# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_20171104TiPNPCl2
_database_code_depnum_ccdc_archive 'CCDC 1847681'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H42 Cl2 N P2 Ti'
_chemical_formula_moiety         'C22 H42 Cl2 N P2 Ti'
_chemical_formula_weight         501.33
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_space_group_IT_number           19
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,-Y,1/2+Z
3 1/2+X,1/2-Y,-Z
4 -X,1/2+Y,1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.5443(3)
_cell_length_b                   14.5948(4)
_cell_length_c                   15.2113(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     2784.91(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23781
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    177
#------------------------------------------------------------------------------
_exptl_crystal_description       chunk
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1068.00
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_T_max  0.951

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      177
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            27304
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         1.934
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6384
_reflns_number_gt                5489
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0555
_refine_ls_wR_factor_gt          0.0533
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6384
_refine_ls_number_parameters     265
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+1.3750P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 2096 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(9)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.26645(4) 0.32162(4) 0.72736(3) 0.02758(11) Uani 1 1 d . . . . .
Cl1 Cl 0.16349(7) 0.31439(7) 0.60434(5) 0.0536(2) Uani 1 1 d . . . . .
Cl2 Cl 0.33834(7) 0.46644(5) 0.72152(6) 0.0473(2) Uani 1 1 d . . . . .
P1 P 0.12031(6) 0.36397(6) 0.84155(5) 0.03556(19) Uani 1 1 d . . . . .
P2 P 0.43493(6) 0.22282(5) 0.68296(5) 0.02961(17) Uani 1 1 d . . . . .
N1 N 0.25764(18) 0.20992(15) 0.80792(15) 0.0305(5) Uani 1 1 d . . . . .
C1 C 0.0746(3) 0.2470(2) 0.8613(2) 0.0426(8) Uani 1 1 d . . . . .
H1A H 0.036366 0.243090 0.918150 0.051 Uiso 1 1 calc R U . . .
H1B H 0.025815 0.226986 0.813917 0.051 Uiso 1 1 calc R U . . .
C2 C 0.1724(2) 0.1880(2) 0.86300(19) 0.0375(7) Uani 1 1 d . . . . .
C3 C 0.1965(3) 0.1133(2) 0.9117(2) 0.0507(10) Uani 1 1 d . . . . .
H3 H 0.152162 0.085043 0.954493 0.061 Uiso 1 1 calc R U . . .
C4 C 0.3002(3) 0.0851(2) 0.8872(2) 0.0504(9) Uani 1 1 d . . . . .
H4 H 0.338158 0.034078 0.910080 0.060 Uiso 1 1 calc R U . . .
C5 C 0.3354(2) 0.1441(2) 0.82514(19) 0.0352(7) Uani 1 1 d . . . . .
C6 C 0.4407(2) 0.1473(2) 0.7792(2) 0.0421(8) Uani 1 1 d . . . . .
H6A H 0.460923 0.084753 0.760309 0.051 Uiso 1 1 calc R U . . .
H6B H 0.495919 0.169799 0.820344 0.051 Uiso 1 1 calc R U . . .
C7 C -0.0013(3) 0.4318(3) 0.8095(3) 0.0640(11) Uani 1 1 d . . . . .
C8 C -0.0634(3) 0.3772(4) 0.7417(3) 0.0864(15) Uani 1 1 d . . . . .
H8A H -0.015822 0.359731 0.693443 0.104 Uiso 1 1 calc R U . . .
H8B H -0.121835 0.414771 0.718669 0.104 Uiso 1 1 calc R U . . .
H8C H -0.092617 0.321950 0.769230 0.104 Uiso 1 1 calc R U . . .
C9 C -0.0761(3) 0.4504(4) 0.8877(3) 0.0940(17) Uani 1 1 d . . . . .
H9A H -0.096652 0.392146 0.914877 0.113 Uiso 1 1 calc R U . . .
H9B H -0.140103 0.482256 0.866819 0.113 Uiso 1 1 calc R U . . .
H9C H -0.039348 0.488650 0.931059 0.113 Uiso 1 1 calc R U . . .
C10 C 0.0349(4) 0.5224(3) 0.7680(4) 0.1023(18) Uani 1 1 d . . . . .
H10A H -0.027517 0.556422 0.747218 0.123 Uiso 1 1 calc R U . . .
H10B H 0.082384 0.509571 0.718346 0.123 Uiso 1 1 calc R U . . .
H10C H 0.073005 0.558968 0.811953 0.123 Uiso 1 1 calc R U . . .
C11 C 0.1800(3) 0.4028(2) 0.9491(2) 0.0494(9) Uani 1 1 d . . . . .
C12 C 0.2930(3) 0.3639(3) 0.9563(2) 0.0586(10) Uani 1 1 d . . . . .
H12A H 0.325780 0.384935 1.011106 0.070 Uiso 1 1 calc R U . . .
H12B H 0.335597 0.384959 0.906211 0.070 Uiso 1 1 calc R U . . .
H12C H 0.289820 0.296765 0.956039 0.070 Uiso 1 1 calc R U . . .
C13 C 0.1167(3) 0.3691(3) 1.0292(2) 0.0715(13) Uani 1 1 d . . . . .
H13A H 0.152922 0.388391 1.083178 0.086 Uiso 1 1 calc R U . . .
H13B H 0.111838 0.302134 1.027760 0.086 Uiso 1 1 calc R U . . .
H13C H 0.044791 0.395421 1.027759 0.086 Uiso 1 1 calc R U . . .
C14 C 0.1901(3) 0.5076(3) 0.9503(3) 0.0732(13) Uani 1 1 d . . . . .
H14A H 0.225894 0.528225 0.896538 0.088 Uiso 1 1 calc R U . . .
H14B H 0.232035 0.526439 1.001609 0.088 Uiso 1 1 calc R U . . .
H14C H 0.118990 0.535139 0.953567 0.088 Uiso 1 1 calc R U . . .
C15 C 0.4118(2) 0.1434(2) 0.5878(2) 0.0377(7) Uani 1 1 d . . . . .
C16 C 0.3101(3) 0.0902(2) 0.6105(2) 0.0496(9) Uani 1 1 d . . . . .
H16A H 0.291995 0.049094 0.561856 0.059 Uiso 1 1 calc R U . . .
H16B H 0.251484 0.133385 0.620264 0.059 Uiso 1 1 calc R U . . .
H16C H 0.321955 0.054162 0.664005 0.059 Uiso 1 1 calc R U . . .
C17 C 0.5022(3) 0.0743(2) 0.5721(3) 0.0541(10) Uani 1 1 d . . . . .
H17A H 0.566322 0.106914 0.552907 0.065 Uiso 1 1 calc R U . . .
H17B H 0.480526 0.030538 0.526594 0.065 Uiso 1 1 calc R U . . .
H17C H 0.517258 0.041259 0.626819 0.065 Uiso 1 1 calc R U . . .
C18 C 0.3921(3) 0.1983(3) 0.5035(2) 0.0558(10) Uani 1 1 d . . . . .
H18A H 0.368188 0.156801 0.456842 0.067 Uiso 1 1 calc R U . . .
H18B H 0.458359 0.228414 0.485438 0.067 Uiso 1 1 calc R U . . .
H18C H 0.337171 0.244637 0.514390 0.067 Uiso 1 1 calc R U . . .
C19 C 0.5701(2) 0.2785(2) 0.6796(3) 0.0464(8) Uani 1 1 d . . . . .
C20 C 0.5774(3) 0.3411(2) 0.5999(3) 0.0670(12) Uani 1 1 d . . . . .
H20A H 0.643702 0.376424 0.602571 0.080 Uiso 1 1 calc R U . . .
H20B H 0.516421 0.383117 0.599489 0.080 Uiso 1 1 calc R U . . .
H20C H 0.576626 0.304045 0.546128 0.080 Uiso 1 1 calc R U . . .
C21 C 0.6637(2) 0.2114(3) 0.6791(3) 0.0726(13) Uani 1 1 d . . . . .
H21A H 0.730716 0.245553 0.683474 0.087 Uiso 1 1 calc R U . . .
H21B H 0.662861 0.176109 0.624332 0.087 Uiso 1 1 calc R U . . .
H21C H 0.657374 0.169574 0.729254 0.087 Uiso 1 1 calc R U . . .
C22 C 0.5789(3) 0.3372(3) 0.7626(3) 0.0688(12) Uani 1 1 d . . . . .
H22A H 0.519258 0.380523 0.764725 0.083 Uiso 1 1 calc R U . . .
H22B H 0.646306 0.371097 0.761668 0.083 Uiso 1 1 calc R U . . .
H22C H 0.576744 0.297573 0.814593 0.083 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 2.042(2) . ?
Ti1 Cl1 2.2761(9) . ?
Ti1 Cl2 2.2996(9) . ?
Ti1 P1 2.6000(9) . ?
Ti1 P2 2.6461(9) . ?
P1 C1 1.826(3) . ?
P1 C7 1.883(4) . ?
P1 C11 1.886(4) . ?
P2 C6 1.834(3) . ?
P2 C15 1.877(3) . ?
P2 C19 1.880(3) . ?
N1 C5 1.394(4) . ?
N1 C2 1.396(4) . ?
C1 C2 1.498(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.353(4) . ?
C3 C4 1.414(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.351(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.495(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.519(6) . ?
C7 C10 1.534(6) . ?
C7 C9 1.539(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.530(5) . ?
C11 C13 1.535(5) . ?
C11 C14 1.536(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.532(4) . ?
C15 C18 1.532(5) . ?
C15 C17 1.536(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.522(5) . ?
C19 C21 1.529(4) . ?
C19 C22 1.529(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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 Ti1 Cl1 115.18(7) . . ?
N1 Ti1 Cl2 141.08(7) . . ?
Cl1 Ti1 Cl2 103.50(4) . . ?
N1 Ti1 P1 75.57(7) . . ?
Cl1 Ti1 P1 99.22(3) . . ?
Cl2 Ti1 P1 94.81(3) . . ?
N1 Ti1 P2 76.19(7) . . ?
Cl1 Ti1 P2 102.60(3) . . ?
Cl2 Ti1 P2 100.24(3) . . ?
P1 Ti1 P2 149.68(3) . . ?
C1 P1 C7 106.26(19) . . ?
C1 P1 C11 105.21(16) . . ?
C7 P1 C11 112.84(19) . . ?
C1 P1 Ti1 96.26(11) . . ?
C7 P1 Ti1 121.57(13) . . ?
C11 P1 Ti1 111.77(12) . . ?
C6 P2 C15 104.49(15) . . ?
C6 P2 C19 104.23(16) . . ?
C15 P2 C19 112.69(14) . . ?
C6 P2 Ti1 98.93(10) . . ?
C15 P2 Ti1 114.19(10) . . ?
C19 P2 Ti1 119.43(10) . . ?
C5 N1 C2 105.4(2) . . ?
C5 N1 Ti1 128.69(19) . . ?
C2 N1 Ti1 125.78(19) . . ?
C2 C1 P1 106.5(2) . . ?
C2 C1 H1A 110.4 . . ?
P1 C1 H1A 110.4 . . ?
C2 C1 H1B 110.4 . . ?
P1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
C3 C2 N1 110.0(3) . . ?
C3 C2 C1 131.0(3) . . ?
N1 C2 C1 119.0(3) . . ?
C2 C3 C4 107.2(3) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
C5 C4 C3 107.4(3) . . ?
C5 C4 H4 126.3 . . ?
C3 C4 H4 126.3 . . ?
C4 C5 N1 110.0(3) . . ?
C4 C5 C6 129.4(3) . . ?
N1 C5 C6 120.6(3) . . ?
C5 C6 P2 110.9(2) . . ?
C5 C6 H6A 109.4 . . ?
P2 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
P2 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C10 108.9(4) . . ?
C8 C7 C9 107.7(4) . . ?
C10 C7 C9 110.3(4) . . ?
C8 C7 P1 108.4(3) . . ?
C10 C7 P1 108.6(3) . . ?
C9 C7 P1 112.8(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C13 107.7(3) . . ?
C12 C11 C14 107.0(3) . . ?
C13 C11 C14 110.6(3) . . ?
C12 C11 P1 108.5(2) . . ?
C13 C11 P1 112.8(2) . . ?
C14 C11 P1 110.0(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C18 108.6(3) . . ?
C16 C15 C17 108.5(3) . . ?
C18 C15 C17 109.4(3) . . ?
C16 C15 P2 105.5(2) . . ?
C18 C15 P2 110.3(2) . . ?
C17 C15 P2 114.3(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C21 109.5(3) . . ?
C20 C19 C22 108.5(3) . . ?
C21 C19 C22 107.9(3) . . ?
C20 C19 P2 109.6(2) . . ?
C21 C19 P2 114.6(2) . . ?
C22 C19 P2 106.6(2) . . ?
C19 C20 H20A 109.5 . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 C1 C2 165.2(2) . . . . ?
C11 P1 C1 C2 -74.9(2) . . . . ?
Ti1 P1 C1 C2 39.7(2) . . . . ?
C5 N1 C2 C3 0.4(3) . . . . ?
Ti1 N1 C2 C3 -175.4(2) . . . . ?
C5 N1 C2 C1 179.4(3) . . . . ?
Ti1 N1 C2 C1 3.6(4) . . . . ?
P1 C1 C2 C3 144.3(3) . . . . ?
P1 C1 C2 N1 -34.5(3) . . . . ?
N1 C2 C3 C4 -0.6(4) . . . . ?
C1 C2 C3 C4 -179.4(3) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C3 C4 C5 N1 -0.3(4) . . . . ?
C3 C4 C5 C6 177.9(3) . . . . ?
C2 N1 C5 C4 -0.1(3) . . . . ?
Ti1 N1 C5 C4 175.6(2) . . . . ?
C2 N1 C5 C6 -178.4(3) . . . . ?
Ti1 N1 C5 C6 -2.7(4) . . . . ?
C4 C5 C6 P2 166.2(3) . . . . ?
N1 C5 C6 P2 -15.9(4) . . . . ?
C15 P2 C6 C5 -97.3(2) . . . . ?
C19 P2 C6 C5 144.2(2) . . . . ?
Ti1 P2 C6 C5 20.7(2) . . . . ?
C1 P1 C7 C8 -46.4(3) . . . . ?
C11 P1 C7 C8 -161.2(3) . . . . ?
Ti1 P1 C7 C8 61.8(3) . . . . ?
C1 P1 C7 C10 -164.6(3) . . . . ?
C11 P1 C7 C10 80.6(3) . . . . ?
Ti1 P1 C7 C10 -56.4(4) . . . . ?
C1 P1 C7 C9 72.8(4) . . . . ?
C11 P1 C7 C9 -42.0(4) . . . . ?
Ti1 P1 C7 C9 -179.0(3) . . . . ?
C1 P1 C11 C12 80.5(3) . . . . ?
C7 P1 C11 C12 -164.1(3) . . . . ?
Ti1 P1 C11 C12 -22.9(3) . . . . ?
C1 P1 C11 C13 -38.8(3) . . . . ?
C7 P1 C11 C13 76.7(3) . . . . ?
Ti1 P1 C11 C13 -142.1(3) . . . . ?
C1 P1 C11 C14 -162.8(3) . . . . ?
C7 P1 C11 C14 -47.3(3) . . . . ?
Ti1 P1 C11 C14 93.9(3) . . . . ?
C6 P2 C15 C16 56.2(2) . . . . ?
C19 P2 C15 C16 168.7(2) . . . . ?
Ti1 P2 C15 C16 -50.8(2) . . . . ?
C6 P2 C15 C18 173.4(2) . . . . ?
C19 P2 C15 C18 -74.1(2) . . . . ?
Ti1 P2 C15 C18 66.4(2) . . . . ?
C6 P2 C15 C17 -62.9(3) . . . . ?
C19 P2 C15 C17 49.7(3) . . . . ?
Ti1 P2 C15 C17 -169.8(2) . . . . ?
C6 P2 C19 C20 177.9(2) . . . . ?
C15 P2 C19 C20 65.2(3) . . . . ?
Ti1 P2 C19 C20 -73.0(3) . . . . ?
C6 P2 C19 C21 54.4(3) . . . . ?
C15 P2 C19 C21 -58.3(3) . . . . ?
Ti1 P2 C19 C21 163.5(3) . . . . ?
C6 P2 C19 C22 -64.9(3) . . . . ?
C15 P2 C19 C22 -177.5(2) . . . . ?
Ti1 P2 C19 C22 44.2(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_20170519-ZrCl3(PNP)
_database_code_depnum_ccdc_archive 'CCDC 1847682'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C44 H84 Cl6 N2 P4 Zr2'
_chemical_formula_moiety         'C44 H84 Cl6 N2 P4 Zr2'
_chemical_formula_weight         1160.21
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'A e a 2'
_space_group_name_Hall           'A 2 -2ab'
_space_group_IT_number           41
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1, z+1/2'
'x+1/2, -y+1, z+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   14.8731(10)
_cell_length_b                   14.7823(9)
_cell_length_c                   25.3833(15)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     5580.7(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20010
_cell_measurement_theta_min      2.10
_cell_measurement_theta_max      27.56
_cell_measurement_temperature    173
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2416.00
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_T_max  0.851

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      173
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            24238
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.739
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6357
_reflns_number_gt                5650
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_max     0.990
_reflns_Friedel_fraction_full    0.991

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1168
_refine_ls_wR_factor_gt          0.1131
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6357
_refine_ls_number_parameters     276
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+31.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.35
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 2212 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Zr Zr -2.9673 0.5597
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Zr1 Zr 0.500000 0.500000 0.54205(3) 0.0414(3) Uani 1 2 d S T P . .
Zr2 Zr 0.500000 0.500000 0.37519(3) 0.0409(3) Uani 1 2 d S T P . .
Cl1 Cl 0.63449(13) 0.5906(2) 0.54121(11) 0.0727(7) Uani 1 1 d . . . . .
Cl2 Cl 0.4087(2) 0.36613(15) 0.37567(14) 0.0842(9) Uani 1 1 d . . . . .
Cl3 Cl 0.57347(11) 0.42502(13) 0.45866(11) 0.0491(4) Uani 1 1 d . . . . .
P1 P 0.41559(16) 0.6611(2) 0.58083(10) 0.0648(7) Uani 1 1 d . . . . .
P2 P 0.6583(2) 0.41249(17) 0.33645(10) 0.0656(7) Uani 1 1 d . . . . .
N1 N 0.500000 0.500000 0.6283(4) 0.055(4) Uani 1 2 d S T P . .
N2 N 0.500000 0.500000 0.2885(5) 0.073(5) Uani 1 2 d S T P . .
C1 C 0.4983(5) 0.5757(8) 0.6610(3) 0.058(2) Uani 1 1 d . . . . .
C2 C 0.4982(7) 0.5484(9) 0.7129(4) 0.072(3) Uani 1 1 d . . . . .
H2 H 0.496102 0.586600 0.742961 0.086 Uiso 1 1 calc R U . . .
C3 C 0.4866(7) 0.6680(9) 0.6398(3) 0.072(3) Uani 1 1 d . . . . .
H3A H 0.545838 0.694241 0.630724 0.086 Uiso 1 1 calc R U . . .
H3B H 0.457819 0.707170 0.666588 0.086 Uiso 1 1 calc R U . . .
C4 C 0.2967(7) 0.6458(9) 0.6047(4) 0.084(4) Uani 1 1 d . . . . .
C5 C 0.2375(7) 0.6194(11) 0.5574(4) 0.107(5) Uani 1 1 d . . . . .
H5A H 0.234298 0.670128 0.532698 0.129 Uiso 1 1 calc R U . . .
H5B H 0.176912 0.604415 0.569843 0.129 Uiso 1 1 calc R U . . .
H5C H 0.263653 0.566671 0.539701 0.129 Uiso 1 1 calc R U . . .
C6 C 0.2572(9) 0.7320(11) 0.6320(5) 0.126(7) Uani 1 1 d . . . . .
H6A H 0.200864 0.716301 0.649803 0.151 Uiso 1 1 calc R U . . .
H6B H 0.245543 0.778512 0.605340 0.151 Uiso 1 1 calc R U . . .
H6C H 0.300392 0.755061 0.657833 0.151 Uiso 1 1 calc R U . . .
C7 C 0.2932(6) 0.5640(12) 0.6446(4) 0.112(5) Uani 1 1 d . . . . .
H7A H 0.318946 0.582675 0.678431 0.134 Uiso 1 1 calc R U . . .
H7B H 0.327940 0.513213 0.630361 0.134 Uiso 1 1 calc R U . . .
H7C H 0.230637 0.545282 0.649739 0.134 Uiso 1 1 calc R U . . .
C8 C 0.4283(9) 0.7771(8) 0.5490(4) 0.084(3) Uani 1 1 d . . . . .
C9 C 0.5175(8) 0.7783(8) 0.5191(4) 0.090(4) Uani 1 1 d . . . . .
H9A H 0.514742 0.735219 0.489801 0.107 Uiso 1 1 calc R U . . .
H9B H 0.566379 0.761214 0.543001 0.107 Uiso 1 1 calc R U . . .
H9C H 0.528550 0.839223 0.505322 0.107 Uiso 1 1 calc R U . . .
C10 C 0.3554(9) 0.7974(9) 0.5094(4) 0.099(4) Uani 1 1 d . . . . .
H10A H 0.368663 0.854798 0.491699 0.119 Uiso 1 1 calc R U . . .
H10B H 0.297406 0.802002 0.527564 0.119 Uiso 1 1 calc R U . . .
H10C H 0.352755 0.748704 0.483296 0.119 Uiso 1 1 calc R U . . .
C11 C 0.4323(13) 0.8539(9) 0.5903(5) 0.137(6) Uani 1 1 d . . . . .
H11A H 0.378142 0.851921 0.612270 0.165 Uiso 1 1 calc R U . . .
H11B H 0.435560 0.912387 0.572233 0.165 Uiso 1 1 calc R U . . .
H11C H 0.485579 0.845979 0.612485 0.165 Uiso 1 1 calc R U . . .
C12 C 0.5741(10) 0.4979(7) 0.2558(3) 0.093(5) Uani 1 1 d . . . . .
C13 C 0.5466(13) 0.4978(11) 0.2044(4) 0.140(9) Uani 1 1 d . . . . .
H13 H 0.584338 0.495359 0.174243 0.168 Uiso 1 1 calc R U . . .
C14 C 0.6647(10) 0.4851(8) 0.2774(4) 0.097(5) Uani 1 1 d . . . . .
H14A H 0.690971 0.544457 0.286794 0.117 Uiso 1 1 calc R U . . .
H14B H 0.703825 0.456431 0.250589 0.117 Uiso 1 1 calc R U . . .
C15 C 0.6410(10) 0.2928(7) 0.3120(4) 0.093(4) Uani 1 1 d . . . . .
C16 C 0.5635(13) 0.2921(8) 0.2708(5) 0.141(8) Uani 1 1 d . . . . .
H16A H 0.509530 0.319211 0.286328 0.170 Uiso 1 1 calc R U . . .
H16B H 0.550530 0.229587 0.260375 0.170 Uiso 1 1 calc R U . . .
H16C H 0.581638 0.326987 0.239753 0.170 Uiso 1 1 calc R U . . .
C17 C 0.6137(10) 0.2342(7) 0.3584(5) 0.103(5) Uani 1 1 d . . . . .
H17A H 0.663822 0.230206 0.383397 0.124 Uiso 1 1 calc R U . . .
H17B H 0.598212 0.173502 0.345894 0.124 Uiso 1 1 calc R U . . .
H17C H 0.561496 0.261167 0.375988 0.124 Uiso 1 1 calc R U . . .
C18 C 0.7271(12) 0.2531(9) 0.2841(5) 0.128(7) Uani 1 1 d . . . . .
H18A H 0.774524 0.243440 0.310296 0.154 Uiso 1 1 calc R U . . .
H18B H 0.748240 0.295749 0.257290 0.154 Uiso 1 1 calc R U . . .
H18C H 0.711973 0.195295 0.267337 0.154 Uiso 1 1 calc R U . . .
C19 C 0.7732(8) 0.4233(8) 0.3681(5) 0.080(3) Uani 1 1 d . . . . .
