 1.483(7) . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?

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 Cl1 113.27(6) . . ?
N1 Zr1 Cl2 118.76(7) . . ?
Cl1 Zr1 Cl2 113.84(3) . . ?
N1 Zr1 N2 74.98(7) . . ?
Cl1 Zr1 N2 79.61(5) . . ?
Cl2 Zr1 N2 77.42(5) . . ?
N1 Zr1 C13 85.69(11) . . ?
Cl1 Zr1 C13 130.08(8) . . ?
Cl2 Zr1 C13 92.37(10) . . ?
N2 Zr1 C13 149.73(9) . . ?
N1 Zr1 C14 118.26(11) . . ?
Cl1 Zr1 C14 111.84(10) . . ?
Cl2 Zr1 C14 75.83(7) . . ?
N2 Zr1 C14 153.25(8) . . ?
C13 Zr1 C14 32.6 . . ?
N1 Zr1 C15A 113.94(12) . . ?
Cl1 Zr1 C15A 76.73(8) . . ?
Cl2 Zr1 C15A 113.10(11) . . ?
N2 Zr1 C15A 156.32(9) . . ?
N1 Zr1 C16A 81.87(11) . . ?
Cl1 Zr1 C16A 94.14(11) . . ?
Cl2 Zr1 C16A 129.95(8) . . ?
N2 Zr1 C16A 151.04(9) . . ?
C15A Zr1 C16A 32.56(5) . . ?
N1 Zr1 C17 74.84(10) . . ?
Cl1 Zr1 C17 105.81(11) . . ?
Cl2 Zr1 C17 124.55(9) . . ?
N2 Zr1 C17 148.91(9) . . ?
C13 Zr1 C17 32.46(5) . . ?
C14 Zr1 C17 53.73(6) . . ?
N1 Zr1 C15 128.07(10) . . ?
Cl1 Zr1 C15 80.72(9) . . ?
Cl2 Zr1 C15 96.20(10) . . ?
N2 Zr1 C15 154.60(9) . . ?
C13 Zr1 C15 53.69(5) . . ?
C14 Zr1 C15 32.4 . . ?
C17 Zr1 C15 53.39(5) . . ?
N1 Zr1 C14A 128.50(9) . . ?
Cl1 Zr1 C14A 96.12(10) . . ?
Cl2 Zr1 C14A 81.70(10) . . ?
N2 Zr1 C14A 154.66(9) . . ?
C15A Zr1 C14A 32.3 . . ?
C16A Zr1 C14A 53.57(6) . . ?
N1 Zr1 C17A 75.42(10) . . ?
Cl1 Zr1 C17A 126.07(10) . . ?
Cl2 Zr1 C17A 104.75(10) . . ?
N2 Zr1 C17A 146.99(9) . . ?
C15A Zr1 C17A 53.57(6) . . ?
C16A Zr1 C17A 32.34(6) . . ?
C14A Zr1 C17A 53.21(5) . . ?
C8 N2 C9 106.69(19) . . ?
C8 N2 C7 108.12(18) . . ?
C9 N2 C7 106.55(18) . . ?
C8 N2 Zr1 113.28(14) . . ?
C9 N2 Zr1 112.81(14) . . ?
C7 N2 Zr1 109.07(13) . . ?
C1 N1 Zr1 141.19(17) . . ?
C1 N1 H1 109.4 . . ?
Zr1 N1 H1 109.4 . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 C7 119.1(2) . . ?
C1 C6 C7 121.6(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C7 C6 114.22(19) . . ?
N2 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C4 C5 C6 121.7(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C1 C6 121.7(2) . . ?
N1 C1 C2 119.7(2) . . ?
C6 C1 C2 118.5(2) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C3 C4 C5 119.1(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C17 C13 C14 108.0 . . ?
C17 C13 C23 123.7(5) . . ?
C14 C13 C23 128.2(5) . . ?
C17 C13 Zr1 74.80(17) . . ?
C14 C13 Zr1 73.89(17) . . ?
C23 C13 Zr1 120.7(4) . . ?
C13 C14 C15 108.0 . . ?
C13 C14 C24 126.8(5) . . ?
C15 C14 C24 124.1(5) . . ?
C13 C14 Zr1 73.50(17) . . ?
C15 C14 Zr1 74.96(15) . . ?
C24 C14 Zr1 126.9(4) . . ?
C14 C15 C16 108.0 . . ?
C14 C15 C25 126.5(5) . . ?
C16 C15 C25 125.5(5) . . ?
C14 C15 Zr1 72.67(15) . . ?
C16 C15 Zr1 74.46(17) . . ?
C25 C15 Zr1 120.1(4) . . ?
C17 C16 C15 108.0 . . ?
C17 C16 C26 125.8(5) . . ?
C15 C16 C26 125.9(5) . . ?
C17 C16 Zr1 73.10(16) . . ?
C15 C16 Zr1 73.44(17) . . ?
C26 C16 Zr1 124.6(4) . . ?
C13 C17 C16 108.0 . . ?
C13 C17 C27 129.4(5) . . ?
C16 C17 C27 121.9(5) . . ?
C13 C17 Zr1 72.74(16) . . ?
C16 C17 Zr1 74.74(15) . . ?
C27 C17 Zr1 125.8(4) . . ?
C13 C23 H23A 109.5 . . ?
C13 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C13 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 C24 H24A 109.5 . . ?
C14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C15 C25 H25A 109.5 . . ?
C15 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C15 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C26 H26A 109.5 . . ?
C16 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C16 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C17 C27 H27A 109.5 . . ?
C17 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C17 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C14A C13A C17A 108.0 . . ?
C14A C13A C23A 124.8(5) . . ?
C17A C13A C23A 126.8(5) . . ?
C14A C13A Zr1 73.23(17) . . ?
C17A C13A Zr1 73.23(18) . . ?
C23A C13A Zr1 125.6(4) . . ?
C15A C14A C13A 108.0 . . ?
C15A C14A C24A 126.8(5) . . ?
C13A C14A C24A 125.1(5) . . ?
C15A C14A Zr1 72.58(16) . . ?
C13A C14A Zr1 74.76(16) . . ?
C24A C14A Zr1 121.6(4) . . ?
C14A C15A C16A 108.0 . . ?
C14A C15A C25A 126.1(5) . . ?
C16A C15A C25A 125.1(5) . . ?
C14A C15A Zr1 75.08(16) . . ?
C16A C15A Zr1 73.72(19) . . ?
C25A C15A Zr1 125.5(4) . . ?
C17A C16A C15A 108.0 . . ?
C17A C16A C26A 123.9(5) . . ?
C15A C16A C26A 127.9(5) . . ?
C17A C16A Zr1 75.08(15) . . ?
C15A C16A Zr1 73.72(18) . . ?
C26A C16A Zr1 120.3(4) . . ?
C16A C17A C13A 108.0 . . ?
C16A C17A C27A 127.4(5) . . ?
C13A C17A C27A 123.9(5) . . ?
C16A C17A Zr1 72.58(15) . . ?
C13A C17A Zr1 74.77(17) . . ?
C27A C17A Zr1 126.3(4) . . ?
C13A C23A H23D 109.5 . . ?
C13A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C13A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C14A C24A H24D 109.5 . . ?
C14A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C14A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C15A C25A H25D 109.5 . . ?
C15A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
C15A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
C16A C26A H26D 109.5 . . ?
C16A C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
C16A C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C17A C27A H27D 109.5 . . ?
C17A C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C17A C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?


# SQUEEZE RESULTS (APPEND TO CIF)
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
1 0.000 -0.017 0.000 197.3 54.4
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.082
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1044555'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H38 Cl2 N2 Zr, 1.5(C7 H8)'
_chemical_formula_sum            'C29.50 H40 Cl2 N2 Zr'
_chemical_formula_weight         584.76

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0950(4)
_cell_length_b                   9.8420(5)
_cell_length_c                   16.5011(16)
_cell_angle_alpha                102.455(5)
_cell_angle_beta                 96.228(5)
_cell_angle_gamma                91.467(4)
_cell_volume                     1431.95(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    10672
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             610
_exptl_absorpt_coefficient_mu    0.591
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.040
0 0 1 0.012
0 -1 0 0.096
0 1 0 0.055
-1 0 0 0.094
1 0 0 0.140
-1 1 0 0.071
-1 -1 1 0.111
1 1 -1 0.101
1 -1 0 0.141


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10597
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5668
_reflns_number_gt                4514
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0227P)²+3.4728P] 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         5668
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1062
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 0.97817(4) 0.86817(4) 0.18885(2) 0.01907(10) Uani 1 1 d . . .
Cl2 Cl 0.86150(11) 0.74382(10) 0.05099(6) 0.0310(2) Uani 1 1 d . . .
Cl1 Cl 1.20709(11) 0.99314(10) 0.17868(8) 0.0400(3) Uani 1 1 d . . .
N2 N 1.1418(3) 0.6675(3) 0.15197(18) 0.0227(6) Uani 1 1 d . . .
N1 N 0.9915(4) 0.7748(3) 0.29178(19) 0.0256(7) Uani 1 1 d . . .
C11 C 0.7509(4) 0.9587(4) 0.2578(2) 0.0273(8) Uani 1 1 d . . .
C10 C 0.8719(4) 1.0503(4) 0.2988(2) 0.0279(8) Uani 1 1 d . . .
C7 C 1.2611(4) 0.6732(4) 0.2223(2) 0.0297(8) Uani 1 1 d . . .
H7A H 1.3362 0.6099 0.2027 0.036 Uiso 1 1 d R . .
H7B H 1.3074 0.7665 0.2382 0.036 Uiso 1 1 d R . .
C13 C 0.8348(4) 1.0747(4) 0.1634(2) 0.0285(8) Uani 1 1 d . . .
C8 C 1.0589(5) 0.5301(4) 0.1356(2) 0.0279(8) Uani 1 1 d . . .
H8A H 0.9917 0.5189 0.0853 0.033 Uiso 1 1 d R . .
H8B H 1.0041 0.5257 0.1816 0.033 Uiso 1 1 d R . .
H8C H 1.1275 0.4571 0.1293 0.033 Uiso 1 1 d R . .
C14 C 0.9220(4) 1.1232(4) 0.2411(2) 0.0272(8) Uani 1 1 d . . .
C1 C 1.0817(4) 0.6890(4) 0.3308(2) 0.0231(8) Uani 1 1 d . . .
C9 C 1.2158(4) 0.6703(4) 0.0764(2) 0.0292(8) Uani 1 1 d . . .
H9A H 1.2628 0.5841 0.0598 0.035 Uiso 1 1 d R . .
H9B H 1.2889 0.7462 0.0887 0.035 Uiso 1 1 d R . .
H9C H 1.1437 0.6822 0.0318 0.035 Uiso 1 1 d R . .
C2 C 1.2095(4) 0.6355(4) 0.2983(2) 0.0261(8) Uani 1 1 d . . .
C6 C 1.0473(5) 0.6552(4) 0.4051(2) 0.0312(9) Uani 1 1 d . . .
H6 H 0.9616 0.6881 0.4269 0.037 Uiso 1 1 d R . .
C5 C 1.1377(5) 0.5745(4) 0.4464(3) 0.0368(10) Uani 1 1 d . . .
H5 H 1.1145 0.5559 0.4966 0.044 Uiso 1 1 d R . .
C12 C 0.7261(4) 0.9745(4) 0.1744(3) 0.0298(9) Uani 1 1 d . . .
C3 C 1.2964(5) 0.5518(4) 0.3396(2) 0.0334(9) Uani 1 1 d . . .
H3 H 1.3806 0.5156 0.3175 0.040 Uiso 1 1 d R . .
C24 C 0.6228(5) 0.4703(4) 0.1278(3) 0.0378(10) Uani 1 1 d . . .
H24 H 0.6626 0.5331 0.1003 0.045 Uiso 1 1 d R . .
C25 C 0.6781(5) 0.4713(5) 0.2103(3) 0.0365(10) Uani 1 1 d . . .
H25 H 0.7568 0.5324 0.2372 0.044 Uiso 1 1 d R . .
C22 C 0.4487(5) 0.2862(4) 0.1291(3) 0.0370(10) Uani 1 1 d . . .
H22 H 0.3699 0.2251 0.1025 0.044 Uiso 1 1 d R . .
C17 C 0.5946(5) 0.9129(5) 0.1143(3) 0.0475(12) Uani 1 1 d . . .
H17A H 0.5842 0.8149 0.1125 0.057 Uiso 1 1 d R . .
H17B H 0.6082 0.9266 0.0597 0.057 Uiso 1 1 d R . .
H17C H 0.5071 0.9571 0.1320 0.057 Uiso 1 1 d R . .
C20 C 0.6185(5) 0.3782(4) 0.2517(3) 0.0327(9) Uani 1 1 d . . .
C15 C 0.9243(6) 1.0805(5) 0.3910(2) 0.0423(11) Uani 1 1 d . . .
H15A H 1.0240 1.1197 0.4002 0.051 Uiso 1 1 d R . .
H15B H 0.9214 0.9960 0.4111 0.051 Uiso 1 1 d R . .
H15C H 0.8613 1.1458 0.4205 0.051 Uiso 1 1 d R . .
C21 C 0.5037(5) 0.2858(4) 0.2097(3) 0.0338(9) Uani 1 1 d . . .
H21 H 0.4635 0.2219 0.2364 0.041 Uiso 1 1 d R . .
C23 C 0.5078(5) 0.3786(5) 0.0880(3) 0.0370(10) Uani 1 1 d . . .
H23 H 0.4708 0.3779 0.0332 0.044 Uiso 1 1 d R . .
C26 C 0.6753(6) 0.3798(6) 0.3407(3) 0.0503(13) Uani 1 1 d . . .
H26A H 0.7735 0.4226 0.3532 0.060 Uiso 1 1 d R . .
H26B H 0.6775 0.2860 0.3486 0.060 Uiso 1 1 d R . .
H26C H 0.6114 0.4319 0.3772 0.060 Uiso 1 1 d R . .
C4 C 1.2617(5) 0.5228(4) 0.4137(3) 0.0420(11) Uani 1 1 d . . .
H4 H 1.3219 0.4676 0.4410 0.050 Uiso 1 1 d R . .
C19 C 1.0338(5) 1.2446(4) 0.2616(3) 0.0443(12) Uani 1 1 d . . .
H19A H 0.9840 1.3303 0.2719 0.053 Uiso 1 1 d R . .
H19B H 1.0907 1.2416 0.2156 0.053 Uiso 1 1 d R . .
H19C H 1.0986 1.2388 0.3106 0.053 Uiso 1 1 d R . .
C18 C 0.8452(6) 1.1263(5) 0.0855(3) 0.0496(13) Uani 1 1 d . . .
H18A H 0.8204 1.0516 0.0374 0.059 Uiso 1 1 d R . .
H18B H 0.9445 1.1619 0.0858 0.059 Uiso 1 1 d R . .
H18C H 0.7778 1.1993 0.0835 0.059 Uiso 1 1 d R . .
C16 C 0.6518(5) 0.8748(5) 0.2984(3) 0.0449(12) Uani 1 1 d . . .
H16A H 0.5500 0.8868 0.2803 0.054 Uiso 1 1 d R . .
H16B H 0.6700 0.9045 0.3581 0.054 Uiso 1 1 d R . .
H16C H 0.6729 0.7783 0.2820 0.054 Uiso 1 1 d R . .
H1 H 0.914(4) 0.806(4) 0.327(2) 0.026(10) Uiso 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 2.093(3) . ?
Zr1 Cl1 2.4310(10) . ?
Zr1 Cl2 2.4511(10) . ?
Zr1 N2 2.513(3) . ?
Zr1 C13 2.528(4) . ?
Zr1 C10 2.551(3) . ?
Zr1 C11 2.555(4) . ?
Zr1 C12 2.553(4) . ?
Zr1 C14 2.555(4) . ?
N2 C9 1.485(4) . ?
N2 C7 1.491(5) . ?
N2 C8 1.489(5) . ?
N1 C1 1.398(5) . ?
N1 H1 0.98(4) . ?
C11 C10 1.416(6) . ?
C11 C12 1.412(6) . ?
C11 C16 1.508(5) . ?
C10 C14 1.414(5) . ?
C10 C15 1.507(5) . ?
C7 C2 1.500(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C13 C14 1.413(6) . ?
C13 C12 1.431(6) . ?
C13 C18 1.491(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C14 C19 1.505(5) . ?
C1 C6 1.401(5) . ?
C1 C2 1.401(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C2 C3 1.387(5) . ?
C6 C5 1.385(6) . ?
C6 H6 0.9300 . ?
C5 C4 1.365(6) . ?
C5 H5 0.9299 . ?
C12 C17 1.493(6) . ?
C3 C4 1.382(6) . ?
C3 H3 0.9300 . ?
C24 C23 1.374(6) . ?
C24 C25 1.397(6) . ?
C24 H24 0.9299 . ?
C25 C20 1.386(6) . ?
C25 H25 0.9300 . ?
C22 C23 1.376(6) . ?
C22 C21 1.370(6) . ?
C22 H22 0.9301 . ?
C17 H17A 0.9601 . ?
C17 H17B 0.9599 . ?
C17 H17C 0.9600 . ?
C20 C21 1.386(6) . ?
C20 C26 1.500(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C21 H21 0.9300 . ?
C23 H23 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C4 H4 0.9301 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9601 . ?
C18 H18A 0.9599 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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 Cl1 112.95(10) . . ?
N1 Zr1 Cl2 121.32(9) . . ?
Cl1 Zr1 Cl2 111.46(4) . . ?
N1 Zr1 N2 75.24(11) . . ?
Cl1 Zr1 N2 79.77(7) . . ?
Cl2 Zr1 N2 77.02(7) . . ?
N1 Zr1 C13 129.42(12) . . ?
Cl1 Zr1 C13 89.59(10) . . ?
Cl2 Zr1 C13 86.45(10) . . ?
N2 Zr1 C13 155.30(11) . . ?
N1 Zr1 C10 77.61(12) . . ?
Cl1 Zr1 C10 99.48(10) . . ?
Cl2 Zr1 C10 129.16(9) . . ?
N2 Zr1 C10 149.97(11) . . ?
C13 Zr1 C10 53.56(12) . . ?
N1 Zr1 C11 78.40(12) . . ?
Cl1 Zr1 C11 129.43(9) . . ?
Cl2 Zr1 C11 100.74(10) . . ?
N2 Zr1 C11 147.02(11) . . ?
C13 Zr1 C11 53.81(12) . . ?
C10 Zr1 C11 32.21(13) . . ?
N1 Zr1 C12 108.64(13) . . ?
Cl1 Zr1 C12 122.29(10) . . ?
Cl2 Zr1 C12 76.06(9) . . ?
N2 Zr1 C12 150.18(12) . . ?
C13 Zr1 C12 32.70(13) . . ?
C10 Zr1 C12 53.22(13) . . ?
C11 Zr1 C12 32.10(12) . . ?
N1 Zr1 C14 107.30(12) . . ?
Cl1 Zr1 C14 76.80(9) . . ?
Cl2 Zr1 C14 118.69(9) . . ?
N2 Zr1 C14 155.41(11) . . ?
C13 Zr1 C14 32.28(13) . . ?
C10 Zr1 C14 32.16(12) . . ?
C11 Zr1 C14 53.40(12) . . ?
C12 Zr1 C14 53.41(13) . . ?
C9 N2 C7 107.0(3) . . ?
C9 N2 C8 106.5(3) . . ?
C7 N2 C8 108.4(3) . . ?
C9 N2 Zr1 113.0(2) . . ?
C7 N2 Zr1 109.3(2) . . ?
C8 N2 Zr1 112.4(2) . . ?
C1 N1 Zr1 140.8(3) . . ?
C1 N1 H1 108(2) . . ?
Zr1 N1 H1 111(2) . . ?
C10 C11 C12 107.8(3) . . ?
C10 C11 C16 126.2(4) . . ?
C12 C11 C16 125.4(4) . . ?
C10 C11 Zr1 73.7(2) . . ?
C12 C11 Zr1 73.9(2) . . ?
C16 C11 Zr1 124.8(3) . . ?
C11 C10 C14 108.4(3) . . ?
C11 C10 C15 125.8(4) . . ?
C14 C10 C15 125.3(4) . . ?
C11 C10 Zr1 74.1(2) . . ?
C14 C10 Zr1 74.1(2) . . ?
C15 C10 Zr1 124.5(3) . . ?
N2 C7 C2 114.4(3) . . ?
N2 C7 H7A 108.5 . . ?
C2 C7 H7A 108.5 . . ?
N2 C7 H7B 108.9 . . ?
C2 C7 H7B 108.7 . . ?
H7A C7 H7B 107.5 . . ?
C14 C13 C12 107.6(3) . . ?
C14 C13 C18 126.5(4) . . ?
C12 C13 C18 125.7(4) . . ?
C14 C13 Zr1 74.9(2) . . ?
C12 C13 Zr1 74.6(2) . . ?
C18 C13 Zr1 120.2(3) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.4 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C13 C14 C10 108.0(3) . . ?
C13 C14 C19 125.6(4) . . ?
C10 C14 C19 125.9(4) . . ?
C13 C14 Zr1 72.8(2) . . ?
C10 C14 Zr1 73.7(2) . . ?
C19 C14 Zr1 125.6(3) . . ?
N1 C1 C6 120.6(3) . . ?
N1 C1 C2 121.7(3) . . ?
C6 C1 C2 117.7(3) . . ?
N2 C9 H9A 109.3 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.6 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 C7 118.4(4) . . ?
C1 C2 C7 121.7(3) . . ?
C5 C6 C1 121.6(4) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 118.9 . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 120.2 . . ?
C11 C12 C13 108.0(4) . . ?
C11 C12 C17 124.4(4) . . ?
C13 C12 C17 127.0(4) . . ?
C11 C12 Zr1 74.0(2) . . ?
C13 C12 Zr1 72.7(2) . . ?
C17 C12 Zr1 126.3(3) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.6 . . ?
C23 C24 C25 120.0(4) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 119.9 . . ?
C20 C25 C24 120.0(4) . . ?
C20 C25 H25 119.7 . . ?
C24 C25 H25 120.2 . . ?
C23 C22 C21 120.3(4) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 119.7 . . ?
C12 C17 H17A 109.2 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.7 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C21 C20 C25 118.7(4) . . ?
C21 C20 C26 120.7(4) . . ?
C25 C20 C26 120.5(4) . . ?
C10 C15 H15A 109.1 . . ?
C10 C15 H15B 109.9 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C22 C21 C20 121.0(4) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.7 . . ?
C24 C23 C22 119.9(4) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.0 . . ?
C20 C26 H26A 109.3 . . ?
C20 C26 H26B 109.6 . . ?
H26A C26 H26B 109.5 . . ?
C20 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.1 . . ?
C14 C19 H19A 109.8 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.1 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C13 C18 H18A 110.0 . . ?
C13 C18 H18B 109.1 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.3 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C16 H16A 109.7 . . ?
C11 C16 H16B 110.1 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 108.6 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
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
1 0.500 1.000 0.500 201.8 36.9
_platon_squeeze_details          
;
;


