# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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. 
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data_pbts150701
_database_code_depnum_ccdc_archive 'CCDC 1427661'
_audit_update_record             
;
2015-09-25 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H82 Li4 N2 P4'
_chemical_formula_sum            'C46 H82 Li4 N2 P4'
_chemical_formula_weight         814.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.4117(13)
_cell_length_b                   8.6059(6)
_cell_length_c                   22.4415(14)
_cell_angle_alpha                90
_cell_angle_beta                 125.229(4)
_cell_angle_gamma                90
_cell_volume                     2589.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4708
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.96

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.175
_shelx_estimated_absorpt_T_min   0.933
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tub'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18475
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.830
_diffrn_reflns_theta_max         28.010
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6245
_reflns_number_gt                4394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0778P)²+2.2709P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6245
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1618
_refine_ls_wR_factor_gt          0.1423
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.88102(16) -0.1978(2) 0.94443(12) 0.0211(5) Uani 1 1 d . . . . .
C2 C 0.96831(17) -0.2919(3) 0.98420(13) 0.0269(5) Uani 1 1 d . . . . .
H2 H 0.9783 -0.3605 1.0211 0.032 Uiso 1 1 calc R U . . .
C3 C 1.03831(18) -0.2826(3) 0.96866(14) 0.0298(6) Uani 1 1 d . . . . .
H3 H 1.0963 -0.3459 0.9947 0.036 Uiso 1 1 calc R U . . .
C4 C 1.02500(18) -0.1823(3) 0.91572(14) 0.0273(5) Uani 1 1 d . . . . .
H4 H 1.0737 -0.1762 0.9056 0.033 Uiso 1 1 calc R U . . .
C5 C 0.93769(16) -0.0881(3) 0.87639(12) 0.0210(5) Uani 1 1 d . . . . .
C6 C 0.81126(16) -0.1976(3) 0.96298(12) 0.0223(5) Uani 1 1 d . . . . .
H6 H 0.8306 -0.2314 1.0097 0.027 Uiso 1 1 calc R U . . .
C7 C 0.61251(18) -0.3181(3) 0.85777(14) 0.0277(5) Uani 1 1 d . . . . .
C8 C 0.6679(2) -0.4124(3) 0.83308(17) 0.0422(7) Uani 1 1 d . . . . .
H8A H 0.7338 -0.4423 0.8759 0.063 Uiso 1 1 calc R U . . .
H8B H 0.6756 -0.3488 0.8004 0.063 Uiso 1 1 calc R U . . .
H8C H 0.6294 -0.5060 0.8073 0.063 Uiso 1 1 calc R U . . .
C9 C 0.5074(2) -0.2836(4) 0.78906(15) 0.0424(7) Uani 1 1 d . . . . .
H9A H 0.4743 -0.3815 0.7647 0.064 Uiso 1 1 calc R U . . .
H9B H 0.5127 -0.2182 0.7557 0.064 Uiso 1 1 calc R U . . .
H9C H 0.4683 -0.2294 0.8030 0.064 Uiso 1 1 calc R U . . .
C10 C 0.6058(2) -0.4162(3) 0.91154(17) 0.0412(7) Uani 1 1 d . . . . .
H10A H 0.5736 -0.5156 0.8888 0.062 Uiso 1 1 calc R U . . .
H10B H 0.5664 -0.3606 0.9249 0.062 Uiso 1 1 calc R U . . .
H10C H 0.6730 -0.4353 0.9554 0.062 Uiso 1 1 calc R U . . .
C11 C 0.64687(18) -0.0210(3) 0.94810(14) 0.0290(5) Uani 1 1 d . . . . .
C12 C 0.5335(2) -0.0022(4) 0.90347(17) 0.0419(7) Uani 1 1 d . . . . .
H12A H 0.5167 0.0771 0.9261 0.063 Uiso 1 1 calc R U . . .
H12B H 0.5031 -0.1014 0.9021 0.063 Uiso 1 1 calc R U . . .
H12C H 0.5080 0.0297 0.8537 0.063 Uiso 1 1 calc R U . . .
C13 C 0.6849(3) -0.0897(4) 1.02299(15) 0.0458(7) Uani 1 1 d . . . . .
H13A H 0.7578 -0.0978 1.0524 0.069 Uiso 1 1 calc R U . . .
H13B H 0.6560 -0.1932 1.0166 0.069 Uiso 1 1 calc R U . . .
H13C H 0.6652 -0.0219 1.0478 0.069 Uiso 1 1 calc R U . . .
C14 C 0.6930(2) 0.1400(3) 0.95895(17) 0.0422(7) Uani 1 1 d . . . . .
H14A H 0.6795 0.2041 0.9885 0.063 Uiso 1 1 calc R U . . .
H14B H 0.6638 0.1894 0.9114 0.063 Uiso 1 1 calc R U . . .
H14C H 0.7652 0.1297 0.9840 0.063 Uiso 1 1 calc R U . . .
C15 C 0.92706(17) 0.0261(3) 0.82638(12) 0.0225(5) Uani 1 1 d . . . . .
C16 C 0.7529(2) 0.0021(3) 0.67583(14) 0.0366(6) Uani 1 1 d . . . . .
C17 C 0.8232(3) -0.0336(6) 0.6549(2) 0.0939(19) Uani 1 1 d . . . . .
H17A H 0.7894 -0.0998 0.6114 0.141 Uiso 1 1 calc R U . . .
H17B H 0.8821 -0.0878 0.6952 0.141 Uiso 1 1 calc R U . . .
H17C H 0.8439 0.0635 0.6445 0.141 Uiso 1 1 calc R U . . .
C18 C 0.6585(2) 0.0764(4) 0.61139(15) 0.0477(8) Uani 1 1 d . . . . .
H18A H 0.6765 0.1639 0.5932 0.071 Uiso 1 1 calc R U . . .
H18B H 0.6172 0.1138 0.6270 0.071 Uiso 1 1 calc R U . . .
H18C H 0.6211 -0.0007 0.5725 0.071 Uiso 1 1 calc R U . . .
C19 C 0.7179(4) -0.1489(4) 0.6923(2) 0.102(2) Uani 1 1 d . . . . .
H19A H 0.6760 -0.1224 0.7089 0.153 Uiso 1 1 calc R U . . .
H19B H 0.7762 -0.2078 0.7305 0.153 Uiso 1 1 calc R U . . .