C20 C 0.7758(7) 0.5126(8) 0.3967(5) 0.094(4) Uani 1 1 d . . . . .
H20A H 0.771034 0.562050 0.371096 0.113 Uiso 1 1 calc R U . . .
H20B H 0.832629 0.517956 0.415961 0.113 Uiso 1 1 calc R U . . .
H20C H 0.725465 0.515951 0.421506 0.113 Uiso 1 1 calc R U . . .
C21 C 0.7916(8) 0.3485(8) 0.4078(4) 0.085(3) Uani 1 1 d . . . . .
H21A H 0.797277 0.290613 0.389247 0.102 Uiso 1 1 calc R U . . .
H21B H 0.741760 0.345075 0.432959 0.102 Uiso 1 1 calc R U . . .
H21C H 0.847553 0.361589 0.426645 0.102 Uiso 1 1 calc R U . . .
C22 C 0.8501(9) 0.4251(12) 0.3276(6) 0.124(6) Uani 1 1 d . . . . .
H22A H 0.845039 0.372613 0.304235 0.149 Uiso 1 1 calc R U . . .
H22B H 0.907988 0.423053 0.346087 0.149 Uiso 1 1 calc R U . . .
H22C H 0.846432 0.480775 0.306793 0.149 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 2.190(10) . ?
Zr1 Cl1 2.407(2) . ?
Zr1 Cl1 2.407(2) 2_665 ?
Zr1 Cl3 2.627(3) 2_665 ?
Zr1 Cl3 2.627(3) . ?
Zr1 P1 2.866(3) 2_665 ?
Zr1 P1 2.866(3) . ?
Zr2 N2 2.201(12) . ?
Zr2 Cl2 2.400(2) . ?
Zr2 Cl2 2.400(2) 2_665 ?
Zr2 Cl3 2.629(3) . ?
Zr2 Cl3 2.629(3) 2_665 ?
Zr2 P2 2.861(3) . ?
Zr2 P2 2.861(3) 2_665 ?
P1 C3 1.836(9) . ?
P1 C4 1.882(10) . ?
P1 C8 1.906(13) . ?
P2 C14 1.847(10) . ?
P2 C15 1.893(11) . ?
P2 C19 1.895(13) . ?
N1 C1 1.392(11) 2_665 ?
N1 C1 1.392(11) . ?
N2 C12 1.380(13) 2_665 ?
N2 C12 1.380(13) . ?
C1 C2 1.378(13) . ?
C1 C3 1.476(16) . ?
C2 C2 1.43(3) 2_665 ?
C2 H2 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.539(15) . ?
C4 C6 1.564(17) . ?
C4 C7 1.578(17) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.509(16) . ?
C8 C9 1.529(16) . ?
C8 C11 1.545(16) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.367(16) . ?
C12 C14 1.467(19) . ?
C13 C13 1.39(4) 2_665 ?
C13 H13 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C17 1.517(19) . ?
C15 C16 1.557(17) . ?
C15 C18 1.577(19) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.507(16) . ?
C19 C21 1.519(15) . ?
C19 C22 1.539(14) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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 90.51(7) . . ?
N1 Zr1 Cl1 90.51(7) . 2_665 ?
Cl1 Zr1 Cl1 178.98(15) . 2_665 ?
N1 Zr1 Cl3 143.67(5) . 2_665 ?
Cl1 Zr1 Cl3 95.96(9) . 2_665 ?
Cl1 Zr1 Cl3 83.22(8) 2_665 2_665 ?
N1 Zr1 Cl3 143.67(5) . . ?
Cl1 Zr1 Cl3 83.22(8) . . ?
Cl1 Zr1 Cl3 95.96(9) 2_665 . ?
Cl3 Zr1 Cl3 72.66(10) 2_665 . ?
N1 Zr1 P1 69.91(6) . 2_665 ?
Cl1 Zr1 P1 95.81(9) . 2_665 ?
Cl1 Zr1 P1 84.54(8) 2_665 2_665 ?
Cl3 Zr1 P1 144.04(9) 2_665 2_665 ?
Cl3 Zr1 P1 75.17(6) . 2_665 ?
N1 Zr1 P1 69.91(6) . . ?
Cl1 Zr1 P1 84.54(8) . . ?
Cl1 Zr1 P1 95.81(9) 2_665 . ?
Cl3 Zr1 P1 75.17(6) 2_665 . ?
Cl3 Zr1 P1 144.03(9) . . ?
P1 Zr1 P1 139.82(12) 2_665 . ?
N2 Zr2 Cl2 90.29(9) . . ?
N2 Zr2 Cl2 90.29(9) . 2_665 ?
Cl2 Zr2 Cl2 179.42(18) . 2_665 ?
N2 Zr2 Cl3 143.70(5) . . ?
Cl2 Zr2 Cl3 83.30(8) . . ?
Cl2 Zr2 Cl3 96.23(11) 2_665 . ?
N2 Zr2 Cl3 143.70(5) . 2_665 ?
Cl2 Zr2 Cl3 96.23(11) . 2_665 ?
Cl2 Zr2 Cl3 83.30(8) 2_665 2_665 ?
Cl3 Zr2 Cl3 72.60(10) . 2_665 ?
N2 Zr2 P2 69.90(6) . . ?
Cl2 Zr2 P2 95.41(10) . . ?
Cl2 Zr2 P2 84.79(9) 2_665 . ?
Cl3 Zr2 P2 75.18(6) . . ?
Cl3 Zr2 P2 144.07(8) 2_665 . ?
N2 Zr2 P2 69.90(6) . 2_665 ?
Cl2 Zr2 P2 84.79(9) . 2_665 ?
Cl2 Zr2 P2 95.41(10) 2_665 2_665 ?
Cl3 Zr2 P2 144.07(8) . 2_665 ?
Cl3 Zr2 P2 75.18(6) 2_665 2_665 ?
P2 Zr2 P2 139.79(11) . 2_665 ?
Zr1 Cl3 Zr2 107.37(6) . . ?
C3 P1 C4 106.5(4) . . ?
C3 P1 C8 103.8(6) . . ?
C4 P1 C8 109.7(6) . . ?
C3 P1 Zr1 94.3(4) . . ?
C4 P1 Zr1 115.0(4) . . ?
C8 P1 Zr1 124.0(4) . . ?
C14 P2 C15 106.5(5) . . ?
C14 P2 C19 104.4(6) . . ?
C15 P2 C19 109.9(5) . . ?
C14 P2 Zr2 93.4(4) . . ?
C15 P2 Zr2 115.1(5) . . ?
C19 P2 Zr2 123.9(3) . . ?
C1 N1 C1 107.0(10) 2_665 . ?
C1 N1 Zr1 126.5(5) 2_665 . ?
C1 N1 Zr1 126.5(5) . . ?
C12 N2 C12 106.1(13) 2_665 . ?
C12 N2 Zr2 127.0(6) 2_665 . ?
C12 N2 Zr2 127.0(6) . . ?
C2 C1 N1 109.5(10) . . ?
C2 C1 C3 128.1(9) . . ?
N1 C1 C3 121.9(7) . . ?
C1 C2 C2 107.0(7) . 2_665 ?
C1 C2 H2 126.5 . . ?
C2 C2 H2 126.5 2_665 . ?
C1 C3 P1 108.2(7) . . ?
C1 C3 H3A 110.1 . . ?
P1 C3 H3A 110.1 . . ?
C1 C3 H3B 110.1 . . ?
P1 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
C5 C4 C6 109.7(9) . . ?
C5 C4 C7 106.6(12) . . ?
C6 C4 C7 109.2(9) . . ?
C5 C4 P1 108.5(6) . . ?
C6 C4 P1 113.4(10) . . ?
C7 C4 P1 109.2(6) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C9 106.9(9) . . ?
C10 C8 C11 109.4(11) . . ?
C9 C8 C11 107.2(12) . . ?
C10 C8 P1 113.0(9) . . ?
C9 C8 P1 107.9(8) . . ?
C11 C8 P1 112.2(8) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N2 109.6(13) . . ?
C13 C12 C14 129.1(11) . . ?
N2 C12 C14 120.8(8) . . ?
C12 C13 C13 107.4(9) . 2_665 ?
C12 C13 H13 126.3 . . ?
C13 C13 H13 126.3 2_665 . ?
C12 C14 P2 109.3(9) . . ?
C12 C14 H14A 109.8 . . ?
P2 C14 H14A 109.8 . . ?
C12 C14 H14B 109.8 . . ?
P2 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
C17 C15 C16 108.7(13) . . ?
C17 C15 C18 110.7(9) . . ?
C16 C15 C18 107.2(10) . . ?
C17 C15 P2 108.4(7) . . ?
C16 C15 P2 109.1(7) . . ?
C18 C15 P2 112.6(11) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C21 108.3(10) . . ?
C20 C19 C22 106.6(11) . . ?
C21 C19 C22 108.7(10) . . ?
C20 C19 P2 107.5(8) . . ?
C21 C19 P2 112.5(9) . . ?
C22 C19 P2 112.9(9) . . ?
C19 C20 H20A 109.5 . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C1 C2 -0.5(5) 2_665 . . . ?
Zr1 N1 C1 C2 179.5(5) . . . . ?
C1 N1 C1 C3 -173.5(9) 2_665 . . . ?
Zr1 N1 C1 C3 6.5(9) . . . . ?
N1 C1 C2 C2 1.2(13) . . . 2_665 ?
C3 C1 C2 C2 173.6(10) . . . 2_665 ?
C2 C1 C3 P1 -139.8(8) . . . . ?
N1 C1 C3 P1 31.9(10) . . . . ?
C4 P1 C3 C1 76.9(8) . . . . ?
C8 P1 C3 C1 -167.3(7) . . . . ?
Zr1 P1 C3 C1 -40.7(6) . . . . ?
C3 P1 C4 C5 -168.0(9) . . . . ?
C8 P1 C4 C5 80.2(10) . . . . ?
Zr1 P1 C4 C5 -65.1(10) . . . . ?
C3 P1 C4 C6 69.9(9) . . . . ?
C8 P1 C4 C6 -41.9(9) . . . . ?
Zr1 P1 C4 C6 172.8(7) . . . . ?
C3 P1 C4 C7 -52.2(10) . . . . ?
C8 P1 C4 C7 -163.9(8) . . . . ?
Zr1 P1 C4 C7 50.8(9) . . . . ?
C12 N2 C12 C13 -0.5(8) 2_665 . . . ?
Zr2 N2 C12 C13 179.5(8) . . . . ?
C12 N2 C12 C14 -173.2(13) 2_665 . . . ?
Zr2 N2 C12 C14 6.8(13) . . . . ?
N2 C12 C13 C13 1(2) . . . 2_665 ?
C14 C12 C13 C13 173.2(16) . . . 2_665 ?
C13 C12 C14 P2 -138.8(14) . . . . ?
N2 C12 C14 P2 32.2(13) . . . . ?
C15 P2 C14 C12 75.9(9) . . . . ?
C19 P2 C14 C12 -167.8(8) . . . . ?
Zr2 P2 C14 C12 -41.5(8) . . . . ?
C14 P2 C15 C17 -166.9(9) . . . . ?
C19 P2 C15 C17 80.5(10) . . . . ?
Zr2 P2 C15 C17 -65.0(9) . . . . ?
C14 P2 C15 C16 -48.8(12) . . . . ?
C19 P2 C15 C16 -161.4(10) . . . . ?
Zr2 P2 C15 C16 53.1(11) . . . . ?
C14 P2 C15 C18 70.2(9) . . . . ?
C19 P2 C15 C18 -42.4(9) . . . . ?
Zr2 P2 C15 C18 172.1(6) . . . . ?
C14 P2 C19 C20 77.8(8) . . . . ?
C15 P2 C19 C20 -168.3(8) . . . . ?
Zr2 P2 C19 C20 -26.5(9) . . . . ?
C14 P2 C19 C21 -163.0(7) . . . . ?
C15 P2 C19 C21 -49.1(9) . . . . ?
Zr2 P2 C19 C21 92.7(8) . . . . ?
C14 P2 C19 C22 -39.6(11) . . . . ?
C15 P2 C19 C22 74.4(11) . . . . ?
Zr2 P2 C19 C22 -143.8(8) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_20170825ZrPNPCpN2
_database_code_depnum_ccdc_archive 'CCDC 1847684'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C68 H110 N4 P4 Zr2'
_chemical_formula_moiety         'C68 H110 N4 P4 Zr2'
_chemical_formula_weight         1289.98
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_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                   27.0349(9)
_cell_length_b                   14.8663(4)
_cell_length_c                   17.7670(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.262(8)
_cell_angle_gamma                90.0000
_cell_volume                     6819.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26384
_cell_measurement_theta_min      1.84
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    173
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2744.00
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_T_max  0.974

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      173
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            31974
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.122
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7781
_reflns_number_gt                6066
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1313
_refine_ls_wR_factor_gt          0.1234
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7781
_refine_ls_number_parameters     330
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+39.2000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Zr Zr -2.9673 0.5597
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Zr1 Zr 0.59723(2) 0.77240(2) 0.29014(2) 0.03007(10) Uani 1 1 d . . . . .
P1 P 0.61980(4) 0.60170(7) 0.23548(5) 0.0340(2) Uani 1 1 d . . . . .
P2 P 0.61878(4) 0.86200(7) 0.44479(6) 0.0343(2) Uani 1 1 d . . . . .
N1 N 0.52471(10) 0.74759(19) 0.26586(16) 0.0314(6) Uani 1 1 d . . . . .
N2 N 0.64023(11) 0.6806(2) 0.39255(16) 0.0314(6) Uani 1 1 d . . . . .
C1 C 0.60819(15) 0.5406(3) 0.3185(2) 0.0374(8) Uani 1 1 d . . . . .
H1A H 0.570765 0.540333 0.313718 0.045 Uiso 1 1 calc R U . . .
H1B H 0.620116 0.477520 0.319240 0.045 Uiso 1 1 calc R U . . .
C2 C 0.63805(13) 0.5883(3) 0.3924(2) 0.0336(8) Uani 1 1 d . . . . .
C3 C 0.66626(14) 0.5543(3) 0.4645(2) 0.0382(8) Uani 1 1 d . . . . .
H3 H 0.670866 0.492691 0.479215 0.046 Uiso 1 1 calc R U . . .
C4 C 0.68690(14) 0.6291(3) 0.5122(2) 0.0371(8) Uani 1 1 d . . . . .
H4 H 0.707935 0.627696 0.565544 0.045 Uiso 1 1 calc R U . . .
C5 C 0.67093(13) 0.7041(3) 0.4671(2) 0.0332(8) Uani 1 1 d . . . . .
C6 C 0.68061(13) 0.8014(3) 0.4866(2) 0.0369(8) Uani 1 1 d . . . . .
H6A H 0.707278 0.824863 0.463786 0.044 Uiso 1 1 calc R U . . .
H6B H 0.693065 0.809746 0.544494 0.044 Uiso 1 1 calc R U . . .
C7 C 0.57559(15) 0.5432(3) 0.1466(2) 0.0418(9) Uani 1 1 d . . . . .
C8 C 0.52067(14) 0.5495(3) 0.1554(2) 0.0446(9) Uani 1 1 d . . . . .
H8A H 0.517537 0.507252 0.196119 0.054 Uiso 1 1 calc R U . . .
H8B H 0.495099 0.534328 0.105137 0.054 Uiso 1 1 calc R U . . .
H8C H 0.514466 0.610843 0.170647 0.054 Uiso 1 1 calc R U . . .
C9 C 0.58777(18) 0.4436(3) 0.1390(3) 0.0557(12) Uani 1 1 d . . . . .
H9A H 0.560771 0.416822 0.095203 0.067 Uiso 1 1 calc R U . . .
H9B H 0.588939 0.412241 0.188067 0.067 Uiso 1 1 calc R U . . .
H9C H 0.621388 0.437955 0.129051 0.067 Uiso 1 1 calc R U . . .
C10 C 0.57500(17) 0.5925(3) 0.0709(2) 0.0530(11) Uani 1 1 d . . . . .
H10A H 0.570021 0.657071 0.077277 0.064 Uiso 1 1 calc R U . . .
H10B H 0.546598 0.569441 0.026970 0.064 Uiso 1 1 calc R U . . .
H10C H 0.608009 0.582765 0.059784 0.064 Uiso 1 1 calc R U . . .
C11 C 0.69038(15) 0.5745(3) 0.2442(2) 0.0416(9) Uani 1 1 d . . . . .
C12 C 0.72450(14) 0.6432(3) 0.3007(2) 0.0455(10) Uani 1 1 d . . . . .
H12A H 0.713884 0.704196 0.281704 0.055 Uiso 1 1 calc R U . . .
H12B H 0.760803 0.633846 0.302993 0.055 Uiso 1 1 calc R U . . .
H12C H 0.720616 0.635520 0.353413 0.055 Uiso 1 1 calc R U . . .
C13 C 0.70660(17) 0.4802(3) 0.2776(3) 0.0552(11) Uani 1 1 d . . . . .
H13A H 0.742639 0.469061 0.279280 0.066 Uiso 1 1 calc R U . . .
H13B H 0.684134 0.435161 0.243839 0.066 Uiso 1 1 calc R U . . .
H13C H 0.703373 0.476106 0.330998 0.066 Uiso 1 1 calc R U . . .
C14 C 0.70109(16) 0.5838(4) 0.1645(2) 0.0545(12) Uani 1 1 d . . . . .
H14A H 0.688271 0.642126 0.140991 0.065 Uiso 1 1 calc R U . . .
H14B H 0.683374 0.535419 0.129259 0.065 Uiso 1 1 calc R U . . .
H14C H 0.738456 0.579783 0.172270 0.065 Uiso 1 1 calc R U . . .
C15 C 0.57750(14) 0.8210(3) 0.5082(2) 0.0400(9) Uani 1 1 d . . . . .
C16 C 0.53475(16) 0.8898(3) 0.5072(3) 0.0510(11) Uani 1 1 d . . . . .
H16A H 0.510343 0.863407 0.532226 0.061 Uiso 1 1 calc R U . . .
H16B H 0.516306 0.905853 0.452598 0.061 Uiso 1 1 calc R U . . .
H16C H 0.550382 0.943834 0.536186 0.061 Uiso 1 1 calc R U . . .
C17 C 0.60820(17) 0.8025(3) 0.5941(2) 0.0488(10) Uani 1 1 d . . . . .
H17A H 0.633689 0.754999 0.596147 0.059 Uiso 1 1 calc R U . . .
H17B H 0.584457 0.783216 0.623292 0.059 Uiso 1 1 calc R U . . .
H17C H 0.626124 0.857504 0.617950 0.059 Uiso 1 1 calc R U . . .
C18 C 0.55085(15) 0.7342(3) 0.4717(2) 0.0408(8) Uani 1 1 d . . . . .
H18A H 0.525708 0.716046 0.498744 0.049 Uiso 1 1 calc R U . . .
H18B H 0.576808 0.686744 0.477112 0.049 Uiso 1 1 calc R U . . .
H18C H 0.532905 0.744222 0.415691 0.049 Uiso 1 1 calc R U . . .
C19 C 0.63777(16) 0.9829(3) 0.4696(2) 0.0452(9) Uani 1 1 d . . . . .
C20 C 0.59290(18) 1.0458(3) 0.4280(3) 0.0604(12) Uani 1 1 d . . . . .
H20A H 0.579133 1.028363 0.372476 0.073 Uiso 1 1 calc R U . . .
H20B H 0.605505 1.107947 0.431398 0.073 Uiso 1 1 calc R U . . .
H20C H 0.565439 1.041294 0.453472 0.073 Uiso 1 1 calc R U . . .
C21 C 0.65552(19) 1.0039(3) 0.5585(3) 0.0594(12) Uani 1 1 d . . . . .
H21A H 0.668813 1.065616 0.566853 0.071 Uiso 1 1 calc R U . . .
H21B H 0.682946 0.961843 0.585559 0.071 Uiso 1 1 calc R U . . .
H21C H 0.626114 0.997698 0.579730 0.071 Uiso 1 1 calc R U . . .
C22 C 0.68492(16) 1.0041(3) 0.4400(3) 0.0514(10) Uani 1 1 d . . . . .
H22A H 0.716055 0.976278 0.475365 0.062 Uiso 1 1 calc R U . . .
H22B H 0.689798 1.069406 0.439315 0.062 Uiso 1 1 calc R U . . .
H22C H 0.678742 0.980103 0.386662 0.062 Uiso 1 1 calc R U . . .
C23 C 0.56846(17) 0.9027(3) 0.1935(2) 0.0486(10) Uani 1 1 d . . . . .
H23 H 0.534315 0.925219 0.184497 0.058 Uiso 1 1 calc R U . . .
C24 C 0.61283(18) 0.9339(3) 0.2505(2) 0.0502(10) Uani 1 1 d . . . . .
H24 H 0.613921 0.981010 0.287122 0.060 Uiso 1 1 calc R U . . .
C25 C 0.65554(16) 0.8836(3) 0.2443(3) 0.0517(11) Uani 1 1 d . . . . .
H25 H 0.690462 0.890415 0.275984 0.062 Uiso 1 1 calc R U . . .
C26 C 0.63726(16) 0.8218(3) 0.1833(2) 0.0487(10) Uani 1 1 d . . . . .
H26 H 0.657780 0.779459 0.165794 0.058 Uiso 1 1 calc R U . . .
C27 C 0.58303(16) 0.8327(3) 0.1519(2) 0.0463(10) Uani 1 1 d . . . . .
H27 H 0.560647 0.798730 0.110272 0.056 Uiso 1 1 calc R U . . .
C28 C 0.6041(4) 0.2841(6) 0.3693(6) 0.121(3) Uiso 1 1 d . . . . .
C29 C 0.6411(5) 0.3022(7) 0.4254(7) 0.153(4) Uiso 1 1 d . . . . .
H29 H 0.632378 0.325571 0.469565 0.184 Uiso 1 1 calc R U . . .
C30 C 0.6956(6) 0.2945(9) 0.4366(8) 0.197(5) Uiso 1 1 d . . . . .
H30 H 0.721070 0.307114 0.485229 0.236 Uiso 1 1 calc R U . . .
C31 C 0.7076(5) 0.2666(7) 0.3693(7) 0.160(4) Uiso 1 1 d . . . . .
H31 H 0.741715 0.267720 0.364603 0.192 Uiso 1 1 calc R U . . .
C32 C 0.6649(5) 0.2369(8) 0.3096(7) 0.175(4) Uiso 1 1 d . . . . .
H32 H 0.671926 0.210153 0.265352 0.210 Uiso 1 1 calc R U . . .
C33 C 0.6148(5) 0.2414(8) 0.3069(7) 0.167(4) Uiso 1 1 d . . . . .
H33 H 0.588175 0.216542 0.264333 0.200 Uiso 1 1 calc R U . . .
C34 C 0.5504(4) 0.2878(7) 0.3627(6) 0.157(4) Uiso 1 1 d . . . . .
H34A H 0.531495 0.245151 0.322363 0.189 Uiso 1 1 calc R U . . .
H34B H 0.537436 0.348819 0.347726 0.189 Uiso 1 1 calc R U . . .
H34C H 0.545328 0.272137 0.413458 0.189 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.914(3) . ?
Zr1 N2 2.295(3) . ?
Zr1 C27 2.534(4) . ?
Zr1 C23 2.552(4) . ?
Zr1 C26 2.556(4) . ?
Zr1 C24 2.572(4) . ?
Zr1 C25 2.577(4) . ?
Zr1 P1 2.8472(10) . ?
Zr1 P2 2.9517(10) . ?
P1 C1 1.837(4) . ?
P1 C7 1.887(4) . ?
P1 C11 1.911(4) . ?
P2 C6 1.849(4) . ?
P2 C19 1.886(4) . ?
P2 C15 1.906(4) . ?
N1 N1 1.287(5) 2_655 ?
N2 C2 1.374(5) . ?
N2 C5 1.383(4) . ?
C1 C2 1.500(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.378(5) . ?
C3 C4 1.409(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.492(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C10 1.528(6) . ?