_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.0
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1044556'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H54 Cl2 Hf2 N4'
_chemical_formula_sum            'C38 H54 Cl2 Hf2 N4'
_chemical_formula_weight         994.73

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'
Hf Hf -0.5830 6.1852 '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'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2969(7)
_cell_length_b                   10.3570(5)
_cell_length_c                   11.6491(5)
_cell_angle_alpha                112.212(4)
_cell_angle_beta                 102.671(6)
_cell_angle_gamma                104.562(4)
_cell_volume                     941.17(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    18255
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_absorpt_coefficient_mu    5.685
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.112
1 0 0 0.073
0 -1 0 0.129
0 1 0 0.077
-1 1 0 0.083
0 0 1 0.011
0 0 -1 0.075


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;


_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18182
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4300
_reflns_number_gt                4076
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0352P)²+0.7920P] where P=(Fo²+2Fc²)/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         4300
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0596
_refine_ls_wR_factor_gt          0.0582
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.004
_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 0.100348(13) 0.150634(13) 1.013126(11) 0.01702(6) Uani 1 1 d . . .
Cl1 Cl 0.37288(9) 0.18472(10) 1.03547(8) 0.02672(17) Uani 1 1 d . . .
N1 N -0.0359(3) -0.0562(3) 0.8655(3) 0.0199(5) Uani 1 1 d . . .
C12 C 0.1352(4) 0.3572(4) 0.9462(3) 0.0243(7) Uani 1 1 d . . .
C19 C -0.2609(4) 0.1940(5) 0.9679(4) 0.0331(8) Uani 1 1 d . . .
H19A H -0.3212 0.2537 0.9559 0.040 Uiso 1 1 d R . .
H19B H -0.2643 0.1816 1.0450 0.040 Uiso 1 1 d R . .
H19C H -0.3052 0.0974 0.8915 0.040 Uiso 1 1 d R . .
C8 C 0.3661(6) -0.0069(8) 0.6239(5) 0.073(2) Uani 1 1 d . . .
H8A H 0.4409 0.0252 0.7098 0.088 Uiso 1 1 d R . .
H8B H 0.3376 0.0754 0.6221 0.088 Uiso 1 1 d R . .
H8C H 0.4131 -0.0401 0.5580 0.088 Uiso 1 1 d R . .
C11 C 0.1719(4) 0.4256(4) 1.0845(3) 0.0234(7) Uani 1 1 d . . .
C15 C 0.0158(5) 0.4276(4) 1.2445(4) 0.0321(8) Uani 1 1 d . . .
H15A H 0.1044 0.4306 1.3075 0.039 Uiso 1 1 d R . .
H15B H -0.0807 0.3599 1.2386 0.039 Uiso 1 1 d R . .
H15C H 0.0123 0.5263 1.2728 0.039 Uiso 1 1 d R . .
N2 N 0.2229(4) -0.1289(4) 0.5959(3) 0.0379(8) Uani 1 1 d . . .
C2 C -0.0290(4) -0.1681(4) 0.6404(3) 0.0209(6) Uani 1 1 d . . .
C1 C -0.1141(4) -0.1485(3) 0.7280(3) 0.0192(6) Uani 1 1 d . . .
C6 C -0.2791(4) -0.2247(4) 0.6751(3) 0.0228(6) Uani 1 1 d . . .
H6 H -0.3365 -0.2105 0.7318 0.027 Uiso 1 1 d R . .
C3 C -0.1101(4) -0.2647(4) 0.5067(3) 0.0284(7) Uani 1 1 d . . .
H3 H -0.0539 -0.2767 0.4490 0.034 Uiso 1 1 d R . .
C16 C 0.3320(4) 0.5374(4) 1.1873(4) 0.0329(8) Uani 1 1 d . . .
H16A H 0.3481 0.6342 1.1905 0.039 Uiso 1 1 d R . .
H16B H 0.4142 0.5046 1.1645 0.039 Uiso 1 1 d R . .
H16C H 0.3351 0.5443 1.2724 0.039 Uiso 1 1 d R . .
C5 C -0.3584(4) -0.3212(4) 0.5412(4) 0.0302(8) Uani 1 1 d . . .
H5 H -0.4681 -0.3695 0.5085 0.036 Uiso 1 1 d R . .
C10 C 0.0327(4) 0.3747(4) 1.1109(3) 0.0237(7) Uani 1 1 d . . .
C13 C -0.0280(4) 0.2619(4) 0.8852(3) 0.0230(6) Uani 1 1 d . . .
C18 C -0.1216(5) 0.1740(4) 0.7387(4) 0.0325(8) Uani 1 1 d . . .
H18A H -0.1659 0.2353 0.7095 0.039 Uiso 1 1 d R . .
H18B H -0.2057 0.0856 0.7215 0.039 Uiso 1 1 d R . .
H18C H -0.0528 0.1453 0.6918 0.039 Uiso 1 1 d R . .
C14 C -0.0910(4) 0.2723(4) 0.9874(3) 0.0231(7) Uani 1 1 d . . .
C17 C 0.2478(5) 0.3848(4) 0.8761(4) 0.0326(8) Uani 1 1 d . . .
H17A H 0.2126 0.2997 0.7908 0.039 Uiso 1 1 d R . .
H17B H 0.3513 0.3985 0.9278 0.039 Uiso 1 1 d R . .
H17C H 0.2524 0.4730 0.8653 0.039 Uiso 1 1 d R . .
C7 C 0.1471(4) -0.0796(4) 0.6925(3) 0.0288(8) Uani 1 1 d . . .
H7A H 0.1641 0.0255 0.7197 0.035 Uiso 1 1 d R . .
H7B H 0.1969 -0.0883 0.7703 0.035 Uiso 1 1 d R . .
C4 C -0.2730(4) -0.3430(5) 0.4564(3) 0.0330(8) Uani 1 1 d . . .
H4 H -0.3243 -0.4109 0.3671 0.040 Uiso 1 1 d R . .
C9 C 0.2577(6) -0.2582(7) 0.5928(5) 0.0591(15) Uani 1 1 d . . .
H9A H 0.3285 -0.2319 0.6785 0.071 Uiso 1 1 d R . .
H9B H 0.3072 -0.2888 0.5283 0.071 Uiso 1 1 d R . .
H9C H 0.1615 -0.3392 0.5696 0.071 Uiso 1 1 d 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 N1 2.012(3) . ?
Hf1 N1 2.106(3) 2_557 ?
Hf1 Cl1 2.4090(8) . ?
Hf1 C14 2.454(3) . ?
Hf1 C10 2.475(3) . ?
Hf1 C13 2.486(3) . ?
Hf1 C11 2.501(3) . ?
Hf1 C12 2.512(3) . ?
Hf1 Hf1 3.0679(3) 2_557 ?
N1 C1 1.411(4) . ?
N1 Hf1 2.106(3) 2_557 ?
C12 C11 1.410(5) . ?
C12 C13 1.422(5) . ?
C12 C17 1.498(5) . ?
C19 C14 1.504(5) . ?
C19 H19A 0.9599 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9601 . ?
C8 N2 1.459(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9601 . ?
C11 C10 1.415(5) . ?
C11 C16 1.515(5) . ?
C15 C10 1.501(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 C9 1.444(7) . ?
N2 C7 1.456(4) . ?
C2 C3 1.387(4) . ?
C2 C1 1.409(4) . ?
C2 C7 1.509(4) . ?
C1 C6 1.402(4) . ?
C6 C5 1.386(5) . ?
C6 H6 0.9300 . ?
C3 C4 1.389(5) . ?
C3 H3 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9601 . ?
C16 H16C 0.9600 . ?
C5 C4 1.386(5) . ?
C5 H5 0.9299 . ?
C10 C14 1.423(5) . ?
C13 C14 1.419(5) . ?
C13 C18 1.508(5) . ?
C18 H18A 0.9599 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C17 H17A 0.9601 . ?
C17 H17B 0.9601 . ?
C17 H17C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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 Hf1 N1 83.71(11) . 2_557 ?
N1 Hf1 Cl1 107.63(8) . . ?
N1 Hf1 Cl1 109.13(8) 2_557 . ?
N1 Hf1 C14 97.75(11) . . ?
N1 Hf1 C14 102.38(11) 2_557 . ?
Cl1 Hf1 C14 141.12(8) . . ?
N1 Hf1 C10 130.34(11) . . ?
N1 Hf1 C10 96.18(11) 2_557 . ?
Cl1 Hf1 C10 118.86(8) . . ?
C14 Hf1 C10 33.55(11) . . ?
N1 Hf1 C13 89.92(11) . . ?
N1 Hf1 C13 133.90(11) 2_557 . ?
Cl1 Hf1 C13 116.27(8) . . ?
C14 Hf1 C13 33.38(11) . . ?
C10 Hf1 C13 55.23(11) . . ?
N1 Hf1 C11 144.59(11) . . ?
N1 Hf1 C11 121.18(11) 2_557 . ?
Cl1 Hf1 C11 88.63(8) . . ?
C14 Hf1 C11 55.10(11) . . ?
C10 Hf1 C11 33.04(11) . . ?
C13 Hf1 C11 54.77(11) . . ?
N1 Hf1 C12 114.95(11) . . ?
N1 Hf1 C12 150.83(11) 2_557 . ?
Cl1 Hf1 C12 87.26(8) . . ?
C14 Hf1 C12 54.99(11) . . ?
C10 Hf1 C12 54.68(11) . . ?
C13 Hf1 C12 33.06(11) . . ?
C11 Hf1 C12 32.66(11) . . ?
N1 Hf1 Hf1 43.03(7) . 2_557 ?
N1 Hf1 Hf1 40.67(7) 2_557 2_557 ?
Cl1 Hf1 Hf1 115.07(2) . 2_557 ?
C14 Hf1 Hf1 103.63(8) . 2_557 ?
C10 Hf1 Hf1 119.89(8) . 2_557 ?
C13 Hf1 Hf1 118.37(8) . 2_557 ?
C11 Hf1 Hf1 152.86(8) . 2_557 ?
C12 Hf1 Hf1 151.17(8) . 2_557 ?
C1 N1 Hf1 147.4(2) . . ?
C1 N1 Hf1 115.6(2) . 2_557 ?
Hf1 N1 Hf1 96.29(11) . 2_557 ?
C11 C12 C13 108.2(3) . . ?
C11 C12 C17 125.6(3) . . ?
C13 C12 C17 126.2(3) . . ?
C11 C12 Hf1 73.24(19) . . ?
C13 C12 Hf1 72.46(18) . . ?
C17 C12 Hf1 121.8(2) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 108.8 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 110.1 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C8 H8A 110.0 . . ?
N2 C8 H8B 108.6 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.8 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C11 C10 108.4(3) . . ?
C12 C11 C16 125.9(3) . . ?
C10 C11 C16 125.7(3) . . ?
C12 C11 Hf1 74.11(19) . . ?
C10 C11 Hf1 72.47(18) . . ?
C16 C11 Hf1 120.6(2) . . ?
C10 C15 H15A 109.9 . . ?
C10 C15 H15B 109.3 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.2 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 N2 C7 110.6(3) . . ?
C9 N2 C8 111.1(4) . . ?
C7 N2 C8 110.8(4) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C7 121.1(3) . . ?
C1 C2 C7 119.7(3) . . ?
C6 C1 C2 118.2(3) . . ?
C6 C1 N1 120.6(3) . . ?
C2 C1 N1 121.2(3) . . ?
C5 C6 C1 121.9(3) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 118.8 . . ?
C2 C3 C4 121.9(3) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.1 . . ?
C11 C16 H16A 109.6 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.3 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C5 C6 119.4(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.1 . . ?
C11 C10 C14 107.7(3) . . ?
C11 C10 C15 126.0(3) . . ?
C14 C10 C15 126.1(3) . . ?
C11 C10 Hf1 74.49(19) . . ?
C14 C10 Hf1 72.40(19) . . ?
C15 C10 Hf1 122.1(2) . . ?
C14 C13 C12 107.6(3) . . ?
C14 C13 C18 125.5(3) . . ?
C12 C13 C18 126.7(3) . . ?
C14 C13 Hf1 72.06(19) . . ?
C12 C13 Hf1 74.49(19) . . ?
C18 C13 Hf1 122.4(2) . . ?
C13 C18 H18A 109.3 . . ?
C13 C18 H18B 109.6 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 C10 108.1(3) . . ?
C13 C14 C19 125.8(3) . . ?
C10 C14 C19 126.1(3) . . ?
C13 C14 Hf1 74.56(19) . . ?
C10 C14 Hf1 74.05(19) . . ?
C19 C14 Hf1 119.5(2) . . ?
C12 C17 H17A 109.4 . . ?
C12 C17 H17B 108.8 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 110.2 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C7 C2 113.3(3) . . ?
N2 C7 H7A 108.9 . . ?
C2 C7 H7A 108.7 . . ?
N2 C7 H7B 109.0 . . ?
C2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.7 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.5 . . ?
N2 C9 H9A 109.2 . . ?
N2 C9 H9B 109.2 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 110.0 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.562
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1044557'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H60 Cl2 N2 Zr2'
_chemical_formula_sum            'C42 H60 Cl2 N2 Zr2'
_chemical_formula_weight         846.26

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2009(5)
_cell_length_b                   10.5211(7)
_cell_length_c                   10.6140(7)
_cell_angle_alpha                113.719(6)
_cell_angle_beta                 103.394(5)
_cell_angle_gamma                98.566(5)
_cell_volume                     976.34(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    20466
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.50

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440
_exptl_absorpt_coefficient_mu    0.702
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.062
-1 0 0 0.117
0 -1 0 0.065
0 1 0 0.071
0 0 -1 0.026
0 0 1 0.024


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20373
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4457
_reflns_number_gt                3929
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0251P)²+0.6391P] where P=(Fo²+2Fc²)/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         4457
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0591
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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 0.119707(18) 0.482912(19) 0.604244(19) 0.01251(6) Uani 1 1 d . . .
Cl1 Cl 0.10957(5) 0.57402(5) 0.84911(5) 0.02184(11) Uani 1 1 d . . .
N1 N 0.07509(16) 0.64042(16) 0.53169(17) 0.0146(3) Uani 1 1 d . . .
C3 C 0.2467(2) 0.2864(2) 0.5632(2) 0.0182(4) Uani 1 1 d . . .
C16 C 0.1599(2) 0.8974(2) 0.8351(2) 0.0189(4) Uani 1 1 d . . .
H16 H 0.0800 0.8124 0.7945 0.023 Uiso 1 1 d R . .
C11 C 0.2440(2) 0.8730(2) 0.7306(2) 0.0173(4) Uani 1 1 d . . .
C10 C 0.19604(19) 0.76001(19) 0.5859(2) 0.0143(4) Uani 1 1 d . . .
C12 C 0.3730(2) 0.9747(2) 0.7792(2) 0.0226(4) Uani 1 1 d . . .
H12 H 0.4056 1.0474 0.8745 0.027 Uiso 1 1 d R . .
C6 C 0.2268(2) 0.2708(2) 0.3075(2) 0.0279(5) Uani 1 1 d . . .
H6A H 0.2018 0.3346 0.2678 0.033 Uiso 1 1 d R . .
H6B H 0.1484 0.1883 0.2703 0.033 Uiso 1 1 d R . .
H6C H 0.3044 0.2400 0.2803 0.033 Uiso 1 1 d R . .
C2 C 0.2672(2) 0.3479(2) 0.4698(2) 0.0185(4) Uani 1 1 d . . .
C21 C 0.3268(2) 0.6242(2) 0.2572(2) 0.0282(5) Uani 1 1 d . . .
H21A H 0.3747 0.7060 0.2507 0.034 Uiso 1 1 d R . .
H21B H 0.2824 0.5456 0.1614 0.034 Uiso 1 1 d R . .
H21C H 0.3929 0.5959 0.3139 0.034 Uiso 1 1 d R . .
C5 C 0.38045(19) 0.5217(2) 0.7065(2) 0.0173(4) Uani 1 1 d . . .
C15 C 0.2749(2) 0.7645(2) 0.4918(2) 0.0159(4) Uani 1 1 d . . .
C4 C 0.3167(2) 0.3934(2) 0.7086(2) 0.0184(4) Uani 1 1 d . . .
C9 C 0.4683(2) 0.6604(2) 0.8363(2) 0.0230(4) Uani 1 1 d . . .
H9A H 0.5610 0.6520 0.8693 0.028 Uiso 1 1 d R . .
H9B H 0.4274 0.6799 0.9127 0.028 Uiso 1 1 d R . .
H9C H 0.4728 0.7378 0.8101 0.028 Uiso 1 1 d R . .
C14 C 0.4025(2) 0.8681(2) 0.5477(2) 0.0217(4) Uani 1 1 d . . .
H14 H 0.4548 0.8681 0.4866 0.026 Uiso 1 1 d R . .
C17 C 0.1048(2) 1.0293(2) 0.8525(3) 0.0276(5) Uani 1 1 d . . .
H17A H 0.1820 1.1144 0.8971 0.033 Uiso 1 1 d R . .
H17B H 0.0457 1.0399 0.9124 0.033 Uiso 1 1 d R . .
H17C H 0.0519 1.0161 0.7585 0.033 Uiso 1 1 d R . .
C1 C 0.3485(2) 0.4933(2) 0.5594(2) 0.0182(4) Uani 1 1 d . . .
H1 H 0.3762 0.5591 0.5264 0.022 Uiso 1 1 d R . .
C7 C 0.1740(2) 0.1328(2) 0.5190(3) 0.0286(5) Uani 1 1 d . . .
H7A H 0.2163 0.1054 0.5914 0.034 Uiso 1 1 d R . .
H7B H 0.1820 0.0707 0.4273 0.034 Uiso 1 1 d R . .
H7C H 0.0769 0.1241 0.5102 0.034 Uiso 1 1 d R . .
C19 C 0.2168(2) 0.6646(2) 0.3303(2) 0.0186(4) Uani 1 1 d . . .
H19 H 0.1559 0.5754 0.3163 0.022 Uiso 1 1 d R . .
C8 C 0.3296(2) 0.3698(2) 0.8408(2) 0.0261(5) Uani 1 1 d . . .
H8A H 0.3917 0.3102 0.8444 0.031 Uiso 1 1 d R . .
H8B H 0.2390 0.3228 0.8358 0.031 Uiso 1 1 d R . .
H8C H 0.3662 0.4609 0.9266 0.031 Uiso 1 1 d R . .
C20 C 0.1264(2) 0.7348(2) 0.2562(2) 0.0257(5) Uani 1 1 d . . .
H20A H 0.0528 0.7533 0.2976 0.031 Uiso 1 1 d R . .
H20B H 0.0863 0.6711 0.1540 0.031 Uiso 1 1 d R . .
H20C H 0.1833 0.8240 0.2707 0.031 Uiso 1 1 d R . .
C18 C 0.2458(2) 0.9227(2) 0.9868(2) 0.0244(4) Uani 1 1 d . . .
H18A H 0.2935 0.8489 0.9774 0.029 Uiso 1 1 d R . .
H18B H 0.1842 0.9194 1.0421 0.029 Uiso 1 1 d R . .
H18C H 0.3132 1.0155 1.0358 0.029 Uiso 1 1 d R . .
C13 C 0.4529(2) 0.9707(2) 0.6911(2) 0.0251(5) Uani 1 1 d . . .
H13 H 0.5404 1.0365 0.7277 0.030 Uiso 1 1 d 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 2.0277(16) 2_566 ?
Zr1 N1 2.1530(16) . ?
Zr1 Cl1 2.4153(5) . ?
Zr1 C1 2.4836(19) . ?
Zr1 C2 2.5136(19) . ?
Zr1 C5 2.5302(19) . ?
Zr1 C3 2.5446(19) . ?
Zr1 C4 2.5541(19) . ?
Zr1 Zr1 3.0641(4) 2_566 ?
N1 C10 1.436(2) . ?
N1 Zr1 2.0276(16) 2_566 ?
C3 C4 1.418(3) . ?
C3 C2 1.420(3) . ?
C3 C7 1.502(3) . ?
C16 C11 1.520(3) . ?
C16 C17 1.534(3) . ?
C16 C18 1.537(3) . ?
C16 H16 0.9800 . ?
C11 C12 1.401(3) . ?
C11 C10 1.421(3) . ?
C10 C15 1.431(3) . ?
C12 C13 1.368(3) . ?
C12 H12 0.9300 . ?
C6 C2 1.498(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C2 C1 1.421(3) . ?
C21 C19 1.524(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C5 C1 1.412(3) . ?
C5 C4 1.420(3) . ?
C5 C9 1.500(3) . ?
C15 C14 1.390(3) . ?
C15 C19 1.513(3) . ?
C4 C8 1.501(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C14 C13 1.377(3) . ?
C14 H14 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C1 H1 0.9299 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9601 . ?
C19 C20 1.532(3) . ?
C19 H19 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9599 . ?
C20 H20C 0.9599 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C13 H13 0.9300 . ?