H19C H 0.6795 -0.2121 0.6479 0.153 Uiso 1 1 calc R U . . .
C20 C 0.83425(19) 0.3208(3) 0.75037(14) 0.0293(5) Uani 1 1 d . . . . .
C21 C 0.8991(3) 0.3947(4) 0.82450(18) 0.0691(12) Uani 1 1 d . . . . .
H21A H 0.9061 0.5059 0.8190 0.104 Uiso 1 1 calc R U . . .
H21B H 0.9650 0.3455 0.8520 0.104 Uiso 1 1 calc R U . . .
H21C H 0.8684 0.3807 0.8508 0.104 Uiso 1 1 calc R U . . .
C22 C 0.8847(3) 0.3358(5) 0.7098(2) 0.0642(10) Uani 1 1 d . . . . .
H22A H 0.8999 0.4453 0.7083 0.096 Uiso 1 1 calc R U . . .
H22B H 0.8396 0.2964 0.6600 0.096 Uiso 1 1 calc R U . . .
H22C H 0.9466 0.2753 0.7356 0.096 Uiso 1 1 calc R U . . .
C23 C 0.7359(2) 0.4100(3) 0.70627(19) 0.0516(8) Uani 1 1 d . . . . .
H23A H 0.7015 0.4011 0.7302 0.077 Uiso 1 1 calc R U . . .
H23B H 0.6937 0.3663 0.6570 0.077 Uiso 1 1 calc R U . . .
H23C H 0.7493 0.5196 0.7034 0.077 Uiso 1 1 calc R U . . .
Li1 Li 0.7454(3) 0.0195(5) 0.8340(2) 0.0318(10) Uani 1 1 d . . . . .
Li2 Li 1.0490(3) 0.1006(6) 0.9411(2) 0.0398(11) Uani 1 1 d . . . . .
P1 P 0.68712(4) -0.13258(7) 0.89680(3) 0.02083(15) Uani 1 1 d . . . . .
P2 P 0.80933(4) 0.11534(7) 0.76394(3) 0.02069(15) Uani 1 1 d . . . . .
N1 N 0.86805(13) -0.0982(2) 0.89176(10) 0.0200(4) Uani 1 1 d . . . . .
H15 H 0.974(2) 0.014(3) 0.8139(15) 0.028(7) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.374(3) . ?
C1 C2 1.425(3) . ?
C1 C6 1.426(3) . ?
C1 Li2 2.284(5) 3_757 ?
C2 C3 1.382(4) . ?
C2 Li2 2.481(6) 3_757 ?
C2 H2 0.9500 . ?
C3 C4 1.380(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.425(3) . ?
C4 Li2 2.480(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.374(3) . ?
C5 C15 1.425(3) . ?
C5 Li2 2.241(5) . ?
C6 P1 1.783(2) . ?
C6 Li2 2.212(5) 3_757 ?
C6 H6 0.9500 . ?
C7 C10 1.528(4) . ?
C7 C8 1.540(4) . ?
C7 C9 1.540(3) . ?
C7 P1 1.892(2) . ?
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 1.530(4) . ?
C11 C12 1.530(4) . ?
C11 C13 1.534(4) . ?
C11 P1 1.887(3) . ?
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 P2 1.778(2) . ?
C15 Li2 2.258(5) . ?
C15 H15 0.96(3) . ?
C16 C17 1.508(5) . ?
C16 C18 1.521(4) . ?
C16 C19 1.549(5) . ?
C16 P2 1.898(3) . ?
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 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.504(4) . ?
C20 C23 1.526(4) . ?
C20 C22 1.549(4) . ?
C20 P2 1.879(3) . ?
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 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
Li1 N1 1.936(4) . ?
Li1 P2 2.481(4) . ?
Li1 P1 2.484(4) . ?
Li2 C6 2.212(5) 3_757 ?
Li2 C1 2.284(5) 3_757 ?
Li2 C2 2.481(6) 3_757 ?

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 C1 C2 119.7(2) . . ?
N1 C1 C6 119.9(2) . . ?
C2 C1 C6 120.3(2) . . ?
N1 C1 Li2 117.87(19) . 3_757 ?
C2 C1 Li2 80.34(19) . 3_757 ?
C6 C1 Li2 68.79(18) . 3_757 ?
C3 C2 C1 119.4(2) . . ?
C3 C2 Li2 124.6(2) . 3_757 ?
C1 C2 Li2 65.18(17) . 3_757 ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
Li2 C2 H2 81.6 3_757 . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.5(2) . . ?
C3 C4 Li2 119.4(2) . . ?
C5 C4 Li2 63.47(17) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
Li2 C4 H4 87.5 . . ?
N1 C5 C15 120.0(2) . . ?
N1 C5 C4 119.6(2) . . ?
C15 C5 C4 120.2(2) . . ?
N1 C5 Li2 111.6(2) . . ?
C15 C5 Li2 72.17(18) . . ?
C4 C5 Li2 81.9(2) . . ?
C1 C6 P1 118.77(16) . . ?
C1 C6 Li2 74.27(18) . 3_757 ?
P1 C6 Li2 137.51(19) . 3_757 ?
C1 C6 H6 120.6 . . ?
P1 C6 H6 120.6 . . ?
Li2 C6 H6 62.8 3_757 . ?
C10 C7 C8 108.6(2) . . ?
C10 C7 C9 110.3(2) . . ?
C8 C7 C9 107.1(2) . . ?
C10 C7 P1 115.02(18) . . ?
C8 C7 P1 104.63(17) . . ?
C9 C7 P1 110.68(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 108.2(2) . . ?
C14 C11 C13 108.9(2) . . ?
C12 C11 C13 109.3(2) . . ?
C14 C11 P1 104.04(18) . . ?
C12 C11 P1 112.09(18) . . ?
C13 C11 P1 114.08(19) . . ?
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 . . ?
C5 C15 P2 120.15(17) . . ?
C5 C15 Li2 70.91(18) . . ?
P2 C15 Li2 128.42(19) . . ?
C5 C15 H15 113.6(16) . . ?
P2 C15 H15 120.2(16) . . ?
Li2 C15 H15 91.7(16) . . ?
C17 C16 C18 109.4(3) . . ?
C17 C16 C19 111.0(4) . . ?
C18 C16 C19 105.4(3) . . ?