C7 C9 1.532(6) . ?
C7 C8 1.542(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.533(6) . ?
C11 C14 1.534(5) . ?
C11 C13 1.535(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C18 1.525(6) . ?
C15 C17 1.530(5) . ?
C15 C16 1.539(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.537(6) . ?
C19 C21 1.540(6) . ?
C19 C22 1.549(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C27 1.399(6) . ?
C23 C24 1.400(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.407(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.415(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.215(12) . ?
C28 C33 1.381(12) . ?
C28 C34 1.422(12) . ?
C29 C30 1.431(14) . ?
C29 H29 0.9500 . ?
C30 C31 1.393(14) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(14) . ?
C31 H31 0.9500 . ?
C32 C33 1.342(14) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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 N2 107.95(11) . . ?
N1 Zr1 C27 89.96(13) . . ?
N2 Zr1 C27 150.90(12) . . ?
N1 Zr1 C23 84.69(13) . . ?
N2 Zr1 C23 165.04(13) . . ?
C27 Zr1 C23 31.92(14) . . ?
N1 Zr1 C26 121.27(13) . . ?
N2 Zr1 C26 122.20(12) . . ?
C27 Zr1 C26 32.27(13) . . ?
C23 Zr1 C26 52.69(14) . . ?
N1 Zr1 C24 111.00(14) . . ?
N2 Zr1 C24 133.33(12) . . ?
C27 Zr1 C24 52.74(14) . . ?
C23 Zr1 C24 31.71(13) . . ?
C26 Zr1 C24 52.31(15) . . ?
N1 Zr1 C25 137.23(13) . . ?
N2 Zr1 C25 114.71(12) . . ?
C27 Zr1 C25 53.00(14) . . ?
C23 Zr1 C25 52.67(14) . . ?
C26 Zr1 C25 31.54(14) . . ?
C24 Zr1 C25 31.73(14) . . ?
N1 Zr1 P1 93.45(9) . . ?
N2 Zr1 P1 68.36(7) . . ?
C27 Zr1 P1 88.32(10) . . ?
C23 Zr1 P1 120.01(10) . . ?
C26 Zr1 P1 79.73(11) . . ?
C24 Zr1 P1 132.03(11) . . ?
C25 Zr1 P1 104.52(11) . . ?
N1 Zr1 P2 101.71(9) . . ?
N2 Zr1 P2 67.46(7) . . ?
C27 Zr1 P2 132.36(10) . . ?
C23 Zr1 P2 102.74(10) . . ?
C26 Zr1 P2 123.47(11) . . ?
C24 Zr1 P2 80.23(10) . . ?
C25 Zr1 P2 91.96(11) . . ?
P1 Zr1 P2 135.77(3) . . ?
C1 P1 C7 103.15(18) . . ?
C1 P1 C11 103.56(18) . . ?
C7 P1 C11 109.85(17) . . ?
C1 P1 Zr1 93.57(12) . . ?
C7 P1 Zr1 123.35(13) . . ?
C11 P1 Zr1 118.08(13) . . ?
C6 P2 C19 102.68(18) . . ?
C6 P2 C15 102.96(17) . . ?
C19 P2 C15 109.43(19) . . ?
C6 P2 Zr1 93.42(12) . . ?
C19 P2 Zr1 127.82(14) . . ?
C15 P2 Zr1 114.68(13) . . ?
N1 N1 Zr1 163.7(2) 2_655 . ?
C2 N2 C5 105.5(3) . . ?
C2 N2 Zr1 125.5(2) . . ?
C5 N2 Zr1 128.9(2) . . ?
C2 C1 P1 107.1(3) . . ?
C2 C1 H1A 110.3 . . ?
P1 C1 H1A 110.3 . . ?
C2 C1 H1B 110.3 . . ?
P1 C1 H1B 110.3 . . ?
H1A C1 H1B 108.6 . . ?
N2 C2 C3 110.7(3) . . ?
N2 C2 C1 119.1(3) . . ?
C3 C2 C1 130.3(4) . . ?
C2 C3 C4 106.3(3) . . ?
C2 C3 H3 126.9 . . ?
C4 C3 H3 126.9 . . ?
C5 C4 C3 107.0(3) . . ?
C5 C4 H4 126.5 . . ?
C3 C4 H4 126.5 . . ?
C4 C5 N2 110.5(3) . . ?
C4 C5 C6 130.7(3) . . ?
N2 C5 C6 118.8(3) . . ?
C5 C6 P2 107.7(2) . . ?
C5 C6 H6A 110.2 . . ?
P2 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
P2 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
C10 C7 C9 109.5(3) . . ?
C10 C7 C8 107.6(3) . . ?
C9 C7 C8 107.8(4) . . ?
C10 C7 P1 110.8(3) . . ?
C9 C7 P1 114.8(3) . . ?
C8 C7 P1 106.1(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C14 107.6(3) . . ?
C12 C11 C13 108.0(3) . . ?
C14 C11 C13 109.2(3) . . ?
C12 C11 P1 107.7(3) . . ?
C14 C11 P1 111.3(3) . . ?
C13 C11 P1 112.9(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 C17 108.7(3) . . ?
C18 C15 C16 107.4(3) . . ?
C17 C15 C16 108.3(3) . . ?
C18 C15 P2 107.7(2) . . ?
C17 C15 P2 114.1(3) . . ?
C16 C15 P2 110.5(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C21 109.4(4) . . ?
C20 C19 C22 108.9(4) . . ?
C21 C19 C22 105.6(3) . . ?
C20 C19 P2 110.3(3) . . ?
C21 C19 P2 114.5(3) . . ?
C22 C19 P2 108.0(3) . . ?
C19 C20 H20A 109.5 . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C27 C23 C24 108.3(4) . . ?
C27 C23 Zr1 73.3(2) . . ?
C24 C23 Zr1 74.9(2) . . ?
C27 C23 H23 125.9 . . ?
C24 C23 H23 125.9 . . ?
Zr1 C23 H23 117.8 . . ?
C23 C24 C25 108.3(4) . . ?
C23 C24 Zr1 73.4(2) . . ?
C25 C24 Zr1 74.3(2) . . ?
C23 C24 H24 125.9 . . ?
C25 C24 H24 125.9 . . ?
Zr1 C24 H24 118.3 . . ?
C26 C25 C24 107.5(4) . . ?
C26 C25 Zr1 73.4(2) . . ?
C24 C25 Zr1 73.9(2) . . ?
C26 C25 H25 126.2 . . ?
C24 C25 H25 126.2 . . ?
Zr1 C25 H25 118.4 . . ?
C25 C26 C27 108.5(4) . . ?
C25 C26 Zr1 75.1(2) . . ?
C27 C26 Zr1 73.0(2) . . ?
C25 C26 H26 125.7 . . ?
C27 C26 H26 125.7 . . ?
Zr1 C26 H26 118.1 . . ?
C23 C27 C26 107.4(4) . . ?
C23 C27 Zr1 74.8(2) . . ?
C26 C27 Zr1 74.7(2) . . ?
C23 C27 H27 126.3 . . ?
C26 C27 H27 126.3 . . ?
Zr1 C27 H27 116.4 . . ?
C29 C28 C33 116.3(12) . . ?
C29 C28 C34 129.1(11) . . ?
C33 C28 C34 113.8(10) . . ?
C28 C29 C30 131.3(13) . . ?
C28 C29 H29 114.4 . . ?
C30 C29 H29 114.4 . . ?
C31 C30 C29 113.4(13) . . ?
C31 C30 H30 123.3 . . ?
C29 C30 H30 123.3 . . ?
C32 C31 C30 113.4(12) . . ?
C32 C31 H31 123.3 . . ?
C30 C31 H31 123.3 . . ?
C33 C32 C31 127.9(13) . . ?
C33 C32 H32 116.0 . . ?
C31 C32 H32 116.0 . . ?
C32 C33 C28 116.3(12) . . ?
C32 C33 H33 121.9 . . ?
C28 C33 H33 121.9 . . ?
C28 C34 H34A 109.5 . . ?
C28 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C28 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 C1 C2 -174.6(2) . . . . ?
C11 P1 C1 C2 70.9(3) . . . . ?
Zr1 P1 C1 C2 -49.1(2) . . . . ?
C5 N2 C2 C3 0.2(4) . . . . ?
Zr1 N2 C2 C3 -176.9(2) . . . . ?
C5 N2 C2 C1 -178.7(3) . . . . ?
Zr1 N2 C2 C1 4.2(4) . . . . ?
P1 C1 C2 N2 38.6(4) . . . . ?
P1 C1 C2 C3 -140.0(3) . . . . ?
N2 C2 C3 C4 0.3(4) . . . . ?
C1 C2 C3 C4 179.0(3) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 N2 0.8(4) . . . . ?
C3 C4 C5 C6 179.5(4) . . . . ?
C2 N2 C5 C4 -0.6(4) . . . . ?
Zr1 N2 C5 C4 176.3(2) . . . . ?
C2 N2 C5 C6 -179.5(3) . . . . ?
Zr1 N2 C5 C6 -2.5(4) . . . . ?
C4 C5 C6 P2 -136.7(4) . . . . ?
N2 C5 C6 P2 41.9(4) . . . . ?
C19 P2 C6 C5 -177.4(3) . . . . ?
C15 P2 C6 C5 68.9(3) . . . . ?
Zr1 P2 C6 C5 -47.3(2) . . . . ?
C1 P1 C7 C10 173.1(3) . . . . ?
C11 P1 C7 C10 -77.0(3) . . . . ?
Zr1 P1 C7 C10 69.8(3) . . . . ?
C1 P1 C7 C9 -62.3(3) . . . . ?
C11 P1 C7 C9 47.6(4) . . . . ?
Zr1 P1 C7 C9 -165.6(3) . . . . ?
C1 P1 C7 C8 56.7(3) . . . . ?
C11 P1 C7 C8 166.6(3) . . . . ?
Zr1 P1 C7 C8 -46.6(3) . . . . ?
C6 P2 C19 C20 171.1(3) . . . . ?
C15 P2 C19 C20 -80.1(3) . . . . ?
Zr1 P2 C19 C20 66.5(4) . . . . ?
C6 P2 C19 C21 -65.1(3) . . . . ?
C15 P2 C19 C21 43.8(4) . . . . ?
Zr1 P2 C19 C21 -169.7(2) . . . . ?
C6 P2 C19 C22 52.2(3) . . . . ?
C15 P2 C19 C22 161.1(3) . . . . ?
Zr1 P2 C19 C22 -52.4(3) . . . . ?
C27 C23 C24 C25 0.4(5) . . . . ?
Zr1 C23 C24 C25 66.7(3) . . . . ?
C27 C23 C24 Zr1 -66.3(3) . . . . ?
C23 C24 C25 C26 0.2(5) . . . . ?
Zr1 C24 C25 C26 66.3(3) . . . . ?
C23 C24 C25 Zr1 -66.1(3) . . . . ?
C24 C25 C26 C27 -0.7(5) . . . . ?
Zr1 C25 C26 C27 65.9(3) . . . . ?
C24 C25 C26 Zr1 -66.6(3) . . . . ?
C24 C23 C27 C26 -0.8(5) . . . . ?
Zr1 C23 C27 C26 -68.2(3) . . . . ?
C24 C23 C27 Zr1 67.4(3) . . . . ?
C25 C26 C27 C23 0.9(5) . . . . ?
Zr1 C26 C27 C23 68.2(3) . . . . ?
C25 C26 C27 Zr1 -67.3(3) . . . . ?
C33 C28 C29 C30 6(2) . . . . ?
C34 C28 C29 C30 175.7(12) . . . . ?
C28 C29 C30 C31 5(2) . . . . ?
C29 C30 C31 C32 -10.7(17) . . . . ?
C30 C31 C32 C33 8(2) . . . . ?
C31 C32 C33 C28 3(2) . . . . ?
C29 C28 C33 C32 -9.9(17) . . . . ?
C34 C28 C33 C32 179.2(10) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_20171122TiPNPClCp
_database_code_depnum_ccdc_archive 'CCDC 1847685'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C27 H47 Cl N P2 Ti'
_chemical_formula_moiety         'C27 H47 Cl N P2 Ti'
_chemical_formula_weight         530.98
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
loop_
_space_group_symop_operation_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                   47.9405(19)
_cell_length_b                   8.5955(3)
_cell_length_c                   13.8464(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.655(7)
_cell_angle_gamma                90.0000
_cell_volume                     5654.9(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19397
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    178
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2280.00
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_T_max  0.990

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      178
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            26064
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6457
_reflns_number_gt                4384
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1373
_refine_ls_wR_factor_gt          0.1258
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6457
_refine_ls_number_parameters     317
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+36.2000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.62275(2) 0.45248(7) 0.55023(5) 0.02702(17) Uani 1 1 d . . . . .
Cl1 Cl 0.63020(2) 0.38162(12) 0.38974(7) 0.0381(2) Uani 1 1 d . . . . .
P1 P 0.68024(2) 0.43279(11) 0.60054(7) 0.0271(2) Uani 1 1 d . . . . .
P2 P 0.57445(2) 0.26030(12) 0.54290(8) 0.0305(2) Uani 1 1 d . . . . .
N1 N 0.63214(6) 0.2770(3) 0.6549(2) 0.0269(7) Uani 1 1 d . . . . .
C1 C 0.67708(8) 0.3987(4) 0.7304(3) 0.0298(8) Uani 1 1 d . . . . .
H1A H 0.695193 0.362679 0.766176 0.036 Uiso 1 1 calc R U . . .
H1B H 0.671223 0.494831 0.761566 0.036 Uiso 1 1 calc R U . . .
C2 C 0.65506(7) 0.2755(4) 0.7291(3) 0.0286(8) Uani 1 1 d . . . . .
C3 C 0.65479(8) 0.1436(4) 0.7840(3) 0.0325(9) Uani 1 1 d . . . . .
H3 H 0.667884 0.116471 0.839092 0.039 Uiso 1 1 calc R U . . .
C4 C 0.63127(8) 0.0552(4) 0.7432(3) 0.0344(9) Uani 1 1 d . . . . .
H4 H 0.625570 -0.042757 0.765622 0.041 Uiso 1 1 calc R U . . .
C5 C 0.61831(7) 0.1369(4) 0.6655(3) 0.0306(8) Uani 1 1 d . . . . .
C6 C 0.59450(8) 0.0891(4) 0.5898(3) 0.0363(10) Uani 1 1 d . . . . .
H6A H 0.581984 0.015964 0.618786 0.044 Uiso 1 1 calc R U . . .
H6B H 0.602051 0.035057 0.535684 0.044 Uiso 1 1 calc R U . . .
C7 C 0.69611(8) 0.2451(4) 0.5588(3) 0.0324(9) Uani 1 1 d . . . . .
C8 C 0.67361(8) 0.1169(4) 0.5371(3) 0.0360(9) Uani 1 1 d . . . . .
H8A H 0.658265 0.155345 0.489182 0.043 Uiso 1 1 calc R U . . .
H8B H 0.666171 0.088939 0.597341 0.043 Uiso 1 1 calc R U . . .
H8C H 0.682112 0.025008 0.510933 0.043 Uiso 1 1 calc R U . . .
C9 C 0.70719(9) 0.2781(5) 0.4620(3) 0.0429(11) Uani 1 1 d . . . . .
H9A H 0.692671 0.332076 0.417857 0.051 Uiso 1 1 calc R U . . .
H9B H 0.711954 0.179698 0.432433 0.051 Uiso 1 1 calc R U . . .
H9C H 0.724029 0.343603 0.473897 0.051 Uiso 1 1 calc R U . . .
C10 C 0.71932(8) 0.1767(5) 0.6339(3) 0.0409(10) Uani 1 1 d . . . . .
H10A H 0.711318 0.147887 0.692976 0.049 Uiso 1 1 calc R U . . .
H10B H 0.734165 0.254364 0.650191 0.049 Uiso 1 1 calc R U . . .
H10C H 0.727277 0.084170 0.606554 0.049 Uiso 1 1 calc R U . . .
C11 C 0.70744(8) 0.5939(4) 0.6023(3) 0.0330(9) Uani 1 1 d . . . . .
C12 C 0.69984(9) 0.7238(5) 0.6710(3) 0.0428(11) Uani 1 1 d . . . . .
H12A H 0.680549 0.759193 0.649993 0.051 Uiso 1 1 calc R U . . .
H12B H 0.712866 0.811262 0.668879 0.051 Uiso 1 1 calc R U . . .
H12C H 0.701268 0.683633 0.737672 0.051 Uiso 1 1 calc R U . . .
C13 C 0.70673(9) 0.6632(5) 0.4994(3) 0.0428(10) Uani 1 1 d . . . . .
H13A H 0.715687 0.590745 0.458341 0.051 Uiso 1 1 calc R U . . .
H13B H 0.716892 0.762398 0.503467 0.051 Uiso 1 1 calc R U . . .
H13C H 0.687146 0.680511 0.470888 0.051 Uiso 1 1 calc R U . . .
C14 C 0.73792(8) 0.5458(5) 0.6400(4) 0.0486(12) Uani 1 1 d . . . . .
H14A H 0.750331 0.636319 0.639417 0.058 Uiso 1 1 calc R U . . .
H14B H 0.743993 0.464343 0.597923 0.058 Uiso 1 1 calc R U . . .
H14C H 0.738820 0.506227 0.706744 0.058 Uiso 1 1 calc R U . . .
C15 C 0.55375(9) 0.1936(5) 0.4237(3) 0.0422(10) Uani 1 1 d . . . . .
C16 C 0.57401(13) 0.1405(11) 0.3583(5) 0.130(4) Uani 1 1 d . . . . .
H16A H 0.590288 0.210492 0.364685 0.156 Uiso 1 1 calc R U . . .
H16B H 0.564830 0.141272 0.290654 0.156 Uiso 1 1 calc R U . . .
H16C H 0.580284 0.034644 0.376295 0.156 Uiso 1 1 calc R U . . .
C17A C 0.54857(19) 0.3558(10) 0.3631(7) 0.044(2) Uani 0.5 1 d . . P . .
C17B C 0.5269(2) 0.2905(14) 0.3913(8) 0.064(3) Uani 0.5 1 d . . P . .
C18A C 0.5278(2) 0.1064(14) 0.4196(8) 0.055(3) Uani 0.5 1 d . . P . .
C18B C 0.5419(2) 0.0144(12) 0.4348(8) 0.055(3) Uani 0.5 1 d . . P . .
C19 C 0.54922(8) 0.2887(5) 0.6365(3) 0.0400(10) Uani 1 1 d . . . . .
C20 C 0.56689(9) 0.3076(5) 0.7361(3) 0.0433(11) Uani 1 1 d . . . . .
H20A H 0.575877 0.208191 0.756131 0.052 Uiso 1 1 calc R U . . .
H20B H 0.554726 0.339779 0.784028 0.052 Uiso 1 1 calc R U . . .
H20C H 0.581384 0.386767 0.731987 0.052 Uiso 1 1 calc R U . . .
C21 C 0.53144(9) 0.4366(7) 0.6143(4) 0.0589(14) Uani 1 1 d . . . . .
H21A H 0.543909 0.526956 0.614164 0.071 Uiso 1 1 calc R U . . .
H21B H 0.518993 0.450541 0.664300 0.071 Uiso 1 1 calc R U . . .
H21C H 0.520106 0.426536 0.550264 0.071 Uiso 1 1 calc R U . . .
C22 C 0.52926(10) 0.1513(7) 0.6459(4) 0.0623(15) Uani 1 1 d . . . . .
H22A H 0.520742 0.162264 0.706080 0.075 Uiso 1 1 calc R U . . .
H22B H 0.539879 0.053683 0.647806 0.075 Uiso 1 1 calc R U . . .
H22C H 0.514434 0.150348 0.589880 0.075 Uiso 1 1 calc R U . . .
C23 C 0.62560(9) 0.6896(4) 0.6334(3) 0.0369(9) Uani 1 1 d . . . . .
H23 H 0.637796 0.696241 0.693217 0.044 Uiso 1 1 calc R U . . .
C24 C 0.59705(9) 0.6436(4) 0.6207(3) 0.0388(10) Uani 1 1 d . . . . .
H24 H 0.586504 0.614242 0.671239 0.047 Uiso 1 1 calc R U . . .
C25 C 0.58682(9) 0.6485(4) 0.5199(3) 0.0411(10) Uani 1 1 d . . . . .
H25 H 0.568364 0.621644 0.490904 0.049 Uiso 1 1 calc R U . . .
C26 C 0.60869(9) 0.6998(4) 0.4707(3) 0.0396(10) Uani 1 1 d . . . . .
H26 H 0.607616 0.715618 0.402364 0.048 Uiso 1 1 calc R U . . .
C27 C 0.63246(9) 0.7241(4) 0.5393(3) 0.0370(10) Uani 1 1 d . . . . .
H27 H 0.650326 0.758104 0.525121 0.044 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 2.099(3) . ?
Ti1 C23 2.336(4) . ?
Ti1 C24 2.343(4) . ?
Ti1 Cl1 2.3766(12) . ?
Ti1 C27 2.389(4) . ?
Ti1 C25 2.406(4) . ?
Ti1 C26 2.448(4) . ?
Ti1 P1 2.7567(11) . ?
Ti1 P2 2.8349(12) . ?
P1 C1 1.848(4) . ?
P1 C11 1.900(4) . ?
P1 C7 1.906(4) . ?
P2 C6 1.829(4) . ?
P2 C15 1.898(4) . ?
P2 C19 1.902(4) . ?
N1 C5 1.392(5) . ?
N1 C2 1.400(5) . ?
C1 C2 1.493(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.367(5) . ?
C3 C4 1.414(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.363(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.501(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C9 1.532(6) . ?
C7 C10 1.535(5) . ?
C7 C8 1.544(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.541(6) . ?
C11 C14 1.541(5) . ?
C11 C12 1.541(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C18A 1.447(9) . ?
C15 C16 1.486(7) . ?
C15 C17B 1.549(10) . ?
C15 C17A 1.629(10) . ?
C15 C18B 1.657(10) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17A C17B 1.287(14) . ?
C17B C18A 1.630(16) . ?
C18A C18B 1.042(13) . ?
C19 C20 1.528(6) . ?
C19 C22 1.537(6) . ?
C19 C21 1.538(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.413(6) . ?
C23 C27 1.416(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.418(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.399(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 C23 107.08(14) . . ?
N1 Ti1 C24 107.01(14) . . ?
C23 Ti1 C24 35.16(14) . . ?
N1 Ti1 Cl1 114.60(9) . . ?
C23 Ti1 Cl1 132.70(11) . . ?
C24 Ti1 Cl1 136.23(12) . . ?
N1 Ti1 C27 136.08(13) . . ?
C23 Ti1 C27 34.86(14) . . ?
C24 Ti1 C27 57.25(15) . . ?
Cl1 Ti1 C27 97.84(11) . . ?
N1 Ti1 C25 134.98(14) . . ?
C23 Ti1 C25 57.90(14) . . ?
C24 Ti1 C25 34.72(15) . . ?
Cl1 Ti1 C25 102.08(12) . . ?
C27 Ti1 C25 56.34(14) . . ?
N1 Ti1 C26 162.96(14) . . ?
C23 Ti1 C26 57.20(15) . . ?
C24 Ti1 C26 56.63(15) . . ?
Cl1 Ti1 C26 82.44(11) . . ?
C27 Ti1 C26 33.59(13) . . ?
C25 Ti1 C26 33.41(15) . . ?
N1 Ti1 P1 70.48(8) . . ?
C23 Ti1 P1 86.45(11) . . ?
C24 Ti1 P1 120.08(11) . . ?
Cl1 Ti1 P1 87.18(4) . . ?
C27 Ti1 P1 83.06(10) . . ?
C25 Ti1 P1 139.06(11) . . ?
C26 Ti1 P1 111.91(11) . . ?
N1 Ti1 P2 72.85(8) . . ?
C23 Ti1 P2 121.33(11) . . ?
C24 Ti1 P2 87.20(11) . . ?
Cl1 Ti1 P2 92.35(4) . . ?
C27 Ti1 P2 137.07(11) . . ?