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 85.78(6) 2_566 . ?
N1 Zr1 Cl1 107.22(5) 2_566 . ?
N1 Zr1 Cl1 106.25(4) . . ?
N1 Zr1 C1 129.95(6) 2_566 . ?
N1 Zr1 C1 93.92(6) . . ?
Cl1 Zr1 C1 120.60(5) . . ?
N1 Zr1 C2 100.64(6) 2_566 . ?
N1 Zr1 C2 109.18(6) . . ?
Cl1 Zr1 C2 136.00(5) . . ?
C1 Zr1 C2 33.02(6) . . ?
N1 Zr1 C5 152.58(6) 2_566 . ?
N1 Zr1 C5 111.61(6) . . ?
Cl1 Zr1 C5 88.66(5) . . ?
C1 Zr1 C5 32.70(6) . . ?
C2 Zr1 C5 54.42(6) . . ?
N1 Zr1 C3 99.14(6) 2_566 . ?
N1 Zr1 C3 141.77(6) . . ?
Cl1 Zr1 C3 108.26(5) . . ?
C1 Zr1 C3 54.12(6) . . ?
C2 Zr1 C3 32.60(6) . . ?
C5 Zr1 C3 53.99(6) . . ?
N1 Zr1 C4 126.04(6) 2_566 . ?
N1 Zr1 C4 143.89(6) . . ?
Cl1 Zr1 C4 82.16(5) . . ?
C1 Zr1 C4 53.78(6) . . ?
C2 Zr1 C4 53.86(6) . . ?
C5 Zr1 C4 32.42(6) . . ?
C3 Zr1 C4 32.31(6) . . ?
N1 Zr1 Zr1 44.49(4) 2_566 2_566 ?
N1 Zr1 Zr1 41.30(4) . 2_566 ?
Cl1 Zr1 Zr1 113.113(16) . 2_566 ?
C1 Zr1 Zr1 118.22(5) . 2_566 ?
C2 Zr1 Zr1 110.67(5) . 2_566 ?
C5 Zr1 Zr1 147.80(5) . 2_566 ?
C3 Zr1 Zr1 131.08(5) . 2_566 ?
C4 Zr1 Zr1 163.14(5) . 2_566 ?
C10 N1 Zr1 153.06(13) . 2_566 ?
C10 N1 Zr1 111.79(11) . . ?
Zr1 N1 Zr1 94.22(6) 2_566 . ?
C4 C3 C2 107.93(17) . . ?
C4 C3 C7 124.86(19) . . ?
C2 C3 C7 127.06(19) . . ?
C4 C3 Zr1 74.22(11) . . ?
C2 C3 Zr1 72.50(11) . . ?
C7 C3 Zr1 122.65(14) . . ?
C11 C16 C17 109.63(17) . . ?
C11 C16 C18 113.06(17) . . ?
C17 C16 C18 108.08(17) . . ?
C11 C16 H16 108.6 . . ?
C17 C16 H16 108.7 . . ?
C18 C16 H16 108.6 . . ?
C12 C11 C10 118.91(18) . . ?
C12 C11 C16 116.84(17) . . ?
C10 C11 C16 124.14(17) . . ?
C11 C10 C15 117.98(17) . . ?
C11 C10 N1 123.18(17) . . ?
C15 C10 N1 118.81(16) . . ?
C13 C12 C11 122.22(19) . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 119.0 . . ?
C2 C6 H6A 109.6 . . ?
C2 C6 H6B 109.4 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C2 C1 107.31(17) . . ?
C3 C2 C6 126.84(19) . . ?
C1 C2 C6 125.46(19) . . ?
C3 C2 Zr1 74.90(11) . . ?
C1 C2 Zr1 72.33(11) . . ?
C6 C2 Zr1 123.90(14) . . ?
C19 C21 H21A 109.4 . . ?
C19 C21 H21B 109.7 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.3 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C1 C5 C4 107.23(17) . . ?
C1 C5 C9 126.48(18) . . ?
C4 C5 C9 126.28(18) . . ?
C1 C5 Zr1 71.84(11) . . ?
C4 C5 Zr1 74.72(11) . . ?
C9 C5 Zr1 120.10(13) . . ?
C14 C15 C10 119.62(18) . . ?
C14 C15 C19 119.44(17) . . ?
C10 C15 C19 120.81(17) . . ?
C3 C4 C5 108.51(17) . . ?
C3 C4 C8 125.11(18) . . ?
C5 C4 C8 126.23(18) . . ?
C3 C4 Zr1 73.48(11) . . ?
C5 C4 Zr1 72.86(11) . . ?
C8 C4 Zr1 123.23(14) . . ?
C5 C9 H9A 109.3 . . ?
C5 C9 H9B 109.6 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C13 C14 C15 121.56(19) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.1 . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.4 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.3 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C5 C1 C2 109.01(17) . . ?
C5 C1 Zr1 75.47(11) . . ?
C2 C1 Zr1 74.65(11) . . ?
C5 C1 H1 125.5 . . ?
C2 C1 H1 125.5 . . ?
Zr1 C1 H1 116.4 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.6 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.3 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C15 C19 C21 114.79(17) . . ?
C15 C19 C20 108.69(16) . . ?
C21 C19 C20 109.66(17) . . ?
C15 C19 H19 107.8 . . ?
C21 C19 H19 107.8 . . ?
C20 C19 H19 107.9 . . ?
C4 C8 H8A 109.4 . . ?
C4 C8 H8B 109.4 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.6 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.4 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.6 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C13 C14 119.26(19) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 1044558'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H64 Cl2 N2 Zr2'
_chemical_formula_sum            'C44 H64 Cl2 N2 Zr2'
_chemical_formula_weight         874.31

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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   21.2253(6)
_cell_length_b                   18.0580(3)
_cell_length_c                   11.1202(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.141(3)
_cell_angle_gamma                90
_cell_volume                     4237.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    17975
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    0.650
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.140
-1 0 0 0.082
1 0 -1 0.110
-1 0 1 0.140
0 1 0 0.199
0 -1 0 0.140
1 0 1 0.150


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17895
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4797
_reflns_number_gt                3584
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0533P)²+23.2009P] where P=(Fo²+2Fc²)/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         4797
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1522
_refine_ls_wR_factor_gt          0.1289
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_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 0.22778(2) 0.29382(2) 0.38370(4) 0.03482(15) Uani 1 1 d . . .
Cl1 Cl 0.21945(7) 0.42693(7) 0.40844(13) 0.0574(3) Uani 1 1 d . . .
C1 C 0.2139(3) 0.2062(3) 0.2116(4) 0.0495(12) Uani 1 1 d . . .
N1 N 0.31349(17) 0.2574(2) 0.4736(4) 0.0406(9) Uani 1 1 d . . .
C11 C 0.3794(2) 0.2635(3) 0.4539(4) 0.0387(10) Uani 1 1 d . . .
C2 C 0.2528(3) 0.2649(4) 0.1729(4) 0.0666(18) Uani 1 1 d . . .
C12 C 0.4098(2) 0.3341(3) 0.4596(4) 0.0435(11) Uani 1 1 d . . .
C16 C 0.4161(2) 0.2010(3) 0.4288(5) 0.0476(11) Uani 1 1 d . . .
C15 C 0.4794(3) 0.2104(4) 0.4117(6) 0.0647(16) Uani 1 1 d . . .
H15 H 0.5032 0.1692 0.3945 0.078 Uiso 1 1 d R . .
C13 C 0.4733(3) 0.3382(4) 0.4415(6) 0.0656(16) Uani 1 1 d . . .
H13 H 0.4929 0.3843 0.4448 0.079 Uiso 1 1 d R . .
C5 C 0.1527(3) 0.2384(4) 0.2164(5) 0.0641(15) Uani 1 1 d . . .
C17 C 0.3769(3) 0.4063(3) 0.4766(7) 0.0652(17) Uani 1 1 d . . .
H17 H 0.3353 0.3958 0.5031 0.078 Uiso 1 1 d R . .
C9 C 0.0961(5) 0.3643(6) 0.1731(9) 0.122(4) Uani 1 1 d . . .
H9A H 0.0644 0.3472 0.2220 0.146 Uiso 1 1 d R . .
H9B H 0.0787 0.3657 0.0898 0.146 Uiso 1 1 d R . .
H9C H 0.1097 0.4131 0.1987 0.146 Uiso 1 1 d R . .
C18 C 0.3658(5) 0.4428(6) 0.3524(11) 0.150(5) Uani 1 1 d . . .
H18A H 0.4062 0.4501 0.3227 0.180 Uiso 1 1 d R . .
H18B H 0.3454 0.4898 0.3590 0.180 Uiso 1 1 d R . .
H18C H 0.3399 0.4117 0.2973 0.180 Uiso 1 1 d R . .
C4 C 0.1519(3) 0.3120(5) 0.1873(6) 0.0757(19) Uani 1 1 d . . .
C6 C 0.2278(3) 0.1262(3) 0.2291(6) 0.0693(17) Uani 1 1 d . . .
H6A H 0.2343 0.1146 0.3138 0.083 Uiso 1 1 d R . .
H6B H 0.2654 0.1145 0.1921 0.083 Uiso 1 1 d R . .
H6C H 0.1929 0.0976 0.1916 0.083 Uiso 1 1 d R . .
C3 C 0.2115(4) 0.3285(3) 0.1585(5) 0.0647(17) Uani 1 1 d . . .
C20 C 0.3911(3) 0.1223(3) 0.4099(6) 0.0664(16) Uani 1 1 d . . .
H20 H 0.3455 0.1225 0.4170 0.080 Uiso 1 1 d R . .
C7 C 0.3178(3) 0.2575(5) 0.1424(6) 0.088(2) Uani 1 1 d . . .
H7A H 0.3312 0.2069 0.1518 0.105 Uiso 1 1 d R . .
H7B H 0.3448 0.2884 0.1961 0.105 Uiso 1 1 d R . .
H7C H 0.3204 0.2729 0.0604 0.105 Uiso 1 1 d R . .
C8 C 0.2320(5) 0.4036(5) 0.1088(7) 0.103(3) Uani 1 1 d . . .
H8A H 0.2084 0.4129 0.0317 0.124 Uiso 1 1 d R . .
H8B H 0.2765 0.4022 0.0996 0.124 Uiso 1 1 d R . .
H8C H 0.2239 0.4424 0.1641 0.124 Uiso 1 1 d R . .
C10 C 0.0933(3) 0.1972(6) 0.2362(8) 0.104(3) Uani 1 1 d . . .
H10A H 0.0751 0.2193 0.3031 0.125 Uiso 1 1 d R . .
H10B H 0.1032 0.1463 0.2543 0.125 Uiso 1 1 d R . .
H10C H 0.0635 0.2000 0.1650 0.125 Uiso 1 1 d R . .
C19 C 0.4123(5) 0.4599(5) 0.5612(12) 0.153(5) Uani 1 1 d . . .
H19A H 0.4274 0.4333 0.6334 0.183 Uiso 1 1 d R . .
H19B H 0.3842 0.4986 0.5809 0.183 Uiso 1 1 d R . .
H19C H 0.4477 0.4811 0.5263 0.183 Uiso 1 1 d R . .
C14 C 0.5082(3) 0.2774(4) 0.4189(8) 0.089(2) Uani 1 1 d . . .
H14 H 0.5508 0.2818 0.4077 0.106 Uiso 1 1 d R . .
C21 C 0.4016(4) 0.0912(4) 0.2826(8) 0.098(3) Uani 1 1 d . . .
H21A H 0.3882 0.1271 0.2215 0.117 Uiso 1 1 d R . .
H21B H 0.3774 0.0465 0.2676 0.117 Uiso 1 1 d R . .
H21C H 0.4458 0.0806 0.2805 0.117 Uiso 1 1 d R . .
C22 C 0.4228(4) 0.0707(5) 0.5025(10) 0.108(3) Uani 1 1 d . . .
H22A H 0.4676 0.0700 0.4967 0.129 Uiso 1 1 d R . .
H22B H 0.4059 0.0217 0.4887 0.129 Uiso 1 1 d R . .
H22C H 0.4150 0.0871 0.5817 0.129 Uiso 1 1 d 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 2.086(4) . ?
Zr1 N1 2.106(4) 7_556 ?
Zr1 Cl1 2.4280(14) . ?
Zr1 C1 2.477(5) . ?
Zr1 C2 2.513(5) . ?
Zr1 C5 2.524(5) . ?
Zr1 C3 2.568(5) . ?
Zr1 C4 2.591(6) . ?
Zr1 Zr1 3.0924(8) 7_556 ?
C1 C5 1.429(9) . ?
C1 C2 1.437(8) . ?
C1 C6 1.483(8) . ?
N1 C11 1.444(5) . ?
N1 Zr1 2.106(4) 7_556 ?
C11 C16 1.415(7) . ?
C11 C12 1.426(7) . ?
C2 C3 1.443(10) . ?
C2 C7 1.463(9) . ?
C12 C13 1.386(7) . ?
C12 C17 1.501(8) . ?
C16 C15 1.389(7) . ?
C16 C20 1.523(8) . ?
C15 C14 1.354(9) . ?
C15 H15 0.9299 . ?
C13 C14 1.364(9) . ?
C13 H13 0.9300 . ?
C5 C4 1.368(10) . ?
C5 C10 1.500(10) . ?
C17 C19 1.495(11) . ?
C17 C18 1.526(11) . ?
C17 H17 0.9798 . ?
C9 C4 1.510(11) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9599 . ?
C9 H9C 0.9600 . ?
C18 H18A 0.9601 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9601 . ?
C4 C3 1.369(10) . ?
C6 H6A 0.9601 . ?
C6 H6B 0.9599 . ?
C6 H6C 0.9601 . ?
C3 C8 1.545(9) . ?
C20 C22 1.494(10) . ?
C20 C21 1.562(10) . ?
C20 H20 0.9801 . ?
C7 H7A 0.9598 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9601 . ?
C8 H8B 0.9599 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9599 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9601 . ?
C14 H14 0.9298 . ?
C21 H21A 0.9601 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9601 . ?
C22 H22B 0.9599 . ?
C22 H22C 0.9601 . ?

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 84.96(14) . 7_556 ?
N1 Zr1 Cl1 109.17(11) . . ?
N1 Zr1 Cl1 107.94(11) 7_556 . ?
N1 Zr1 C1 101.22(17) . . ?
N1 Zr1 C1 106.07(16) 7_556 . ?
Cl1 Zr1 C1 135.74(13) . . ?
N1 Zr1 C2 96.96(19) . . ?
N1 Zr1 C2 139.24(19) 7_556 . ?
Cl1 Zr1 C2 109.69(18) . . ?
C1 Zr1 C2 33.47(19) . . ?
N1 Zr1 C5 132.66(19) . . ?
N1 Zr1 C5 95.76(19) 7_556 . ?
Cl1 Zr1 C5 115.37(16) . . ?
C1 Zr1 C5 33.2(2) . . ?
C2 Zr1 C5 53.8(2) . . ?
N1 Zr1 C3 124.3(2) . . ?
N1 Zr1 C3 144.9(2) 7_556 . ?
Cl1 Zr1 C3 82.27(14) . . ?
C1 Zr1 C3 53.83(18) . . ?
C2 Zr1 C3 33.0(2) . . ?
C5 Zr1 C3 50.9(2) . . ?
N1 Zr1 C4 151.0(2) . . ?
N1 Zr1 C4 114.8(2) 7_556 . ?
Cl1 Zr1 C4 85.64(18) . . ?
C1 Zr1 C4 54.4(2) . . ?
C2 Zr1 C4 54.2(2) . . ?
C5 Zr1 C4 31.0(2) . . ?
C3 Zr1 C4 30.8(2) . . ?
N1 Zr1 Zr1 42.72(10) . 7_556 ?
N1 Zr1 Zr1 42.23(11) 7_556 7_556 ?
Cl1 Zr1 Zr1 115.55(4) . 7_556 ?
C1 Zr1 Zr1 108.65(13) . 7_556 ?
C2 Zr1 Zr1 126.71(18) . 7_556 ?
C5 Zr1 Zr1 121.71(16) . 7_556 ?
C3 Zr1 Zr1 159.61(15) . 7_556 ?
C4 Zr1 Zr1 151.17(19) . 7_556 ?
C5 C1 C2 105.3(6) . . ?
C5 C1 C6 124.1(6) . . ?
C2 C1 C6 130.2(6) . . ?
C5 C1 Zr1 75.2(3) . . ?
C2 C1 Zr1 74.6(3) . . ?
C6 C1 Zr1 121.0(3) . . ?
C11 N1 Zr1 135.5(3) . . ?
C11 N1 Zr1 129.5(3) . 7_556 ?
Zr1 N1 Zr1 95.05(14) . 7_556 ?
C16 C11 C12 117.8(4) . . ?
C16 C11 N1 122.1(4) . . ?
C12 C11 N1 120.2(4) . . ?
C1 C2 C3 105.0(5) . . ?
C1 C2 C7 126.1(7) . . ?
C3 C2 C7 128.5(7) . . ?
C1 C2 Zr1 71.9(3) . . ?
C3 C2 Zr1 75.6(3) . . ?
C7 C2 Zr1 122.3(4) . . ?
C13 C12 C11 118.9(5) . . ?
C13 C12 C17 116.3(5) . . ?
C11 C12 C17 124.6(4) . . ?
C15 C16 C11 119.4(5) . . ?
C15 C16 C20 115.0(5) . . ?
C11 C16 C20 125.5(4) . . ?
C14 C15 C16 122.5(6) . . ?
C14 C15 H15 118.4 . . ?
C16 C15 H15 119.1 . . ?
C14 C13 C12 122.6(6) . . ?
C14 C13 H13 118.6 . . ?
C12 C13 H13 118.8 . . ?
C4 C5 C1 112.0(6) . . ?
C4 C5 C10 121.9(7) . . ?
C1 C5 C10 125.8(7) . . ?
C4 C5 Zr1 77.2(4) . . ?
C1 C5 Zr1 71.6(3) . . ?
C10 C5 Zr1 124.2(5) . . ?
C19 C17 C12 115.7(7) . . ?
C19 C17 C18 108.0(8) . . ?
C12 C17 C18 106.8(6) . . ?
C19 C17 H17 110.2 . . ?
C12 C17 H17 108.4 . . ?
C18 C17 H17 107.4 . . ?
C4 C9 H9A 109.3 . . ?
C4 C9 H9B 109.6 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.6 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C17 C18 H18A 108.3 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 110.3 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C5 C4 C3 106.2(6) . . ?
C5 C4 C9 128.4(8) . . ?
C3 C4 C9 125.0(8) . . ?
C5 C4 Zr1 71.8(3) . . ?
C3 C4 Zr1 73.7(3) . . ?
C9 C4 Zr1 125.3(5) . . ?
C1 C6 H6A 110.3 . . ?
C1 C6 H6B 108.7 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.4 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C3 C2 111.5(6) . . ?
C4 C3 C8 125.2(7) . . ?
C2 C3 C8 123.2(7) . . ?
C4 C3 Zr1 75.5(4) . . ?
C2 C3 Zr1 71.4(3) . . ?
C8 C3 Zr1 123.3(4) . . ?
C22 C20 C16 111.3(6) . . ?
C22 C20 C21 107.6(6) . . ?
C16 C20 C21 112.3(5) . . ?
C22 C20 H20 108.8 . . ?
C16 C20 H20 108.5 . . ?
C21 C20 H20 108.2 . . ?
C2 C7 H7A 109.7 . . ?
C2 C7 H7B 108.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 110.2 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.4 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C10 H10A 108.8 . . ?
C5 C10 H10B 109.7 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 110.0 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C17 C19 H19A 107.6 . . ?
C17 C19 H19B 109.4 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 111.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C14 C13 118.7(5) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.8 . . ?
C20 C21 H21A 109.8 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.1 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.8 . . ?
C20 C22 H22B 109.4 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.3 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.098
####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 1044559'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H60 Cl2 Hf2 N2'
_chemical_formula_sum            'C42 H60 Cl2 Hf2 N2'
_chemical_formula_weight         1020.80

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'
Hf Hf -0.5830 6.1852 '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'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1859(5)
_cell_length_b                   10.5241(9)
_cell_length_c                   10.6120(7)
_cell_angle_alpha                113.815(5)
_cell_angle_beta                 103.680(4)
_cell_angle_gamma                98.356(5)
_cell_volume                     973.38(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    20069
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504
_exptl_absorpt_coefficient_mu    5.498
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.056
1 0 0 0.025
0 0 1 0.053
0 0 -1 0.012
0 -1 0 0.020
0 1 0 0.065