C17 C16 P2 115.3(2) . . ?
C18 C16 P2 113.1(2) . . ?
C19 C16 P2 102.0(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C23 108.3(3) . . ?
C21 C20 C22 109.7(3) . . ?
C23 C20 C22 107.5(3) . . ?
C21 C20 P2 107.44(19) . . ?
C23 C20 P2 109.29(18) . . ?
C22 C20 P2 114.4(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 Li1 P2 86.67(16) . . ?
N1 Li1 P1 86.33(16) . . ?
P2 Li1 P1 167.6(2) . . ?
C6 Li2 C5 154.6(3) 3_757 . ?
C6 Li2 C15 163.0(3) 3_757 . ?
C5 Li2 C15 36.92(11) . . ?
C6 Li2 C1 36.94(11) 3_757 3_757 ?
C5 Li2 C1 133.4(2) . 3_757 ?
C15 Li2 C1 157.8(3) . 3_757 ?
C6 Li2 C4 122.1(2) 3_757 . ?
C5 Li2 C4 34.67(11) . . ?
C15 Li2 C4 62.65(14) . . ?
C1 Li2 C4 121.8(2) 3_757 . ?
C6 Li2 C2 63.28(14) 3_757 3_757 ?
C5 Li2 C2 123.4(2) . 3_757 ?
C15 Li2 C2 125.9(2) . 3_757 ?
C1 Li2 C2 34.48(10) 3_757 3_757 ?
C4 Li2 C2 137.9(2) . 3_757 ?
C6 P1 C11 106.58(11) . . ?
C6 P1 C7 104.15(11) . . ?
C11 P1 C7 110.54(12) . . ?
C6 P1 Li1 90.52(12) . . ?
C11 P1 Li1 117.58(14) . . ?
C7 P1 Li1 122.70(14) . . ?
C15 P2 C20 107.15(11) . . ?
C15 P2 C16 104.76(12) . . ?
C20 P2 C16 109.59(12) . . ?
C15 P2 Li1 91.24(12) . . ?
C20 P2 Li1 128.80(14) . . ?
C16 P2 Li1 111.02(15) . . ?
C1 N1 C5 121.13(19) . . ?
C1 N1 Li1 119.21(19) . . ?
C5 N1 Li1 119.53(19) . . ?

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 C1 C2 C3 -0.6(3) . . . . ?
C6 C1 C2 C3 -175.6(2) . . . . ?
Li2 C1 C2 C3 -117.2(3) 3_757 . . . ?
N1 C1 C2 Li2 116.7(2) . . . 3_757 ?
C6 C1 C2 Li2 -58.4(2) . . . 3_757 ?
C1 C2 C3 C4 0.6(4) . . . . ?
Li2 C2 C3 C4 -78.0(3) 3_757 . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C2 C3 C4 Li2 74.0(3) . . . . ?
C3 C4 C5 N1 0.1(3) . . . . ?
Li2 C4 C5 N1 -110.3(2) . . . . ?
C3 C4 C5 C15 174.2(2) . . . . ?
Li2 C4 C5 C15 63.8(2) . . . . ?
C3 C4 C5 Li2 110.4(3) . . . . ?
N1 C1 C6 P1 25.2(3) . . . . ?
C2 C1 C6 P1 -159.80(17) . . . . ?
Li2 C1 C6 P1 136.0(2) 3_757 . . . ?
N1 C1 C6 Li2 -110.8(2) . . . 3_757 ?
C2 C1 C6 Li2 64.2(2) . . . 3_757 ?
N1 C5 C15 P2 -18.8(3) . . . . ?
C4 C5 C15 P2 167.05(18) . . . . ?
Li2 C5 C15 P2 -124.0(2) . . . . ?
N1 C5 C15 Li2 105.2(2) . . . . ?
C4 C5 C15 Li2 -68.9(2) . . . . ?
C1 C6 P1 C11 -142.22(19) . . . . ?
Li2 C6 P1 C11 -44.1(3) 3_757 . . . ?
C1 C6 P1 C7 100.86(19) . . . . ?
Li2 C6 P1 C7 -161.0(3) 3_757 . . . ?
C1 C6 P1 Li1 -23.2(2) . . . . ?
Li2 C6 P1 Li1 75.0(3) 3_757 . . . ?
C14 C11 P1 C6 81.31(19) . . . . ?
C12 C11 P1 C6 -162.07(19) . . . . ?
C13 C11 P1 C6 -37.2(2) . . . . ?
C14 C11 P1 C7 -166.11(17) . . . . ?
C12 C11 P1 C7 -49.5(2) . . . . ?
C13 C11 P1 C7 75.4(2) . . . . ?
C14 C11 P1 Li1 -18.3(2) . . . . ?
C12 C11 P1 Li1 98.4(2) . . . . ?
C13 C11 P1 Li1 -136.7(2) . . . . ?
C10 C7 P1 C6 65.4(2) . . . . ?
C8 C7 P1 C6 -53.7(2) . . . . ?
C9 C7 P1 C6 -168.75(19) . . . . ?
C10 C7 P1 C11 -48.8(2) . . . . ?
C8 C7 P1 C11 -167.85(18) . . . . ?
C9 C7 P1 C11 77.1(2) . . . . ?
C10 C7 P1 Li1 165.34(19) . . . . ?
C8 C7 P1 Li1 46.2(2) . . . . ?
C9 C7 P1 Li1 -68.8(2) . . . . ?
C5 C15 P2 C20 146.56(19) . . . . ?
Li2 C15 P2 C20 57.8(2) . . . . ?
C5 C15 P2 C16 -97.1(2) . . . . ?
Li2 C15 P2 C16 174.2(2) . . . . ?
C5 C15 P2 Li1 15.1(2) . . . . ?
Li2 C15 P2 Li1 -73.7(2) . . . . ?
C21 C20 P2 C15 -54.3(3) . . . . ?
C23 C20 P2 C15 -171.6(2) . . . . ?
C22 C20 P2 C15 67.8(2) . . . . ?
C21 C20 P2 C16 -167.5(2) . . . . ?
C23 C20 P2 C16 75.2(2) . . . . ?
C22 C20 P2 C16 -45.4(3) . . . . ?
C21 C20 P2 Li1 51.7(3) . . . . ?
C23 C20 P2 Li1 -65.5(3) . . . . ?