C25 Ti1 P2 80.77(11) . . ?
C26 Ti1 P2 108.39(11) . . ?
P1 Ti1 P2 139.25(4) . . ?
C1 P1 C11 104.37(17) . . ?
C1 P1 C7 104.39(17) . . ?
C11 P1 C7 108.64(17) . . ?
C1 P1 Ti1 92.69(12) . . ?
C11 P1 Ti1 128.31(12) . . ?
C7 P1 Ti1 113.67(12) . . ?
C6 P2 C15 104.77(19) . . ?
C6 P2 C19 102.3(2) . . ?
C15 P2 C19 108.96(19) . . ?
C6 P2 Ti1 93.91(12) . . ?
C15 P2 Ti1 122.48(15) . . ?
C19 P2 Ti1 119.41(14) . . ?
C5 N1 C2 104.7(3) . . ?
C5 N1 Ti1 129.3(2) . . ?
C2 N1 Ti1 126.0(2) . . ?
C2 C1 P1 104.4(2) . . ?
C2 C1 H1A 110.9 . . ?
P1 C1 H1A 110.9 . . ?
C2 C1 H1B 110.9 . . ?
P1 C1 H1B 110.9 . . ?
H1A C1 H1B 108.9 . . ?
C3 C2 N1 110.5(3) . . ?
C3 C2 C1 129.8(3) . . ?
N1 C2 C1 119.2(3) . . ?
C2 C3 C4 106.8(3) . . ?
C2 C3 H3 126.6 . . ?
C4 C3 H3 126.6 . . ?
C5 C4 C3 107.1(3) . . ?
C5 C4 H4 126.5 . . ?
C3 C4 H4 126.5 . . ?
C4 C5 N1 110.8(3) . . ?
C4 C5 C6 129.4(3) . . ?
N1 C5 C6 119.5(3) . . ?
C5 C6 P2 110.0(3) . . ?
C5 C6 H6A 109.7 . . ?
P2 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
P2 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C9 C7 C10 111.0(3) . . ?
C9 C7 C8 106.0(3) . . ?
C10 C7 C8 106.4(3) . . ?
C9 C7 P1 107.9(3) . . ?
C10 C7 P1 113.7(3) . . ?
C8 C7 P1 111.5(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C14 108.7(3) . . ?
C13 C11 C12 108.2(3) . . ?
C14 C11 C12 106.1(3) . . ?
C13 C11 P1 109.8(3) . . ?
C14 C11 P1 115.3(3) . . ?
C12 C11 P1 108.5(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18A C15 C16 116.4(6) . . ?
C18A C15 C17B 65.8(7) . . ?
C16 C15 C17B 125.1(6) . . ?
C18A C15 C17A 110.6(6) . . ?
C16 C15 C17A 90.9(6) . . ?
C17B C15 C17A 47.7(5) . . ?
C18A C15 C18B 38.5(5) . . ?
C16 C15 C18B 91.8(6) . . ?
C17B C15 C18B 104.1(7) . . ?
C17A C15 C18B 144.4(6) . . ?
C18A C15 P2 122.5(5) . . ?
C16 C15 P2 108.3(3) . . ?
C17B C15 P2 114.0(5) . . ?
C17A C15 P2 102.5(4) . . ?
C18B C15 P2 110.3(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17B C17A C15 62.9(6) . . ?
C17A C17B C15 69.4(6) . . ?
C17A C17B C18A 119.9(9) . . ?
C15 C17B C18A 54.1(5) . . ?
C18B C18A C15 81.7(8) . . ?
C18B C18A C17B 141.4(10) . . ?
C15 C18A C17B 60.1(6) . . ?
C18A C18B C15 59.8(7) . . ?
C20 C19 C22 106.3(4) . . ?
C20 C19 C21 108.6(4) . . ?
C22 C19 C21 108.5(4) . . ?
C20 C19 P2 107.6(3) . . ?
C22 C19 P2 114.8(3) . . ?
C21 C19 P2 110.8(3) . . ?
C19 C20 H20A 109.5 . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C27 106.5(4) . . ?
C24 C23 Ti1 72.7(2) . . ?
C27 C23 Ti1 74.6(2) . . ?
C24 C23 H23 126.7 . . ?
C27 C23 H23 126.7 . . ?
Ti1 C23 H23 118.1 . . ?
C23 C24 C25 108.4(4) . . ?
C23 C24 Ti1 72.2(2) . . ?
C25 C24 Ti1 75.1(2) . . ?
C23 C24 H24 125.8 . . ?
C25 C24 H24 125.8 . . ?
Ti1 C24 H24 118.8 . . ?
C26 C25 C24 107.8(4) . . ?
C26 C25 Ti1 74.9(2) . . ?
C24 C25 Ti1 70.2(2) . . ?
C26 C25 H25 126.1 . . ?
C24 C25 H25 126.1 . . ?
Ti1 C25 H25 120.6 . . ?
C25 C26 C27 108.2(4) . . ?
C25 C26 Ti1 71.7(2) . . ?
C27 C26 Ti1 70.9(2) . . ?
C25 C26 H26 125.9 . . ?
C27 C26 H26 125.9 . . ?
Ti1 C26 H26 123.2 . . ?
C26 C27 C23 109.0(4) . . ?
C26 C27 Ti1 75.5(2) . . ?
C23 C27 Ti1 70.5(2) . . ?
C26 C27 H27 125.5 . . ?
C23 C27 H27 125.5 . . ?
Ti1 C27 H27 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 P1 C1 C2 178.3(2) . . . . ?
C7 P1 C1 C2 -67.7(3) . . . . ?
Ti1 P1 C1 C2 47.6(2) . . . . ?
C5 N1 C2 C3 -1.7(4) . . . . ?
Ti1 N1 C2 C3 -179.9(3) . . . . ?
C5 N1 C2 C1 171.0(3) . . . . ?
Ti1 N1 C2 C1 -7.1(5) . . . . ?
P1 C1 C2 C3 134.5(4) . . . . ?
P1 C1 C2 N1 -36.6(4) . . . . ?
N1 C2 C3 C4 1.1(4) . . . . ?
C1 C2 C3 C4 -170.7(4) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C3 C4 C5 N1 -1.1(5) . . . . ?
C3 C4 C5 C6 172.2(4) . . . . ?
C2 N1 C5 C4 1.7(4) . . . . ?
Ti1 N1 C5 C4 179.8(3) . . . . ?
C2 N1 C5 C6 -172.3(3) . . . . ?
Ti1 N1 C5 C6 5.8(5) . . . . ?
C4 C5 C6 P2 151.8(4) . . . . ?
N1 C5 C6 P2 -35.4(4) . . . . ?
C15 P2 C6 C5 162.0(3) . . . . ?
C19 P2 C6 C5 -84.3(3) . . . . ?
Ti1 P2 C6 C5 36.9(3) . . . . ?
C6 P2 C15 C18A 80.7(7) . . . . ?
C19 P2 C15 C18A -28.2(7) . . . . ?
Ti1 P2 C15 C18A -174.8(6) . . . . ?
C6 P2 C15 C16 -59.5(5) . . . . ?
C19 P2 C15 C16 -168.4(5) . . . . ?
Ti1 P2 C15 C16 45.1(5) . . . . ?
C6 P2 C15 C17B 156.3(6) . . . . ?
C19 P2 C15 C17B 47.4(6) . . . . ?
Ti1 P2 C15 C17B -99.1(6) . . . . ?
C6 P2 C15 C17A -154.7(4) . . . . ?
C19 P2 C15 C17A 96.4(4) . . . . ?
Ti1 P2 C15 C17A -50.1(4) . . . . ?
C6 P2 C15 C18B 39.6(5) . . . . ?
C19 P2 C15 C18B -69.2(5) . . . . ?
Ti1 P2 C15 C18B 144.2(5) . . . . ?
C18A C15 C17A C17B 20.9(9) . . . . ?
C16 C15 C17A C17B 139.7(7) . . . . ?
C18B C15 C17A C17B 45.3(13) . . . . ?
P2 C15 C17A C17B -111.3(7) . . . . ?
C15 C17A C17B C18A -20.0(8) . . . . ?
C18A C15 C17B C17A -158.5(9) . . . . ?
C16 C15 C17B C17A -52.2(9) . . . . ?
C18B C15 C17B C17A -154.7(7) . . . . ?
P2 C15 C17B C17A 85.1(7) . . . . ?
C16 C15 C17B C18A 106.3(8) . . . . ?
C17A C15 C17B C18A 158.5(9) . . . . ?
C18B C15 C17B C18A 3.8(7) . . . . ?
P2 C15 C17B C18A -116.4(6) . . . . ?
C16 C15 C18A C18B 55.4(11) . . . . ?
C17B C15 C18A C18B 174.1(11) . . . . ?
C17A C15 C18A C18B 157.3(9) . . . . ?
P2 C15 C18A C18B -81.8(10) . . . . ?
C16 C15 C18A C17B -118.7(8) . . . . ?
C17A C15 C18A C17B -16.8(7) . . . . ?
C18B C15 C18A C17B -174.1(11) . . . . ?
P2 C15 C18A C17B 104.1(6) . . . . ?
C17A C17B C18A C18B 14(2) . . . . ?
C15 C17B C18A C18B -9.4(18) . . . . ?
C17A C17B C18A C15 23.3(9) . . . . ?
C17B C18A C18B C15 8.2(16) . . . . ?
C16 C15 C18B C18A -132.5(10) . . . . ?
C17B C15 C18B C18A -5.5(11) . . . . ?
C17A C15 C18B C18A -38.3(15) . . . . ?
P2 C15 C18B C18A 117.2(9) . . . . ?
C27 C23 C24 C25 0.6(4) . . . . ?
Ti1 C23 C24 C25 -66.9(3) . . . . ?
C27 C23 C24 Ti1 67.5(3) . . . . ?
C23 C24 C25 C26 -1.0(4) . . . . ?
Ti1 C24 C25 C26 -66.0(3) . . . . ?
C23 C24 C25 Ti1 65.0(3) . . . . ?
C24 C25 C26 C27 1.1(4) . . . . ?
Ti1 C25 C26 C27 -61.9(3) . . . . ?
C24 C25 C26 Ti1 62.9(3) . . . . ?
C25 C26 C27 C23 -0.7(4) . . . . ?
Ti1 C26 C27 C23 -63.0(3) . . . . ?
C25 C26 C27 Ti1 62.3(3) . . . . ?
C24 C23 C27 C26 0.1(4) . . . . ?
Ti1 C23 C27 C26 66.2(3) . . . . ?
C24 C23 C27 Ti1 -66.2(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_20170902ZrPNPCl2Cp
_database_code_depnum_ccdc_archive 'CCDC 1847683'
_audit_update_record             
;
2018-06-28 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C27 H47 Cl2 N P2 Zr'
_chemical_formula_moiety         'C27 H47 Cl2 N P2 Zr'
_chemical_formula_weight         609.75
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
_space_group_IT_number           15
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
#------------------------------------------------------------------------------
_cell_length_a                   21.3223(6)
_cell_length_b                   9.8821(3)
_cell_length_c                   28.558(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 104.499(7)
_cell_angle_gamma                90.0000
_cell_volume                     5825.7(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    20683
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    173
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.101
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2560.00
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_T_max  0.933

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      173
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            27118
_diffrn_reflns_av_unetI/netI     ?
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.189
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6664
_reflns_number_gt                5842
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.1034
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6664
_refine_ls_number_parameters     330
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+38.2000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Zr Zr -2.9673 0.5597
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
Zr1 Zr 0.45195(2) 0.32682(3) 0.37680(2) 0.01619(9) Uani 1 1 d . . . . .
Cl1 Cl 0.42258(4) 0.27329(8) 0.28879(3) 0.02431(17) Uani 1 1 d . . . . .
Cl2 Cl 0.46087(4) 0.30469(9) 0.46518(3) 0.02611(18) Uani 1 1 d . . . . .
P1 P 0.54075(4) 0.09859(8) 0.39509(3) 0.01922(17) Uani 1 1 d . . . . .
P2 P 0.31513(4) 0.38882(8) 0.35785(3) 0.01733(17) Uani 1 1 d . . . . .
N1 N 0.39654(12) 0.1338(3) 0.37771(9) 0.0185(5) Uani 1 1 d . . . . .
C1 C 0.49013(16) -0.0053(3) 0.42448(12) 0.0225(7) Uani 1 1 d . . . . .
H1A H 0.501997 -0.101775 0.423141 0.027 Uiso 1 1 calc R U . . .
H1B H 0.497898 0.021101 0.458907 0.027 Uiso 1 1 calc R U . . .
C2 C 0.41978(16) 0.0135(3) 0.39965(12) 0.0211(6) Uani 1 1 d . . . . .
C3 C 0.37097(17) -0.0804(3) 0.39341(13) 0.0264(7) Uani 1 1 d . . . . .
H3 H 0.374725 -0.170723 0.405182 0.032 Uiso 1 1 calc R U . . .
C4 C 0.31423(16) -0.0173(3) 0.36620(13) 0.0261(7) Uani 1 1 d . . . . .
H4 H 0.272393 -0.056799 0.356102 0.031 Uiso 1 1 calc R U . . .
C5 C 0.33109(15) 0.1122(3) 0.35711(12) 0.0202(6) Uani 1 1 d . . . . .
C6 C 0.28797(15) 0.2234(3) 0.33172(12) 0.0219(7) Uani 1 1 d . . . . .
H6A H 0.243109 0.206898 0.334167 0.026 Uiso 1 1 calc R U . . .
H6B H 0.287793 0.223268 0.297018 0.026 Uiso 1 1 calc R U . . .
C7 C 0.54923(18) -0.0030(4) 0.34048(13) 0.0296(8) Uani 1 1 d . . . . .
C8 C 0.5929(2) -0.1282(4) 0.35273(16) 0.0442(10) Uani 1 1 d . . . . .
H8A H 0.637909 -0.099498 0.365782 0.053 Uiso 1 1 calc R U . . .
H8B H 0.589767 -0.181890 0.323370 0.053 Uiso 1 1 calc R U . . .
H8C H 0.578990 -0.183197 0.376848 0.053 Uiso 1 1 calc R U . . .
C9 C 0.48206(18) -0.0552(4) 0.31331(13) 0.0324(8) Uani 1 1 d . . . . .
H9A H 0.467622 -0.124531 0.332817 0.039 Uiso 1 1 calc R U . . .
H9B H 0.484594 -0.094385 0.282316 0.039 Uiso 1 1 calc R U . . .
H9C H 0.451129 0.020045 0.307479 0.039 Uiso 1 1 calc R U . . .
C10 C 0.5754(2) 0.0917(5) 0.30684(14) 0.0402(10) Uani 1 1 d . . . . .
H10A H 0.579356 0.041352 0.278133 0.048 Uiso 1 1 calc R U . . .
H10B H 0.618093 0.126083 0.324060 0.048 Uiso 1 1 calc R U . . .
H10C H 0.545556 0.167700 0.296950 0.048 Uiso 1 1 calc R U . . .
C11 C 0.62162(16) 0.1016(4) 0.44230(13) 0.0270(7) Uani 1 1 d . . . . .
C12 C 0.67571(18) 0.1505(5) 0.42023(17) 0.0463(11) Uani 1 1 d . . . . .
H12A H 0.714874 0.167419 0.446052 0.056 Uiso 1 1 calc R U . . .
H12B H 0.662268 0.234404 0.402204 0.056 Uiso 1 1 calc R U . . .
H12C H 0.684767 0.081227 0.398268 0.056 Uiso 1 1 calc R U . . .
C13 C 0.61585(19) 0.1999(4) 0.48226(15) 0.0400(10) Uani 1 1 d . . . . .
H13A H 0.606834 0.291019 0.468680 0.048 Uiso 1 1 calc R U . . .
H13B H 0.656566 0.200775 0.507519 0.048 Uiso 1 1 calc R U . . .
H13C H 0.580464 0.171093 0.496228 0.048 Uiso 1 1 calc R U . . .
C14 C 0.64010(19) -0.0359(4) 0.46695(15) 0.0382(9) Uani 1 1 d . . . . .
H14A H 0.682051 -0.028225 0.490637 0.046 Uiso 1 1 calc R U . . .
H14B H 0.643063 -0.103661 0.442549 0.046 Uiso 1 1 calc R U . . .
H14C H 0.606978 -0.063502 0.483414 0.046 Uiso 1 1 calc R U . . .
C15 C 0.27026(16) 0.5093(3) 0.30922(12) 0.0246(7) Uani 1 1 d . . . . .
C16 C 0.30367(18) 0.5066(4) 0.26739(13) 0.0326(8) Uani 1 1 d . . . . .
H16A H 0.348712 0.536402 0.279158 0.039 Uiso 1 1 calc R U . . .
H16B H 0.280834 0.567396 0.241615 0.039 Uiso 1 1 calc R U . . .
H16C H 0.302781 0.414265 0.254707 0.039 Uiso 1 1 calc R U . . .
C17 C 0.19873(17) 0.4694(4) 0.28759(14) 0.0338(8) Uani 1 1 d . . . . .
H17A H 0.173905 0.484158 0.311753 0.041 Uiso 1 1 calc R U . . .
H17B H 0.196334 0.373657 0.278325 0.041 Uiso 1 1 calc R U . . .
H17C H 0.180610 0.524996 0.258997 0.041 Uiso 1 1 calc R U . . .
C18 C 0.2733(2) 0.6541(4) 0.32848(14) 0.0353(9) Uani 1 1 d . . . . .
H18A H 0.252742 0.715486 0.302150 0.042 Uiso 1 1 calc R U . . .
H18B H 0.318594 0.680457 0.341431 0.042 Uiso 1 1 calc R U . . .
H18C H 0.250346 0.659076 0.354202 0.042 Uiso 1 1 calc R U . . .
C19 C 0.28223(16) 0.4026(3) 0.41333(12) 0.0240(7) Uani 1 1 d . . . . .
C20 C 0.31784(18) 0.5184(4) 0.44499(13) 0.0306(8) Uani 1 1 d . . . . .
H20A H 0.364455 0.499683 0.453999 0.037 Uiso 1 1 calc R U . . .
H20B H 0.302015 0.525822 0.474285 0.037 Uiso 1 1 calc R U . . .
H20C H 0.309757 0.603556 0.426891 0.037 Uiso 1 1 calc R U . . .
C21 C 0.29430(17) 0.2693(4) 0.44140(13) 0.0285(8) Uani 1 1 d . . . . .
H21A H 0.265709 0.199084 0.423378 0.034 Uiso 1 1 calc R U . . .
H21B H 0.285367 0.281403 0.473172 0.034 Uiso 1 1 calc R U . . .
H21C H 0.339555 0.241897 0.445631 0.034 Uiso 1 1 calc R U . . .
C22 C 0.20905(17) 0.4304(4) 0.40226(14) 0.0320(8) Uani 1 1 d . . . . .
H22A H 0.199751 0.519389 0.386987 0.038 Uiso 1 1 calc R U . . .
H22B H 0.195055 0.428777 0.432430 0.038 Uiso 1 1 calc R U . . .
H22C H 0.185692 0.360562 0.380308 0.038 Uiso 1 1 calc R U . . .
C23A C 0.4744(4) 0.5744(6) 0.4009(4) 0.042(2) Uani 0.7 1 d . . P . .
C23B C 0.5435(9) 0.4634(16) 0.3563(8) 0.025(4) Uiso 0.3 1 d . . P . .
C24A C 0.4630(5) 0.5720(10) 0.3495(5) 0.053(3) Uani 0.7 1 d . . P . .
C24B C 0.5491(8) 0.4807(18) 0.4070(7) 0.024(4) Uiso 0.3 1 d . . P . .
C25A C 0.5125(7) 0.4968(12) 0.3372(3) 0.054(3) Uani 0.7 1 d . . P . .
C25B C 0.4970(11) 0.5570(19) 0.4114(6) 0.021(4) Uiso 0.3 1 d . . P . .
C26A C 0.5555(3) 0.4574(6) 0.3816(5) 0.0373(15) Uani 0.7 1 d . . P . .
C26B C 0.4570(11) 0.581(2) 0.3657(8) 0.022(4) Uiso 0.3 1 d . . P . .
C27A C 0.5322(5) 0.5089(7) 0.4196(2) 0.0307(14) Uani 0.7 1 d . . P . .
C27B C 0.4877(10) 0.528(2) 0.3324(8) 0.027(4) Uiso 0.3 1 d . . P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 2.247(3) . ?
Zr1 Cl1 2.4901(8) . ?
Zr1 Cl2 2.4929(8) . ?
Zr1 C26A 2.531(5) . ?
Zr1 C26B 2.54(2) . ?
Zr1 C24B 2.541(15) . ?
Zr1 C25A 2.549(7) . ?
Zr1 C23A 2.554(6) . ?
Zr1 C23B 2.560(16) . ?
Zr1 C25B 2.569(16) . ?
Zr1 C27A 2.572(5) . ?
Zr1 C24A 2.574(7) . ?
P1 C1 1.837(3) . ?
P1 C7 1.901(4) . ?
P1 C11 1.905(3) . ?
P2 C6 1.829(3) . ?
P2 C19 1.891(3) . ?
P2 C15 1.896(3) . ?
N1 C2 1.377(4) . ?
N1 C5 1.388(4) . ?
C1 C2 1.502(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.372(5) . ?
C3 C4 1.409(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.498(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.536(5) . ?
C7 C9 1.537(5) . ?
C7 C10 1.542(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.525(5) . ?
C11 C13 1.527(5) . ?
C11 C14 1.535(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C18 1.529(5) . ?
C15 C16 1.537(5) . ?
C15 C17 1.547(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.531(5) . ?
C19 C20 1.536(5) . ?
C19 C22 1.537(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23A C25B 0.529(18) . ?
C23A C26B 0.980(19) . ?
C23A C27A 1.377(10) . ?
C23A C24A 1.427(14) . ?
C23A C24B 1.814(19) . ?
C23B C26A 0.708(16) . ?
C23B C25A 0.813(15) . ?
C23B C27B 1.37(2) . ?
C23B C24B 1.43(2) . ?
C23B C27A 1.937(19) . ?
C23B C24A 1.993(19) . ?
C24A C26B 0.52(2) . ?
C24A C27B 0.91(2) . ?
C24A C25A 1.405(16) . ?
C24A C25B 1.743(18) . ?
C24B C27A 0.634(17) . ?
C24B C26A 0.804(17) . ?
C24B C25B 1.38(2) . ?
C24B C25A 1.956(19) . ?
C25A C27B 0.599(18) . ?
C25A C26A 1.420(12) . ?
C25A C26B 1.80(2) . ?
C25B C27A 0.871(18) . ?
C25B C26B 1.39(2) . ?
C25B C26A 1.94(2) . ?
C26A C27A 1.397(10) . ?
C26A C27B 1.88(2) . ?
C26B C27B 1.39(2) . ?

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 80.29(7) . . ?
N1 Zr1 Cl2 79.68(7) . . ?
Cl1 Zr1 Cl2 159.96(3) . . ?
N1 Zr1 C26A 152.38(15) . . ?
Cl1 Zr1 C26A 99.1(3) . . ?
Cl2 Zr1 C26A 98.3(3) . . ?
N1 Zr1 C26B 151.7(5) . . ?
Cl1 Zr1 C26B 95.3(5) . . ?
Cl2 Zr1 C26B 102.6(5) . . ?
C26A Zr1 C26B 55.8(5) . . ?
N1 Zr1 C24B 152.9(4) . . ?
Cl1 Zr1 C24B 116.6(5) . . ?
Cl2 Zr1 C24B 81.9(5) . . ?
C26A Zr1 C24B 18.2(4) . . ?
C26B Zr1 C24B 52.7(6) . . ?
N1 Zr1 C25A 153.0(2) . . ?
Cl1 Zr1 C25A 73.74(18) . . ?
Cl2 Zr1 C25A 126.00(18) . . ?
C26A Zr1 C25A 32.5(3) . . ?
C26B Zr1 C25A 41.4(5) . . ?
C24B Zr1 C25A 45.2(4) . . ?
N1 Zr1 C23A 150.88(17) . . ?