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19985
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4456
_reflns_number_gt                4166
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0390P)²+1.0782P] where P=(Fo²+2Fc²)/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         4456
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_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 0.381583(13) 0.019147(14) 0.397465(14) 0.01304(6) Uani 1 1 d . . .
Cl1 Cl 0.39195(9) -0.07379(10) 0.15487(9) 0.02173(18) Uani 1 1 d . . .
C5 C 0.8716(4) 0.4773(4) 0.7793(4) 0.0215(8) Uani 1 1 d . . .
H5 H 0.9037 0.5507 0.8745 0.026 Uiso 1 1 d R . .
N1 N 0.5778(3) 0.1383(3) 0.5342(3) 0.0135(5) Uani 1 1 d . . .
C16 C 0.1855(4) 0.1070(4) 0.2911(4) 0.0195(7) Uani 1 1 d . . .
C7 C 0.7167(4) 0.1630(4) 0.3300(4) 0.0190(7) Uani 1 1 d . . .
H7 H 0.6558 0.0740 0.3161 0.023 Uiso 1 1 d R . .
C9 C 0.6255(4) 0.2320(4) 0.2541(4) 0.0261(8) Uani 1 1 d . . .
H9A H 0.5539 0.2547 0.2974 0.031 Uiso 1 1 d R . .
H9B H 0.5826 0.1655 0.1525 0.031 Uiso 1 1 d R . .
H9C H 0.6831 0.3187 0.2645 0.031 Uiso 1 1 d R . .
C17 C 0.1220(4) -0.0212(4) 0.2943(4) 0.0191(7) Uani 1 1 d . . .
C15 C 0.2555(4) 0.2142(4) 0.4379(4) 0.0201(7) Uani 1 1 d . . .
C14 C 0.2365(4) 0.1531(4) 0.5321(4) 0.0188(7) Uani 1 1 d . . .
C1 C 0.6963(3) 0.2598(4) 0.5864(4) 0.0151(7) Uani 1 1 d . . .
C13 C 0.1543(4) 0.0081(4) 0.4420(4) 0.0196(7) Uani 1 1 d . . .
H13 H 0.1261 -0.0573 0.4751 0.023 Uiso 1 1 d R . .
C3 C 0.9010(4) 0.3687(4) 0.5470(4) 0.0220(8) Uani 1 1 d . . .
H3 H 0.9530 0.3681 0.4857 0.026 Uiso 1 1 d R . .
C8 C 0.8270(5) 0.1228(5) 0.2575(5) 0.0296(9) Uani 1 1 d . . .
H8A H 0.8752 0.2043 0.2512 0.036 Uiso 1 1 d R . .
H8B H 0.7818 0.0444 0.1613 0.036 Uiso 1 1 d R . .
H8C H 0.8932 0.0939 0.3139 0.036 Uiso 1 1 d R . .
C6 C 0.7433(4) 0.3739(4) 0.7309(4) 0.0172(7) Uani 1 1 d . . .
C2 C 0.7742(4) 0.2649(4) 0.4923(4) 0.0175(7) Uani 1 1 d . . .
C10 C 0.6606(4) 0.3986(4) 0.8367(4) 0.0191(7) Uani 1 1 d . . .
H10 H 0.5803 0.3139 0.7962 0.023 Uiso 1 1 d R . .
C21 C 0.0325(4) -0.1604(4) 0.1635(4) 0.0239(8) Uani 1 1 d . . .
H21A H 0.0340 -0.2388 0.1879 0.029 Uiso 1 1 d R . .
H21B H 0.0687 -0.1767 0.0842 0.029 Uiso 1 1 d R . .
H21C H -0.0622 -0.1543 0.1353 0.029 Uiso 1 1 d R . .
C11 C 0.7479(4) 0.4222(4) 0.9872(4) 0.0241(8) Uani 1 1 d . . .
H11A H 0.8018 0.3531 0.9759 0.029 Uiso 1 1 d R . .
H11B H 0.6869 0.4105 1.0406 0.029 Uiso 1 1 d R . .
H11C H 0.8101 0.5180 1.0396 0.029 Uiso 1 1 d R . .
C4 C 0.9515(4) 0.4735(4) 0.6912(5) 0.0264(8) Uani 1 1 d . . .
H4 H 1.0385 0.5401 0.7274 0.032 Uiso 1 1 d R . .
C12 C 0.6052(4) 0.5309(4) 0.8552(5) 0.0278(9) Uani 1 1 d . . .
H12A H 0.6830 0.6153 0.8986 0.033 Uiso 1 1 d R . .
H12B H 0.5480 0.5426 0.9170 0.033 Uiso 1 1 d R . .
H12C H 0.5502 0.5177 0.7617 0.033 Uiso 1 1 d R . .
C20 C 0.1707(5) 0.1295(5) 0.1572(5) 0.0289(9) Uani 1 1 d . . .
H20A H 0.1392 0.0376 0.0720 0.035 Uiso 1 1 d R . .
H20B H 0.2600 0.1815 0.1645 0.035 Uiso 1 1 d R . .
H20C H 0.1037 0.1838 0.1500 0.035 Uiso 1 1 d R . .
C19 C 0.3289(5) 0.3675(4) 0.4827(5) 0.0280(9) Uani 1 1 d . . .
H19A H 0.3188 0.4298 0.5732 0.034 Uiso 1 1 d R . .
H19B H 0.2877 0.3940 0.4089 0.034 Uiso 1 1 d R . .
H19C H 0.4268 0.3770 0.4943 0.034 Uiso 1 1 d R . .
C18 C 0.2759(4) 0.2308(5) 0.6945(4) 0.0285(9) Uani 1 1 d . . .
H18A H 0.3546 0.3134 0.7327 0.034 Uiso 1 1 d R . .
H18B H 0.3004 0.1672 0.7348 0.034 Uiso 1 1 d R . .
H18C H 0.1976 0.2616 0.7201 0.034 Uiso 1 1 d 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 N1 2.026(3) . ?
Hf1 N1 2.115(3) 2_656 ?
Hf1 Cl1 2.3918(9) . ?
Hf1 C13 2.466(3) . ?
Hf1 C14 2.488(4) . ?
Hf1 C17 2.509(3) . ?
Hf1 C15 2.522(4) . ?
Hf1 C16 2.536(4) . ?
Hf1 Hf1 3.0373(3) 2_656 ?
C5 C4 1.370(6) . ?
C5 C6 1.405(5) . ?
C5 H5 0.9300 . ?
N1 C1 1.435(4) . ?
N1 Hf1 2.115(3) 2_656 ?
C16 C15 1.424(5) . ?
C16 C17 1.426(5) . ?
C16 C20 1.510(6) . ?
C7 C2 1.519(5) . ?
C7 C8 1.522(5) . ?
C7 C9 1.533(5) . ?
C7 H7 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9601 . ?
C17 C13 1.412(5) . ?
C17 C21 1.509(5) . ?
C15 C14 1.423(5) . ?
C15 C19 1.500(5) . ?
C14 C13 1.420(5) . ?
C14 C18 1.496(5) . ?
C1 C6 1.422(5) . ?
C1 C2 1.427(5) . ?
C13 H13 0.9300 . ?
C3 C4 1.386(6) . ?
C3 C2 1.386(5) . ?
C3 H3 0.9299 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9599 . ?
C8 H8C 0.9600 . ?
C6 C10 1.520(5) . ?
C10 C11 1.532(5) . ?
C10 C12 1.535(5) . ?
C10 H10 0.9800 . ?
C21 H21A 0.9601 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C4 H4 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9599 . ?
C18 H18C 0.9601 . ?

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 Hf1 N1 85.65(11) . 2_656 ?
N1 Hf1 Cl1 107.14(8) . . ?
N1 Hf1 Cl1 105.14(8) 2_656 . ?
N1 Hf1 C13 130.32(12) . . ?
N1 Hf1 C13 92.98(11) 2_656 . ?
Cl1 Hf1 C13 120.92(9) . . ?
N1 Hf1 C14 101.11(12) . . ?
N1 Hf1 C14 108.80(11) 2_656 . ?
Cl1 Hf1 C14 136.97(9) . . ?
C13 Hf1 C14 33.30(12) . . ?
N1 Hf1 C17 154.08(12) . . ?
N1 Hf1 C17 110.31(11) 2_656 . ?
Cl1 Hf1 C17 88.78(9) . . ?
C13 Hf1 C17 32.97(13) . . ?
C14 Hf1 C17 55.07(12) . . ?
N1 Hf1 C15 100.30(12) . . ?
N1 Hf1 C15 141.78(12) 2_656 . ?
Cl1 Hf1 C15 108.87(9) . . ?
C13 Hf1 C15 54.49(12) . . ?
C14 Hf1 C15 32.98(12) . . ?
C17 Hf1 C15 54.45(12) . . ?
N1 Hf1 C16 127.48(12) . . ?
N1 Hf1 C16 143.06(11) 2_656 . ?
Cl1 Hf1 C16 82.24(9) . . ?
C13 Hf1 C16 54.44(12) . . ?
C14 Hf1 C16 54.76(12) . . ?
C17 Hf1 C16 32.82(12) . . ?
C15 Hf1 C16 32.71(12) . . ?
N1 Hf1 Hf1 43.97(8) . 2_656 ?
N1 Hf1 Hf1 41.68(8) 2_656 2_656 ?
Cl1 Hf1 Hf1 112.24(2) . 2_656 ?
C13 Hf1 Hf1 117.89(9) . 2_656 ?
C14 Hf1 Hf1 110.66(9) . 2_656 ?
C17 Hf1 Hf1 147.30(9) . 2_656 ?
C15 Hf1 Hf1 131.78(9) . 2_656 ?
C16 Hf1 Hf1 164.22(9) . 2_656 ?
C4 C5 C6 122.3(4) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.9 . . ?
C1 N1 Hf1 150.2(2) . . ?
C1 N1 Hf1 114.7(2) . 2_656 ?
Hf1 N1 Hf1 94.35(11) . 2_656 ?
C15 C16 C17 107.7(3) . . ?
C15 C16 C20 125.9(3) . . ?
C17 C16 C20 126.2(4) . . ?
C15 C16 Hf1 73.1(2) . . ?
C17 C16 Hf1 72.6(2) . . ?
C20 C16 Hf1 124.0(3) . . ?
C2 C7 C8 115.2(3) . . ?
C2 C7 C9 108.4(3) . . ?
C8 C7 C9 109.4(3) . . ?
C2 C7 H7 107.8 . . ?
C8 C7 H7 108.0 . . ?
C9 C7 H7 107.8 . . ?
C7 C9 H9A 109.7 . . ?
C7 C9 H9B 109.3 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.4 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C13 C17 C16 107.5(3) . . ?
C13 C17 C21 126.6(3) . . ?
C16 C17 C21 125.9(4) . . ?
C13 C17 Hf1 71.81(19) . . ?
C16 C17 Hf1 74.6(2) . . ?
C21 C17 Hf1 120.9(2) . . ?
C14 C15 C16 108.5(3) . . ?
C14 C15 C19 126.7(4) . . ?
C16 C15 C19 124.7(4) . . ?
C14 C15 Hf1 72.2(2) . . ?
C16 C15 Hf1 74.2(2) . . ?
C19 C15 Hf1 122.4(3) . . ?
C13 C14 C15 106.9(3) . . ?
C13 C14 C18 125.5(4) . . ?
C15 C14 C18 127.0(4) . . ?
C13 C14 Hf1 72.5(2) . . ?
C15 C14 Hf1 74.8(2) . . ?
C18 C14 Hf1 124.8(3) . . ?
C6 C1 C2 118.0(3) . . ?
C6 C1 N1 122.7(3) . . ?
C2 C1 N1 119.3(3) . . ?
C17 C13 C14 109.3(3) . . ?
C17 C13 Hf1 75.2(2) . . ?
C14 C13 Hf1 74.2(2) . . ?
C17 C13 H13 125.4 . . ?
C14 C13 H13 125.3 . . ?
Hf1 C13 H13 117.2 . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.3 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C6 C1 118.8(3) . . ?
C5 C6 C10 116.4(3) . . ?
C1 C6 C10 124.7(3) . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 C7 118.8(3) . . ?
C1 C2 C7 121.0(3) . . ?
C6 C10 C11 113.0(3) . . ?
C6 C10 C12 109.7(3) . . ?
C11 C10 C12 108.5(3) . . ?
C6 C10 H10 108.7 . . ?
C11 C10 H10 108.4 . . ?
C12 C10 H10 108.5 . . ?
C17 C21 H21A 109.4 . . ?
C17 C21 H21B 109.6 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.3 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.3 . . ?
C10 C12 H12A 109.3 . . ?
C10 C12 H12B 109.6 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C16 C20 H20A 109.6 . . ?
C16 C20 H20B 109.3 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.6 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C19 H19A 109.4 . . ?
C15 C19 H19B 109.2 . . ?
H19A C19 H19B 109.5 . . ?
C15 C19 H19C 109.8 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C18 H18A 109.6 . . ?
C14 C18 H18B 109.6 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.2 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.763
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.156
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 1044560'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H64 Cl2 Hf2 N2'
_chemical_formula_sum            'C44 H64 Cl2 Hf2 N2'
_chemical_formula_weight         1048.85

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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   21.2660(3)
_cell_length_b                   18.0465(6)
_cell_length_c                   11.0391(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.851(4)
_cell_angle_gamma                90
_cell_volume                     4214.48(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    19301
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    5.082
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.075
0 1 1 0.110
0 -1 1 0.085
0 1 -1 0.079
1 0 0 0.117
-1 0 0 0.028


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19227
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4806
_reflns_number_gt                3852
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0283P)²+34.6111P] where P=(Fo²+2Fc²)/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         4806
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_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 0.273806(11) 0.293162(12) 0.11545(2) 0.02912(9) Uani 1 1 d . . .
Cl1 Cl 0.28165(8) 0.42479(9) 0.08706(16) 0.0464(4) Uani 1 1 d . . .
N1 N 0.1878(2) 0.2572(3) 0.0319(4) 0.0318(10) Uani 1 1 d . . .
C11 C 0.1218(3) 0.2629(3) 0.0504(5) 0.0313(11) Uani 1 1 d . . .
C1 C 0.2893(4) 0.3317(4) 0.3390(5) 0.0444(15) Uani 1 1 d . . .
C12 C 0.0858(3) 0.1993(4) 0.0773(6) 0.0389(14) Uani 1 1 d . . .
C5 C 0.2503(3) 0.2671(4) 0.3285(5) 0.0416(15) Uani 1 1 d . . .
C16 C 0.0906(3) 0.3324(4) 0.0439(6) 0.0388(13) Uani 1 1 d . . .
C15 C 0.0264(3) 0.3361(4) 0.0571(7) 0.0504(17) Uani 1 1 d . . .
H15 H 0.0067 0.3821 0.0508 0.060 Uiso 1 1 d R . .
C3 C 0.3490(3) 0.2375(4) 0.2795(6) 0.0473(16) Uani 1 1 d . . .
C2 C 0.3502(3) 0.3115(4) 0.3085(6) 0.0478(16) Uani 1 1 d . . .
C20 C 0.1241(4) 0.4057(4) 0.0325(7) 0.0517(17) Uani 1 1 d . . .
H20 H 0.1646 0.3955 0.0004 0.062 Uiso 1 1 d R . .
C17 C 0.1107(3) 0.1215(4) 0.0992(7) 0.0479(16) Uani 1 1 d . . .
H17 H 0.1562 0.1224 0.0920 0.057 Uiso 1 1 d R . .
C9 C 0.2694(4) 0.1276(4) 0.2761(7) 0.0582(19) Uani 1 1 d . . .
H9A H 0.2887 0.1052 0.2102 0.070 Uiso 1 1 d R . .
H9B H 0.2242 0.1238 0.2605 0.070 Uiso 1 1 d R . .
H9C H 0.2832 0.1024 0.3507 0.070 Uiso 1 1 d R . .
C19 C 0.0801(4) 0.0670(5) 0.0062(9) 0.070(2) Uani 1 1 d . . .
H19A H 0.0354 0.0647 0.0120 0.084 Uiso 1 1 d R . .
H19B H 0.0982 0.0186 0.0207 0.084 Uiso 1 1 d R . .
H19C H 0.0876 0.0835 -0.0737 0.084 Uiso 1 1 d R . .
C4 C 0.2872(3) 0.2074(4) 0.2879(5) 0.0396(14) Uani 1 1 d . . .
C18 C 0.1006(4) 0.0935(5) 0.2275(8) 0.061(2) Uani 1 1 d . . .
H18A H 0.1146 0.1306 0.2866 0.073 Uiso 1 1 d R . .
H18B H 0.1246 0.0489 0.2440 0.073 Uiso 1 1 d R . .
H18C H 0.0566 0.0834 0.2320 0.073 Uiso 1 1 d R . .
C14 C -0.0088(4) 0.2751(5) 0.0779(8) 0.064(2) Uani 1 1 d . . .
H14 H -0.0519 0.2792 0.0855 0.077 Uiso 1 1 d R . .
C13 C 0.0212(3) 0.2085(4) 0.0883(8) 0.0556(19) Uani 1 1 d . . .
H13 H -0.0024 0.1667 0.1032 0.067 Uiso 1 1 d R . .
C8 C 0.4066(4) 0.1922(5) 0.2576(8) 0.069(2) Uani 1 1 d . . .
H8A H 0.3946 0.1418 0.2397 0.082 Uiso 1 1 d R . .
H8B H 0.4368 0.1936 0.3285 0.082 Uiso 1 1 d R . .
H8C H 0.4251 0.2132 0.1896 0.082 Uiso 1 1 d R . .
C7 C 0.4059(4) 0.3634(6) 0.3188(8) 0.074(3) Uani 1 1 d . . .
H7A H 0.3919 0.4119 0.2928 0.089 Uiso 1 1 d R . .
H7B H 0.4370 0.3462 0.2681 0.089 Uiso 1 1 d R . .
H7C H 0.4242 0.3655 0.4019 0.089 Uiso 1 1 d R . .
C10 C 0.1843(4) 0.2609(5) 0.3626(6) 0.0562(19) Uani 1 1 d . . .
H10A H 0.1569 0.2425 0.2948 0.067 Uiso 1 1 d R . .
H10B H 0.1701 0.3089 0.3853 0.067 Uiso 1 1 d R . .
H10C H 0.1836 0.2275 0.4303 0.067 Uiso 1 1 d R . .
C6 C 0.2720(5) 0.4052(5) 0.3905(7) 0.065(2) Uani 1 1 d . . .
H6A H 0.2930 0.4114 0.4710 0.078 Uiso 1 1 d R . .
H6B H 0.2270 0.4067 0.3937 0.078 Uiso 1 1 d R . .
H6C H 0.2843 0.4444 0.3391 0.078 Uiso 1 1 d R . .
C21 C 0.1377(5) 0.4369(6) 0.1621(10) 0.091(3) Uani 1 1 d . . .
H21A H 0.0990 0.4414 0.1994 0.110 Uiso 1 1 d R . .
H21B H 0.1571 0.4847 0.1585 0.110 Uiso 1 1 d R . .
H21C H 0.1658 0.4039 0.2094 0.110 Uiso 1 1 d R . .
C22 C 0.0894(5) 0.4638(5) -0.0479(11) 0.091(3) Uani 1 1 d . . .
H22A H 0.0709 0.4407 -0.1214 0.109 Uiso 1 1 d R . .
H22B H 0.1187 0.5013 -0.0677 0.109 Uiso 1 1 d R . .
H22C H 0.0568 0.4860 -0.0059 0.109 Uiso 1 1 d 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 N1 2.067(5) . ?
Hf1 N1 2.100(5) 7 ?
Hf1 Cl1 2.4040(16) . ?
Hf1 C4 2.448(6) . ?
Hf1 C5 2.498(6) . ?
Hf1 C3 2.502(7) . ?
Hf1 C1 2.552(6) . ?
Hf1 C2 2.566(7) . ?
Hf1 Hf1 3.0696(4) 7 ?
N1 C11 1.443(7) . ?
N1 Hf1 2.100(5) 7 ?
C11 C16 1.418(9) . ?
C11 C12 1.427(8) . ?
C1 C2 1.420(10) . ?
C1 C5 1.428(10) . ?
C1 C6 1.504(10) . ?
C12 C13 1.401(9) . ?
C12 C17 1.511(9) . ?
C5 C4 1.432(9) . ?
C5 C10 1.494(10) . ?
C16 C15 1.388(9) . ?
C16 C20 1.513(10) . ?
C15 C14 1.364(11) . ?
C15 H15 0.9301 . ?
C3 C2 1.373(11) . ?
C3 C4 1.435(10) . ?
C3 C8 1.511(11) . ?
C2 C7 1.506(11) . ?
C20 C22 1.516(12) . ?
C20 C21 1.538(12) . ?
C20 H20 0.9802 . ?
C17 C19 1.520(11) . ?
C17 C18 1.539(10) . ?
C17 H17 0.9799 . ?
C9 C4 1.492(10) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9599 . ?
C19 H19A 0.9599 . ?
C19 H19B 0.9601 . ?
C19 H19C 0.9601 . ?
C18 H18A 0.9599 . ?
C18 H18B 0.9599 . ?
C18 H18C 0.9601 . ?
C14 C13 1.361(11) . ?
C14 H14 0.9301 . ?
C13 H13 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9601 . ?
C8 H8C 0.9601 . ?
C7 H7A 0.9599 . ?
C7 H7B 0.9601 . ?
C7 H7C 0.9599 . ?
C10 H10A 0.9599 . ?
C10 H10B 0.9601 . ?
C10 H10C 0.9600 . ?
C6 H6A 0.9599 . ?
C6 H6B 0.9601 . ?
C6 H6C 0.9600 . ?
C21 H21A 0.9599 . ?
C21 H21B 0.9601 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9601 . ?