C22 C20 P2 Li1 173.8(2) . . . . ?
C17 C16 P2 C15 -43.8(3) . . . . ?
C18 C16 P2 C15 -170.8(2) . . . . ?
C19 C16 P2 C15 76.6(3) . . . . ?
C17 C16 P2 C20 70.9(3) . . . . ?
C18 C16 P2 C20 -56.1(3) . . . . ?
C19 C16 P2 C20 -168.8(3) . . . . ?
C17 C16 P2 Li1 -141.0(3) . . . . ?
C18 C16 P2 Li1 92.0(2) . . . . ?
C19 C16 P2 Li1 -20.6(3) . . . . ?
C2 C1 N1 C5 0.3(3) . . . . ?
C6 C1 N1 C5 175.4(2) . . . . ?
Li2 C1 N1 C5 95.1(3) 3_757 . . . ?
C2 C1 N1 Li1 176.2(2) . . . . ?
C6 C1 N1 Li1 -8.7(3) . . . . ?
Li2 C1 N1 Li1 -89.1(3) 3_757 . . . ?
C15 C5 N1 C1 -174.2(2) . . . . ?
C4 C5 N1 C1 -0.1(3) . . . . ?
Li2 C5 N1 C1 -92.9(2) . . . . ?
C15 C5 N1 Li1 9.9(3) . . . . ?
C4 C5 N1 Li1 -175.9(2) . . . . ?
Li2 C5 N1 Li1 91.2(3) . . . . ?

_refine_diff_density_max         0.919
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_pbts150804
_database_code_depnum_ccdc_archive 'CCDC 1427662'
_audit_update_record             
;
2015-09-25 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H82 Cl2 Cr3 N2 P4'
_chemical_formula_sum            'C46 H82 Cl2 Cr3 N2 P4'
_chemical_formula_weight         1013.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   17.0266(14)
_cell_length_b                   18.1629(15)
_cell_length_c                   19.1642(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5926.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4430
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      26.27

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_F_000             2152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.766
_shelx_estimated_absorpt_T_min   0.831
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5286
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39878
_diffrn_reflns_av_unetI/netI     0.1927
_diffrn_reflns_av_R_equivalents  0.1268
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.545
_diffrn_reflns_theta_max         28.011
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14278
_reflns_number_gt                7075
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0514P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2168 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(18)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         14278
_refine_ls_number_parameters     538
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.1396
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_restrained_S_all      0.898
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1558(4) 0.2367(4) 0.7841(4) 0.0228(18) Uani 1 1 d . . . . .
C2 C 0.1761(5) 0.1737(4) 0.8210(4) 0.033(2) Uani 1 1 d . . . . .
H2 H 0.2208 0.1733 0.8507 0.040 Uiso 1 1 calc R U . . .
C3 C 0.1282(5) 0.1095(4) 0.8133(4) 0.029(2) Uani 1 1 d . . . . .
H3 H 0.1428 0.0648 0.8355 0.035 Uiso 1 1 calc R U . . .
C4 C 0.0631(5) 0.1128(4) 0.7750(4) 0.0272(19) Uani 1 1 d . . . . .
H4 H 0.0329 0.0693 0.7686 0.033 Uiso 1 1 calc R U . . .
C5 C 0.0370(5) 0.1803(4) 0.7430(4) 0.0287(19) Uani 1 1 d . . . . .
C6 C 0.2053(5) 0.3008(4) 0.7932(4) 0.0277(19) Uani 1 1 d . . . . .
H6 H 0.2611 0.2844 0.7880 0.033 Uiso 1 1 calc R U . . .
C7 C 0.2114(5) 0.4621(5) 0.7652(5) 0.0405(16) Uani 1 1 d . . . . .
C8 C 0.2161(7) 0.5218(5) 0.7097(6) 0.069(3) Uani 1 1 d . . . . .
H8A H 0.1716 0.5169 0.6777 0.104 Uiso 1 1 calc R U . . .
H8B H 0.2653 0.5166 0.6837 0.104 Uiso 1 1 calc R U . . .
H8C H 0.2145 0.5703 0.7321 0.104 Uiso 1 1 calc R U . . .
C9 C 0.1411(6) 0.4784(5) 0.8128(4) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.1521 0.5224 0.8408 0.074 Uiso 1 1 calc R U . . .
H9B H 0.1320 0.4364 0.8438 0.074 Uiso 1 1 calc R U . . .
H9C H 0.0943 0.4869 0.7842 0.074 Uiso 1 1 calc R U . . .
C10 C 0.2878(5) 0.4606(5) 0.8082(5) 0.055(3) Uani 1 1 d . . . . .
H10A H 0.3326 0.4529 0.7770 0.083 Uiso 1 1 calc R U . . .
H10B H 0.2853 0.4204 0.8422 0.083 Uiso 1 1 calc R U . . .
H10C H 0.2940 0.5075 0.8328 0.083 Uiso 1 1 calc R U . . .
C11 C 0.2510(5) 0.3477(5) 0.6490(4) 0.0405(16) Uani 1 1 d . . . . .
C12 C 0.3386(6) 0.3606(6) 0.6597(5) 0.070(3) Uani 1 1 d . . . . .
H12A H 0.3568 0.3318 0.6998 0.104 Uiso 1 1 calc R U . . .
H12B H 0.3480 0.4130 0.6685 0.104 Uiso 1 1 calc R U . . .
H12C H 0.3672 0.3453 0.6178 0.104 Uiso 1 1 calc R U . . .
C13 C 0.2379(6) 0.2660(5) 0.6344(5) 0.059(3) Uani 1 1 d . . . . .
H13A H 0.2659 0.2520 0.5917 0.088 Uiso 1 1 calc R U . . .
H13B H 0.1817 0.2566 0.6285 0.088 Uiso 1 1 calc R U . . .
H13C H 0.2579 0.2369 0.6736 0.088 Uiso 1 1 calc R U . . .
C14 C 0.2198(6) 0.3892(6) 0.5854(5) 0.063(3) Uani 1 1 d . . . . .
H14A H 0.2297 0.4420 0.5912 0.094 Uiso 1 1 calc R U . . .
H14B H 0.1632 0.3807 0.5810 0.094 Uiso 1 1 calc R U . . .
H14C H 0.2465 0.3716 0.5433 0.094 Uiso 1 1 calc R U . . .