Cl1 Zr1 C23A 117.2(3) . . ?
Cl2 Zr1 C23A 81.4(3) . . ?
C26A Zr1 C23A 52.8(2) . . ?
C26B Zr1 C23A 22.2(4) . . ?
C24B Zr1 C23A 41.7(4) . . ?
C25A Zr1 C23A 53.6(3) . . ?
N1 Zr1 C23B 152.1(4) . . ?
Cl1 Zr1 C23B 83.9(5) . . ?
Cl2 Zr1 C23B 114.1(5) . . ?
C26A Zr1 C23B 16.0(4) . . ?
C26B Zr1 C23B 52.5(6) . . ?
C24B Zr1 C23B 32.7(5) . . ?
C25A Zr1 C23B 18.3(3) . . ?
C23A Zr1 C23B 56.9(4) . . ?
N1 Zr1 C25B 153.4(4) . . ?
Cl1 Zr1 C25B 123.5(4) . . ?
Cl2 Zr1 C25B 76.2(4) . . ?
C26A Zr1 C25B 44.8(4) . . ?
C26B Zr1 C25B 31.6(5) . . ?
C24B Zr1 C25B 31.2(5) . . ?
C25A Zr1 C25B 53.5(4) . . ?
C23A Zr1 C25B 11.8(4) . . ?
C23B Zr1 C25B 52.3(5) . . ?
N1 Zr1 C27A 151.33(15) . . ?
Cl1 Zr1 C27A 126.72(16) . . ?
Cl2 Zr1 C27A 72.95(15) . . ?
C26A Zr1 C27A 31.8(2) . . ?
C26B Zr1 C27A 47.4(5) . . ?
C24B Zr1 C27A 14.2(4) . . ?
C25A Zr1 C27A 53.1(2) . . ?
C23A Zr1 C27A 31.2(2) . . ?
C23B Zr1 C27A 44.3(4) . . ?
C25B Zr1 C27A 19.5(4) . . ?
N1 Zr1 C24A 152.9(2) . . ?
Cl1 Zr1 C24A 85.0(3) . . ?
Cl2 Zr1 C24A 113.6(3) . . ?
C26A Zr1 C24A 52.6(3) . . ?
C26B Zr1 C24A 11.6(4) . . ?
C24B Zr1 C24A 53.9(4) . . ?
C25A Zr1 C24A 31.8(4) . . ?
C23A Zr1 C24A 32.3(3) . . ?
C23B Zr1 C24A 45.7(4) . . ?
C25B Zr1 C24A 39.6(4) . . ?
C27A Zr1 C24A 52.1(2) . . ?
C1 P1 C7 105.51(16) . . ?
C1 P1 C11 102.50(15) . . ?
C7 P1 C11 109.49(16) . . ?
C1 P1 Zr1 94.86(11) . . ?
C7 P1 Zr1 116.98(12) . . ?
C11 P1 Zr1 123.28(12) . . ?
C6 P2 C19 105.09(15) . . ?
C6 P2 C15 102.23(15) . . ?
C19 P2 C15 110.08(15) . . ?
C6 P2 Zr1 95.07(10) . . ?
C19 P2 Zr1 115.23(11) . . ?
C15 P2 Zr1 124.71(11) . . ?
C2 N1 C5 105.6(3) . . ?
C2 N1 Zr1 127.4(2) . . ?
C5 N1 Zr1 126.9(2) . . ?
C2 C1 P1 110.3(2) . . ?
C2 C1 H1A 109.6 . . ?
P1 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
P1 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C3 C2 N1 110.5(3) . . ?
C3 C2 C1 127.8(3) . . ?
N1 C2 C1 121.6(3) . . ?
C2 C3 C4 106.9(3) . . ?
C2 C3 H3 126.6 . . ?
C4 C3 H3 126.6 . . ?
C5 C4 C3 106.7(3) . . ?
C5 C4 H4 126.6 . . ?
C3 C4 H4 126.6 . . ?
C4 C5 N1 110.3(3) . . ?
C4 C5 C6 128.2(3) . . ?
N1 C5 C6 121.5(3) . . ?
C5 C6 P2 111.4(2) . . ?
C5 C6 H6A 109.4 . . ?
P2 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
P2 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C9 106.3(3) . . ?
C8 C7 C10 109.7(3) . . ?
C9 C7 C10 109.1(3) . . ?
C8 C7 P1 114.5(3) . . ?
C9 C7 P1 108.9(2) . . ?
C10 C7 P1 108.3(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C13 108.5(3) . . ?
C12 C11 C14 109.7(3) . . ?
C13 C11 C14 106.2(3) . . ?
C12 C11 P1 110.9(3) . . ?
C13 C11 P1 108.1(2) . . ?
C14 C11 P1 113.2(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 C16 108.1(3) . . ?
C18 C15 C17 109.3(3) . . ?
C16 C15 C17 106.7(3) . . ?
C18 C15 P2 110.9(2) . . ?
C16 C15 P2 108.2(2) . . ?
C17 C15 P2 113.5(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C20 109.8(3) . . ?
C21 C19 C22 106.9(3) . . ?
C20 C19 C22 108.4(3) . . ?
C21 C19 P2 109.1(2) . . ?
C20 C19 P2 108.3(2) . . ?
C22 C19 P2 114.3(2) . . ?
C19 C20 H20A 109.5 . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25B C23A C26B 131(3) . . ?
C25B C23A C27A 13(2) . . ?
C26B C23A C27A 120.1(15) . . ?
C25B C23A C24A 119(2) . . ?
C26B C23A C24A 12.9(15) . . ?
C27A C23A C24A 107.4(7) . . ?
C25B C23A C24B 29(2) . . ?
C26B C23A C24B 103.3(15) . . ?
C27A C23A C24B 16.8(6) . . ?
C24A C23A C24B 90.6(8) . . ?
C25B C23A Zr1 86(2) . . ?
C26B C23A Zr1 77.8(13) . . ?
C27A C23A Zr1 75.2(3) . . ?
C24A C23A Zr1 74.6(4) . . ?
C24B C23A Zr1 68.8(5) . . ?
C26A C23B C25A 138(3) . . ?
C26A C23B C27B 126(2) . . ?
C25A C23B C27B 11.6(14) . . ?
C26A C23B C24B 19.6(12) . . ?
C25A C23B C24B 118.4(19) . . ?
C27B C23B C24B 106.8(17) . . ?
C26A C23B C27A 32.9(12) . . ?
C25A C23B C27A 105.1(16) . . ?
C27B C23B C27A 93.5(14) . . ?
C24B C23B C27A 13.3(7) . . ?
C26A C23B C24A 103.1(17) . . ?
C25A C23B C24A 34.9(11) . . ?
C27B C23B C24A 23.3(10) . . ?
C24B C23B C24A 83.5(10) . . ?
C27A C23B C24A 70.2(7) . . ?
C26A C23B Zr1 79.7(14) . . ?
C25A C23B Zr1 80.1(12) . . ?
C27B C23B Zr1 75.1(13) . . ?
C24B C23B Zr1 72.9(9) . . ?
C27A C23B Zr1 68.2(5) . . ?
C24A C23B Zr1 67.5(5) . . ?
C26B C24A C27B 150(4) . . ?
C26B C24A C25A 133(4) . . ?
C27B C24A C25A 17.3(14) . . ?
C26B C24A C23A 25(3) . . ?
C27B C24A C23A 125.8(16) . . ?
C25A C24A C23A 108.6(7) . . ?
C26B C24A C25B 40(3) . . ?
C27B C24A C25B 110.7(16) . . ?
C25A C24A C25B 93.4(9) . . ?
C23A C24A C25B 15.5(7) . . ?
C26B C24A C23B 114(3) . . ?
C27B C24A C23B 36.6(13) . . ?
C25A C24A C23B 19.3(6) . . ?
C23A C24A C23B 89.3(7) . . ?
C25B C24A C23B 74.1(9) . . ?
C26B C24A Zr1 80(3) . . ?
C27B C24A Zr1 79.9(15) . . ?
C25A C24A Zr1 73.1(4) . . ?
C23A C24A Zr1 73.1(4) . . ?
C25B C24A Zr1 70.0(6) . . ?
C23B C24A Zr1 66.8(5) . . ?
C27A C24B C26A 152(3) . . ?
C27A C24B C25B 28.3(14) . . ?
C26A C24B C25B 124.2(17) . . ?
C27A C24B C23B 135(2) . . ?
C26A C24B C23B 17.2(10) . . ?
C25B C24B C23B 107.0(14) . . ?
C27A C24B C23A 38.8(14) . . ?
C26A C24B C23A 113.6(15) . . ?
C25B C24B C23A 10.8(7) . . ?
C23B C24B C23A 96.5(11) . . ?
C27A C24B C25A 113.8(19) . . ?
C26A C24B C25A 38.6(10) . . ?
C25B C24B C25A 85.6(10) . . ?
C23B C24B C25A 21.4(7) . . ?
C23A C24B C25A 75.1(7) . . ?
C27A C24B Zr1 85.7(16) . . ?
C26A C24B Zr1 80.2(12) . . ?
C25B C24B Zr1 75.5(10) . . ?
C23B C24B Zr1 74.4(10) . . ?
C23A C24B Zr1 69.5(5) . . ?
C25A C24B Zr1 67.6(5) . . ?
C27B C25A C23B 153(3) . . ?
C27B C25A C24A 27(2) . . ?
C23B C25A C24A 125.8(16) . . ?
C27B C25A C26A 133(3) . . ?
C23B C25A C26A 19.5(13) . . ?
C24A C25A C26A 106.3(7) . . ?
C27B C25A C26B 39(3) . . ?
C23B C25A C26B 113.7(16) . . ?
C24A C25A C26B 12.2(9) . . ?
C26A C25A C26B 94.2(9) . . ?
C27B C25A C24B 112(3) . . ?
C23B C25A C24B 40.2(13) . . ?
C24A C25A C24B 85.6(8) . . ?
C26A C25A C24B 20.7(5) . . ?
C26B C25A C24B 73.5(9) . . ?
C27B C25A Zr1 86(3) . . ?
C23B C25A Zr1 81.6(13) . . ?
C24A C25A Zr1 75.1(4) . . ?
C26A C25A Zr1 73.1(4) . . ?
C26B C25A Zr1 68.9(7) . . ?
C24B C25A Zr1 67.2(5) . . ?
C23A C25B C27A 159(3) . . ?
C23A C25B C24B 140(3) . . ?
C27A C25B C24B 20.2(10) . . ?
C23A C25B C26B 32(2) . . ?
C27A C25B C26B 129.1(18) . . ?
C24B C25B C26B 109.1(14) . . ?
C23A C25B C24A 46.0(19) . . ?
C27A C25B C24A 115.6(15) . . ?
C24B C25B C24A 95.4(12) . . ?
C26B C25B C24A 14.0(10) . . ?
C23A C25B C26A 120(2) . . ?
C27A C25B C26A 40.2(9) . . ?
C24B C25B C26A 20.0(7) . . ?
C26B C25B C26A 89.1(11) . . ?
C24A C25B C26A 75.4(8) . . ?
C23A C25B Zr1 82(2) . . ?
C27A C25B Zr1 80.5(12) . . ?
C24B C25B Zr1 73.3(10) . . ?
C26B C25B Zr1 72.9(11) . . ?
C24A C25B Zr1 70.4(6) . . ?
C26A C25B Zr1 66.5(5) . . ?
C23B C26A C24B 143(2) . . ?
C23B C26A C27A 131.1(17) . . ?
C24B C26A C27A 12.2(12) . . ?
C23B C26A C25A 22.5(14) . . ?
C24B C26A C25A 120.7(14) . . ?
C27A C26A C25A 108.6(7) . . ?
C23B C26A C27B 36.0(17) . . ?
C24B C26A C27B 107.3(15) . . ?
C27A C26A C27B 95.2(7) . . ?
C25A C26A C27B 13.4(9) . . ?
C23B C26A C25B 107.4(16) . . ?
C24B C26A C25B 35.8(12) . . ?
C27A C26A C25B 23.7(5) . . ?
C25A C26A C25B 84.9(7) . . ?
C27B C26A C25B 71.5(8) . . ?
C23B C26A Zr1 84.4(15) . . ?
C24B C26A Zr1 81.6(12) . . ?
C27A C26A Zr1 75.8(3) . . ?
C25A C26A Zr1 74.5(4) . . ?
C27B C26A Zr1 69.7(7) . . ?
C25B C26A Zr1 68.6(5) . . ?
C24A C26B C23A 142(4) . . ?
C24A C26B C27B 19(3) . . ?
C23A C26B C27B 124(2) . . ?
C24A C26B C25B 126(4) . . ?
C23A C26B C25B 16.6(11) . . ?
C27B C26B C25B 107.3(18) . . ?
C24A C26B C25A 35(3) . . ?
C23A C26B C25A 108.0(18) . . ?
C27B C26B C25A 15.8(9) . . ?
C25B C26B C25A 91.6(14) . . ?
C24A C26B Zr1 88(3) . . ?
C23A C26B Zr1 80.0(13) . . ?
C27B C26B Zr1 75.9(14) . . ?
C25B C26B Zr1 75.6(12) . . ?
C25A C26B Zr1 69.7(7) . . ?
C24B C27A C25B 131(2) . . ?
C24B C27A C23A 124.5(18) . . ?
C25B C27A C23A 8.0(12) . . ?
C24B C27A C26A 15.5(16) . . ?
C25B C27A C26A 116.1(12) . . ?
C23A C27A C26A 109.0(6) . . ?
C24B C27A C23B 31.4(17) . . ?
C25B C27A C23B 100.1(12) . . ?
C23A C27A C23B 93.1(7) . . ?
C26A C27A C23B 16.0(6) . . ?
C24B C27A Zr1 80.1(16) . . ?
C25B C27A Zr1 80.0(11) . . ?
C23A C27A Zr1 73.7(3) . . ?
C26A C27A Zr1 72.5(3) . . ?
C23B C27A Zr1 67.5(5) . . ?
C25A C27B C24A 136(4) . . ?
C25A C27B C23B 15.8(19) . . ?
C24A C27B C23B 120(2) . . ?
C25A C27B C26B 125(3) . . ?
C24A C27B C26B 10.9(13) . . ?
C23B C27B C26B 109(2) . . ?
C25A C27B C26A 33(2) . . ?
C24A C27B C26A 102.4(17) . . ?
C23B C27B C26A 17.6(8) . . ?
C26B C27B C26A 91.8(16) . . ?
C25A C27B Zr1 81(3) . . ?
C24A C27B Zr1 79.7(15) . . ?
C23B C27B Zr1 73.9(12) . . ?
C26B C27B Zr1 72.6(14) . . ?
C26A C27B Zr1 67.1(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 C1 C2 -82.0(3) . . . . ?
C11 P1 C1 C2 163.4(2) . . . . ?
Zr1 P1 C1 C2 37.8(2) . . . . ?
C5 N1 C2 C3 -0.3(4) . . . . ?
Zr1 N1 C2 C3 178.4(2) . . . . ?
C5 N1 C2 C1 177.5(3) . . . . ?
Zr1 N1 C2 C1 -3.9(4) . . . . ?
P1 C1 C2 C3 146.6(3) . . . . ?
P1 C1 C2 N1 -30.7(4) . . . . ?
N1 C2 C3 C4 0.2(4) . . . . ?
C1 C2 C3 C4 -177.4(3) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C3 C4 C5 N1 -0.2(4) . . . . ?
C3 C4 C5 C6 -176.6(3) . . . . ?
C2 N1 C5 C4 0.3(4) . . . . ?
Zr1 N1 C5 C4 -178.4(2) . . . . ?
C2 N1 C5 C6 177.0(3) . . . . ?
Zr1 N1 C5 C6 -1.6(4) . . . . ?
C4 C5 C6 P2 145.4(3) . . . . ?
N1 C5 C6 P2 -30.8(4) . . . . ?
C19 P2 C6 C5 -81.3(3) . . . . ?
C15 P2 C6 C5 163.7(2) . . . . ?
Zr1 P2 C6 C5 36.6(2) . . . . ?
C6 P2 C15 C18 166.5(3) . . . . ?
C19 P2 C15 C18 55.2(3) . . . . ?
Zr1 P2 C15 C18 -88.4(3) . . . . ?
C6 P2 C15 C16 -75.2(3) . . . . ?
C19 P2 C15 C16 173.5(2) . . . . ?
Zr1 P2 C15 C16 29.9(3) . . . . ?
C6 P2 C15 C17 43.1(3) . . . . ?
C19 P2 C15 C17 -68.2(3) . . . . ?
Zr1 P2 C15 C17 148.1(2) . . . . ?
C6 P2 C19 C21 44.9(3) . . . . ?
C15 P2 C19 C21 154.3(2) . . . . ?
Zr1 P2 C19 C21 -58.3(2) . . . . ?
C6 P2 C19 C20 164.5(2) . . . . ?
C15 P2 C19 C20 -86.1(3) . . . . ?
Zr1 P2 C19 C20 61.3(3) . . . . ?
C6 P2 C19 C22 -74.6(3) . . . . ?
C15 P2 C19 C22 34.8(3) . . . . ?
Zr1 P2 C19 C22 -177.8(2) . . . . ?
C25B C23A C24A C26B 179(7) . . . . ?
C27A C23A C24A C26B 171(7) . . . . ?
C24B C23A C24A C26B 171(7) . . . . ?
Zr1 C23A C24A C26B 103(7) . . . . ?
C25B C23A C24A C27B 13(3) . . . . ?
C26B C23A C24A C27B -166(7) . . . . ?
C27A C23A C24A C27B 5.1(19) . . . . ?
C24B C23A C24A C27B 4.2(19) . . . . ?
Zr1 C23A C24A C27B -63.5(18) . . . . ?
C25B C23A C24A C25A 11(3) . . . . ?
C26B C23A C24A C25A -168(7) . . . . ?
C27A C23A C24A C25A 3.7(7) . . . . ?
C24B C23A C24A C25A 2.8(8) . . . . ?
Zr1 C23A C24A C25A -65.0(5) . . . . ?
C26B C23A C24A C25B -179(7) . . . . ?
C27A C23A C24A C25B -8(2) . . . . ?
C24B C23A C24A C25B -9(3) . . . . ?
Zr1 C23A C24A C25B -76(3) . . . . ?
C25B C23A C24A C23B 10(3) . . . . ?
C26B C23A C24A C23B -169(7) . . . . ?
C27A C23A C24A C23B 2.8(7) . . . . ?
C24B C23A C24A C23B 1.9(8) . . . . ?
Zr1 C23A C24A C23B -65.9(5) . . . . ?
C25B C23A C24A Zr1 76(3) . . . . ?
C26B C23A C24A Zr1 -103(7) . . . . ?
C27A C23A C24A Zr1 68.7(4) . . . . ?
C24B C23A C24A Zr1 67.8(5) . . . . ?
C26A C23B C24B C27A -174(5) . . . . ?
C25A C23B C24B C27A 1(4) . . . . ?
C27B C23B C24B C27A 1(4) . . . . ?
C24A C23B C24B C27A 2(3) . . . . ?
Zr1 C23B C24B C27A -67(3) . . . . ?
C25A C23B C24B C26A 176(4) . . . . ?
C27B C23B C24B C26A 176(4) . . . . ?
C27A C23B C24B C26A 174(5) . . . . ?
C24A C23B C24B C26A 176(3) . . . . ?
Zr1 C23B C24B C26A 108(3) . . . . ?
C26A C23B C24B C25B -177(4) . . . . ?
C25A C23B C24B C25B -1(3) . . . . ?
C27B C23B C24B C25B -1(2) . . . . ?
C27A C23B C24B C25B -2(2) . . . . ?
C24A C23B C24B C25B -0.6(13) . . . . ?
Zr1 C23B C24B C25B -69.1(12) . . . . ?
C26A C23B C24B C23A -174(3) . . . . ?
C25A C23B C24B C23A 2(2) . . . . ?
C27B C23B C24B C23A 1.5(18) . . . . ?
C27A C23B C24B C23A 0(3) . . . . ?
C24A C23B C24B C23A 1.9(8) . . . . ?
Zr1 C23B C24B C23A -66.6(6) . . . . ?
C26A C23B C24B C25A -176(4) . . . . ?
C27B C23B C24B C25A -0.1(15) . . . . ?
C27A C23B C24B C25A -1(4) . . . . ?
C24A C23B C24B C25A 0.2(15) . . . . ?
Zr1 C23B C24B C25A -68.2(18) . . . . ?
C26A C23B C24B Zr1 -108(3) . . . . ?
C25A C23B C24B Zr1 68.2(18) . . . . ?
C27B C23B C24B Zr1 68.1(15) . . . . ?
C27A C23B C24B Zr1 67(3) . . . . ?
C24A C23B C24B Zr1 68.4(5) . . . . ?
C25B C23A C24B C27A 13(4) . . . . ?
C26B C23A C24B C27A 179(2) . . . . ?
C24A C23A C24B C27A 177(2) . . . . ?
Zr1 C23A C24B C27A -110(2) . . . . ?
C25B C23A C24B C26A -169(5) . . . . ?
C26B C23A C24B C26A -2(2) . . . . ?
C27A C23A C24B C26A 178(3) . . . . ?
C24A C23A C24B C26A -4.5(16) . . . . ?
Zr1 C23A C24B C26A 68.7(15) . . . . ?
C26B C23A C24B C25B 167(5) . . . . ?
C27A C23A C24B C25B -13(4) . . . . ?
C24A C23A C24B C25B 165(5) . . . . ?
Zr1 C23A C24B C25B -122(4) . . . . ?
C25B C23A C24B C23B -167(5) . . . . ?
C26B C23A C24B C23B -0.4(17) . . . . ?
C27A C23A C24B C23B -180(3) . . . . ?
C24A C23A C24B C23B -2.6(11) . . . . ?
Zr1 C23A C24B C23B 70.6(10) . . . . ?
C25B C23A C24B C25A -166(4) . . . . ?
C26B C23A C24B C25A 0.2(14) . . . . ?
C27A C23A C24B C25A -179(2) . . . . ?
C24A C23A C24B C25A -2.0(5) . . . . ?
Zr1 C23A C24B C25A 71.3(4) . . . . ?
C25B C23A C24B Zr1 122(4) . . . . ?
C26B C23A C24B Zr1 -71.1(14) . . . . ?
C27A C23A C24B Zr1 110(2) . . . . ?
C24A C23A C24B Zr1 -73.2(4) . . . . ?
C26A C23B C25A C27B 1(8) . . . . ?
C24B C23B C25A C27B -1(7) . . . . ?
C27A C23B C25A C27B 0(7) . . . . ?
C24A C23B C25A C27B -1(6) . . . . ?
Zr1 C23B C25A C27B 64(6) . . . . ?
C26A C23B C25A C24A 2(5) . . . . ?
C27B C23B C25A C24A 1(6) . . . . ?
C24B C23B C25A C24A 0(3) . . . . ?
C27A C23B C25A C24A 0.7(19) . . . . ?
Zr1 C23B C25A C24A 64.7(12) . . . . ?
C27B C23B C25A C26A -1(8) . . . . ?
C24B C23B C25A C26A -2(2) . . . . ?
C27A C23B C25A C26A -2(3) . . . . ?
C24A C23B C25A C26A -2(5) . . . . ?
Zr1 C23B C25A C26A 62(3) . . . . ?
C26A C23B C25A C26B 0(4) . . . . ?
C27B C23B C25A C26B -1(6) . . . . ?
C24B C23B C25A C26B -2(2) . . . . ?
C27A C23B C25A C26B -1.6(16) . . . . ?
C24A C23B C25A C26B -2.3(11) . . . . ?
Zr1 C23B C25A C26B 62.4(10) . . . . ?
C26A C23B C25A C24B 2(2) . . . . ?
C27B C23B C25A C24B 1(7) . . . . ?
C27A C23B C25A C24B 0.3(10) . . . . ?
C24A C23B C25A C24B 0(3) . . . . ?
Zr1 C23B C25A C24B 64.3(16) . . . . ?
C26A C23B C25A Zr1 -62(3) . . . . ?