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 Hf1 N1 85.12(18) . 7 ?
N1 Hf1 Cl1 108.79(14) . . ?
N1 Hf1 Cl1 106.80(13) 7 . ?
N1 Hf1 C4 100.1(2) . . ?
N1 Hf1 C4 107.78(19) 7 . ?
Cl1 Hf1 C4 136.24(16) . . ?
N1 Hf1 C5 96.2(2) . . ?
N1 Hf1 C5 141.1(2) 7 . ?
Cl1 Hf1 C5 109.38(17) . . ?
C4 Hf1 C5 33.6(2) . . ?
N1 Hf1 C3 131.9(2) . . ?
N1 Hf1 C3 96.7(2) 7 . ?
Cl1 Hf1 C3 116.33(19) . . ?
C4 Hf1 C3 33.7(2) . . ?
C5 Hf1 C3 54.4(2) . . ?
N1 Hf1 C1 122.5(2) . . ?
N1 Hf1 C1 147.6(2) 7 . ?
Cl1 Hf1 C1 81.55(16) . . ?
C4 Hf1 C1 55.0(2) . . ?
C5 Hf1 C1 32.8(2) . . ?
C3 Hf1 C1 53.1(2) . . ?
N1 Hf1 C2 150.2(2) . . ?
N1 Hf1 C2 115.8(2) 7 . ?
Cl1 Hf1 C2 86.25(18) . . ?
C4 Hf1 C2 54.7(2) . . ?
C5 Hf1 C2 54.1(2) . . ?
C3 Hf1 C2 31.4(2) . . ?
C1 Hf1 C2 32.2(2) . . ?
N1 Hf1 Hf1 42.97(13) . 7 ?
N1 Hf1 Hf1 42.15(13) 7 7 ?
Cl1 Hf1 Hf1 114.49(4) . 7 ?
C4 Hf1 Hf1 109.10(15) . 7 ?
C5 Hf1 Hf1 127.27(17) . 7 ?
C3 Hf1 Hf1 121.98(18) . 7 ?
C1 Hf1 Hf1 160.07(16) . 7 ?
C2 Hf1 Hf1 151.91(17) . 7 ?
C11 N1 Hf1 138.1(4) . . ?
C11 N1 Hf1 127.0(4) . 7 ?
Hf1 N1 Hf1 94.88(18) . 7 ?
C16 C11 C12 117.7(5) . . ?
C16 C11 N1 120.8(5) . . ?
C12 C11 N1 121.5(5) . . ?
C2 C1 C5 107.9(6) . . ?
C2 C1 C6 125.5(7) . . ?
C5 C1 C6 126.0(7) . . ?
C2 C1 Hf1 74.4(4) . . ?
C5 C1 Hf1 71.5(3) . . ?
C6 C1 Hf1 126.4(5) . . ?
C13 C12 C11 118.3(6) . . ?
C13 C12 C17 115.3(6) . . ?
C11 C12 C17 126.5(5) . . ?
C1 C5 C4 108.0(6) . . ?
C1 C5 C10 126.4(6) . . ?
C4 C5 C10 125.5(7) . . ?
C1 C5 Hf1 75.7(4) . . ?
C4 C5 Hf1 71.3(3) . . ?
C10 C5 Hf1 122.3(4) . . ?
C15 C16 C11 119.8(6) . . ?
C15 C16 C20 116.3(6) . . ?
C11 C16 C20 123.7(5) . . ?
C14 C15 C16 122.8(7) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.5 . . ?
C2 C3 C4 110.4(6) . . ?
C2 C3 C8 124.5(7) . . ?
C4 C3 C8 124.7(7) . . ?
C2 C3 Hf1 76.9(4) . . ?
C4 C3 Hf1 71.1(4) . . ?
C8 C3 Hf1 124.8(5) . . ?
C3 C2 C1 108.1(7) . . ?
C3 C2 C7 128.2(7) . . ?
C1 C2 C7 123.5(7) . . ?
C3 C2 Hf1 71.7(4) . . ?
C1 C2 Hf1 73.4(4) . . ?
C7 C2 Hf1 124.7(5) . . ?
C16 C20 C22 116.6(7) . . ?
C16 C20 C21 106.7(7) . . ?
C22 C20 C21 108.9(8) . . ?
C16 C20 H20 107.7 . . ?
C22 C20 H20 108.1 . . ?
C21 C20 H20 108.5 . . ?
C12 C17 C19 112.0(6) . . ?
C12 C17 C18 111.9(6) . . ?
C19 C17 C18 108.6(6) . . ?
C12 C17 H17 107.7 . . ?
C19 C17 H17 108.4 . . ?
C18 C17 H17 108.2 . . ?
C4 C9 H9A 110.3 . . ?
C4 C9 H9B 108.9 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.2 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C17 C19 H19A 109.9 . . ?
C17 C19 H19B 109.8 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 108.7 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C4 C3 105.7(6) . . ?
C5 C4 C9 127.8(7) . . ?
C3 C4 C9 125.9(6) . . ?
C5 C4 Hf1 75.1(3) . . ?
C3 C4 Hf1 75.2(4) . . ?
C9 C4 Hf1 122.3(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.7 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 C15 117.7(7) . . ?
C13 C14 H14 121.3 . . ?
C15 C14 H14 121.0 . . ?
C14 C13 C12 123.6(7) . . ?
C14 C13 H13 118.2 . . ?
C12 C13 H13 118.1 . . ?
C3 C8 H8A 110.0 . . ?
C3 C8 H8B 110.0 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 108.4 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C7 H7A 109.1 . . ?
C2 C7 H7B 109.7 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.6 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C10 H10A 109.9 . . ?
C5 C10 H10B 109.0 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C1 C6 H6A 110.1 . . ?
C1 C6 H6B 108.8 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C20 C21 H21A 110.1 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.0 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.1 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.8 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.622
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.146
####################################################################### 
# 
# 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_15
_database_code_depnum_ccdc_archive 'CCDC 1044561'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H50 Cl2 N4 Zr2'
_chemical_formula_sum            'C36 H50 Cl2 N4 Zr2'
_chemical_formula_weight         792.14

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7960(11)
_cell_length_b                   11.405(2)
_cell_length_c                   14.398(3)
_cell_angle_alpha                90.892(13)
_cell_angle_beta                 90.032(11)
_cell_angle_gamma                105.131(12)
_cell_volume                     1711.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    20105
_cell_measurement_theta_min      1
_cell_measurement_theta_max      25.6

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    0.797
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -1 0.060
-1 0 1 0.020
0 0 -1 0.066
1 0 1 0.026
0 1 0 0.060
0 -1 0 0.019
0 0 1 0.014
-1 0 -1 0.058
0 -1 1 0.012
-1 1 -1 0.079


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20051
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.60
_reflns_number_total             6396
_reflns_number_gt                4748
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'


_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)+(0.0000P)²+20.5593P] where P=(Fo²+2Fc²)/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         6396
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.1731
_refine_ls_wR_factor_gt          0.1587
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_restrained_S_all      1.225
_refine_ls_shift/su_max          0.000
_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 0.83933(8) 0.69692(7) 0.23433(6) 0.0176(2) Uani 1 1 d . . .
Zr2 Zr 0.66977(7) 0.89185(7) 0.25217(6) 0.0160(2) Uani 1 1 d . . .
Cl1 Cl 1.0265(2) 0.7454(2) 0.12507(16) 0.0301(5) Uani 1 1 d . . .
Cl2 Cl 0.7656(2) 1.0501(2) 0.37466(16) 0.0297(5) Uani 1 1 d . . .
N1 N 0.7367(7) 0.7735(6) 0.3326(5) 0.0181(15) Uani 1 1 d . . .
N3 N 0.7473(6) 0.7958(6) 0.1497(5) 0.0197(15) Uani 1 1 d . . .
C22 C 0.8153(9) 0.4872(8) 0.3161(7) 0.026(2) Uani 1 1 d . . .
N4 N 0.7756(6) 1.0558(6) 0.1489(5) 0.0199(15) Uani 1 1 d . . .
C36 C 0.4766(10) 1.1028(9) 0.3238(7) 0.035(2) Uani 1 1 d . . .
H36A H 0.4808 1.1600 0.2750 0.041 Uiso 1 1 d R . .
H36B H 0.5514 1.1287 0.3627 0.041 Uiso 1 1 d R . .
H36C H 0.4012 1.0981 0.3603 0.041 Uiso 1 1 d R . .
C10 C 0.7535(8) 0.8094(8) 0.0525(6) 0.0201(18) Uani 1 1 d . . .
C23 C 0.6946(8) 0.4980(7) 0.2831(6) 0.0216(18) Uani 1 1 d . . .
H23 H 0.6279 0.5084 0.3205 0.026 Uiso 1 1 d R . .
C32 C 0.4742(8) 0.9521(9) 0.1861(6) 0.025(2) Uani 1 1 d . . .
H32 H 0.4883 1.0095 0.1394 0.030 Uiso 1 1 d R . .
C29 C 0.4381(8) 0.7725(8) 0.2606(7) 0.0231(19) Uani 1 1 d . . .
N2 N 1.0222(7) 0.8055(7) 0.3444(5) 0.0261(17) Uani 1 1 d . . .
C30 C 0.4512(8) 0.8671(9) 0.3285(6) 0.026(2) Uani 1 1 d . . .
C11 C 0.7532(8) 0.9170(8) 0.0064(6) 0.026(2) Uani 1 1 d . . .
C35 C 0.4377(9) 0.8545(9) 0.4323(6) 0.031(2) Uani 1 1 d . . .
H35A H 0.4098 0.7700 0.4474 0.038 Uiso 1 1 d R . .
H35B H 0.3750 0.8951 0.4533 0.038 Uiso 1 1 d R . .
H35C H 0.5184 0.8905 0.4623 0.038 Uiso 1 1 d R . .
C14 C 0.7585(9) 0.7103(9) -0.0998(6) 0.029(2) Uani 1 1 d . . .
H14 H 0.7604 0.6412 -0.1343 0.034 Uiso 1 1 d R . .
C1 C 0.7413(8) 0.7408(8) 0.4247(6) 0.0226(19) Uani 1 1 d . . .
C16 C 0.7406(9) 1.0352(8) 0.0533(7) 0.028(2) Uani 1 1 d . . .
H16A H 0.7915 1.1027 0.0182 0.034 Uiso 1 1 d R . .
H16B H 0.6517 1.0374 0.0475 0.034 Uiso 1 1 d R . .
C26 C 1.0230(9) 0.4605(9) 0.2373(9) 0.044(3) Uani 1 1 d . . .
H26A H 1.0165 0.3752 0.2422 0.053 Uiso 1 1 d R . .
H26B H 1.0718 0.5033 0.2889 0.053 Uiso 1 1 d R . .
H26C H 1.0651 0.4900 0.1804 0.053 Uiso 1 1 d R . .
C2 C 0.8601(9) 0.7820(8) 0.4737(6) 0.0242(19) Uani 1 1 d . . .
C17 C 0.9187(9) 1.0734(9) 0.1549(7) 0.032(2) Uani 1 1 d . . .
H17A H 0.9387 0.9991 0.1364 0.038 Uiso 1 1 d R . .
H17B H 0.9478 1.0945 0.2174 0.038 Uiso 1 1 d R . .
H17C H 0.9608 1.1372 0.1141 0.038 Uiso 1 1 d R . .
C15 C 0.7559(8) 0.7085(9) -0.0050(6) 0.028(2) Uani 1 1 d . . .
H15 H 0.7554 0.6358 0.0234 0.034 Uiso 1 1 d R . .
C25 C 0.8534(9) 0.4620(8) 0.0583(7) 0.033(2) Uani 1 1 d . . .
H25A H 0.8982 0.5383 0.0323 0.039 Uiso 1 1 d R . .
H25B H 0.7780 0.4267 0.0218 0.039 Uiso 1 1 d R . .
H25C H 0.9084 0.4081 0.0580 0.039 Uiso 1 1 d R . .
C19 C 0.6920(8) 0.4926(7) 0.1854(6) 0.0225(19) Uani 1 1 d . . .
C34 C 0.3952(8) 0.6395(8) 0.2779(7) 0.029(2) Uani 1 1 d . . .
H34A H 0.3351 0.6014 0.2304 0.035 Uiso 1 1 d R . .
H34B H 0.3546 0.6256 0.3375 0.035 Uiso 1 1 d R . .
H34C H 0.4678 0.6056 0.2765 0.035 Uiso 1 1 d R . .
C13 C 0.7578(9) 0.8193(10) -0.1453(6) 0.032(2) Uani 1 1 d . . .
H13 H 0.7586 0.8235 -0.2097 0.039 Uiso 1 1 d R . .
C24 C 0.5737(9) 0.4737(9) 0.1254(7) 0.033(2) Uani 1 1 d . . .
H24A H 0.4992 0.4386 0.1619 0.040 Uiso 1 1 d R . .
H24B H 0.5786 0.4200 0.0743 0.040 Uiso 1 1 d R . .
H24C H 0.5678 0.5504 0.1021 0.040 Uiso 1 1 d R . .
C31 C 0.4712(9) 0.9793(8) 0.2809(7) 0.027(2) Uani 1 1 d . . .
C27 C 0.8438(10) 0.4623(9) 0.4143(7) 0.039(3) Uani 1 1 d . . .
H27A H 0.7997 0.3803 0.4294 0.047 Uiso 1 1 d R . .
H27B H 0.8155 0.5175 0.4549 0.047 Uiso 1 1 d R . .
H27C H 0.9345 0.4737 0.4219 0.047 Uiso 1 1 d R . .
C21 C 0.8894(9) 0.4808(8) 0.2360(7) 0.029(2) Uani 1 1 d . . .
C3 C 0.8688(10) 0.7511(9) 0.5661(6) 0.033(2) Uani 1 1 d . . .
H3 H 0.9460 0.7793 0.5980 0.039 Uiso 1 1 d R . .
C5 C 0.6470(10) 0.6414(9) 0.5641(7) 0.033(2) Uani 1 1 d . . .
H5 H 0.5755 0.5946 0.5945 0.040 Uiso 1 1 d R . .
C7 C 0.9720(9) 0.8636(8) 0.4263(6) 0.027(2) Uani 1 1 d . . .
H7A H 1.0411 0.8910 0.4710 0.033 Uiso 1 1 d R . .
H7B H 0.9471 0.9347 0.4053 0.033 Uiso 1 1 d R . .
C8 C 1.1174(9) 0.9077(8) 0.3012(7) 0.030(2) Uani 1 1 d . . .
H8A H 1.1702 0.9559 0.3488 0.037 Uiso 1 1 d R . .
H8B H 1.0736 0.9571 0.2677 0.037 Uiso 1 1 d R . .
H8C H 1.1701 0.8760 0.2592 0.037 Uiso 1 1 d R . .
C28 C 0.4539(8) 0.8285(9) 0.1716(7) 0.028(2) Uani 1 1 d . . .
C6 C 0.6363(9) 0.6708(8) 0.4727(7) 0.028(2) Uani 1 1 d . . .
H6 H 0.5570 0.6453 0.4431 0.034 Uiso 1 1 d R . .
C20 C 0.8151(8) 0.4828(7) 0.1565(7) 0.0234(19) Uani 1 1 d . . .
C18 C 0.7551(11) 1.1769(9) 0.1752(8) 0.042(3) Uani 1 1 d . . .
H18A H 0.8078 1.2382 0.1368 0.050 Uiso 1 1 d R . .
H18B H 0.7797 1.1939 0.2391 0.050 Uiso 1 1 d R . .
H18C H 0.6667 1.1767 0.1674 0.050 Uiso 1 1 d R . .
C12 C 0.7570(8) 0.9192(10) -0.0911(7) 0.031(2) Uani 1 1 d . . .
H12 H 0.7576 0.9914 -0.1205 0.037 Uiso 1 1 d R . .
C33 C 0.4313(10) 0.7581(9) 0.0808(7) 0.036(2) Uani 1 1 d . . .
H33A H 0.3412 0.7360 0.0663 0.043 Uiso 1 1 d R . .
H33B H 0.4605 0.6859 0.0866 0.043 Uiso 1 1 d R . .
H33C H 0.4776 0.8069 0.0319 0.043 Uiso 1 1 d R . .
C9 C 1.0885(10) 0.7225(9) 0.3802(8) 0.039(3) Uani 1 1 d . . .
H9A H 1.1219 0.6851 0.3292 0.047 Uiso 1 1 d R . .
H9B H 1.0299 0.6611 0.4150 0.047 Uiso 1 1 d R . .
H9C H 1.1578 0.7649 0.4198 0.047 Uiso 1 1 d R . .
C4 C 0.7632(10) 0.6805(10) 0.6113(7) 0.036(2) Uani 1 1 d . . .
H4 H 0.7699 0.6581 0.6726 0.043 Uiso 1 1 d 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 N3 2.090(7) . ?
Zr1 N1 2.111(7) . ?
Zr1 C23 2.507(8) . ?
Zr1 Cl1 2.512(2) . ?
Zr1 C19 2.544(9) . ?
Zr1 N2 2.569(7) . ?
Zr1 C20 2.621(8) . ?
Zr1 C22 2.634(8) . ?
Zr1 C21 2.658(9) . ?
Zr1 Zr2 3.2352(12) . ?
Zr2 N1 2.060(7) . ?
Zr2 N3 2.123(7) . ?
Zr2 N4 2.447(7) . ?
Zr2 C29 2.520(8) . ?
Zr2 Cl2 2.522(2) . ?
Zr2 C28 2.528(8) . ?
Zr2 C30 2.553(8) . ?
Zr2 C32 2.571(8) . ?
Zr2 C31 2.620(9) . ?
N1 C1 1.387(11) . ?
N3 C10 1.411(10) . ?
C22 C21 1.416(13) . ?
C22 C23 1.423(12) . ?
C22 C27 1.494(13) . ?
N4 C16 1.426(12) . ?
N4 C18 1.497(11) . ?
N4 C17 1.508(11) . ?
C36 C31 1.516(13) . ?
C36 H36A 0.9599 . ?
C36 H36B 0.9601 . ?
C36 H36C 0.9600 . ?
C10 C11 1.405(12) . ?
C10 C15 1.412(13) . ?
C23 C19 1.406(12) . ?
C23 H23 0.9301 . ?
C32 C28 1.381(13) . ?
C32 C31 1.397(13) . ?
C32 H32 0.9301 . ?
C29 C30 1.424(13) . ?
C29 C28 1.431(13) . ?
C29 C34 1.491(12) . ?
N2 C9 1.429(13) . ?
N2 C8 1.482(11) . ?
N2 C7 1.512(11) . ?
C30 C31 1.426(13) . ?
C30 C35 1.508(12) . ?
C11 C12 1.406(13) . ?
C11 C16 1.536(13) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9599 . ?
C14 C15 1.367(13) . ?
C14 C13 1.415(14) . ?
C14 H14 0.9300 . ?
C1 C6 1.396(12) . ?
C1 C2 1.427(12) . ?
C16 H16A 0.9701 . ?
C16 H16B 0.9700 . ?
C26 C21 1.519(12) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9601 . ?
C26 H26C 0.9600 . ?
C2 C3 1.390(12) . ?
C2 C7 1.493(13) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9601 . ?
C17 H17C 0.9600 . ?
C15 H15 0.9300 . ?
C25 C20 1.506(13) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9599 . ?
C19 C20 1.424(12) . ?
C19 C24 1.508(13) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C13 C12 1.373(14) . ?
C13 H13 0.9299 . ?
C24 H24A 0.9599 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9601 . ?
C21 C20 1.402(13) . ?
C3 C4 1.382(14) . ?
C3 H3 0.9299 . ?
C5 C6 1.375(13) . ?
C5 C4 1.391(15) . ?
C5 H5 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C28 C33 1.510(13) . ?
C6 H6 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9599 . ?
C18 H18C 0.9600 . ?
C12 H12 0.9299 . ?
C33 H33A 0.9601 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9599 . ?
C4 H4 0.9301 . ?