C15 C -0.0334(5) 0.1835(4) 0.7080(4) 0.0287(19) Uani 1 1 d . . . . .
H15 H -0.0630 0.1399 0.7005 0.034 Uiso 1 1 calc R U . . .
C16 C -0.1609(6) 0.2903(5) 0.7257(5) 0.045(2) Uani 1 1 d . . . . .
C17 C -0.2302(6) 0.2429(6) 0.7035(6) 0.072(3) Uani 1 1 d . . . . .
H17A H -0.2154 0.1908 0.7060 0.108 Uiso 1 1 calc R U . . .
H17B H -0.2449 0.2552 0.6554 0.108 Uiso 1 1 calc R U . . .
H17C H -0.2748 0.2522 0.7345 0.108 Uiso 1 1 calc R U . . .
C18 C -0.1823(6) 0.3715(5) 0.7170(5) 0.056(3) Uani 1 1 d . . . . .
H18A H -0.2263 0.3836 0.7479 0.085 Uiso 1 1 calc R U . . .
H18B H -0.1975 0.3808 0.6685 0.085 Uiso 1 1 calc R U . . .
H18C H -0.1369 0.4021 0.7291 0.085 Uiso 1 1 calc R U . . .
C19 C -0.1424(6) 0.2773(6) 0.8016(4) 0.059(3) Uani 1 1 d . . . . .
H19A H -0.1860 0.2951 0.8304 0.088 Uiso 1 1 calc R U . . .
H19B H -0.0943 0.3039 0.8140 0.088 Uiso 1 1 calc R U . . .
H19C H -0.1348 0.2245 0.8097 0.088 Uiso 1 1 calc R U . . .
C20 C -0.0868(5) 0.2574(5) 0.5812(4) 0.039(2) Uani 1 1 d . . . . .
C21 C -0.0042(5) 0.2554(5) 0.5488(5) 0.054(3) Uani 1 1 d . . . . .
H21A H 0.0283 0.2196 0.5740 0.080 Uiso 1 1 calc R U . . .
H21B H 0.0199 0.3043 0.5522 0.080 Uiso 1 1 calc R U . . .
H21C H -0.0080 0.2409 0.4996 0.080 Uiso 1 1 calc R U . . .
C22 C -0.1260(6) 0.1838(5) 0.5644(5) 0.058(3) Uani 1 1 d . . . . .
H22A H -0.1798 0.1839 0.5825 0.086 Uiso 1 1 calc R U . . .
H22B H -0.0962 0.1438 0.5862 0.086 Uiso 1 1 calc R U . . .
H22C H -0.1271 0.1766 0.5137 0.086 Uiso 1 1 calc R U . . .
C23 C -0.1324(6) 0.3216(5) 0.5495(5) 0.055(3) Uani 1 1 d . . . . .
H23A H -0.1316 0.3177 0.4985 0.083 Uiso 1 1 calc R U . . .
H23B H -0.1080 0.3681 0.5637 0.083 Uiso 1 1 calc R U . . .
H23C H -0.1868 0.3203 0.5660 0.083 Uiso 1 1 calc R U . . .
C24 C 0.1328(4) 0.3341(4) 1.0036(4) 0.0227(17) Uani 1 1 d . . . . .
C25 C 0.2077(4) 0.3611(4) 0.9861(4) 0.030(2) Uani 1 1 d . . . . .
H25 H 0.2496 0.3282 0.9760 0.035 Uiso 1 1 calc R U . . .
C26 C 0.2194(5) 0.4382(4) 0.9838(4) 0.034(2) Uani 1 1 d . . . . .
H26 H 0.2705 0.4578 0.9765 0.041 Uiso 1 1 calc R U . . .
C27 C 0.1589(5) 0.4828(4) 0.9917(4) 0.030(2) Uani 1 1 d . . . . .
H27 H 0.1679 0.5345 0.9911 0.037 Uiso 1 1 calc R U . . .
C28 C 0.0794(5) 0.4566(4) 1.0014(4) 0.0287(19) Uani 1 1 d . . . . .
C29 C 0.1215(4) 0.2554(4) 1.0049(4) 0.0273(19) Uani 1 1 d . . . . .
H29 H 0.1652 0.2343 1.0334 0.033 Uiso 1 1 calc R U . . .
C30 C 0.0531(5) 0.2115(5) 1.1390(4) 0.037(2) Uani 1 1 d . . . . .
C31 C -0.0237(5) 0.2020(6) 1.1812(4) 0.061(3) Uani 1 1 d . . . . .
H31A H -0.0517 0.1582 1.1647 0.092 Uiso 1 1 calc R U . . .
H31B H -0.0569 0.2455 1.1748 0.092 Uiso 1 1 calc R U . . .
H31C H -0.0110 0.1963 1.2308 0.092 Uiso 1 1 calc R U . . .
C32 C 0.1084(6) 0.1476(5) 1.1549(5) 0.053(3) Uani 1 1 d . . . . .
H32A H 0.1533 0.1493 1.1230 0.079 Uiso 1 1 calc R U . . .
H32B H 0.0803 0.1010 1.1489 0.079 Uiso 1 1 calc R U . . .
H32C H 0.1271 0.1516 1.2031 0.079 Uiso 1 1 calc R U . . .
C33 C 0.0904(5) 0.2826(5) 1.1648(4) 0.048(3) Uani 1 1 d . . . . .
H33A H 0.0981 0.2797 1.2154 0.072 Uiso 1 1 calc R U . . .
H33B H 0.0558 0.3241 1.1539 0.072 Uiso 1 1 calc R U . . .
H33C H 0.1412 0.2897 1.1418 0.072 Uiso 1 1 calc R U . . .
C34 C 0.0029(5) 0.1378(4) 0.9994(4) 0.0296(19) Uani 1 1 d . . . . .
C35 C -0.0311(5) 0.1632(4) 0.9292(4) 0.035(2) Uani 1 1 d . . . . .
H35A H -0.0466 0.1201 0.9017 0.052 Uiso 1 1 calc R U . . .
H35B H 0.0088 0.1913 0.9036 0.052 Uiso 1 1 calc R U . . .
H35C H -0.0771 0.1944 0.9374 0.052 Uiso 1 1 calc R U . . .
C36 C -0.0620(5) 0.0980(4) 1.0392(5) 0.040(2) Uani 1 1 d . . . . .