C27B C23B C25A Zr1 -64(6) . . . . ?
C24B C23B C25A Zr1 -64.3(16) . . . . ?
C27A C23B C25A Zr1 -64.0(8) . . . . ?
C24A C23B C25A Zr1 -64.7(12) . . . . ?
C26B C24A C25A C27B 169(6) . . . . ?
C23A C24A C25A C27B 176(5) . . . . ?
C25B C24A C25A C27B 179(5) . . . . ?
C23B C24A C25A C27B 179(6) . . . . ?
Zr1 C24A C25A C27B 111(5) . . . . ?
C26B C24A C25A C23B -10(5) . . . . ?
C27B C24A C25A C23B -179(6) . . . . ?
C23A C24A C25A C23B -2.8(19) . . . . ?
C25B C24A C25A C23B 0.2(18) . . . . ?
Zr1 C24A C25A C23B -67.8(17) . . . . ?
C26B C24A C25A C26A -9(5) . . . . ?
C27B C24A C25A C26A -178(5) . . . . ?
C23A C24A C25A C26A -2.0(8) . . . . ?
C25B C24A C25A C26A 1.0(8) . . . . ?
C23B C24A C25A C26A 0.9(16) . . . . ?
Zr1 C24A C25A C26A -66.9(4) . . . . ?
C27B C24A C25A C26B -169(6) . . . . ?
C23A C24A C25A C26B 7(4) . . . . ?
C25B C24A C25A C26B 10(4) . . . . ?
C23B C24A C25A C26B 10(5) . . . . ?
Zr1 C24A C25A C26B -58(4) . . . . ?
C26B C24A C25A C24B -10(4) . . . . ?
C27B C24A C25A C24B -179(5) . . . . ?
C23A C24A C25A C24B -2.6(7) . . . . ?
C25B C24A C25A C24B 0.4(8) . . . . ?
C23B C24A C25A C24B 0.2(17) . . . . ?
Zr1 C24A C25A C24B -67.5(5) . . . . ?
C26B C24A C25A Zr1 58(4) . . . . ?
C27B C24A C25A Zr1 -111(5) . . . . ?
C23A C24A C25A Zr1 64.9(5) . . . . ?
C25B C24A C25A Zr1 67.9(6) . . . . ?
C23B C24A C25A Zr1 67.8(17) . . . . ?
C26B C23A C25B C27A -33(10) . . . . ?
C24A C23A C25B C27A -34(10) . . . . ?
C24B C23A C25B C27A -16(5) . . . . ?
Zr1 C23A C25B C27A 36(9) . . . . ?
C26B C23A C25B C24B -17(6) . . . . ?
C27A C23A C25B C24B 16(5) . . . . ?
C24A C23A C25B C24B -18(5) . . . . ?
Zr1 C23A C25B C24B 52(4) . . . . ?
C27A C23A C25B C26B 33(10) . . . . ?
C24A C23A C25B C26B 0(2) . . . . ?
C24B C23A C25B C26B 17(6) . . . . ?
Zr1 C23A C25B C26B 70(3) . . . . ?
C26B C23A C25B C24A 0(2) . . . . ?
C27A C23A C25B C24A 34(10) . . . . ?
C24B C23A C25B C24A 18(5) . . . . ?
Zr1 C23A C25B C24A 69.9(15) . . . . ?
C26B C23A C25B C26A -13(4) . . . . ?
C27A C23A C25B C26A 21(7) . . . . ?
C24A C23A C25B C26A -13(3) . . . . ?
C24B C23A C25B C26A 5(2) . . . . ?
Zr1 C23A C25B C26A 57.0(18) . . . . ?
C26B C23A C25B Zr1 -70(3) . . . . ?
C27A C23A C25B Zr1 -36(9) . . . . ?
C24A C23A C25B Zr1 -69.9(14) . . . . ?
C24B C23A C25B Zr1 -52(4) . . . . ?
C27A C24B C25B C23A -163(6) . . . . ?
C26A C24B C25B C23A 12(5) . . . . ?
C23B C24B C25B C23A 13(5) . . . . ?
C25A C24B C25B C23A 13(4) . . . . ?
Zr1 C24B C25B C23A -55(4) . . . . ?
C26A C24B C25B C27A 176(4) . . . . ?
C23B C24B C25B C27A 177(3) . . . . ?
C23A C24B C25B C27A 163(5) . . . . ?
C25A C24B C25B C27A 176(3) . . . . ?
Zr1 C24B C25B C27A 108(3) . . . . ?
C27A C24B C25B C26B -173(3) . . . . ?
C26A C24B C25B C26B 3(3) . . . . ?
C23B C24B C25B C26B 4(2) . . . . ?
C23A C24B C25B C26B -10(3) . . . . ?
C25A C24B C25B C26B 3.5(15) . . . . ?
Zr1 C24B C25B C26B -64.6(14) . . . . ?
C27A C24B C25B C24A -176(3) . . . . ?
C26A C24B C25B C24A 0(2) . . . . ?
C23B C24B C25B C24A 0.7(15) . . . . ?
C23A C24B C25B C24A -13(4) . . . . ?
C25A C24B C25B C24A 0.4(8) . . . . ?
Zr1 C24B C25B C24A -67.6(6) . . . . ?
C27A C24B C25B C26A -176(4) . . . . ?
C23B C24B C25B C26A 1.2(13) . . . . ?
C23A C24B C25B C26A -12(5) . . . . ?
C25A C24B C25B C26A 0.9(16) . . . . ?
Zr1 C24B C25B C26A -67.1(19) . . . . ?
C27A C24B C25B Zr1 -108(3) . . . . ?
C26A C24B C25B Zr1 67.1(19) . . . . ?
C23B C24B C25B Zr1 68.3(12) . . . . ?
C23A C24B C25B Zr1 55(4) . . . . ?
C25A C24B C25B Zr1 68.0(5) . . . . ?
C26B C24A C25B C23A -1(5) . . . . ?
C27B C24A C25B C23A -169(3) . . . . ?
C25A C24A C25B C23A -169(3) . . . . ?
C23B C24A C25B C23A -169(3) . . . . ?
Zr1 C24A C25B C23A -99(3) . . . . ?
C26B C24A C25B C27A 167(5) . . . . ?
C27B C24A C25B C27A -2(2) . . . . ?
C25A C24A C25B C27A -2.1(16) . . . . ?
C23A C24A C25B C27A 167(4) . . . . ?
C23B C24A C25B C27A -2.0(14) . . . . ?
Zr1 C24A C25B C27A 68.5(15) . . . . ?
C26B C24A C25B C24B 168(5) . . . . ?
C27B C24A C25B C24B -0.3(19) . . . . ?
C25A C24A C25B C24B -0.6(11) . . . . ?
C23A C24A C25B C24B 169(3) . . . . ?
C23B C24A C25B C24B -0.5(11) . . . . ?
Zr1 C24A C25B C24B 70.1(10) . . . . ?
C27B C24A C25B C26B -168(5) . . . . ?
C25A C24A C25B C26B -169(5) . . . . ?
C23A C24A C25B C26B 1(5) . . . . ?
C23B C24A C25B C26B -169(5) . . . . ?
Zr1 C24A C25B C26B -98(5) . . . . ?
C26B C24A C25B C26A 168(5) . . . . ?
C27B C24A C25B C26A -0.5(16) . . . . ?
C25A C24A C25B C26A -0.7(5) . . . . ?
C23A C24A C25B C26A 169(3) . . . . ?
C23B C24A C25B C26A -0.7(6) . . . . ?
Zr1 C24A C25B C26A 69.9(4) . . . . ?
C26B C24A C25B Zr1 98(5) . . . . ?
C27B C24A C25B Zr1 -70.3(16) . . . . ?
C25A C24A C25B Zr1 -70.6(5) . . . . ?
C23A C24A C25B Zr1 99(3) . . . . ?
C23B C24A C25B Zr1 -70.6(6) . . . . ?
C25A C23B C26A C24B -6(6) . . . . ?
C27B C23B C26A C24B -5(5) . . . . ?
C27A C23B C26A C24B -2(2) . . . . ?
C24A C23B C26A C24B -4(4) . . . . ?
Zr1 C23B C26A C24B -68(3) . . . . ?
C25A C23B C26A C27A -3(5) . . . . ?
C27B C23B C26A C27A -3(4) . . . . ?
C24B C23B C26A C27A 2(2) . . . . ?
C24A C23B C26A C27A -2(2) . . . . ?
Zr1 C23B C26A C27A -65.5(15) . . . . ?
C27B C23B C26A C25A 0(2) . . . . ?
C24B C23B C26A C25A 6(6) . . . . ?
C27A C23B C26A C25A 3(5) . . . . ?
C24A C23B C26A C25A 1(3) . . . . ?
Zr1 C23B C26A C25A -62(3) . . . . ?
C25A C23B C26A C27B 0(2) . . . . ?
C24B C23B C26A C27B 5(5) . . . . ?
C27A C23B C26A C27B 3(4) . . . . ?
C24A C23B C26A C27B 1.1(18) . . . . ?
Zr1 C23B C26A C27B -63(2) . . . . ?
C25A C23B C26A C25B -3(4) . . . . ?
C27B C23B C26A C25B -3(3) . . . . ?
C24B C23B C26A C25B 2(3) . . . . ?
C27A C23B C26A C25B 0.0(11) . . . . ?
C24A C23B C26A C25B -1.7(15) . . . . ?
Zr1 C23B C26A C25B -65.5(8) . . . . ?
C25A C23B C26A Zr1 62(3) . . . . ?
C27B C23B C26A Zr1 63(2) . . . . ?
C24B C23B C26A Zr1 68(3) . . . . ?
C27A C23B C26A Zr1 65.5(15) . . . . ?
C24A C23B C26A Zr1 63.8(8) . . . . ?
C27A C24B C26A C23B 8(8) . . . . ?
C25B C24B C26A C23B 4(4) . . . . ?
C23A C24B C26A C23B 6(4) . . . . ?
C25A C24B C26A C23B 2(3) . . . . ?
Zr1 C24B C26A C23B 69(3) . . . . ?
C25B C24B C26A C27A -5(4) . . . . ?
C23B C24B C26A C27A -8(8) . . . . ?
C23A C24B C26A C27A -2(5) . . . . ?
C25A C24B C26A C27A -6(6) . . . . ?
Zr1 C24B C26A C27A 60(6) . . . . ?
C27A C24B C26A C25A 6(6) . . . . ?
C25B C24B C26A C25A 1(3) . . . . ?
C23B C24B C26A C25A -2(3) . . . . ?
C23A C24B C26A C25A 3.9(19) . . . . ?
Zr1 C24B C26A C25A 66.3(9) . . . . ?
C27A C24B C26A C27B 5(6) . . . . ?
C25B C24B C26A C27B 1(2) . . . . ?
C23B C24B C26A C27B -3(3) . . . . ?
C23A C24B C26A C27B 3.2(16) . . . . ?
C25A C24B C26A C27B -0.7(10) . . . . ?
Zr1 C24B C26A C27B 65.6(9) . . . . ?
C27A C24B C26A C25B 5(4) . . . . ?
C23B C24B C26A C25B -4(4) . . . . ?
C23A C24B C26A C25B 2.5(11) . . . . ?
C25A C24B C26A C25B -1(3) . . . . ?
Zr1 C24B C26A C25B 64.9(18) . . . . ?
C27A C24B C26A Zr1 -60(6) . . . . ?
C25B C24B C26A Zr1 -64.9(18) . . . . ?
C23B C24B C26A Zr1 -69(3) . . . . ?
C23A C24B C26A Zr1 -62.4(10) . . . . ?
C25A C24B C26A Zr1 -66.3(10) . . . . ?
C27B C25A C26A C23B -179(5) . . . . ?
C24A C25A C26A C23B -178(4) . . . . ?
C26B C25A C26A C23B -180(4) . . . . ?
C24B C25A C26A C23B -176(4) . . . . ?
Zr1 C25A C26A C23B 114(4) . . . . ?
C27B C25A C26A C24B -3(4) . . . . ?
C23B C25A C26A C24B 176(4) . . . . ?
C24A C25A C26A C24B -1.8(16) . . . . ?
C26B C25A C26A C24B -3.7(16) . . . . ?
Zr1 C25A C26A C24B -70.1(15) . . . . ?
C27B C25A C26A C27A -2(4) . . . . ?
C23B C25A C26A C27A 177(4) . . . . ?
C24A C25A C26A C27A -0.4(7) . . . . ?
C26B C25A C26A C27A -2.3(8) . . . . ?
C24B C25A C26A C27A 1.3(14) . . . . ?
Zr1 C25A C26A C27A -68.7(4) . . . . ?
C23B C25A C26A C27B 179(5) . . . . ?
C24A C25A C26A C27B 1(3) . . . . ?
C26B C25A C26A C27B -1(4) . . . . ?
C24B C25A C26A C27B 3(4) . . . . ?
Zr1 C25A C26A C27B -67(4) . . . . ?
C27B C25A C26A C25B -2(4) . . . . ?
C23B C25A C26A C25B 177(4) . . . . ?
C24A C25A C26A C25B -0.9(7) . . . . ?
C26B C25A C26A C25B -2.8(9) . . . . ?
C24B C25A C26A C25B 0.8(15) . . . . ?
Zr1 C25A C26A C25B -69.2(5) . . . . ?
C27B C25A C26A Zr1 67(4) . . . . ?
C23B C25A C26A Zr1 -114(4) . . . . ?
C24A C25A C26A Zr1 68.3(5) . . . . ?
C26B C25A C26A Zr1 66.4(7) . . . . ?
C24B C25A C26A Zr1 70.1(15) . . . . ?
C27B C24A C26B C23A 22(11) . . . . ?
C25A C24A C26B C23A 16(9) . . . . ?
C25B C24A C26B C23A 0(3) . . . . ?
C23B C24A C26B C23A 12(7) . . . . ?
Zr1 C24A C26B C23A 71(6) . . . . ?
C25A C24A C26B C27B -6(4) . . . . ?
C23A C24A C26B C27B -22(11) . . . . ?
C25B C24A C26B C27B -22(9) . . . . ?
C23B C24A C26B C27B -10(5) . . . . ?
Zr1 C24A C26B C27B 49(6) . . . . ?
C27B C24A C26B C25B 22(9) . . . . ?
C25A C24A C26B C25B 16(7) . . . . ?
C23A C24A C26B C25B 0(3) . . . . ?
C23B C24A C26B C25B 12(5) . . . . ?
Zr1 C24A C26B C25B 71(3) . . . . ?
C27B C24A C26B C25A 6(4) . . . . ?
C23A C24A C26B C25A -16(9) . . . . ?
C25B C24A C26B C25A -16(7) . . . . ?
C23B C24A C26B C25A -3.5(18) . . . . ?
Zr1 C24A C26B C25A 55(4) . . . . ?
C27B C24A C26B Zr1 -49(6) . . . . ?
C25A C24A C26B Zr1 -55(3) . . . . ?
C23A C24A C26B Zr1 -71(6) . . . . ?
C25B C24A C26B Zr1 -71(3) . . . . ?
C23B C24A C26B Zr1 -59.0(19) . . . . ?
C25B C23A C26B C24A -1(8) . . . . ?
C27A C23A C26B C24A -9(7) . . . . ?
C24B C23A C26B C24A -10(7) . . . . ?
Zr1 C23A C26B C24A -74(7) . . . . ?
C25B C23A C26B C27B 8(5) . . . . ?
C27A C23A C26B C27B -1(3) . . . . ?
C24A C23A C26B C27B 9(5) . . . . ?
C24B C23A C26B C27B -1(3) . . . . ?
Zr1 C23A C26B C27B -65(2) . . . . ?
C27A C23A C26B C25B -8(3) . . . . ?
C24A C23A C26B C25B 1(8) . . . . ?
C24B C23A C26B C25B -9(3) . . . . ?
Zr1 C23A C26B C25B -73(3) . . . . ?
C25B C23A C26B C25A 8(4) . . . . ?
C27A C23A C26B C25A 0(2) . . . . ?
C24A C23A C26B C25A 10(5) . . . . ?
C24B C23A C26B C25A -0.2(16) . . . . ?
Zr1 C23A C26B C25A -64.6(11) . . . . ?
C25B C23A C26B Zr1 73(3) . . . . ?
C27A C23A C26B Zr1 64.7(10) . . . . ?
C24A C23A C26B Zr1 74(7) . . . . ?
C24B C23A C26B Zr1 64.4(7) . . . . ?
C23A C25B C26B C24A 179(6) . . . . ?
C27A C25B C26B C24A -16(6) . . . . ?
C24B C25B C26B C24A -13(5) . . . . ?
C26A C25B C26B C24A -12(5) . . . . ?
Zr1 C25B C26B C24A -77(4) . . . . ?
C27A C25B C26B C23A 165(5) . . . . ?
C24B C25B C26B C23A 168(4) . . . . ?
C24A C25B C26B C23A -179(6) . . . . ?
C26A C25B C26B C23A 169(4) . . . . ?
Zr1 C25B C26B C23A 103(3) . . . . ?
C23A C25B C26B C27B -173(4) . . . . ?
C27A C25B C26B C27B -8(3) . . . . ?
C24B C25B C26B C27B -5(2) . . . . ?
C24A C25B C26B C27B 7(3) . . . . ?
C26A C25B C26B C27B -4.2(19) . . . . ?
Zr1 C25B C26B C27B -69.9(17) . . . . ?
C23A C25B C26B C25A -172(4) . . . . ?
C27A C25B C26B C25A -7(3) . . . . ?
C24B C25B C26B C25A -3.7(17) . . . . ?
C24A C25B C26B C25A 9(4) . . . . ?
C26A C25B C26B C25A -2.9(9) . . . . ?
Zr1 C25B C26B C25A -68.5(7) . . . . ?
C23A C25B C26B Zr1 -103(3) . . . . ?
C27A C25B C26B Zr1 62(2) . . . . ?
C24B C25B C26B Zr1 64.8(13) . . . . ?
C24A C25B C26B Zr1 77(4) . . . . ?
C26A C25B C26B Zr1 65.7(5) . . . . ?
C27B C25A C26B C24A -8(5) . . . . ?
C23B C25A C26B C24A 171(4) . . . . ?
C26A C25A C26B C24A 171(4) . . . . ?
C24B C25A C26B C24A 170(5) . . . . ?
Zr1 C25A C26B C24A -119(5) . . . . ?
C27B C25A C26B C23A -178(5) . . . . ?
C23B C25A C26B C23A 1(2) . . . . ?
C24A C25A C26B C23A -170(6) . . . . ?
C26A C25A C26B C23A 1.6(17) . . . . ?
C24B C25A C26B C23A 0.2(15) . . . . ?
Zr1 C25A C26B C23A 71.6(15) . . . . ?
C23B C25A C26B C27B 179(4) . . . . ?
C24A C25A C26B C27B 8(5) . . . . ?
C26A C25A C26B C27B 179(4) . . . . ?
C24B C25A C26B C27B 178(4) . . . . ?
Zr1 C25A C26B C27B -111(4) . . . . ?
C27B C25A C26B C25B -175(5) . . . . ?
C23B C25A C26B C25B 4(2) . . . . ?
C24A C25A C26B C25B -167(5) . . . . ?
C26A C25A C26B C25B 3.9(13) . . . . ?
C24B C25A C26B C25B 2.6(12) . . . . ?
Zr1 C25A C26B C25B 74.0(11) . . . . ?
C27B C25A C26B Zr1 111(4) . . . . ?
C23B C25A C26B Zr1 -70.1(15) . . . . ?
C24A C25A C26B Zr1 119(5) . . . . ?
C26A C25A C26B Zr1 -70.0(5) . . . . ?
C24B C25A C26B Zr1 -71.4(6) . . . . ?
C26A C24B C27A C25B -8(7) . . . . ?
C23B C24B C27A C25B -4(4) . . . . ?
C23A C24B C27A C25B -4.9(16) . . . . ?
C25A C24B C27A C25B -4(3) . . . . ?
Zr1 C24B C27A C25B -67(2) . . . . ?
C26A C24B C27A C23A -3(7) . . . . ?
C25B C24B C27A C23A 4.9(16) . . . . ?
C23B C24B C27A C23A 1(4) . . . . ?
C25A C24B C27A C23A 1(2) . . . . ?
Zr1 C24B C27A C23A -62.2(14) . . . . ?
C25B C24B C27A C26A 8(7) . . . . ?
C23B C24B C27A C26A 4(3) . . . . ?
C23A C24B C27A C26A 3(7) . . . . ?
C25A C24B C27A C26A 4(4) . . . . ?
Zr1 C24B C27A C26A -59(5) . . . . ?
C26A C24B C27A C23B -4(3) . . . . ?
C25B C24B C27A C23B 4(4) . . . . ?
C23A C24B C27A C23B -1(4) . . . . ?
C25A C24B C27A C23B 0.5(17) . . . . ?
Zr1 C24B C27A C23B -63(3) . . . . ?
C26A C24B C27A Zr1 59(5) . . . . ?
C25B C24B C27A Zr1 67(2) . . . . ?
C23B C24B C27A Zr1 63(3) . . . . ?
C23A C24B C27A Zr1 62.2(14) . . . . ?
C25A C24B C27A Zr1 63.2(11) . . . . ?
C23A C25B C27A C24B 31(10) . . . . ?
C26B C25B C27A C24B 9(4) . . . . ?
C24A C25B C27A C24B 4(3) . . . . ?
C26A C25B C27A C24B 2(2) . . . . ?
Zr1 C25B C27A C24B 67(2) . . . . ?
C24B C25B C27A C23A -31(10) . . . . ?
C26B C25B C27A C23A -22(7) . . . . ?
C24A C25B C27A C23A -26(8) . . . . ?
C26A C25B C27A C23A -28(9) . . . . ?
Zr1 C25B C27A C23A 37(9) . . . . ?
C23A C25B C27A C26A 28(9) . . . . ?
C24B C25B C27A C26A -2(2) . . . . ?
C26B C25B C27A C26A 6(3) . . . . ?
C24A C25B C27A C26A 2.0(18) . . . . ?
Zr1 C25B C27A C26A 64.7(8) . . . . ?
C23A C25B C27A C23B 28(9) . . . . ?
C24B C25B C27A C23B -2(2) . . . . ?
C26B C25B C27A C23B 6(2) . . . . ?
C24A C25B C27A C23B 2.0(14) . . . . ?
C26A C25B C27A C23B 0.0(7) . . . . ?
Zr1 C25B C27A C23B 64.8(6) . . . . ?
C23A C25B C27A Zr1 -37(9) . . . . ?
C24B C25B C27A Zr1 -67(2) . . . . ?
C26B C25B C27A Zr1 -59(2) . . . . ?
C24A C25B C27A Zr1 -62.7(11) . . . . ?
C26A C25B C27A Zr1 -64.7(8) . . . . ?
C25B C23A C27A C24B -152(9) . . . . ?
C26B C23A C27A C24B -1(3) . . . . ?
C24A C23A C27A C24B -3(2) . . . . ?
Zr1 C23A C27A C24B 65(2) . . . . ?
C26B C23A C27A C25B 152(9) . . . . ?
C24A C23A C27A C25B 149(9) . . . . ?
C24B C23A C27A C25B 152(9) . . . . ?
Zr1 C23A C27A C25B -142(9) . . . . ?
C25B C23A C27A C26A -153(9) . . . . ?
C26B C23A C27A C26A -1.7(17) . . . . ?
C24A C23A C27A C26A -3.9(6) . . . . ?
C24B C23A C27A C26A -0.9(19) . . . . ?
Zr1 C23A C27A C26A 64.3(4) . . . . ?
C25B C23A C27A C23B -152(9) . . . . ?
C26B C23A C27A C23B -0.6(17) . . . . ?
C24A C23A C27A C23B -2.8(7) . . . . ?
C24B C23A C27A C23B 0(2) . . . . ?
Zr1 C23A C27A C23B 65.5(5) . . . . ?
C25B C23A C27A Zr1 142(9) . . . . ?
C26B C23A C27A Zr1 -66.1(16) . . . . ?
C24A C23A C27A Zr1 -68.3(4) . . . . ?