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 N1 78.2(3) . . ?
N3 Zr1 C23 113.0(3) . . ?
N1 Zr1 C23 84.7(3) . . ?
N3 Zr1 Cl1 88.7(2) . . ?
N1 Zr1 Cl1 143.69(19) . . ?
C23 Zr1 Cl1 131.3(2) . . ?
N3 Zr1 C19 93.9(3) . . ?
N1 Zr1 C19 106.4(3) . . ?
C23 Zr1 C19 32.3(3) . . ?
Cl1 Zr1 C19 108.1(2) . . ?
N3 Zr1 N2 120.9(3) . . ?
N1 Zr1 N2 79.4(3) . . ?
C23 Zr1 N2 118.4(3) . . ?
Cl1 Zr1 N2 78.74(17) . . ?
C19 Zr1 N2 145.0(3) . . ?
N3 Zr1 C20 108.2(3) . . ?
N1 Zr1 C20 136.4(3) . . ?
C23 Zr1 C20 52.5(3) . . ?
Cl1 Zr1 C20 79.85(19) . . ?
C19 Zr1 C20 32.0(3) . . ?
N2 Zr1 C20 125.3(3) . . ?
N3 Zr1 C22 144.5(3) . . ?
N1 Zr1 C22 97.5(3) . . ?
C23 Zr1 C22 32.0(3) . . ?
Cl1 Zr1 C22 111.9(2) . . ?
C19 Zr1 C22 53.1(3) . . ?
N2 Zr1 C22 92.2(3) . . ?
C20 Zr1 C22 51.9(3) . . ?
N3 Zr1 C21 139.0(3) . . ?
N1 Zr1 C21 128.6(3) . . ?
C23 Zr1 C21 51.9(3) . . ?
Cl1 Zr1 C21 82.7(2) . . ?
C19 Zr1 C21 52.2(3) . . ?
N2 Zr1 C21 96.6(3) . . ?
C20 Zr1 C21 30.8(3) . . ?
C22 Zr1 C21 31.0(3) . . ?
N3 Zr1 Zr2 40.2(2) . . ?
N1 Zr1 Zr2 38.57(18) . . ?
C23 Zr1 Zr2 105.71(19) . . ?
Cl1 Zr1 Zr2 117.32(6) . . ?
C19 Zr1 Zr2 108.48(19) . . ?
N2 Zr1 Zr2 97.37(17) . . ?
C20 Zr1 Zr2 137.0(2) . . ?
C22 Zr1 Zr2 130.7(2) . . ?
C21 Zr1 Zr2 157.5(2) . . ?
N1 Zr2 N3 78.6(3) . . ?
N1 Zr2 N4 133.0(2) . . ?
N3 Zr2 N4 78.5(2) . . ?
N1 Zr2 C29 94.7(3) . . ?
N3 Zr2 C29 103.3(3) . . ?
N4 Zr2 C29 130.4(3) . . ?
N1 Zr2 Cl2 85.8(2) . . ?
N3 Zr2 Cl2 134.31(19) . . ?
N4 Zr2 Cl2 81.79(19) . . ?
C29 Zr2 Cl2 120.7(2) . . ?
N1 Zr2 C28 121.8(3) . . ?
N3 Zr2 C28 89.9(3) . . ?
N4 Zr2 C28 98.5(3) . . ?
C29 Zr2 C28 32.9(3) . . ?
Cl2 Zr2 C28 133.8(2) . . ?
N1 Zr2 C30 98.8(3) . . ?
N3 Zr2 C30 135.9(3) . . ?
N4 Zr2 C30 125.9(3) . . ?
C29 Zr2 C30 32.6(3) . . ?
Cl2 Zr2 C30 88.6(2) . . ?
C28 Zr2 C30 53.7(3) . . ?
N1 Zr2 C32 147.4(3) . . ?
N3 Zr2 C32 110.1(3) . . ?
N4 Zr2 C32 79.4(3) . . ?
C29 Zr2 C32 52.9(3) . . ?
Cl2 Zr2 C32 106.1(2) . . ?
C28 Zr2 C32 31.4(3) . . ?
C30 Zr2 C32 52.5(3) . . ?
N1 Zr2 C31 128.6(3) . . ?
N3 Zr2 C31 140.6(3) . . ?
N4 Zr2 C31 94.0(3) . . ?
C29 Zr2 C31 53.3(3) . . ?
Cl2 Zr2 C31 81.2(2) . . ?
C28 Zr2 C31 52.6(3) . . ?
C30 Zr2 C31 32.0(3) . . ?
C32 Zr2 C31 31.2(3) . . ?
N1 Zr2 Zr1 39.72(19) . . ?
N3 Zr2 Zr1 39.47(18) . . ?
N4 Zr2 Zr1 104.32(15) . . ?
C29 Zr2 Zr1 107.01(19) . . ?
Cl2 Zr2 Zr1 109.83(6) . . ?
C28 Zr2 Zr1 114.7(2) . . ?
C30 Zr2 Zr1 128.8(2) . . ?
C32 Zr2 Zr1 144.0(2) . . ?
C31 Zr2 Zr1 159.7(2) . . ?
C1 N1 Zr2 140.2(6) . . ?
C1 N1 Zr1 117.8(5) . . ?
Zr2 N1 Zr1 101.7(3) . . ?
C10 N3 Zr1 129.2(5) . . ?
C10 N3 Zr2 129.8(5) . . ?
Zr1 N3 Zr2 100.3(3) . . ?
C21 C22 C23 105.9(8) . . ?
C21 C22 C27 128.0(9) . . ?
C23 C22 C27 125.0(9) . . ?
C21 C22 Zr1 75.4(5) . . ?
C23 C22 Zr1 69.1(5) . . ?
C27 C22 Zr1 129.4(6) . . ?
C16 N4 C18 106.5(7) . . ?
C16 N4 C17 107.0(7) . . ?
C18 N4 C17 104.9(7) . . ?
C16 N4 Zr2 114.8(5) . . ?
C18 N4 Zr2 113.9(5) . . ?
C17 N4 Zr2 109.0(5) . . ?
C31 C36 H36A 108.9 . . ?
C31 C36 H36B 109.8 . . ?
H36A C36 H36B 109.5 . . ?
C31 C36 H36C 109.7 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C11 C10 N3 124.6(8) . . ?
C11 C10 C15 116.0(8) . . ?
N3 C10 C15 119.4(8) . . ?
C19 C23 C22 109.8(8) . . ?
C19 C23 Zr1 75.3(5) . . ?
C22 C23 Zr1 78.9(5) . . ?
C19 C23 H23 125.1 . . ?
C22 C23 H23 125.0 . . ?
Zr1 C23 H23 112.0 . . ?
C28 C32 C31 110.6(8) . . ?
C28 C32 Zr2 72.6(5) . . ?
C31 C32 Zr2 76.3(5) . . ?
C28 C32 H32 124.8 . . ?
C31 C32 H32 124.6 . . ?
Zr2 C32 H32 117.9 . . ?
C30 C29 C28 107.0(8) . . ?
C30 C29 C34 126.2(8) . . ?
C28 C29 C34 126.1(9) . . ?
C30 C29 Zr2 75.0(5) . . ?
C28 C29 Zr2 73.8(5) . . ?
C34 C29 Zr2 124.1(6) . . ?
C9 N2 C8 108.5(7) . . ?
C9 N2 C7 107.6(7) . . ?
C8 N2 C7 104.1(7) . . ?
C9 N2 Zr1 111.2(6) . . ?
C8 N2 Zr1 113.8(5) . . ?
C7 N2 Zr1 111.3(5) . . ?
C29 C30 C31 108.0(8) . . ?
C29 C30 C35 127.6(9) . . ?
C31 C30 C35 124.3(9) . . ?
C29 C30 Zr2 72.4(5) . . ?
C31 C30 Zr2 76.6(5) . . ?
C35 C30 Zr2 120.2(6) . . ?
C10 C11 C12 119.6(9) . . ?
C10 C11 C16 125.5(8) . . ?
C12 C11 C16 114.8(8) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 108.8 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 110.1 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C15 C14 C13 119.0(9) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.2 . . ?
N1 C1 C6 123.9(8) . . ?
N1 C1 C2 118.3(8) . . ?
C6 C1 C2 117.8(8) . . ?
N4 C16 C11 118.3(7) . . ?
N4 C16 H16A 108.2 . . ?
C11 C16 H16A 107.8 . . ?
N4 C16 H16B 107.5 . . ?
C11 C16 H16B 107.5 . . ?
H16A C16 H16B 107.1 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 110.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 108.4 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 C2 C1 120.1(9) . . ?
C3 C2 C7 120.7(9) . . ?
C1 C2 C7 119.2(8) . . ?
N4 C17 H17A 109.1 . . ?
N4 C17 H17B 109.9 . . ?
H17A C17 H17B 109.5 . . ?
N4 C17 H17C 109.4 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C15 C10 124.4(9) . . ?
C14 C15 H15 117.5 . . ?
C10 C15 H15 118.0 . . ?
C20 C25 H25A 109.2 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.7 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C19 C20 106.7(8) . . ?
C23 C19 C24 125.6(8) . . ?
C20 C19 C24 126.5(8) . . ?
C23 C19 Zr1 72.4(5) . . ?
C20 C19 Zr1 77.0(5) . . ?
C24 C19 Zr1 125.7(6) . . ?
C29 C34 H34A 109.0 . . ?
C29 C34 H34B 109.8 . . ?
H34A C34 H34B 109.5 . . ?
C29 C34 H34C 109.6 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C12 C13 C14 117.9(9) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 121.3 . . ?
C19 C24 H24A 109.3 . . ?
C19 C24 H24B 109.7 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.4 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 C30 106.8(8) . . ?
C32 C31 C36 126.2(9) . . ?
C30 C31 C36 126.8(9) . . ?
C32 C31 Zr2 72.5(5) . . ?
C30 C31 Zr2 71.4(5) . . ?
C36 C31 Zr2 125.2(6) . . ?
C22 C27 H27A 109.9 . . ?
C22 C27 H27B 109.1 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.4 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C20 C21 C22 109.3(8) . . ?
C20 C21 C26 125.8(9) . . ?
C22 C21 C26 124.6(9) . . ?
C20 C21 Zr1 73.1(5) . . ?
C22 C21 Zr1 73.5(5) . . ?
C26 C21 Zr1 125.0(6) . . ?
C4 C3 C2 120.6(9) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.7 . . ?
C6 C5 C4 120.9(9) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.7 . . ?
C2 C7 N2 114.4(7) . . ?
C2 C7 H7A 108.8 . . ?
N2 C7 H7A 108.5 . . ?
C2 C7 H7B 108.4 . . ?
N2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.6 . . ?
N2 C8 H8A 109.4 . . ?
N2 C8 H8B 109.6 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.4 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C32 C28 C29 107.6(8) . . ?
C32 C28 C33 128.3(9) . . ?
C29 C28 C33 123.5(9) . . ?
C32 C28 Zr2 76.0(5) . . ?
C29 C28 Zr2 73.2(5) . . ?
C33 C28 Zr2 123.4(6) . . ?
C5 C6 C1 121.1(9) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.6 . . ?
C21 C20 C19 108.2(8) . . ?
C21 C20 C25 125.5(8) . . ?
C19 C20 C25 125.9(9) . . ?
C21 C20 Zr1 76.1(5) . . ?
C19 C20 Zr1 71.0(5) . . ?
C25 C20 Zr1 124.7(6) . . ?
N4 C18 H18A 109.2 . . ?
N4 C18 H18B 108.3 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 110.8 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C12 C11 123.1(9) . . ?
C13 C12 H12 118.3 . . ?
C11 C12 H12 118.5 . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.0 . . ?
H33A C33 H33B 109.5 . . ?
C28 C33 H33C 109.9 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C9 H9A 108.9 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 110.0 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C4 C5 119.4(9) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.1 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.60
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.265
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.156
####################################################################### 
# 
# 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_16
_database_code_depnum_ccdc_archive 'CCDC 1044562'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H54 Cl2 N4 Zr2'
_chemical_formula_sum            'C38 H54 Cl2 N4 Zr2'
_chemical_formula_weight         820.19

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3661(7)
_cell_length_b                   10.4020(8)
_cell_length_c                   11.5359(7)
_cell_angle_alpha                111.082(4)
_cell_angle_beta                 103.324(5)
_cell_angle_gamma                105.615(5)
_cell_volume                     940.61(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    20294
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    0.728
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.138
0 -1 0 0.107
0 0 -1 0.082
0 0 1 0.007
1 0 -1 0.052
-1 0 1 0.033
-1 0 0 0.067
1 0 0 0.023
0 1 -1 0.166
0 -1 1 0.091


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20263
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4314
_reflns_number_gt                3813
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0327P)²+0.7287P] where P=(Fo²+2Fc²)/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         4314
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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 0.10504(2) 0.65650(2) 0.52188(2) 0.01623(7) Uani 1 1 d . . .
Cl1 Cl 0.38194(6) 0.69904(7) 0.54357(6) 0.02624(13) Uani 1 1 d . . .
N1 N -0.0257(2) 0.4548(2) 0.36673(18) 0.0183(4) Uani 1 1 d . . .
C1 C -0.1073(3) 0.3586(2) 0.2296(2) 0.0183(4) Uani 1 1 d . . .
C13 C 0.0365(3) 0.8789(2) 0.6170(2) 0.0215(5) Uani 1 1 d . . .
C6 C -0.2724(3) 0.2818(3) 0.1775(2) 0.0219(5) Uani 1 1 d . . .
H6 H -0.3295 0.2996 0.2336 0.026 Uiso 1 1 d R . .
C12 C -0.0889(3) 0.7749(3) 0.4941(2) 0.0225(5) Uani 1 1 d . . .
C10 C 0.1340(3) 0.8622(2) 0.4487(2) 0.0215(5) Uani 1 1 d . . .
C14 C 0.1755(3) 0.9316(2) 0.5898(2) 0.0223(5) Uani 1 1 d . . .
C2 C -0.0235(3) 0.3359(3) 0.1413(2) 0.0205(4) Uani 1 1 d . . .
C15 C 0.2436(3) 0.8909(3) 0.3769(3) 0.0298(5) Uani 1 1 d . . .
H15A H 0.2042 0.8077 0.2902 0.036 Uiso 1 1 d R . .
H15B H 0.3479 0.9034 0.4268 0.036 Uiso 1 1 d R . .
H15C H 0.2490 0.9800 0.3676 0.036 Uiso 1 1 d R . .
C18 C 0.0248(4) 0.9320(3) 0.7520(3) 0.0320(6) Uani 1 1 d . . .
H18A H 0.0142 1.0265 0.7768 0.038 Uiso 1 1 d R . .
H18B H 0.1193 0.9433 0.8159 0.038 Uiso 1 1 d R . .
H18C H -0.0664 0.8605 0.7502 0.038 Uiso 1 1 d R . .
C17 C -0.2585(3) 0.6946(3) 0.4760(3) 0.0321(6) Uani 1 1 d . . .
H17A H -0.2605 0.6823 0.5543 0.038 Uiso 1 1 d R . .
H17B H -0.3031 0.5982 0.4000 0.038 Uiso 1 1 d R . .
H17C H -0.3198 0.7519 0.4623 0.038 Uiso 1 1 d R . .
C16 C -0.1247(3) 0.6758(3) 0.2431(2) 0.0300(5) Uani 1 1 d . . .
H16A H -0.1628 0.7377 0.2103 0.036 Uiso 1 1 d R . .
H16B H -0.2136 0.5918 0.2283 0.036 Uiso 1 1 d R . .
H16C H -0.0593 0.6410 0.1969 0.036 Uiso 1 1 d R . .
C3 C -0.1071(3) 0.2343(3) 0.0082(2) 0.0260(5) Uani 1 1 d . . .
H3 H -0.0526 0.2194 -0.0502 0.031 Uiso 1 1 d R . .
N2 N 0.2274(3) 0.3793(3) 0.0964(2) 0.0347(5) Uani 1 1 d . . .
C11 C -0.0287(3) 0.7647(3) 0.3900(2) 0.0226(5) Uani 1 1 d . . .
C7 C 0.1527(3) 0.4271(3) 0.1928(2) 0.0276(5) Uani 1 1 d . . .
H7A H 0.1695 0.5311 0.2181 0.033 Uiso 1 1 d R . .
H7B H 0.2044 0.4202 0.2722 0.033 Uiso 1 1 d R . .
C19 C 0.3351(3) 1.0451(3) 0.6901(3) 0.0317(6) Uani 1 1 d . . .
H19A H 0.3411 1.1434 0.7037 0.038 Uiso 1 1 d R . .
H19B H 0.4164 1.0253 0.6577 0.038 Uiso 1 1 d R . .
H19C H 0.3505 1.0394 0.7730 0.038 Uiso 1 1 d R . .
C5 C -0.3530(3) 0.1794(3) 0.0445(3) 0.0290(5) Uani 1 1 d . . .
H5 H -0.4627 0.1281 0.0125 0.035 Uiso 1 1 d R . .
C4 C -0.2702(3) 0.1538(3) -0.0404(3) 0.0319(6) Uani 1 1 d . . .
H4 H -0.3234 0.0832 -0.1293 0.038 Uiso 1 1 d R . .
C8 C 0.3684(4) 0.5039(5) 0.1214(4) 0.0649(12) Uani 1 1 d . . .
H8A H 0.4450 0.5393 0.2087 0.078 Uiso 1 1 d R . .
H8B H 0.3381 0.5833 0.1161 0.078 Uiso 1 1 d R . .
H8C H 0.4145 0.4709 0.0557 0.078 Uiso 1 1 d R . .
C9 C 0.2673(4) 0.2544(4) 0.0990(3) 0.0551(9) Uani 1 1 d . . .
H9A H 0.3417 0.2844 0.1858 0.066 Uiso 1 1 d R . .
H9B H 0.3138 0.2228 0.0334 0.066 Uiso 1 1 d R . .
H9C H 0.1722 0.1731 0.0794 0.066 Uiso 1 1 d 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 2.0024(19) . ?
Zr1 N1 2.1427(19) 2_566 ?
Zr1 Cl1 2.4471(6) . ?
Zr1 C12 2.477(2) . ?
Zr1 C13 2.503(2) . ?
Zr1 C11 2.503(2) . ?
Zr1 C14 2.524(2) . ?
Zr1 C10 2.541(2) . ?
Zr1 Zr1 3.1045(5) 2_566 ?
N1 C1 1.407(3) . ?
N1 Zr1 2.1427(19) 2_566 ?
C1 C6 1.396(3) . ?
C1 C2 1.416(3) . ?
C13 C12 1.416(3) . ?
C13 C14 1.421(3) . ?
C13 C18 1.496(3) . ?
C6 C5 1.385(3) . ?
C6 H6 0.9300 . ?
C12 C11 1.423(3) . ?
C12 C17 1.508(3) . ?
C10 C11 1.417(3) . ?
C10 C14 1.426(3) . ?
C10 C15 1.494(3) . ?
C14 C19 1.496(3) . ?
C2 C3 1.385(3) . ?
C2 C7 1.509(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 C11 1.503(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9599 . ?
C16 H16C 0.9600 . ?
C3 C4 1.389(4) . ?
C3 H3 0.9301 . ?
N2 C9 1.454(4) . ?
N2 C7 1.456(3) . ?
N2 C8 1.463(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C5 C4 1.380(4) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9601 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9601 . ?
C9 H9C 0.9600 . ?

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 83.06(8) . 2_566 ?
N1 Zr1 Cl1 105.72(5) . . ?
N1 Zr1 Cl1 112.97(5) 2_566 . ?
N1 Zr1 C12 98.04(8) . . ?
N1 Zr1 C12 101.17(7) 2_566 . ?
Cl1 Zr1 C12 140.12(6) . . ?
N1 Zr1 C13 130.70(8) . . ?
N1 Zr1 C13 98.19(7) 2_566 . ?
Cl1 Zr1 C13 118.32(6) . . ?
C12 Zr1 C13 33.03(8) . . ?
N1 Zr1 C11 87.82(8) . . ?
N1 Zr1 C11 131.27(8) 2_566 . ?
Cl1 Zr1 C11 115.59(6) . . ?
C12 Zr1 C11 33.20(8) . . ?
C13 Zr1 C11 54.63(8) . . ?
N1 Zr1 C14 141.78(8) . . ?
N1 Zr1 C14 124.68(7) 2_566 . ?
Cl1 Zr1 C14 88.07(6) . . ?
C12 Zr1 C14 54.68(8) . . ?
C13 Zr1 C14 32.84(8) . . ?
C11 Zr1 C14 54.43(8) . . ?
N1 Zr1 C10 111.17(8) . . ?
N1 Zr1 C10 152.21(7) 2_566 . ?
Cl1 Zr1 C10 86.83(6) . . ?
C12 Zr1 C10 54.49(8) . . ?
C13 Zr1 C10 54.26(7) . . ?
C11 Zr1 C10 32.62(7) . . ?
C14 Zr1 C10 32.70(7) . . ?
N1 Zr1 Zr1 43.25(5) . 2_566 ?
N1 Zr1 Zr1 39.81(5) 2_566 2_566 ?
Cl1 Zr1 Zr1 116.370(18) . 2_566 ?
C12 Zr1 Zr1 102.94(6) . 2_566 ?
C13 Zr1 Zr1 121.27(6) . 2_566 ?
C11 Zr1 Zr1 115.51(6) . 2_566 ?
C14 Zr1 Zr1 154.08(6) . 2_566 ?
C10 Zr1 Zr1 147.52(5) . 2_566 ?
C1 N1 Zr1 152.80(15) . . ?
C1 N1 Zr1 109.04(14) . 2_566 ?
Zr1 N1 Zr1 96.94(8) . 2_566 ?
C6 C1 N1 121.0(2) . . ?
C6 C1 C2 118.4(2) . . ?
N1 C1 C2 120.7(2) . . ?
C12 C13 C14 108.2(2) . . ?
C12 C13 C18 126.5(2) . . ?
C14 C13 C18 125.2(2) . . ?
C12 C13 Zr1 72.50(12) . . ?
C14 C13 Zr1 74.43(12) . . ?
C18 C13 Zr1 121.68(15) . . ?
C5 C6 C1 121.6(2) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
C13 C12 C11 108.0(2) . . ?
C13 C12 C17 126.0(2) . . ?
C11 C12 C17 125.9(2) . . ?
C13 C12 Zr1 74.47(13) . . ?
C11 C12 Zr1 74.39(13) . . ?
C17 C12 Zr1 119.39(15) . . ?
C11 C10 C14 108.0(2) . . ?
C11 C10 C15 126.6(2) . . ?
C14 C10 C15 125.4(2) . . ?
C11 C10 Zr1 72.21(13) . . ?
C14 C10 Zr1 73.02(13) . . ?
C15 C10 Zr1 121.51(16) . . ?
C13 C14 C10 107.8(2) . . ?
C13 C14 C19 126.4(2) . . ?
C10 C14 C19 125.8(2) . . ?
C13 C14 Zr1 72.73(12) . . ?
C10 C14 Zr1 74.28(13) . . ?
C19 C14 Zr1 120.91(16) . . ?
C3 C2 C1 118.9(2) . . ?
C3 C2 C7 121.6(2) . . ?
C1 C2 C7 119.4(2) . . ?
C10 C15 H15A 109.4 . . ?
C10 C15 H15B 109.4 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.6 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C18 H18A 109.4 . . ?
C13 C18 H18B 109.4 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.6 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C17 H17A 109.4 . . ?
C12 C17 H17B 109.4 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.6 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C16 H16A 109.6 . . ?
C11 C16 H16B 109.3 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C2 C3 C4 121.8(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.0 . . ?
C9 N2 C7 110.6(2) . . ?
C9 N2 C8 111.0(3) . . ?
C7 N2 C8 110.7(2) . . ?
C10 C11 C12 108.0(2) . . ?
C10 C11 C16 126.0(2) . . ?
C12 C11 C16 125.7(2) . . ?
C10 C11 Zr1 75.17(13) . . ?
C12 C11 Zr1 72.42(13) . . ?
C16 C11 Zr1 122.16(15) . . ?
N2 C7 C2 113.5(2) . . ?
N2 C7 H7A 108.9 . . ?
C2 C7 H7A 108.9 . . ?
N2 C7 H7B 108.8 . . ?
C2 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C14 C19 H19A 109.6 . . ?
C14 C19 H19B 109.3 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.6 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.0 . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.5 . . ?
N2 C8 H8A 109.6 . . ?
N2 C8 H8B 109.2 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.7 . . ?
N2 C9 H9B 109.4 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.3 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.080
####################################################################### 
# 
# 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_17
_database_code_depnum_ccdc_archive 'CCDC 1044563'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H38 Cl Hf N3'
_chemical_formula_sum            'C27 H38 Cl Hf N3'
_chemical_formula_weight         618.54