H36A H -0.0840 0.0589 1.0098 0.060 Uiso 1 1 calc R U . . .
H36B H -0.1035 0.1330 1.0514 0.060 Uiso 1 1 calc R U . . .
H36C H -0.0403 0.0763 1.0818 0.060 Uiso 1 1 calc R U . . .
C37 C 0.0728(5) 0.0861(4) 0.9875(4) 0.034(2) Uani 1 1 d . . . . .
H37A H 0.0930 0.0691 1.0326 0.050 Uiso 1 1 calc R U . . .
H37B H 0.1143 0.1124 0.9624 0.050 Uiso 1 1 calc R U . . .
H37C H 0.0557 0.0435 0.9599 0.050 Uiso 1 1 calc R U . . .
C38 C 0.0161(4) 0.5046(4) 1.0054(4) 0.030(2) Uani 1 1 d . . . . .
H38 H 0.0247 0.5562 1.0021 0.036 Uiso 1 1 calc R U . . .
C39 C -0.1356(6) 0.5006(6) 0.9386(7) 0.062(3) Uani 1 1 d . . . . .
C40 C -0.1448(7) 0.5812(6) 0.9247(7) 0.088(4) Uani 1 1 d . . . . .
H40A H -0.1808 0.5885 0.8854 0.132 Uiso 1 1 calc R U . . .
H40B H -0.0935 0.6026 0.9134 0.132 Uiso 1 1 calc R U . . .
H40C H -0.1661 0.6054 0.9663 0.132 Uiso 1 1 calc R U . . .
C41 C -0.2104(8) 0.4567(8) 0.9239(9) 0.066(5) Uani 0.7 1 d . . P A 1
H41A H -0.2483 0.4649 0.9616 0.098 Uiso 0.7 1 calc R U P A 1
H41B H -0.1977 0.4041 0.9212 0.098 Uiso 0.7 1 calc R U P A 1
H41C H -0.2332 0.4729 0.8795 0.098 Uiso 0.7 1 calc R U P A 1
C41B C -0.226(2) 0.490(2) 0.972(2) 0.066(5) Uani 0.3 1 d . . P A 2
H41D H -0.2291 0.5139 1.0180 0.098 Uiso 0.3 1 calc R U P A 2
H41E H -0.2376 0.4371 0.9778 0.098 Uiso 0.3 1 calc R U P A 2
H41F H -0.2651 0.5119 0.9409 0.098 Uiso 0.3 1 calc R U P A 2
C42 C -0.0862(10) 0.4709(8) 0.8758(7) 0.127(6) Uani 1 1 d . . . . .
H42A H -0.1144 0.4803 0.8321 0.190 Uiso 1 1 calc R U . . .
H42B H -0.0779 0.4178 0.8813 0.190 Uiso 1 1 calc R U . . .
H42C H -0.0353 0.4960 0.8746 0.190 Uiso 1 1 calc R U . . .
C43 C -0.1167(7) 0.5146(6) 1.0959(7) 0.069(4) Uani 1 1 d D . . . .
C44 C -0.1070(7) 0.5977(5) 1.1002(7) 0.079(4) Uani 1 1 d . . . . .
H44A H -0.1138 0.6136 1.1487 0.119 Uiso 1 1 calc R U . . .
H44B H -0.1467 0.6215 1.0709 0.119 Uiso 1 1 calc R U . . .
H44C H -0.0545 0.6114 1.0839 0.119 Uiso 1 1 calc R U . . .
C45 C -0.0771(11) 0.4748(9) 1.1542(9) 0.093(5) Uani 0.7 1 d D . P B 1
H45A H -0.0215 0.4678 1.1429 0.140 Uiso 0.7 1 calc R U P B 1
H45B H -0.1021 0.4268 1.1610 0.140 Uiso 0.7 1 calc R U P B 1
H45C H -0.0817 0.5038 1.1972 0.140 Uiso 0.7 1 calc R U P B 1
C46 C -0.2051(12) 0.4977(10) 1.1000(10) 0.093(5) Uani 0.7 1 d . . P B 1
H46A H -0.2143 0.4462 1.0871 0.140 Uiso 0.7 1 calc R U P B 1
H46B H -0.2337 0.5300 1.0678 0.140 Uiso 0.7 1 calc R U P B 1
H46C H -0.2238 0.5061 1.1477 0.140 Uiso 0.7 1 calc R U P B 1
C45B C -0.0477(19) 0.502(2) 1.1488(18) 0.093(5) Uani 0.3 1 d D . P B 2
H45D H 0.0025 0.5103 1.1253 0.140 Uiso 0.3 1 calc R U P B 2
H45E H -0.0497 0.4512 1.1663 0.140 Uiso 0.3 1 calc R U P B 2
H45F H -0.0530 0.5362 1.1880 0.140 Uiso 0.3 1 calc R U P B 2
C46B C -0.185(3) 0.488(3) 1.143(2) 0.093(5) Uani 0.3 1 d . . P B 2
H46D H -0.1813 0.5122 1.1891 0.140 Uiso 0.3 1 calc R U P B 2
H46E H -0.1827 0.4348 1.1492 0.140 Uiso 0.3 1 calc R U P B 2
H46F H -0.2356 0.5016 1.1217 0.140 Uiso 0.3 1 calc R U P B 2
N1 N 0.0845(3) 0.2434(3) 0.7489(3) 0.0230(15) Uani 1 1 d . . . . .
N2 N 0.0677(3) 0.3802(3) 1.0076(3) 0.0227(14) Uani 1 1 d . . . . .
P1 P 0.18686(13) 0.37053(11) 0.72703(11) 0.0298(5) Uani 1 1 d . . . . .
P2 P -0.06855(13) 0.26874(12) 0.67717(11) 0.0304(5) Uani 1 1 d . . . . .
P3 P 0.03172(12) 0.22541(11) 1.04377(10) 0.0235(5) Uani 1 1 d . . . . .
P4 P -0.07813(13) 0.47163(12) 1.01642(14) 0.0382(6) Uani 1 1 d . . . . .
Cl1 Cl 0.01419(15) 0.44646(12) 0.64520(12) 0.0518(7) Uani 1 1 d . . . . .
Cl2 Cl -0.16816(13) 0.29431(11) 1.04958(13) 0.0443(6) Uani 1 1 d . . . . .