C24B C23A C27A Zr1 -65(2) . . . . ?
C23B C26A C27A C24B -173(6) . . . . ?
C25A C26A C27A C24B -175(6) . . . . ?
C27B C26A C27A C24B -175(6) . . . . ?
C25B C26A C27A C24B -173(6) . . . . ?
Zr1 C26A C27A C24B 118(6) . . . . ?
C23B C26A C27A C25B 0(3) . . . . ?
C24B C26A C27A C25B 173(6) . . . . ?
C25A C26A C27A C25B -1.2(14) . . . . ?
C27B C26A C27A C25B -1.6(15) . . . . ?
Zr1 C26A C27A C25B -69.1(13) . . . . ?
C23B C26A C27A C23A 4(2) . . . . ?
C24B C26A C27A C23A 177(6) . . . . ?
C25A C26A C27A C23A 2.8(6) . . . . ?
C27B C26A C27A C23A 2.4(8) . . . . ?
C25B C26A C27A C23A 4.0(13) . . . . ?
Zr1 C26A C27A C23A -65.1(4) . . . . ?
C24B C26A C27A C23B 173(6) . . . . ?
C25A C26A C27A C23B -1(2) . . . . ?
C27B C26A C27A C23B -2(2) . . . . ?
C25B C26A C27A C23B 0(3) . . . . ?
Zr1 C26A C27A C23B -69(2) . . . . ?
C23B C26A C27A Zr1 69(2) . . . . ?
C24B C26A C27A Zr1 -118(6) . . . . ?
C25A C26A C27A Zr1 67.9(4) . . . . ?
C27B C26A C27A Zr1 67.5(7) . . . . ?
C25B C26A C27A Zr1 69.1(13) . . . . ?
C23B C25A C27B C24A 2(10) . . . . ?
C26A C25A C27B C24A 3(7) . . . . ?
C26B C25A C27B C24A 4(2) . . . . ?
C24B C25A C27B C24A 1(6) . . . . ?
Zr1 C25A C27B C24A 65(5) . . . . ?
C24A C25A C27B C23B -2(10) . . . . ?
C26A C25A C27B C23B 1(4) . . . . ?
C26B C25A C27B C23B 2(9) . . . . ?
C24B C25A C27B C23B 0(5) . . . . ?
Zr1 C25A C27B C23B 63(6) . . . . ?
C23B C25A C27B C26B -2(9) . . . . ?
C24A C25A C27B C26B -4(2) . . . . ?
C26A C25A C27B C26B -1(6) . . . . ?
C24B C25A C27B C26B -2(5) . . . . ?
Zr1 C25A C27B C26B 61(3) . . . . ?
C23B C25A C27B C26A -1(4) . . . . ?
C24A C25A C27B C26A -3(7) . . . . ?
C26B C25A C27B C26A 1(6) . . . . ?
C24B C25A C27B C26A -1.1(16) . . . . ?
Zr1 C25A C27B C26A 62(3) . . . . ?
C23B C25A C27B Zr1 -63(6) . . . . ?
C24A C25A C27B Zr1 -65(5) . . . . ?
C26A C25A C27B Zr1 -62(3) . . . . ?
C26B C25A C27B Zr1 -61(3) . . . . ?
C24B C25A C27B Zr1 -63.2(14) . . . . ?
C26B C24A C27B C25A -16(9) . . . . ?
C23A C24A C27B C25A -5(6) . . . . ?
C25B C24A C27B C25A -1(6) . . . . ?
C23B C24A C27B C25A -1(3) . . . . ?
Zr1 C24A C27B C25A -65(5) . . . . ?
C26B C24A C27B C23B -15(8) . . . . ?
C25A C24A C27B C23B 1(3) . . . . ?
C23A C24A C27B C23B -4(3) . . . . ?
C25B C24A C27B C23B 0(3) . . . . ?
Zr1 C24A C27B C23B -64(2) . . . . ?
C25A C24A C27B C26B 16(9) . . . . ?
C23A C24A C27B C26B 11(6) . . . . ?
C25B C24A C27B C26B 15(6) . . . . ?
C23B C24A C27B C26B 15(8) . . . . ?
Zr1 C24A C27B C26B -49(7) . . . . ?
C26B C24A C27B C26A -15(7) . . . . ?
C25A C24A C27B C26A 1(4) . . . . ?
C23A C24A C27B C26A -3(2) . . . . ?
C25B C24A C27B C26A 0.5(17) . . . . ?
C23B C24A C27B C26A 0.8(14) . . . . ?
Zr1 C24A C27B C26A -63.6(9) . . . . ?
C26B C24A C27B Zr1 49(7) . . . . ?
C25A C24A C27B Zr1 65(5) . . . . ?
C23A C24A C27B Zr1 60.4(13) . . . . ?
C25B C24A C27B Zr1 64.0(9) . . . . ?
C23B C24A C27B Zr1 64(2) . . . . ?
C26A C23B C27B C25A -179(7) . . . . ?
C24B C23B C27B C25A 179(6) . . . . ?
C27A C23B C27B C25A 180(6) . . . . ?
C24A C23B C27B C25A 178(8) . . . . ?
Zr1 C23B C27B C25A -114(6) . . . . ?
C26A C23B C27B C24A 3(4) . . . . ?
C25A C23B C27B C24A -178(8) . . . . ?
C24B C23B C27B C24A 1(3) . . . . ?
C27A C23B C27B C24A 1(3) . . . . ?
Zr1 C23B C27B C24A 67(2) . . . . ?
C26A C23B C27B C26B 0(4) . . . . ?
C25A C23B C27B C26B 178(8) . . . . ?
C24B C23B C27B C26B -2(3) . . . . ?
C27A C23B C27B C26B -2(2) . . . . ?
C24A C23B C27B C26B -3.1(15) . . . . ?
Zr1 C23B C27B C26B 64.4(18) . . . . ?
C25A C23B C27B C26A 179(7) . . . . ?
C24B C23B C27B C26A -1.8(17) . . . . ?
C27A C23B C27B C26A -2(2) . . . . ?
C24A C23B C27B C26A -3(4) . . . . ?
Zr1 C23B C27B C26A 65(3) . . . . ?
C26A C23B C27B Zr1 -65(3) . . . . ?
C25A C23B C27B Zr1 114(6) . . . . ?
C24B C23B C27B Zr1 -66.6(13) . . . . ?
C27A C23B C27B Zr1 -66.3(6) . . . . ?
C24A C23B C27B Zr1 -67(2) . . . . ?
C24A C26B C27B C25A 166(8) . . . . ?
C23A C26B C27B C25A 3(6) . . . . ?
C25B C26B C27B C25A 5(5) . . . . ?
Zr1 C26B C27B C25A -65(4) . . . . ?
C23A C26B C27B C24A -164(9) . . . . ?
C25B C26B C27B C24A -161(8) . . . . ?
C25A C26B C27B C24A -166(8) . . . . ?
Zr1 C26B C27B C24A 129(7) . . . . ?
C24A C26B C27B C23B 166(7) . . . . ?
C23A C26B C27B C23B 2(4) . . . . ?
C25B C26B C27B C23B 4(3) . . . . ?
C25A C26B C27B C23B -1(3) . . . . ?
Zr1 C26B C27B C23B -65.2(17) . . . . ?
C24A C26B C27B C26A 166(7) . . . . ?
C23A C26B C27B C26A 2(3) . . . . ?
C25B C26B C27B C26A 4(2) . . . . ?
C25A C26B C27B C26A -1(3) . . . . ?
Zr1 C26B C27B C26A -65.3(7) . . . . ?
C24A C26B C27B Zr1 -129(7) . . . . ?
C23A C26B C27B Zr1 67(2) . . . . ?
C25B C26B C27B Zr1 69.7(15) . . . . ?
C25A C26B C27B Zr1 65(4) . . . . ?
C23B C26A C27B C25A 1(3) . . . . ?
C24B C26A C27B C25A 177(4) . . . . ?
C27A C26A C27B C25A 178(4) . . . . ?
C25B C26A C27B C25A 178(4) . . . . ?
Zr1 C26A C27B C25A -109(4) . . . . ?
C23B C26A C27B C24A -178(4) . . . . ?
C24B C26A C27B C24A -1(2) . . . . ?
C27A C26A C27B C24A 0.3(17) . . . . ?
C25A C26A C27B C24A -178(5) . . . . ?
C25B C26A C27B C24A -0.4(15) . . . . ?
Zr1 C26A C27B C24A 73.0(16) . . . . ?
C24B C26A C27B C23B 177(3) . . . . ?
C27A C26A C27B C23B 178(3) . . . . ?
C25A C26A C27B C23B -1(3) . . . . ?
C25B C26A C27B C23B 177(3) . . . . ?
Zr1 C26A C27B C23B -109(3) . . . . ?
C23B C26A C27B C26B 180(4) . . . . ?
C24B C26A C27B C26B -4(2) . . . . ?
C27A C26A C27B C26B -2.5(15) . . . . ?
C25A C26A C27B C26B 179(5) . . . . ?
C25B C26A C27B C26B -3.1(14) . . . . ?
Zr1 C26A C27B C26B 70.3(14) . . . . ?
C23B C26A C27B Zr1 109(3) . . . . ?
C24B C26A C27B Zr1 -73.8(13) . . . . ?
C27A C26A C27B Zr1 -72.7(4) . . . . ?
C25A C26A C27B Zr1 109(4) . . . . ?
C25B C26A C27B Zr1 -73.4(6) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_20171203Ti2PNP2Cp2N2
_database_code_depnum_ccdc_archive 'CCDC 1847686'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C54 H94 N4 P4 Ti2'
_chemical_formula_moiety         'C54 H94 N4 P4 Ti2'
_chemical_formula_weight         1019.06
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_space_group_IT_number           19
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,-Y,1/2+Z
3 1/2+X,1/2-Y,-Z
4 -X,1/2+Y,1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.9662(3)
_cell_length_b                   22.1194(4)
_cell_length_c                   22.1259(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     6345.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    53470
_cell_measurement_theta_min      1.82
_cell_measurement_theta_max      27.46
_cell_measurement_temperature    183
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.188
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200.00
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_T_max  0.930

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      183
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            62392
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         2.058
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             14499
_reflns_number_gt                12772
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0694
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         14499
_refine_ls_number_parameters     602
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0364P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.17
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.00000

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.17767(3) 0.59688(2) 0.39660(2) 0.02462(10) Uani 1 1 d . . . . .
Ti2 Ti 0.42899(3) 0.44894(2) 0.43606(2) 0.02237(10) Uani 1 1 d . . . . .
P1 P 0.19815(5) 0.63328(3) 0.27963(3) 0.02642(15) Uani 1 1 d . . . . .
P2 P 0.18996(5) 0.65450(3) 0.52663(3) 0.02474(14) Uani 1 1 d . . . . .
P3 P 0.60971(5) 0.49023(3) 0.39256(3) 0.02248(14) Uani 1 1 d . . . . .
P4 P 0.27345(6) 0.33826(3) 0.41083(3) 0.03162(17) Uani 1 1 d . . . . .
N1 N 0.21492(15) 0.69103(9) 0.39574(8) 0.0228(4) Uani 1 1 d . . . . .
N2 N 0.47857(17) 0.38708(9) 0.36760(9) 0.0265(5) Uani 1 1 d . . . . .
N3 N 0.29652(15) 0.55345(9) 0.39666(9) 0.0250(4) Uani 1 1 d . . . . .
N4 N 0.35485(15) 0.50887(9) 0.40137(9) 0.0235(4) Uani 1 1 d . . . . .
C1 C 0.3083(2) 0.68175(12) 0.29882(10) 0.0293(6) Uani 1 1 d . . . . .
H1A H 0.369042 0.657075 0.310113 0.035 Uiso 1 1 calc R U . . .
H1B H 0.327050 0.708024 0.264297 0.035 Uiso 1 1 calc R U . . .
C2 C 0.2720(2) 0.71879(12) 0.35143(10) 0.0269(6) Uani 1 1 d . . . . .
C3 C 0.2780(2) 0.77984(12) 0.36151(12) 0.0364(7) Uani 1 1 d . . . . .
H3 H 0.312119 0.808867 0.336975 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2233(2) 0.79102(12) 0.41571(11) 0.0344(7) Uani 1 1 d . . . . .
H4 H 0.214269 0.829088 0.434857 0.041 Uiso 1 1 calc R U . . .
C5 C 0.1862(2) 0.73675(11) 0.43524(10) 0.0257(5) Uani 1 1 d . . . . .
C6 C 0.1296(2) 0.72114(11) 0.49178(11) 0.0262(6) Uani 1 1 d . . . . .
H6A H 0.056498 0.712407 0.482361 0.031 Uiso 1 1 calc R U . . .
H6B H 0.131961 0.755680 0.520208 0.031 Uiso 1 1 calc R U . . .
C7 C 0.1004(2) 0.68920(14) 0.24691(12) 0.0367(7) Uani 1 1 d . . . . .
C8 C 0.0222(3) 0.65612(16) 0.20654(14) 0.0521(9) Uani 1 1 d . . . . .
H8A H 0.055951 0.643530 0.168974 0.063 Uiso 1 1 calc R U . . .
H8B H -0.035281 0.683320 0.197094 0.063 Uiso 1 1 calc R U . . .
H8C H -0.004050 0.620429 0.227811 0.063 Uiso 1 1 calc R U . . .
C9 C 0.1514(3) 0.74064(15) 0.21088(14) 0.0506(9) Uani 1 1 d . . . . .
H9A H 0.097990 0.767313 0.194447 0.061 Uiso 1 1 calc R U . . .
H9B H 0.191936 0.723503 0.177645 0.061 Uiso 1 1 calc R U . . .
H9C H 0.196853 0.763858 0.237608 0.061 Uiso 1 1 calc R U . . .
C10 C 0.0397(2) 0.71872(14) 0.29898(12) 0.0409(7) Uani 1 1 d . . . . .
H10A H 0.006061 0.687229 0.323082 0.049 Uiso 1 1 calc R U . . .
H10B H -0.012607 0.745986 0.282323 0.049 Uiso 1 1 calc R U . . .
H10C H 0.087199 0.741724 0.324660 0.049 Uiso 1 1 calc R U . . .
C11 C 0.2490(2) 0.58233(13) 0.21762(11) 0.0338(6) Uani 1 1 d . . . . .
C12 C 0.3420(2) 0.54912(15) 0.24464(13) 0.0438(8) Uani 1 1 d . . . . .
H12A H 0.322099 0.530320 0.283001 0.053 Uiso 1 1 calc R U . . .
H12B H 0.398054 0.578006 0.251734 0.053 Uiso 1 1 calc R U . . .
H12C H 0.365407 0.517829 0.216432 0.053 Uiso 1 1 calc R U . . .
C13 C 0.1685(3) 0.53462(14) 0.19964(13) 0.0460(8) Uani 1 1 d . . . . .
H13A H 0.199754 0.505531 0.171708 0.055 Uiso 1 1 calc R U . . .
H13B H 0.109970 0.554498 0.179877 0.055 Uiso 1 1 calc R U . . .
H13C H 0.144430 0.513411 0.235881 0.055 Uiso 1 1 calc R U . . .
C14 C 0.2850(3) 0.61670(15) 0.16175(12) 0.0470(8) Uani 1 1 d . . . . .
H14A H 0.332552 0.648915 0.173873 0.056 Uiso 1 1 calc R U . . .
H14B H 0.225227 0.634433 0.141221 0.056 Uiso 1 1 calc R U . . .
H14C H 0.320300 0.588830 0.134227 0.056 Uiso 1 1 calc R U . . .
C15 C 0.1055(2) 0.64431(13) 0.59644(12) 0.0362(7) Uani 1 1 d . . . . .
C16 C -0.0075(2) 0.64209(15) 0.57674(13) 0.0448(8) Uani 1 1 d . . . . .
H16A H -0.029135 0.682268 0.563047 0.054 Uiso 1 1 calc R U . . .
H16B H -0.050432 0.629517 0.610949 0.054 Uiso 1 1 calc R U . . .
H16C H -0.015295 0.613058 0.543595 0.054 Uiso 1 1 calc R U . . .
C17 C 0.1155(3) 0.69521(15) 0.64325(13) 0.0485(8) Uani 1 1 d . . . . .
H17A H 0.186406 0.696505 0.658546 0.058 Uiso 1 1 calc R U . . .
H17B H 0.067956 0.687641 0.676838 0.058 Uiso 1 1 calc R U . . .
H17C H 0.098522 0.733974 0.624254 0.058 Uiso 1 1 calc R U . . .
C18 C 0.1318(3) 0.58365(14) 0.62724(14) 0.0487(8) Uani 1 1 d . . . . .
H18A H 0.202854 0.584904 0.642320 0.058 Uiso 1 1 calc R U . . .
H18B H 0.124841 0.550724 0.597892 0.058 Uiso 1 1 calc R U . . .
H18C H 0.084453 0.576805 0.661070 0.058 Uiso 1 1 calc R U . . .
C19 C 0.3226(2) 0.68279(11) 0.55055(11) 0.0310(6) Uani 1 1 d . . . . .
C20 C 0.3269(2) 0.75019(12) 0.56788(13) 0.0382(7) Uani 1 1 d . . . . .
H20A H 0.279333 0.757874 0.601411 0.046 Uiso 1 1 calc R U . . .
H20B H 0.306981 0.774856 0.532995 0.046 Uiso 1 1 calc R U . . .
H20C H 0.397256 0.760707 0.580246 0.046 Uiso 1 1 calc R U . . .
C21 C 0.3661(2) 0.64539(13) 0.60266(13) 0.0407(7) Uani 1 1 d . . . . .
H21A H 0.326306 0.653548 0.639443 0.049 Uiso 1 1 calc R U . . .
H21B H 0.438415 0.656313 0.609317 0.049 Uiso 1 1 calc R U . . .
H21C H 0.361326 0.602320 0.592672 0.049 Uiso 1 1 calc R U . . .
C22 C 0.3944(2) 0.67390(13) 0.49566(12) 0.0333(6) Uani 1 1 d . . . . .
H22A H 0.388945 0.632133 0.481235 0.040 Uiso 1 1 calc R U . . .
H22B H 0.465740 0.682252 0.507610 0.040 Uiso 1 1 calc R U . . .
H22C H 0.374014 0.701669 0.463279 0.040 Uiso 1 1 calc R U . . .
C23 C 0.0109(2) 0.56634(14) 0.36111(14) 0.0392(7) Uani 1 1 d . . . . .
H23 H -0.019007 0.586002 0.327197 0.047 Uiso 1 1 calc R U . . .
C24 C -0.0007(2) 0.58388(13) 0.42204(14) 0.0369(7) Uani 1 1 d . . . . .
H24 H -0.039123 0.617387 0.436687 0.044 Uiso 1 1 calc R U . . .
C25 C 0.0557(2) 0.54211(13) 0.45700(13) 0.0367(7) Uani 1 1 d . . . . .
H25 H 0.062003 0.542703 0.499779 0.044 Uiso 1 1 calc R U . . .
C26 C 0.1007(2) 0.49994(13) 0.41864(14) 0.0381(7) Uani 1 1 d . . . . .
H26 H 0.142264 0.466706 0.430731 0.046 Uiso 1 1 calc R U . . .
C27 C 0.0743(2) 0.51480(13) 0.35912(14) 0.0393(7) Uani 1 1 d . . . . .
H27 H 0.095401 0.493835 0.323747 0.047 Uiso 1 1 calc R U . . .
C28 C 0.5743(2) 0.46823(12) 0.31520(11) 0.0291(6) Uani 1 1 d . . . . .
H28A H 0.518085 0.494277 0.299743 0.035 Uiso 1 1 calc R U . . .
H28B H 0.634385 0.471851 0.287834 0.035 Uiso 1 1 calc R U . . .
C29 C 0.5395(2) 0.40405(13) 0.31920(11) 0.0311(6) Uani 1 1 d . . . . .
C30 C 0.5631(2) 0.35487(14) 0.28405(13) 0.0445(8) Uani 1 1 d . . . . .
H30 H 0.603907 0.354677 0.248386 0.053 Uiso 1 1 calc R U . . .
C31 C 0.5147(3) 0.30442(14) 0.31147(14) 0.0472(8) Uani 1 1 d . . . . .
H31 H 0.517036 0.263788 0.297622 0.057 Uiso 1 1 calc R U . . .
C32 C 0.4640(2) 0.32503(13) 0.36149(13) 0.0363(7) Uani 1 1 d . . . . .
C33 C 0.3918(2) 0.29298(12) 0.40337(13) 0.0361(7) Uani 1 1 d . . . . .
H33A H 0.424527 0.287737 0.443439 0.043 Uiso 1 1 calc R U . . .
H33B H 0.374914 0.252484 0.387077 0.043 Uiso 1 1 calc R U . . .
C34 C 0.6416(2) 0.57336(11) 0.38665(12) 0.0280(6) Uani 1 1 d . . . . .
C35 C 0.5459(2) 0.60466(13) 0.35991(15) 0.0424(7) Uani 1 1 d . . . . .
H35A H 0.538508 0.593276 0.317326 0.051 Uiso 1 1 calc R U . . .
H35B H 0.553989 0.648601 0.363043 0.051 Uiso 1 1 calc R U . . .
H35C H 0.484413 0.592041 0.382326 0.051 Uiso 1 1 calc R U . . .
C36 C 0.6601(3) 0.60092(14) 0.44958(13) 0.0457(8) Uani 1 1 d . . . . .
H36A H 0.721823 0.582774 0.467605 0.055 Uiso 1 1 calc R U . . .
H36B H 0.600345 0.592866 0.475472 0.055 Uiso 1 1 calc R U . . .
H36C H 0.669968 0.644681 0.445749 0.055 Uiso 1 1 calc R U . . .
C37 C 0.7327(2) 0.58774(13) 0.34587(14) 0.0402(7) Uani 1 1 d . . . . .
H37A H 0.738323 0.631630 0.340770 0.048 Uiso 1 1 calc R U . . .
H37B H 0.722380 0.568693 0.306342 0.048 Uiso 1 1 calc R U . . .
H37C H 0.796178 0.572179 0.364212 0.048 Uiso 1 1 calc R U . . .
C38 C 0.7324(2) 0.44508(13) 0.40741(13) 0.0341(6) Uani 1 1 d . . . . .
C39 C 0.7938(2) 0.47345(14) 0.45952(14) 0.0466(8) Uani 1 1 d . . . . .
H39A H 0.822714 0.512224 0.446391 0.056 Uiso 1 1 calc R U . . .
H39B H 0.849888 0.446204 0.471326 0.056 Uiso 1 1 calc R U . . .
H39C H 0.747971 0.480048 0.494121 0.056 Uiso 1 1 calc R U . . .
C40 C 0.8020(2) 0.43928(14) 0.35175(16) 0.0488(8) Uani 1 1 d . . . . .
H40A H 0.822062 0.479653 0.337806 0.059 Uiso 1 1 calc R U . . .
H40B H 0.764496 0.418334 0.319488 0.059 Uiso 1 1 calc R U . . .
H40C H 0.863852 0.416156 0.362344 0.059 Uiso 1 1 calc R U . . .
C41 C 0.7026(2) 0.38037(12) 0.42634(14) 0.0409(7) Uani 1 1 d . . . . .
H41A H 0.764598 0.358361 0.438947 0.049 Uiso 1 1 calc R U . . .
H41B H 0.670642 0.359505 0.392059 0.049 Uiso 1 1 calc R U . . .
H41C H 0.653704 0.382091 0.460053 0.049 Uiso 1 1 calc R U . . .
C42 C 0.2149(2) 0.33453(13) 0.33210(12) 0.0363(7) Uani 1 1 d . . . . .
C43 C 0.2634(2) 0.38651(13) 0.29543(12) 0.0396(7) Uani 1 1 d . . . . .
H43A H 0.228776 0.389742 0.256198 0.048 Uiso 1 1 calc R U . . .
H43B H 0.336915 0.378286 0.289127 0.048 Uiso 1 1 calc R U . . .
H43C H 0.255457 0.424552 0.317647 0.048 Uiso 1 1 calc R U . . .