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'
Hf Hf -0.5830 6.1852 '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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   10.7501(7)
_cell_length_b                   9.0630(6)
_cell_length_c                   27.246(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.570(6)
_cell_angle_gamma                90
_cell_volume                     2590.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    21236
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    4.149
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.249
0 -1 0 0.117
0 0 1 0.028
0 0 -1 0.015
-1 0 1 0.086
1 0 -1 0.069
-1 1 1 0.184


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21173
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5822
_reflns_number_gt                4760
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0000P)²+8.6542P] 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         5822
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.146
_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 0.272643(18) 0.54104(2) 0.160077(7) 0.01594(6) Uani 1 1 d . . .
Cl1 Cl 0.43050(12) 0.57875(14) 0.23839(5) 0.0259(3) Uani 1 1 d . . .
C4 C 0.0622(5) 0.0836(6) 0.0687(2) 0.0287(12) Uani 1 1 d . . .
H4 H 0.0213 0.0013 0.0522 0.034 Uiso 1 1 d R . .
C19 C 0.0747(5) 0.6863(5) 0.1567(2) 0.0225(11) Uani 1 1 d . . .
H19 H 0.0152 0.6511 0.1741 0.027 Uiso 1 1 d R . .
C20 C 0.1758(5) 0.7817(5) 0.17657(19) 0.0218(10) Uani 1 1 d . . .
C22 C 0.1799(5) 0.7281(5) 0.09434(19) 0.0205(10) Uani 1 1 d . . .
N1 N 0.1815(4) 0.3828(4) 0.21681(15) 0.0198(8) Uani 1 1 d . . .
C3 C 0.0370(5) 0.1282(6) 0.1139(2) 0.0255(11) Uani 1 1 d . . .
H3 H -0.0199 0.0751 0.1283 0.031 Uiso 1 1 d R . .
C25 C 0.3542(5) 0.9109(5) 0.1417(2) 0.0255(11) Uani 1 1 d . . .
H25A H 0.4071 0.8771 0.1197 0.031 Uiso 1 1 d R . .
H25B H 0.4028 0.9122 0.1757 0.031 Uiso 1 1 d R . .
H25C H 0.3241 1.0087 0.1320 0.031 Uiso 1 1 d R . .
C8 C 0.2768(5) 0.2656(5) 0.23739(19) 0.0237(11) Uani 1 1 d . . .
H8A H 0.3476 0.3091 0.2604 0.028 Uiso 1 1 d R . .
H8B H 0.3062 0.2203 0.2101 0.028 Uiso 1 1 d R . .
H8C H 0.2378 0.1923 0.2546 0.028 Uiso 1 1 d R . .
C1 C 0.1858(4) 0.3368(5) 0.11737(18) 0.0198(10) Uani 1 1 d . . .
C26 C 0.2100(5) 0.7328(6) 0.0428(2) 0.0285(12) Uani 1 1 d . . .
H26A H 0.1989 0.6365 0.0278 0.034 Uiso 1 1 d R . .
H26B H 0.2966 0.7642 0.0457 0.034 Uiso 1 1 d R . .
H26C H 0.1536 0.8012 0.0220 0.034 Uiso 1 1 d R . .
C6 C 0.2088(5) 0.2840(5) 0.07164(19) 0.0241(11) Uani 1 1 d . . .
H6 H 0.2676 0.3333 0.0571 0.029 Uiso 1 1 d R . .
C7 C 0.0674(5) 0.3091(5) 0.18567(19) 0.0216(10) Uani 1 1 d . . .
H7A H -0.0026 0.3789 0.1780 0.026 Uiso 1 1 d R . .
H7B H 0.0412 0.2273 0.2041 0.026 Uiso 1 1 d R . .
C9 C 0.1447(5) 0.4561(6) 0.26001(18) 0.0273(11) Uani 1 1 d . . .
H9A H 0.1129 0.3844 0.2802 0.033 Uiso 1 1 d R . .
H9B H 0.0796 0.5278 0.2478 0.033 Uiso 1 1 d R . .
H9C H 0.2179 0.5043 0.2800 0.033 Uiso 1 1 d R . .
C24 C 0.2032(5) 0.8523(6) 0.2276(2) 0.0286(12) Uani 1 1 d . . .
H24A H 0.1517 0.9392 0.2269 0.034 Uiso 1 1 d R . .
H24B H 0.2917 0.8788 0.2370 0.034 Uiso 1 1 d R . .
H24C H 0.1835 0.7838 0.2517 0.034 Uiso 1 1 d R . .
C2 C 0.0976(5) 0.2539(5) 0.13768(19) 0.0206(10) Uani 1 1 d . . .
C21 C 0.2422(5) 0.8081(5) 0.13763(19) 0.0207(10) Uani 1 1 d . . .
C23 C 0.0754(5) 0.6526(5) 0.10598(19) 0.0223(11) Uani 1 1 d . . .
C27 C -0.0244(5) 0.5698(6) 0.0700(2) 0.0320(13) Uani 1 1 d . . .
H27A H -0.0816 0.6387 0.0498 0.038 Uiso 1 1 d R . .
H27B H -0.0710 0.5088 0.0885 0.038 Uiso 1 1 d R . .
H27C H 0.0142 0.5090 0.0486 0.038 Uiso 1 1 d R . .
C5 C 0.1473(5) 0.1609(6) 0.0473(2) 0.0304(13) Uani 1 1 d . . .
H5 H 0.1641 0.1306 0.0168 0.036 Uiso 1 1 d R . .
N2 N 0.4125(3) 0.5437(5) 0.11928(14) 0.0198(8) Uani 1 1 d . . .
H2 H 0.4229 0.6336 0.1029 0.024 Uiso 1 1 d R . .
N3 N 0.5794(4) 0.7434(5) 0.07653(16) 0.0228(9) Uani 1 1 d . . .
C11 C 0.5920(4) 0.4678(5) 0.08288(17) 0.0196(9) Uani 1 1 d . . .
C10 C 0.5077(4) 0.4431(5) 0.11553(17) 0.0178(9) Uani 1 1 d . . .
C12 C 0.6817(5) 0.3598(6) 0.07923(19) 0.0254(11) Uani 1 1 d . . .
H12 H 0.7375 0.3757 0.0580 0.030 Uiso 1 1 d R . .
C16 C 0.5812(5) 0.6027(6) 0.05021(19) 0.0241(11) Uani 1 1 d . . .
H16A H 0.6533 0.6036 0.0342 0.029 Uiso 1 1 d R . .
H16B H 0.5046 0.5956 0.0239 0.029 Uiso 1 1 d R . .
C15 C 0.5214(5) 0.3121(6) 0.1433(2) 0.0253(11) Uani 1 1 d . . .
H15 H 0.4691 0.2961 0.1659 0.030 Uiso 1 1 d R . .
C14 C 0.6096(5) 0.2067(6) 0.1388(2) 0.0281(12) Uani 1 1 d . . .
H14 H 0.6144 0.1202 0.1574 0.034 Uiso 1 1 d R . .
C13 C 0.6913(5) 0.2287(6) 0.1066(2) 0.0282(12) Uani 1 1 d . . .
H13 H 0.7509 0.1572 0.1032 0.034 Uiso 1 1 d R . .
C18 C 0.5636(6) 0.8651(6) 0.0405(2) 0.0364(14) Uani 1 1 d . . .
H18A H 0.5479 0.9544 0.0571 0.044 Uiso 1 1 d R . .
H18B H 0.4928 0.8452 0.0131 0.044 Uiso 1 1 d R . .
H18C H 0.6397 0.8760 0.0278 0.044 Uiso 1 1 d R . .
C17 C 0.6921(6) 0.7653(6) 0.1159(2) 0.0400(15) Uani 1 1 d . . .
H17A H 0.7022 0.6836 0.1389 0.048 Uiso 1 1 d R . .
H17B H 0.6828 0.8547 0.1337 0.048 Uiso 1 1 d R . .
H17C H 0.7657 0.7727 0.1015 0.048 Uiso 1 1 d 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 2.055(4) . ?
Hf1 C1 2.276(5) . ?
Hf1 Cl1 2.4440(13) . ?
Hf1 N1 2.463(4) . ?
Hf1 C19 2.487(5) . ?
Hf1 C20 2.500(5) . ?
Hf1 C21 2.501(5) . ?
Hf1 C22 2.510(5) . ?
Hf1 C23 2.516(5) . ?
C4 C3 1.377(8) . ?
C4 C5 1.379(8) . ?
C4 H4 0.9299 . ?
C19 C20 1.401(7) . ?
C19 C23 1.418(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.422(7) . ?
C20 C24 1.501(7) . ?
C22 C23 1.409(7) . ?
C22 C21 1.422(7) . ?
C22 C26 1.510(7) . ?
N1 C9 1.478(6) . ?
N1 C7 1.489(6) . ?
N1 C8 1.497(6) . ?
C3 C2 1.400(7) . ?
C3 H3 0.9301 . ?
C25 C21 1.507(7) . ?
C25 H25A 0.9602 . ?
C25 H25B 0.9599 . ?
C25 H25C 0.9600 . ?
C8 H8A 0.9601 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C1 C6 1.407(7) . ?
C1 C2 1.413(7) . ?
C26 H26A 0.9601 . ?
C26 H26B 0.9601 . ?
C26 H26C 0.9599 . ?
C6 C5 1.389(7) . ?
C6 H6 0.9300 . ?
C7 C2 1.500(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9701 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9599 . ?
C23 C27 1.489(7) . ?
C27 H27A 0.9601 . ?
C27 H27B 0.9599 . ?
C27 H27C 0.9600 . ?
C5 H5 0.9301 . ?
N2 C10 1.392(6) . ?
N2 H2 0.9474 . ?
N3 C17 1.447(7) . ?
N3 C18 1.462(7) . ?
N3 C16 1.464(6) . ?
C11 C12 1.392(7) . ?
C11 C10 1.419(6) . ?
C11 C16 1.502(7) . ?
C10 C15 1.399(7) . ?
C12 C13 1.394(7) . ?
C12 H12 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9699 . ?
C15 C14 1.370(7) . ?
C15 H15 0.9300 . ?
C14 C13 1.384(8) . ?
C14 H14 0.9299 . ?
C13 H13 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9601 . ?
C18 H18C 0.9600 . ?
C17 H17A 0.9599 . ?
C17 H17B 0.9601 . ?
C17 H17C 0.9599 . ?

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 C1 90.01(17) . . ?
N2 Hf1 Cl1 91.14(11) . . ?
C1 Hf1 Cl1 133.62(12) . . ?
N2 Hf1 N1 141.65(15) . . ?
C1 Hf1 N1 70.87(15) . . ?
Cl1 Hf1 N1 80.15(10) . . ?
N2 Hf1 C19 134.00(16) . . ?
C1 Hf1 C19 99.17(17) . . ?
Cl1 Hf1 C19 112.57(12) . . ?
N1 Hf1 C19 82.95(15) . . ?
N2 Hf1 C20 117.98(17) . . ?
C1 Hf1 C20 131.38(17) . . ?
Cl1 Hf1 C20 87.61(12) . . ?
N1 Hf1 C20 99.04(15) . . ?
C19 Hf1 C20 32.64(16) . . ?
N2 Hf1 C21 85.90(16) . . ?
C1 Hf1 C21 130.15(16) . . ?
Cl1 Hf1 C21 96.16(12) . . ?
N1 Hf1 C21 131.94(15) . . ?
C19 Hf1 C21 54.06(16) . . ?
C20 Hf1 C21 33.04(16) . . ?
N2 Hf1 C22 80.19(16) . . ?
C1 Hf1 C22 97.44(17) . . ?
Cl1 Hf1 C22 128.39(12) . . ?
N1 Hf1 C22 133.70(15) . . ?
C19 Hf1 C22 54.02(17) . . ?
C20 Hf1 C22 54.72(16) . . ?
C21 Hf1 C22 32.97(16) . . ?
N2 Hf1 C23 107.50(16) . . ?
C1 Hf1 C23 80.06(16) . . ?
Cl1 Hf1 C23 142.36(12) . . ?
N1 Hf1 C23 101.66(15) . . ?
C19 Hf1 C23 32.93(16) . . ?
C20 Hf1 C23 54.82(16) . . ?
C21 Hf1 C23 54.48(16) . . ?
C22 Hf1 C23 32.57(16) . . ?
C3 C4 C5 120.4(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 119.3 . . ?
C20 C19 C23 109.9(5) . . ?
C20 C19 Hf1 74.2(3) . . ?
C23 C19 Hf1 74.7(3) . . ?
C20 C19 H19 125.2 . . ?
C23 C19 H19 124.8 . . ?
Hf1 C19 H19 118.5 . . ?
C19 C20 C21 106.8(4) . . ?
C19 C20 C24 126.9(5) . . ?
C21 C20 C24 126.2(5) . . ?
C19 C20 Hf1 73.2(3) . . ?
C21 C20 Hf1 73.5(3) . . ?
C24 C20 Hf1 122.2(3) . . ?
C23 C22 C21 108.4(4) . . ?
C23 C22 C26 124.5(5) . . ?
C21 C22 C26 126.9(5) . . ?
C23 C22 Hf1 74.0(3) . . ?
C21 C22 Hf1 73.2(3) . . ?
C26 C22 Hf1 123.4(3) . . ?
C9 N1 C7 109.0(4) . . ?
C9 N1 C8 107.5(4) . . ?
C7 N1 C8 107.8(4) . . ?
C9 N1 Hf1 116.8(3) . . ?
C7 N1 Hf1 107.1(3) . . ?
C8 N1 Hf1 108.4(3) . . ?
C4 C3 C2 119.4(5) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.5 . . ?
C21 C25 H25A 109.2 . . ?
C21 C25 H25B 109.7 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.6 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.1 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.8 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C1 C2 115.3(4) . . ?
C6 C1 Hf1 126.7(4) . . ?
C2 C1 Hf1 117.9(3) . . ?
C22 C26 H26A 109.8 . . ?
C22 C26 H26B 109.3 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.3 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C5 C6 C1 122.6(5) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.7 . . ?
N1 C7 C2 109.8(4) . . ?
N1 C7 H7A 109.5 . . ?
C2 C7 H7A 109.5 . . ?
N1 C7 H7B 110.1 . . ?
C2 C7 H7B 109.8 . . ?
H7A C7 H7B 108.1 . . ?
N1 C9 H9A 110.0 . . ?
N1 C9 H9B 109.2 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.2 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.7 . . ?
H24A C24 H24B 109.5 . . ?
C20 C24 H24C 109.2 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C3 C2 C1 122.4(5) . . ?
C3 C2 C7 120.5(5) . . ?
C1 C2 C7 117.1(4) . . ?
C22 C21 C20 108.1(4) . . ?
C22 C21 C25 126.9(5) . . ?
C20 C21 C25 124.9(5) . . ?
C22 C21 Hf1 73.9(3) . . ?
C20 C21 Hf1 73.4(3) . . ?
C25 C21 Hf1 121.4(3) . . ?
C22 C23 C19 106.8(5) . . ?
C22 C23 C27 126.3(5) . . ?
C19 C23 C27 126.5(5) . . ?
C22 C23 Hf1 73.5(3) . . ?
C19 C23 Hf1 72.4(3) . . ?
C27 C23 Hf1 125.3(3) . . ?
C23 C27 H27A 109.2 . . ?
C23 C27 H27B 109.1 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 110.1 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C4 C5 C6 119.8(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.0 . . ?
C10 N2 Hf1 132.0(3) . . ?
C10 N2 H2 111.4 . . ?
Hf1 N2 H2 116.1 . . ?
C17 N3 C18 110.5(4) . . ?
C17 N3 C16 112.6(4) . . ?
C18 N3 C16 109.9(4) . . ?
C12 C11 C10 118.7(5) . . ?
C12 C11 C16 119.7(4) . . ?
C10 C11 C16 121.5(4) . . ?
N2 C10 C15 120.6(4) . . ?
N2 C10 C11 121.5(4) . . ?
C15 C10 C11 117.8(4) . . ?
C11 C12 C13 122.2(5) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 118.7 . . ?
N3 C16 C11 115.2(4) . . ?
N3 C16 H16A 108.1 . . ?
C11 C16 H16A 107.9 . . ?
N3 C16 H16B 108.7 . . ?
C11 C16 H16B 109.1 . . ?
H16A C16 H16B 107.5 . . ?
C14 C15 C10 122.4(5) . . ?
C14 C15 H15 118.8 . . ?
C10 C15 H15 118.8 . . ?
C15 C14 C13 120.3(5) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 120.1 . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.9 . . ?
N3 C18 H18A 109.1 . . ?
N3 C18 H18B 109.7 . . ?
H18A C18 H18B 109.5 . . ?
N3 C18 H18C 109.6 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C17 H17A 109.6 . . ?
N3 C17 H17B 109.1 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.7 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 N3 0.95 2.21 2.960(6) 135.9 .