Cr1 Cr 0.05053(8) 0.33953(7) 0.70127(6) 0.0279(3) Uani 1 1 d . . . . .
Cr2 Cr -0.04323(7) 0.34007(6) 1.02678(6) 0.0267(3) Uani 1 1 d . . . . .
Cr3 Cr 0.16901(8) 0.27601(7) 0.89948(7) 0.0359(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.389(10) . ?
C1 N1 1.394(9) . ?
C1 C6 1.449(10) . ?
C1 Cr3 2.334(7) . ?
C2 C3 1.430(11) . ?
C2 Cr3 2.393(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.331(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.441(10) . ?
C4 H4 0.9500 . ?
C5 C15 1.374(10) . ?
C5 N1 1.408(9) . ?
C6 P1 1.820(8) . ?
C6 Cr3 2.175(8) . ?
C6 H6 1.0000 . ?
C7 C8 1.521(12) . ?
C7 C9 1.534(12) . ?
C7 C10 1.539(12) . ?
C7 P1 1.864(8) . ?
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 1.523(13) . ?
C11 C13 1.527(12) . ?
C11 C14 1.528(12) . ?
C11 P1 1.898(9) . ?
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 P2 1.761(7) . ?
C15 H15 0.9500 . ?
C16 C19 1.506(12) . ?
C16 C17 1.521(13) . ?
C16 C18 1.528(12) . ?
C16 P2 1.869(10) . ?
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 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C23 1.525(11) . ?
C20 C22 1.528(12) . ?
C20 C21 1.539(12) . ?
C20 P2 1.877(8) . ?
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 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N2 1.390(9) . ?
C24 C25 1.408(10) . ?
C24 C29 1.442(10) . ?
C24 Cr3 2.340(7) . ?
C25 C26 1.416(10) . ?
C25 Cr3 2.362(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.320(10) . ?
C26 H26 0.9500 . ?
C27 C28 1.446(10) . ?
C27 H27 0.9500 . ?
C28 C38 1.389(10) . ?
C28 N2 1.408(9) . ?
C29 P3 1.786(8) . ?
C29 Cr3 2.208(8) . ?
C29 H29 1.0000 . ?
C30 C33 1.522(12) . ?
C30 C32 1.525(11) . ?
C30 C31 1.547(12) . ?
C30 P3 1.877(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.525(11) . ?
C34 C37 1.534(10) . ?
C34 C35 1.535(10) . ?
C34 P3 1.869(8) . ?
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 P4 1.725(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.497(13) . ?
C39 C41 1.529(16) . ?
C39 C42 1.564(17) . ?
C39 C41B 1.69(4) . ?
C39 P4 1.859(11) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C45 1.492(18) . ?
C43 C44 1.520(13) . ?
C43 C46 1.54(2) . ?
C43 C46B 1.56(4) . ?
C43 C45B 1.57(3) . ?
C43 P4 1.833(11) . ?
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 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?
C46B H46D 0.9800 . ?
C46B H46E 0.9800 . ?
C46B H46F 0.9800 . ?
N1 Cr1 2.052(6) . ?
N2 Cr2 2.058(6) . ?
P1 Cr1 2.439(3) . ?
P2 Cr1 2.445(3) . ?
P3 Cr2 2.464(2) . ?
P4 Cr2 2.470(2) . ?
Cl1 Cr1 2.304(2) . ?
Cl2 Cr2 2.325(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
C2 C1 N1 122.4(7) . . ?
C2 C1 C6 117.1(7) . . ?
N1 C1 C6 119.7(7) . . ?
C2 C1 Cr3 75.2(4) . . ?
N1 C1 Cr3 121.1(5) . . ?
C6 C1 Cr3 65.4(4) . . ?
C1 C2 C3 118.5(7) . . ?
C1 C2 Cr3 70.6(4) . . ?
C3 C2 Cr3 132.0(6) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
Cr3 C2 H2 70.8 . . ?
C4 C3 C2 119.7(7) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 122.0(7) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 H4 119.0 . . ?
C15 C5 N1 120.3(7) . . ?
C15 C5 C4 120.9(7) . . ?
N1 C5 C4 118.8(7) . . ?
C1 C6 P1 112.0(5) . . ?
C1 C6 Cr3 77.3(4) . . ?
P1 C6 Cr3 138.4(4) . . ?
C1 C6 H6 107.6 . . ?
P1 C6 H6 107.6 . . ?
Cr3 C6 H6 107.6 . . ?
C8 C7 C9 108.6(8) . . ?
C8 C7 C10 110.0(8) . . ?
C9 C7 C10 110.1(7) . . ?
C8 C7 P1 111.9(6) . . ?
C9 C7 P1 103.3(6) . . ?
C10 C7 P1 112.6(6) . . ?
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(8) . . ?
C12 C11 C14 111.9(8) . . ?
C13 C11 C14 106.5(8) . . ?
C12 C11 P1 115.0(6) . . ?
C13 C11 P1 105.8(6) . . ?
C14 C11 P1 108.6(6) . . ?
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 . . ?
C5 C15 P2 119.9(6) . . ?
C5 C15 H15 120.1 . . ?
P2 C15 H15 120.1 . . ?
C19 C16 C17 110.2(8) . . ?
C19 C16 C18 107.8(8) . . ?
C17 C16 C18 109.3(8) . . ?
C19 C16 P2 105.8(6) . . ?
C17 C16 P2 113.2(7) . . ?
C18 C16 P2 110.4(7) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C23 C20 C22 111.3(7) . . ?
C23 C20 C21 108.9(8) . . ?
C22 C20 C21 107.0(8) . . ?
C23 C20 P2 113.0(6) . . ?
C22 C20 P2 112.0(6) . . ?
C21 C20 P2 104.2(6) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C25 121.7(7) . . ?
N2 C24 C29 119.3(6) . . ?
C25 C24 C29 118.0(7) . . ?
N2 C24 Cr3 122.0(5) . . ?
C25 C24 Cr3 73.4(4) . . ?
C29 C24 Cr3 66.6(4) . . ?
C24 C25 C26 118.7(7) . . ?
C24 C25 Cr3 71.7(4) . . ?
C26 C25 Cr3 131.7(6) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
Cr3 C25 H25 69.9 . . ?
C27 C26 C25 119.6(8) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C28 122.9(7) . . ?