C44 C 0.0990(2) 0.34744(15) 0.33510(15) 0.0487(8) Uani 1 1 d . . . . .
H44A H 0.072116 0.353092 0.294098 0.058 Uiso 1 1 calc R U . . .
H44B H 0.087089 0.384204 0.358805 0.058 Uiso 1 1 calc R U . . .
H44C H 0.063751 0.313302 0.354307 0.058 Uiso 1 1 calc R U . . .
C45 C 0.2329(3) 0.27509(14) 0.29819(14) 0.0457(8) Uani 1 1 d . . . . .
H45A H 0.203857 0.241521 0.321543 0.055 Uiso 1 1 calc R U . . .
H45B H 0.307169 0.268712 0.292785 0.055 Uiso 1 1 calc R U . . .
H45C H 0.199360 0.276993 0.258560 0.055 Uiso 1 1 calc R U . . .
C46 C 0.1923(3) 0.29008(13) 0.46419(13) 0.0432(7) Uani 1 1 d . . . . .
C47 C 0.2578(3) 0.27487(15) 0.51946(13) 0.0575(10) Uani 1 1 d . . . . .
H47A H 0.289669 0.311875 0.535090 0.069 Uiso 1 1 calc R U . . .
H47B H 0.311785 0.246061 0.507990 0.069 Uiso 1 1 calc R U . . .
H47C H 0.214004 0.256910 0.550771 0.069 Uiso 1 1 calc R U . . .
C48 C 0.0982(3) 0.32762(17) 0.48617(16) 0.0632(10) Uani 1 1 d . . . . .
H48A H 0.050474 0.333899 0.452417 0.076 Uiso 1 1 calc R U . . .
H48B H 0.122007 0.366867 0.501283 0.076 Uiso 1 1 calc R U . . .
H48C H 0.062882 0.305786 0.518664 0.076 Uiso 1 1 calc R U . . .
C49 C 0.1533(3) 0.22994(15) 0.43796(16) 0.0568(9) Uani 1 1 d . . . . .
H49A H 0.106236 0.238061 0.404295 0.068 Uiso 1 1 calc R U . . .
H49B H 0.116881 0.207260 0.469444 0.068 Uiso 1 1 calc R U . . .
H49C H 0.212084 0.206150 0.423427 0.068 Uiso 1 1 calc R U . . .
C50 C 0.5156(2) 0.44545(15) 0.53314(11) 0.0403(7) Uani 1 1 d . . . . .
H50 H 0.588004 0.439269 0.535693 0.048 Uiso 1 1 calc R U . . .
C51 C 0.4408(3) 0.40043(13) 0.53274(11) 0.0390(7) Uani 1 1 d . . . . .
H51 H 0.452622 0.358085 0.534577 0.047 Uiso 1 1 calc R U . . .
C52 C 0.3436(2) 0.42950(13) 0.52907(11) 0.0341(7) Uani 1 1 d . . . . .
H52 H 0.278467 0.409886 0.527990 0.041 Uiso 1 1 calc R U . . .
C53 C 0.3598(2) 0.49125(13) 0.52732(11) 0.0325(6) Uani 1 1 d . . . . .
H53 H 0.307666 0.521378 0.525258 0.039 Uiso 1 1 calc R U . . .
C54 C 0.4657(2) 0.50161(13) 0.52912(11) 0.0366(7) Uani 1 1 d . . . . .
H54 H 0.498508 0.540005 0.527850 0.044 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 N3 1.816(2) . ?
Ti1 N1 2.138(2) . ?
Ti1 C24 2.398(3) . ?
Ti1 C23 2.398(3) . ?
Ti1 C25 2.399(3) . ?
Ti1 C27 2.404(3) . ?
Ti1 C26 2.415(3) . ?
Ti1 P1 2.7234(8) . ?
Ti2 N4 1.808(2) . ?
Ti2 N2 2.140(2) . ?
Ti2 C52 2.376(3) . ?
Ti2 C51 2.398(3) . ?
Ti2 C53 2.400(2) . ?
Ti2 C54 2.413(3) . ?
Ti2 C50 2.425(3) . ?
Ti2 P3 2.6928(8) . ?
P1 C1 1.836(3) . ?
P1 C11 1.894(3) . ?
P1 C7 1.913(3) . ?
P2 C6 1.838(2) . ?
P2 C19 1.905(3) . ?
P2 C15 1.907(3) . ?
P3 C28 1.838(2) . ?
P3 C34 1.889(3) . ?
P3 C38 1.907(3) . ?
P4 C33 1.839(3) . ?
P4 C42 1.902(3) . ?
P4 C46 1.907(3) . ?
N1 C2 1.373(3) . ?
N1 C5 1.388(3) . ?
N2 C29 1.382(3) . ?
N2 C32 1.392(3) . ?
N3 N4 1.247(3) . ?
C1 C2 1.499(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.371(4) . ?
C3 C4 1.415(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.490(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.537(4) . ?
C7 C9 1.539(4) . ?
C7 C10 1.540(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.524(4) . ?
C11 C12 1.534(4) . ?
C11 C13 1.536(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.530(4) . ?
C15 C17 1.535(4) . ?
C15 C18 1.543(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.527(4) . ?
C19 C20 1.540(4) . ?
C19 C22 1.543(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C27 1.406(4) . ?
C23 C24 1.411(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.410(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.400(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.492(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.372(4) . ?
C30 C31 1.417(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.365(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.496(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C37 1.520(4) . ?
C34 C35 1.539(4) . ?
C34 C36 1.539(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40 1.532(4) . ?
C38 C39 1.535(4) . ?
C38 C41 1.541(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C44 1.530(4) . ?
C42 C45 1.532(4) . ?
C42 C43 1.542(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.526(5) . ?
C46 C49 1.537(4) . ?
C46 C48 1.554(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.390(4) . ?
C50 C54 1.403(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.417(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.382(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.394(4) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ti1 N1 108.88(9) . . ?
N3 Ti1 C24 139.03(10) . . ?
N1 Ti1 C24 109.68(9) . . ?
N3 Ti1 C23 128.06(10) . . ?
N1 Ti1 C23 118.38(10) . . ?
C24 Ti1 C23 34.23(10) . . ?
N3 Ti1 C25 106.97(10) . . ?
N1 Ti1 C25 130.23(9) . . ?
C24 Ti1 C25 34.19(10) . . ?
C23 Ti1 C25 56.34(10) . . ?
N3 Ti1 C27 94.24(10) . . ?
N1 Ti1 C27 149.14(9) . . ?
C24 Ti1 C27 56.82(10) . . ?
C23 Ti1 C27 34.05(10) . . ?
C25 Ti1 C27 56.18(10) . . ?
N3 Ti1 C26 83.16(10) . . ?
N1 Ti1 C26 163.76(9) . . ?
C24 Ti1 C26 56.46(10) . . ?
C23 Ti1 C26 56.17(10) . . ?
C25 Ti1 C26 33.55(10) . . ?
C27 Ti1 C26 33.77(10) . . ?
N3 Ti1 P1 94.27(7) . . ?
N1 Ti1 P1 71.43(5) . . ?
C24 Ti1 P1 110.65(7) . . ?
C23 Ti1 P1 81.95(7) . . ?
C25 Ti1 P1 138.00(7) . . ?
C27 Ti1 P1 87.13(7) . . ?
C26 Ti1 P1 119.65(8) . . ?
N4 Ti2 N2 109.14(9) . . ?
N4 Ti2 C52 104.63(10) . . ?
N2 Ti2 C52 129.59(9) . . ?
N4 Ti2 C51 137.77(10) . . ?
N2 Ti2 C51 109.03(9) . . ?
C52 Ti2 C51 34.53(10) . . ?
N4 Ti2 C53 82.67(9) . . ?
N2 Ti2 C53 163.19(9) . . ?
C52 Ti2 C53 33.64(9) . . ?
C51 Ti2 C53 56.48(10) . . ?
N4 Ti2 C54 96.50(10) . . ?
N2 Ti2 C54 148.56(10) . . ?
C52 Ti2 C54 55.97(10) . . ?
C51 Ti2 C54 56.10(10) . . ?
C53 Ti2 C54 33.66(9) . . ?
N4 Ti2 C50 130.20(10) . . ?
N2 Ti2 C50 117.87(9) . . ?
C52 Ti2 C50 56.15(10) . . ?
C51 Ti2 C50 33.50(10) . . ?
C53 Ti2 C50 55.97(10) . . ?
C54 Ti2 C50 33.72(10) . . ?
N4 Ti2 P3 93.57(7) . . ?
N2 Ti2 P3 72.69(6) . . ?
C52 Ti2 P3 140.93(7) . . ?
C51 Ti2 P3 114.52(8) . . ?
C53 Ti2 P3 119.60(7) . . ?
C54 Ti2 P3 88.24(7) . . ?
C50 Ti2 P3 85.66(8) . . ?
C1 P1 C11 104.14(12) . . ?
C1 P1 C7 103.03(13) . . ?
C11 P1 C7 109.95(12) . . ?
C1 P1 Ti1 91.65(8) . . ?
C11 P1 Ti1 123.12(9) . . ?
C7 P1 Ti1 119.08(9) . . ?
C6 P2 C19 103.73(12) . . ?
C6 P2 C15 100.97(12) . . ?
C19 P2 C15 109.39(13) . . ?
C28 P3 C34 104.36(12) . . ?
C28 P3 C38 103.31(13) . . ?
C34 P3 C38 109.82(12) . . ?
C28 P3 Ti2 91.47(9) . . ?
C34 P3 Ti2 123.04(8) . . ?
C38 P3 Ti2 119.13(9) . . ?
C33 P4 C42 103.13(13) . . ?
C33 P4 C46 102.20(14) . . ?
C42 P4 C46 108.82(14) . . ?
C2 N1 C5 105.6(2) . . ?
C2 N1 Ti1 124.31(16) . . ?
C5 N1 Ti1 130.06(16) . . ?
C29 N2 C32 105.6(2) . . ?
C29 N2 Ti2 123.12(17) . . ?
C32 N2 Ti2 131.19(18) . . ?
N4 N3 Ti1 158.91(18) . . ?
N3 N4 Ti2 159.63(18) . . ?
C2 C1 P1 104.72(18) . . ?
C2 C1 H1A 110.8 . . ?
P1 C1 H1A 110.8 . . ?
C2 C1 H1B 110.8 . . ?
P1 C1 H1B 110.8 . . ?
H1A C1 H1B 108.9 . . ?
C3 C2 N1 110.8(2) . . ?
C3 C2 C1 130.3(2) . . ?
N1 C2 C1 118.6(2) . . ?
C2 C3 C4 106.4(2) . . ?
C2 C3 H3 126.8 . . ?
C4 C3 H3 126.8 . . ?
C5 C4 C3 107.0(2) . . ?
C5 C4 H4 126.5 . . ?
C3 C4 H4 126.5 . . ?
C4 C5 N1 110.3(2) . . ?
C4 C5 C6 130.1(2) . . ?
N1 C5 C6 119.5(2) . . ?
C5 C6 P2 109.18(17) . . ?
C5 C6 H6A 109.8 . . ?
P2 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
P2 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C8 C7 C9 109.6(2) . . ?
C8 C7 C10 107.4(2) . . ?
C9 C7 C10 107.1(2) . . ?
C8 C7 P1 110.4(2) . . ?
C9 C7 P1 112.9(2) . . ?
C10 C7 P1 109.23(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C12 108.3(2) . . ?
C14 C11 C13 109.9(2) . . ?
C12 C11 C13 107.8(2) . . ?
C14 C11 P1 113.4(2) . . ?
C12 C11 P1 106.04(18) . . ?
C13 C11 P1 111.1(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 107.2(2) . . ?
C16 C15 C18 108.0(3) . . ?
C17 C15 C18 108.7(2) . . ?
C16 C15 P2 108.84(18) . . ?
C17 C15 P2 114.3(2) . . ?
C18 C15 P2 109.50(19) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C20 108.8(2) . . ?
C21 C19 C22 107.6(2) . . ?
C20 C19 C22 107.3(2) . . ?
C21 C19 P2 111.41(19) . . ?
C20 C19 P2 114.83(19) . . ?
C22 C19 P2 106.50(17) . . ?
C19 C20 H20A 109.5 . . ?
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 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C27 C23 C24 108.4(3) . . ?
C27 C23 Ti1 73.23(16) . . ?
C24 C23 Ti1 72.88(16) . . ?
C27 C23 H23 125.8 . . ?
C24 C23 H23 125.8 . . ?
Ti1 C23 H23 119.9 . . ?
C25 C24 C23 106.8(3) . . ?
C25 C24 Ti1 72.95(15) . . ?
C23 C24 Ti1 72.89(16) . . ?
C25 C24 H24 126.6 . . ?
C23 C24 H24 126.6 . . ?
Ti1 C24 H24 119.5 . . ?
C26 C25 C24 108.8(3) . . ?
C26 C25 Ti1 73.86(16) . . ?
C24 C25 Ti1 72.87(15) . . ?
C26 C25 H25 125.6 . . ?
C24 C25 H25 125.6 . . ?
Ti1 C25 H25 119.5 . . ?
C25 C26 C27 108.3(3) . . ?
C25 C26 Ti1 72.58(16) . . ?
C27 C26 Ti1 72.70(16) . . ?
C25 C26 H26 125.8 . . ?
C27 C26 H26 125.8 . . ?
Ti1 C26 H26 120.6 . . ?
C26 C27 C23 107.7(3) . . ?
C26 C27 Ti1 73.53(16) . . ?
C23 C27 Ti1 72.72(16) . . ?
C26 C27 H27 126.2 . . ?
C23 C27 H27 126.2 . . ?
Ti1 C27 H27 119.5 . . ?
C29 C28 P3 105.80(17) . . ?
C29 C28 H28A 110.6 . . ?
P3 C28 H28A 110.6 . . ?
C29 C28 H28B 110.6 . . ?
P3 C28 H28B 110.6 . . ?
H28A C28 H28B 108.7 . . ?
C30 C29 N2 110.6(2) . . ?
C30 C29 C28 130.8(2) . . ?
N2 C29 C28 118.5(2) . . ?
C29 C30 C31 106.4(3) . . ?
C29 C30 H30 126.8 . . ?
C31 C30 H30 126.8 . . ?
C32 C31 C30 107.3(3) . . ?
C32 C31 H31 126.4 . . ?
C30 C31 H31 126.4 . . ?
C31 C32 N2 110.1(3) . . ?
C31 C32 C33 130.2(3) . . ?
N2 C32 C33 119.4(2) . . ?
C32 C33 P4 108.66(19) . . ?
C32 C33 H33A 110.0 . . ?
P4 C33 H33A 110.0 . . ?
C32 C33 H33B 110.0 . . ?
P4 C33 H33B 110.0 . . ?
H33A C33 H33B 108.3 . . ?
C37 C34 C35 107.7(2) . . ?
C37 C34 C36 109.4(2) . . ?
C35 C34 C36 107.2(2) . . ?
C37 C34 P3 114.51(19) . . ?
C35 C34 P3 106.76(18) . . ?
C36 C34 P3 110.92(18) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40 C38 C39 109.5(2) . . ?
C40 C38 C41 106.8(2) . . ?
C39 C38 C41 107.8(2) . . ?
C40 C38 P3 113.4(2) . . ?
C39 C38 P3 110.3(2) . . ?
C41 C38 P3 108.91(18) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C44 C42 C45 109.4(2) . . ?
C44 C42 C43 106.5(2) . . ?
C45 C42 C43 108.7(2) . . ?
C44 C42 P4 110.1(2) . . ?
C45 C42 P4 115.1(2) . . ?
C43 C42 P4 106.66(18) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 C49 107.1(3) . . ?
C47 C46 C48 107.7(3) . . ?
C49 C46 C48 108.8(3) . . ?
C47 C46 P4 108.2(2) . . ?
C49 C46 P4 115.5(2) . . ?
C48 C46 P4 109.2(2) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C54 108.2(3) . . ?
C51 C50 Ti2 72.17(15) . . ?
C54 C50 Ti2 72.68(15) . . ?
C51 C50 H50 125.9 . . ?
C54 C50 H50 125.9 . . ?
Ti2 C50 H50 121.0 . . ?
C50 C51 C52 107.2(3) . . ?
C50 C51 Ti2 74.32(16) . . ?
C52 C51 Ti2 71.89(15) . . ?
C50 C51 H51 126.4 . . ?
C52 C51 H51 126.4 . . ?
Ti2 C51 H51 119.3 . . ?
C53 C52 C51 108.4(3) . . ?
C53 C52 Ti2 74.13(15) . . ?
C51 C52 Ti2 73.59(15) . . ?
C53 C52 H52 125.8 . . ?
C51 C52 H52 125.8 . . ?
Ti2 C52 H52 118.4 . . ?
C52 C53 C54 108.1(3) . . ?
C52 C53 Ti2 72.23(15) . . ?
C54 C53 Ti2 73.70(15) . . ?
C52 C53 H53 125.9 . . ?
C54 C53 H53 125.9 . . ?
Ti2 C53 H53 119.9 . . ?
C53 C54 C50 108.1(3) . . ?
C53 C54 Ti2 72.64(15) . . ?
C50 C54 Ti2 73.60(15) . . ?
C53 C54 H54 125.9 . . ?
C50 C54 H54 125.9 . . ?
Ti2 C54 H54 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ti1 N3 N4 167.2(5) . . . . ?
C24 Ti1 N3 N4 7.7(6) . . . . ?
C23 Ti1 N3 N4 -37.9(5) . . . . ?
C25 Ti1 N3 N4 22.3(5) . . . . ?
C27 Ti1 N3 N4 -33.6(5) . . . . ?
C26 Ti1 N3 N4 -1.6(5) . . . . ?
P1 Ti1 N3 N4 -121.0(5) . . . . ?
Ti1 N3 N4 Ti2 -73.6(8) . . . . ?
N2 Ti2 N4 N3 167.6(5) . . . . ?
C52 Ti2 N4 N3 25.6(5) . . . . ?
C51 Ti2 N4 N3 13.9(6) . . . . ?
C53 Ti2 N4 N3 -0.1(5) . . . . ?
C54 Ti2 N4 N3 -30.9(5) . . . . ?
C50 Ti2 N4 N3 -32.2(6) . . . . ?
P3 Ti2 N4 N3 -119.5(5) . . . . ?
C11 P1 C1 C2 -175.38(17) . . . . ?
C7 P1 C1 C2 69.82(19) . . . . ?
Ti1 P1 C1 C2 -50.57(16) . . . . ?
C5 N1 C2 C3 -1.0(3) . . . . ?
Ti1 N1 C2 C3 176.60(18) . . . . ?
C5 N1 C2 C1 -175.6(2) . . . . ?
Ti1 N1 C2 C1 2.1(3) . . . . ?
P1 C1 C2 C3 -131.9(3) . . . . ?
P1 C1 C2 N1 41.4(3) . . . . ?
N1 C2 C3 C4 1.1(3) . . . . ?
C1 C2 C3 C4 174.8(3) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C3 C4 C5 N1 0.1(3) . . . . ?
C3 C4 C5 C6 175.3(3) . . . . ?
C2 N1 C5 C4 0.6(3) . . . . ?
Ti1 N1 C5 C4 -176.88(18) . . . . ?
C2 N1 C5 C6 -175.2(2) . . . . ?
Ti1 N1 C5 C6 7.4(3) . . . . ?
C4 C5 C6 P2 -131.3(3) . . . . ?
N1 C5 C6 P2 43.5(3) . . . . ?
C19 P2 C6 C5 66.6(2) . . . . ?
C15 P2 C6 C5 179.87(19) . . . . ?
C1 P1 C11 C14 -60.4(2) . . . . ?
C7 P1 C11 C14 49.4(2) . . . . ?
Ti1 P1 C11 C14 -161.96(17) . . . . ?
C1 P1 C11 C12 58.3(2) . . . . ?
C7 P1 C11 C12 168.1(2) . . . . ?
Ti1 P1 C11 C12 -43.2(2) . . . . ?
C1 P1 C11 C13 175.17(19) . . . . ?
C7 P1 C11 C13 -75.0(2) . . . . ?
Ti1 P1 C11 C13 73.7(2) . . . . ?
C27 C23 C24 C25 -0.4(3) . . . . ?
Ti1 C23 C24 C25 -65.58(19) . . . . ?
C27 C23 C24 Ti1 65.1(2) . . . . ?
C23 C24 C25 C26 -0.1(3) . . . . ?
Ti1 C24 C25 C26 -65.65(19) . . . . ?
C23 C24 C25 Ti1 65.54(19) . . . . ?
C24 C25 C26 C27 0.6(3) . . . . ?
Ti1 C25 C26 C27 -64.4(2) . . . . ?
C24 C25 C26 Ti1 65.00(19) . . . . ?
C25 C26 C27 C23 -0.9(3) . . . . ?
Ti1 C26 C27 C23 -65.2(2) . . . . ?
C25 C26 C27 Ti1 64.31(19) . . . . ?
C24 C23 C27 C26 0.8(3) . . . . ?
Ti1 C23 C27 C26 65.7(2) . . . . ?
C24 C23 C27 Ti1 -64.9(2) . . . . ?
C34 P3 C28 C29 -175.04(18) . . . . ?
C38 P3 C28 C29 70.1(2) . . . . ?
Ti2 P3 C28 C29 -50.32(17) . . . . ?
C32 N2 C29 C30 -0.3(3) . . . . ?
Ti2 N2 C29 C30 177.3(2) . . . . ?
C32 N2 C29 C28 -176.3(2) . . . . ?
Ti2 N2 C29 C28 1.4(3) . . . . ?
P3 C28 C29 C30 -133.8(3) . . . . ?
P3 C28 C29 N2 41.2(3) . . . . ?
N2 C29 C30 C31 0.1(3) . . . . ?
C28 C29 C30 C31 175.4(3) . . . . ?
C29 C30 C31 C32 0.2(4) . . . . ?
C30 C31 C32 N2 -0.4(4) . . . . ?
C30 C31 C32 C33 172.9(3) . . . . ?
C29 N2 C32 C31 0.4(3) . . . . ?
Ti2 N2 C32 C31 -177.0(2) . . . . ?
C29 N2 C32 C33 -173.6(2) . . . . ?
Ti2 N2 C32 C33 9.0(4) . . . . ?
C31 C32 C33 P4 -128.4(3) . . . . ?
N2 C32 C33 P4 44.3(3) . . . . ?
C42 P4 C33 C32 66.4(2) . . . . ?
C46 P4 C33 C32 179.32(19) . . . . ?
C28 P3 C34 C37 -62.6(2) . . . . ?
C38 P3 C34 C37 47.6(2) . . . . ?
Ti2 P3 C34 C37 -164.00(16) . . . . ?
C28 P3 C34 C35 56.5(2) . . . . ?
C38 P3 C34 C35 166.68(19) . . . . ?
Ti2 P3 C34 C35 -44.9(2) . . . . ?
C28 P3 C34 C36 173.0(2) . . . . ?
C38 P3 C34 C36 -76.9(2) . . . . ?
Ti2 P3 C34 C36 71.5(2) . . . . ?
C54 C50 C51 C52 -0.6(3) . . . . ?
Ti2 C50 C51 C52 -64.85(17) . . . . ?
C54 C50 C51 Ti2 64.23(19) . . . . ?
C50 C51 C52 C53 0.0(3) . . . . ?
Ti2 C51 C52 C53 -66.52(18) . . . . ?
C50 C51 C52 Ti2 66.49(18) . . . . ?
C51 C52 C53 C54 0.7(3) . . . . ?
Ti2 C52 C53 C54 -65.48(19) . . . . ?
C51 C52 C53 Ti2 66.17(18) . . . . ?
C52 C53 C54 C50 -1.1(3) . . . . ?
Ti2 C53 C54 C50 -65.58(19) . . . . ?
C52 C53 C54 Ti2 64.52(18) . . . . ?
C51 C50 C54 C53 1.0(3) . . . . ?
Ti2 C50 C54 C53 64.95(19) . . . . ?
C51 C50 C54 Ti2 -63.90(18) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================
#     End of CIF
#==============================================================================