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.152
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1044564'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H69 N3 Zr'
_chemical_formula_sum            'C46 H69 N3 Zr'
_chemical_formula_weight         755.26

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'
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'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5520(9)
_cell_length_b                   11.3391(10)
_cell_length_c                   19.2680(15)
_cell_angle_alpha                89.837(6)
_cell_angle_beta                 85.731(5)
_cell_angle_gamma                70.379(7)
_cell_volume                     2164.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    43774
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    0.286
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.089
-1 -1 0 0.119
0 -1 0 0.116
0 1 0 0.124
0 0 1 0.042
0 0 -1 0.034
1 0 0 0.095
-1 0 0 0.114


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43669
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9893
_reflns_number_gt                8380
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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+1.0987P] where P=(Fo²+2Fc²)/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         9893
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0856
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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 0.263444(18) 0.049170(16) 0.235159(9) 0.02438(6) Uani 1 1 d . . .
N3 N 0.21200(16) -0.05923(15) 0.16298(8) 0.0301(3) Uani 1 1 d . . .
H3 H 0.2535 -0.0576 0.1230 0.036 Uiso 1 1 d R . .
N2 N 0.19290(17) 0.00641(17) 0.33142(8) 0.0365(4) Uani 1 1 d . . .
H2 H 0.1065 0.0405 0.3356 0.044 Uiso 1 1 d R . .
C35 C 0.12966(19) -0.13521(17) 0.15897(10) 0.0295(4) Uani 1 1 d . . .
N1 N 0.13561(17) 0.23177(15) 0.22543(9) 0.0346(4) Uani 1 1 d . . .
H1 H 0.1624 0.2796 0.2509 0.041 Uiso 1 1 d R . .
C36 C 0.1849(2) -0.25645(19) 0.12760(11) 0.0349(4) Uani 1 1 d . . .
C11 C 0.0211(2) 0.30819(17) 0.19281(11) 0.0343(4) Uani 1 1 d . . .
C16 C -0.0920(2) 0.38612(19) 0.23463(13) 0.0414(5) Uani 1 1 d . . .
C1 C 0.4499(2) 0.13833(19) 0.20059(12) 0.0370(5) Uani 1 1 d . . .
C2 C 0.4580(2) 0.1148(2) 0.27202(11) 0.0398(5) Uani 1 1 d . . .
C4 C 0.5167(2) -0.0733(2) 0.21403(13) 0.0410(5) Uani 1 1 d . . .
C3 C 0.5002(2) -0.0162(2) 0.28019(12) 0.0432(5) Uani 1 1 d . . .
C40 C -0.0059(2) -0.09188(19) 0.18596(11) 0.0358(4) Uani 1 1 d . . .
C12 C 0.0182(2) 0.30656(18) 0.12012(12) 0.0383(5) Uani 1 1 d . . .
C5 C 0.48382(19) 0.0221(2) 0.16450(11) 0.0365(5) Uani 1 1 d . . .
C23 C 0.2352(2) -0.0594(2) 0.39309(11) 0.0411(5) Uani 1 1 d . . .
C30 C 0.3965(4) -0.3910(3) 0.3169(2) 0.0929(11) Uani 1 1 d . . .
H30A H 0.4811 -0.3789 0.3220 0.111 Uiso 1 1 d R . .
H30B H 0.3976 -0.4256 0.2713 0.111 Uiso 1 1 d R . .
H30C H 0.3827 -0.4475 0.3515 0.111 Uiso 1 1 d R . .
C41 C 0.3270(2) -0.3007(2) 0.09295(12) 0.0424(5) Uani 1 1 d . . .
H41 H 0.3809 -0.2654 0.1203 0.051 Uiso 1 1 d R . .
C19 C 0.0996(3) 0.1337(2) 0.02751(13) 0.0510(6) Uani 1 1 d . . .
H19A H 0.0704 0.0788 0.0577 0.061 Uiso 1 1 d R . .
H19B H 0.1773 0.0855 -0.0018 0.061 Uiso 1 1 d R . .
H19C H 0.0282 0.1774 -0.0009 0.061 Uiso 1 1 d R . .
C13 C -0.0968(2) 0.3837(2) 0.09057(14) 0.0513(6) Uani 1 1 d . . .
H13 H -0.0990 0.3837 0.0424 0.062 Uiso 1 1 d R . .
C17 C 0.1361(2) 0.2288(2) 0.07107(12) 0.0413(5) Uani 1 1 d . . .
H17 H 0.2087 0.1817 0.0996 0.050 Uiso 1 1 d R . .
C24 C 0.2868(2) -0.1910(2) 0.39109(12) 0.0477(6) Uani 1 1 d . . .
C44 C -0.0785(2) 0.0411(2) 0.21305(13) 0.0437(5) Uani 1 1 d . . .
H44 H -0.0122 0.0845 0.2121 0.052 Uiso 1 1 d R . .
C37 C 0.1051(2) -0.3325(2) 0.12779(12) 0.0457(5) Uani 1 1 d . . .
H37 H 0.1411 -0.4126 0.1079 0.055 Uiso 1 1 d R . .
C39 C -0.0805(2) -0.1724(2) 0.18441(13) 0.0474(6) Uani 1 1 d . . .
H39 H -0.1698 -0.1447 0.2028 0.057 Uiso 1 1 d R . .
C20 C -0.0896(3) 0.3906(2) 0.31303(14) 0.0540(6) Uani 1 1 d . . .
H20 H -0.0378 0.3061 0.3272 0.065 Uiso 1 1 d R . .
C18 C 0.1900(3) 0.3116(2) 0.02311(14) 0.0558(6) Uani 1 1 d . . .
H18A H 0.2680 0.2603 -0.0049 0.067 Uiso 1 1 d R . .
H18B H 0.2143 0.3698 0.0508 0.067 Uiso 1 1 d R . .
H18C H 0.1216 0.3568 -0.0065 0.067 Uiso 1 1 d R . .
C38 C -0.0258(3) -0.2920(2) 0.15663(13) 0.0512(6) Uani 1 1 d . . .
H38 H -0.0769 -0.3448 0.1572 0.061 Uiso 1 1 d R . .
C6 C 0.4245(3) 0.2639(2) 0.16861(17) 0.0611(7) Uani 1 1 d . . .
H6A H 0.3417 0.3221 0.1894 0.073 Uiso 1 1 d R . .
H6B H 0.4181 0.2568 0.1195 0.073 Uiso 1 1 d R . .
H6C H 0.4977 0.2934 0.1764 0.073 Uiso 1 1 d R . .
C10 C 0.5007(3) 0.0031(3) 0.08712(13) 0.0626(7) Uani 1 1 d . . .
H10A H 0.5916 -0.0057 0.0707 0.075 Uiso 1 1 d R . .
H10B H 0.4391 0.0740 0.0660 0.075 Uiso 1 1 d R . .
H10C H 0.4821 -0.0712 0.0750 0.075 Uiso 1 1 d R . .
C28 C 0.2287(3) 0.0074(3) 0.45568(12) 0.0513(6) Uani 1 1 d . . .
C43 C 0.3310(3) -0.2505(3) 0.01978(13) 0.0581(7) Uani 1 1 d . . .
H43A H 0.2832 -0.2868 -0.0093 0.070 Uiso 1 1 d R . .
H43B H 0.4232 -0.2724 0.0013 0.070 Uiso 1 1 d R . .
H43C H 0.2895 -0.1610 0.0212 0.070 Uiso 1 1 d R . .
C46 C -0.1876(3) 0.1109(3) 0.16494(17) 0.0640(7) Uani 1 1 d . . .
H46A H -0.1486 0.1044 0.1179 0.077 Uiso 1 1 d R . .
H46B H -0.2249 0.1976 0.1792 0.077 Uiso 1 1 d R . .
H46C H -0.2577 0.0744 0.1677 0.077 Uiso 1 1 d R . .
C25 C 0.3362(3) -0.2526(3) 0.45090(15) 0.0659(8) Uani 1 1 d . . .
H25 H 0.3730 -0.3396 0.4498 0.079 Uiso 1 1 d R . .
C27 C 0.2781(3) -0.0600(3) 0.51419(14) 0.0712(9) Uani 1 1 d . . .
H27 H 0.2742 -0.0170 0.5557 0.085 Uiso 1 1 d R . .
C14 C -0.2066(3) 0.4592(2) 0.13078(16) 0.0587(7) Uani 1 1 d . . .
H14 H -0.2823 0.5096 0.1100 0.070 Uiso 1 1 d R . .
C15 C -0.2040(2) 0.4595(2) 0.20207(16) 0.0540(6) Uani 1 1 d . . .
H15 H -0.2789 0.5104 0.2292 0.065 Uiso 1 1 d R . .
C29 C 0.2828(3) -0.2652(2) 0.32646(13) 0.0532(6) Uani 1 1 d . . .
H29 H 0.2900 -0.2146 0.2860 0.064 Uiso 1 1 d R . .
C45 C -0.1403(3) 0.0482(3) 0.28771(15) 0.0645(8) Uani 1 1 d . . .
H45A H -0.2133 0.0154 0.2891 0.077 Uiso 1 1 d R . .
H45B H -0.1736 0.1338 0.3041 0.077 Uiso 1 1 d R . .
H45C H -0.0727 -0.0004 0.3169 0.077 Uiso 1 1 d R . .
C8 C 0.5451(3) -0.0840(3) 0.34608(16) 0.0786(10) Uani 1 1 d . . .
H8A H 0.5344 -0.1648 0.3450 0.094 Uiso 1 1 d R . .
H8B H 0.4914 -0.0357 0.3853 0.094 Uiso 1 1 d R . .
H8C H 0.6383 -0.0942 0.3501 0.094 Uiso 1 1 d R . .
C42 C 0.3946(3) -0.4424(2) 0.09100(18) 0.0721(8) Uani 1 1 d . . .
H42A H 0.3851 -0.4743 0.1365 0.086 Uiso 1 1 d R . .
H42B H 0.4887 -0.4626 0.0766 0.086 Uiso 1 1 d R . .
H42C H 0.3532 -0.4794 0.0587 0.086 Uiso 1 1 d R . .
C32 C 0.1652(3) 0.1485(3) 0.45942(13) 0.0585(7) Uani 1 1 d . . .
H32 H 0.1825 0.1795 0.4134 0.070 Uiso 1 1 d R . .
C7 C 0.4377(3) 0.2122(3) 0.32833(17) 0.0758(9) Uani 1 1 d . . .
H7A H 0.5169 0.2358 0.3288 0.091 Uiso 1 1 d R . .
H7B H 0.4215 0.1783 0.3725 0.091 Uiso 1 1 d R . .
H7C H 0.3615 0.2845 0.3198 0.091 Uiso 1 1 d R . .
C26 C 0.3324(4) -0.1875(3) 0.51155(16) 0.0786(10) Uani 1 1 d . . .
H26 H 0.3667 -0.2305 0.5509 0.094 Uiso 1 1 d R . .
C9 C 0.5756(3) -0.2120(2) 0.1986(2) 0.0735(9) Uani 1 1 d . . .
H9A H 0.6519 -0.2480 0.2254 0.088 Uiso 1 1 d R . .
H9B H 0.6039 -0.2262 0.1499 0.088 Uiso 1 1 d R . .
H9C H 0.5086 -0.2501 0.2106 0.088 Uiso 1 1 d R . .
C31 C 0.1471(3) -0.2848(3) 0.32755(16) 0.0717(8) Uani 1 1 d . . .
H31A H 0.1351 -0.3296 0.3684 0.086 Uiso 1 1 d R . .
H31B H 0.1439 -0.3321 0.2869 0.086 Uiso 1 1 d R . .
H31C H 0.0765 -0.2049 0.3284 0.086 Uiso 1 1 d R . .
C21 C -0.0151(4) 0.4776(3) 0.33517(18) 0.0803(9) Uani 1 1 d . . .
H21A H 0.0746 0.4505 0.3128 0.096 Uiso 1 1 d R . .
H21B H -0.0106 0.4750 0.3848 0.096 Uiso 1 1 d R . .
H21C H -0.0627 0.5617 0.3220 0.096 Uiso 1 1 d R . .
C34 C 0.0122(3) 0.1861(3) 0.47399(17) 0.0823(10) Uani 1 1 d . . .
H34A H -0.0235 0.1509 0.4381 0.099 Uiso 1 1 d R . .
H34B H -0.0276 0.2757 0.4745 0.099 Uiso 1 1 d R . .
H34C H -0.0082 0.1549 0.5183 0.099 Uiso 1 1 d R . .
C22 C -0.2286(3) 0.4272(3) 0.35266(18) 0.0848(10) Uani 1 1 d . . .
H22A H -0.2762 0.5148 0.3474 0.102 Uiso 1 1 d R . .
H22B H -0.2181 0.4099 0.4011 0.102 Uiso 1 1 d R . .
H22C H -0.2787 0.3792 0.3344 0.102 Uiso 1 1 d R . .
C33 C 0.2234(4) 0.2135(4) 0.51236(18) 0.0948(12) Uani 1 1 d . . .
H33A H 0.1982 0.1935 0.5586 0.114 Uiso 1 1 d R . .
H33B H 0.1880 0.3025 0.5068 0.114 Uiso 1 1 d R . .
H33C H 0.3200 0.1852 0.5049 0.114 Uiso 1 1 d 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 N2 2.0642(16) . ?
Zr1 N1 2.0740(16) . ?
Zr1 N3 2.0760(15) . ?
Zr1 C5 2.5312(19) . ?
Zr1 C1 2.5439(19) . ?
Zr1 C2 2.553(2) . ?
Zr1 C4 2.566(2) . ?
Zr1 C3 2.573(2) . ?
N3 C35 1.420(2) . ?
N3 H3 0.8599 . ?
N2 C23 1.421(3) . ?
N2 H2 0.8599 . ?
C35 C40 1.406(3) . ?
C35 C36 1.417(3) . ?
N1 C11 1.419(3) . ?
N1 H1 0.8600 . ?
C36 C37 1.392(3) . ?
C36 C41 1.514(3) . ?
C11 C12 1.403(3) . ?
C11 C16 1.417(3) . ?
C16 C15 1.389(3) . ?
C16 C20 1.514(4) . ?
C1 C2 1.405(3) . ?
C1 C5 1.414(3) . ?
C1 C6 1.498(3) . ?
C2 C3 1.412(3) . ?
C2 C7 1.502(3) . ?
C4 C3 1.404(3) . ?
C4 C5 1.412(3) . ?
C4 C9 1.505(3) . ?
C3 C8 1.505(3) . ?
C40 C39 1.393(3) . ?
C40 C44 1.518(3) . ?
C12 C13 1.396(3) . ?
C12 C17 1.520(3) . ?
C5 C10 1.496(3) . ?
C23 C24 1.406(3) . ?
C23 C28 1.411(3) . ?
C30 C29 1.526(4) . ?
C30 H30A 0.9599 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C41 C43 1.522(3) . ?
C41 C42 1.523(3) . ?
C41 H41 0.9801 . ?
C19 C17 1.531(3) . ?
C19 H19A 0.9599 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9601 . ?
C13 C14 1.371(4) . ?
C13 H13 0.9301 . ?
C17 C18 1.528(3) . ?
C17 H17 0.9800 . ?
C24 C25 1.389(3) . ?
C24 C29 1.516(4) . ?
C44 C45 1.525(4) . ?
C44 C46 1.534(4) . ?
C44 H44 0.9800 . ?
C37 C38 1.374(3) . ?
C37 H37 0.9300 . ?
C39 C38 1.375(3) . ?
C39 H39 0.9300 . ?
C20 C22 1.527(4) . ?
C20 C21 1.532(4) . ?
C20 H20 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C38 H38 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9601 . ?
C6 H6C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C28 C27 1.394(4) . ?
C28 C32 1.513(4) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9601 . ?
C43 H43C 0.9600 . ?
C46 H46A 0.9599 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9601 . ?
C25 C26 1.375(4) . ?
C25 H25 0.9300 . ?
C27 C26 1.364(5) . ?
C27 H27 0.9299 . ?
C14 C15 1.376(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9301 . ?
C29 C31 1.520(4) . ?
C29 H29 0.9800 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9599 . ?
C8 H8A 0.9601 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C32 C34 1.529(4) . ?
C32 C33 1.537(4) . ?
C32 H32 0.9800 . ?
C7 H7A 0.9599 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C26 H26 0.9301 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9599 . ?
C9 H9C 0.9601 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9601 . ?
C21 H21C 0.9600 . ?
C34 H34A 0.9601 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9599 . ?
C22 H22C 0.9601 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9599 . ?

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 Zr1 N1 100.91(7) . . ?
N2 Zr1 N3 106.07(6) . . ?
N1 Zr1 N3 106.64(6) . . ?
N2 Zr1 C5 140.17(7) . . ?
N1 Zr1 C5 108.49(7) . . ?
N3 Zr1 C5 90.81(6) . . ?
N2 Zr1 C1 131.04(7) . . ?
N1 Zr1 C1 84.46(7) . . ?
N3 Zr1 C1 118.98(7) . . ?
C5 Zr1 C1 32.36(7) . . ?
N2 Zr1 C2 99.22(7) . . ?
N1 Zr1 C2 93.99(7) . . ?
N3 Zr1 C2 143.24(7) . . ?
C5 Zr1 C2 53.33(7) . . ?
C1 Zr1 C2 31.99(7) . . ?
N2 Zr1 C4 109.57(7) . . ?
N1 Zr1 C4 137.36(7) . . ?
N3 Zr1 C4 93.02(7) . . ?
C5 Zr1 C4 32.15(7) . . ?
C1 Zr1 C4 53.06(7) . . ?
C2 Zr1 C4 52.93(7) . . ?
N2 Zr1 C3 88.06(7) . . ?
N1 Zr1 C3 125.67(7) . . ?
N3 Zr1 C3 122.14(7) . . ?
C5 Zr1 C3 53.01(7) . . ?
C1 Zr1 C3 52.86(7) . . ?
C2 Zr1 C3 31.98(7) . . ?
C4 Zr1 C3 31.70(8) . . ?
C35 N3 Zr1 139.77(13) . . ?
C35 N3 H3 110.1 . . ?
Zr1 N3 H3 110.2 . . ?
C23 N2 Zr1 142.84(14) . . ?
C23 N2 H2 108.6 . . ?
Zr1 N2 H2 108.5 . . ?
C40 C35 C36 119.53(17) . . ?
C40 C35 N3 120.84(17) . . ?
C36 C35 N3 119.63(17) . . ?
C11 N1 Zr1 144.15(13) . . ?
C11 N1 H1 107.9 . . ?
Zr1 N1 H1 107.9 . . ?
C37 C36 C35 118.8(2) . . ?
C37 C36 C41 120.85(19) . . ?
C35 C36 C41 120.30(17) . . ?
C12 C11 C16 119.92(19) . . ?
C12 C11 N1 120.92(18) . . ?
C16 C11 N1 119.15(19) . . ?
C15 C16 C11 118.6(2) . . ?
C15 C16 C20 120.9(2) . . ?
C11 C16 C20 120.6(2) . . ?
C2 C1 C5 108.09(18) . . ?
C2 C1 C6 125.2(2) . . ?
C5 C1 C6 126.4(2) . . ?
C2 C1 Zr1 74.37(11) . . ?
C5 C1 Zr1 73.33(11) . . ?
C6 C1 Zr1 123.32(15) . . ?
C1 C2 C3 107.89(19) . . ?
C1 C2 C7 125.3(2) . . ?
C3 C2 C7 126.6(2) . . ?
C1 C2 Zr1 73.64(11) . . ?
C3 C2 Zr1 74.77(11) . . ?
C7 C2 Zr1 121.79(16) . . ?
C3 C4 C5 108.01(19) . . ?
C3 C4 C9 125.4(2) . . ?
C5 C4 C9 126.2(2) . . ?
C3 C4 Zr1 74.40(12) . . ?
C5 C4 Zr1 72.55(11) . . ?
C9 C4 Zr1 124.55(15) . . ?
C4 C3 C2 108.22(19) . . ?
C4 C3 C8 125.1(2) . . ?
C2 C3 C8 125.8(2) . . ?
C4 C3 Zr1 73.90(11) . . ?
C2 C3 Zr1 73.25(12) . . ?
C8 C3 Zr1 127.44(15) . . ?
C39 C40 C35 118.75(19) . . ?
C39 C40 C44 117.76(19) . . ?
C35 C40 C44 123.39(17) . . ?
C13 C12 C11 118.7(2) . . ?
C13 C12 C17 117.7(2) . . ?
C11 C12 C17 123.58(18) . . ?
C4 C5 C1 107.76(19) . . ?
C4 C5 C10 125.9(2) . . ?
C1 C5 C10 125.8(2) . . ?
C4 C5 Zr1 75.30(12) . . ?
C1 C5 Zr1 74.31(11) . . ?
C10 C5 Zr1 122.76(15) . . ?
C24 C23 C28 120.2(2) . . ?
C24 C23 N2 119.8(2) . . ?
C28 C23 N2 120.0(2) . . ?
C29 C30 H30A 109.2 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.4 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C41 C43 111.39(19) . . ?
C36 C41 C42 113.9(2) . . ?
C43 C41 C42 109.8(2) . . ?
C36 C41 H41 107.1 . . ?
C43 C41 H41 107.0 . . ?
C42 C41 H41 107.3 . . ?
C17 C19 H19A 109.7 . . ?
C17 C19 H19B 109.4 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.3 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C13 C12 121.6(2) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.1 . . ?
C12 C17 C18 111.47(19) . . ?
C12 C17 C19 112.31(19) . . ?
C18 C17 C19 109.8(2) . . ?
C12 C17 H17 107.7 . . ?
C18 C17 H17 107.8 . . ?
C19 C17 H17 107.6 . . ?
C25 C24 C23 118.5(2) . . ?
C25 C24 C29 120.2(2) . . ?
C23 C24 C29 121.1(2) . . ?
C40 C44 C45 113.4(2) . . ?
C40 C44 C46 110.4(2) . . ?
C45 C44 C46 110.0(2) . . ?
C40 C44 H44 107.8 . . ?
C45 C44 H44 107.7 . . ?
C46 C44 H44 107.5 . . ?
C38 C37 C36 121.6(2) . . ?
C38 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C38 C39 C40 121.9(2) . . ?
C38 C39 H39 119.0 . . ?
C40 C39 H39 119.1 . . ?
C16 C20 C22 114.4(2) . . ?
C16 C20 C21 111.0(2) . . ?
C22 C20 C21 109.8(2) . . ?
C16 C20 H20 107.1 . . ?
C22 C20 H20 107.3 . . ?
C21 C20 H20 107.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.3 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.6 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C37 C38 C39 119.3(2) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.4 . . ?
C1 C6 H6A 109.6 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.4 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.4 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.6 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C27 C28 C23 118.4(3) . . ?
C27 C28 C32 121.1(2) . . ?
C23 C28 C32 120.5(2) . . ?
C41 C43 H43A 109.4 . . ?
C41 C43 H43B 109.3 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.7 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C46 H46A 109.6 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.3 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C26 C25 C24 121.3(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.3 . . ?
C26 C27 C28 121.3(3) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.1 . . ?
C13 C14 C15 119.5(2) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 121.7(2) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.1 . . ?
C24 C29 C31 109.4(2) . . ?
C24 C29 C30 114.4(3) . . ?
C31 C29 C30 109.8(3) . . ?
C24 C29 H29 107.7 . . ?
C31 C29 H29 107.6 . . ?
C30 C29 H29 107.7 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.4 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C3 C8 H8A 109.9 . . ?
C3 C8 H8B 109.2 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.3 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.7 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C28 C32 C34 110.2(2) . . ?
C28 C32 C33 114.5(3) . . ?
C34 C32 C33 110.2(3) . . ?
C28 C32 H32 107.1 . . ?
C34 C32 H32 107.4 . . ?
C33 C32 H32 107.2 . . ?
C2 C7 H7A 109.7 . . ?
C2 C7 H7B 109.2 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.4 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C29 C31 H31A 109.2 . . ?
C29 C31 H31B 109.9 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.3 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C32 C34 H34A 109.1 . . ?
C32 C34 H34B 109.7 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.6 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C20 C22 H22A 109.8 . . ?
C20 C22 H22B 109.3 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.2 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.7 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.314 0.447 0.472 41 4 ' '
2 0.687 0.553 0.529 42 4 ' '
_platon_squeeze_details          ?


_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.055

#END