C26 C27 H27 118.5 . . ?
C28 C27 H27 118.5 . . ?
C38 C28 N2 120.3(7) . . ?
C38 C28 C27 121.8(7) . . ?
N2 C28 C27 117.9(7) . . ?
C24 C29 P3 115.1(6) . . ?
C24 C29 Cr3 76.6(4) . . ?
P3 C29 Cr3 138.3(4) . . ?
C24 C29 H29 107.0 . . ?
P3 C29 H29 107.0 . . ?
Cr3 C29 H29 107.0 . . ?
C33 C30 C32 108.8(7) . . ?
C33 C30 C31 106.1(7) . . ?
C32 C30 C31 109.4(8) . . ?
C33 C30 P3 106.4(6) . . ?
C32 C30 P3 114.7(6) . . ?
C31 C30 P3 111.1(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C37 110.2(6) . . ?
C36 C34 C35 107.9(7) . . ?
C37 C34 C35 110.2(6) . . ?
C36 C34 P3 111.6(6) . . ?
C37 C34 P3 112.7(5) . . ?
C35 C34 P3 104.0(5) . . ?
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 . . ?
C28 C38 P4 120.7(6) . . ?
C28 C38 H38 119.6 . . ?
P4 C38 H38 119.6 . . ?
C40 C39 C41 113.0(10) . . ?
C40 C39 C42 104.9(10) . . ?
C41 C39 C42 97.3(11) . . ?
C40 C39 C41B 94.9(15) . . ?
C42 C39 C41B 138.4(18) . . ?
C40 C39 P4 118.3(8) . . ?
C41 C39 P4 116.0(8) . . ?
C42 C39 P4 103.7(7) . . ?
C41B C39 P4 98.1(15) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C41B H41D 109.5 . . ?
C39 C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C39 C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C45 C43 C44 113.0(13) . . ?
C45 C43 C46 107.9(12) . . ?
C44 C43 C46 107.5(11) . . ?
C44 C43 C46B 110.6(18) . . ?
C44 C43 C45B 91.7(18) . . ?
C46B C43 C45B 98(3) . . ?
C45 C43 P4 104.8(8) . . ?
C44 C43 P4 115.4(8) . . ?
C46 C43 P4 108.0(10) . . ?
C46B C43 P4 128.7(19) . . ?
C45B C43 P4 101.9(16) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C45B H45D 109.5 . . ?
C43 C45B H45E 109.5 . . ?
H45D C45B H45E 109.5 . . ?
C43 C45B H45F 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?
C43 C46B H46D 109.5 . . ?
C43 C46B H46E 109.5 . . ?
H46D C46B H46E 109.5 . . ?
C43 C46B H46F 109.5 . . ?
H46D C46B H46F 109.5 . . ?
H46E C46B H46F 109.5 . . ?
C1 N1 C5 117.8(6) . . ?
C1 N1 Cr1 122.4(5) . . ?
C5 N1 Cr1 119.7(5) . . ?
C24 N2 C28 118.4(6) . . ?
C24 N2 Cr2 121.9(5) . . ?
C28 N2 Cr2 119.6(5) . . ?
C6 P1 C7 108.0(4) . . ?
C6 P1 C11 107.3(4) . . ?
C7 P1 C11 112.0(4) . . ?
C6 P1 Cr1 98.3(3) . . ?
C7 P1 Cr1 119.9(3) . . ?
C11 P1 Cr1 109.7(3) . . ?
C15 P2 C16 107.6(4) . . ?
C15 P2 C20 106.8(4) . . ?
C16 P2 C20 111.8(4) . . ?
C15 P2 Cr1 96.7(3) . . ?
C16 P2 Cr1 119.6(3) . . ?
C20 P2 Cr1 112.3(3) . . ?
C29 P3 C34 107.2(4) . . ?
C29 P3 C30 106.3(4) . . ?
C34 P3 C30 112.2(4) . . ?
C29 P3 Cr2 97.5(3) . . ?
C34 P3 Cr2 121.5(3) . . ?
C30 P3 Cr2 110.0(3) . . ?
C38 P4 C43 106.7(5) . . ?
C38 P4 C39 107.0(4) . . ?
C43 P4 C39 111.0(6) . . ?
C38 P4 Cr2 97.0(3) . . ?
C43 P4 Cr2 115.5(4) . . ?
C39 P4 Cr2 117.7(4) . . ?
N1 Cr1 Cl1 178.5(2) . . ?
N1 Cr1 P1 80.69(18) . . ?
Cl1 Cr1 P1 98.94(9) . . ?
N1 Cr1 P2 82.55(18) . . ?
Cl1 Cr1 P2 97.61(9) . . ?
P1 Cr1 P2 161.60(9) . . ?
N2 Cr2 Cl2 179.38(19) . . ?
N2 Cr2 P3 81.22(17) . . ?
Cl2 Cr2 P3 98.44(8) . . ?
N2 Cr2 P4 82.19(17) . . ?
Cl2 Cr2 P4 98.09(9) . . ?
P3 Cr2 P4 162.32(9) . . ?
C6 Cr3 C29 174.7(3) . . ?
C6 Cr3 C1 37.3(3) . . ?
C29 Cr3 C1 141.2(3) . . ?
C6 Cr3 C24 141.2(3) . . ?
C29 Cr3 C24 36.8(3) . . ?
C1 Cr3 C24 156.9(3) . . ?
C6 Cr3 C25 116.3(3) . . ?
C29 Cr3 C25 64.5(3) . . ?
C1 Cr3 C25 153.2(3) . . ?
C24 Cr3 C25 34.8(2) . . ?
C6 Cr3 C2 63.8(3) . . ?
C29 Cr3 C2 117.5(3) . . ?
C1 Cr3 C2 34.1(2) . . ?
C24 Cr3 C2 154.1(3) . . ?
C25 Cr3 C2 159.3(3) . . ?

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 C1 C2 C3 10.3(11) . . . . ?
C6 C1 C2 C3 179.8(7) . . . . ?
Cr3 C1 C2 C3 128.0(7) . . . . ?
N1 C1 C2 Cr3 -117.7(7) . . . . ?
C6 C1 C2 Cr3 51.8(6) . . . . ?
C1 C2 C3 C4 -4.3(12) . . . . ?
Cr3 C2 C3 C4 84.6(10) . . . . ?
C2 C3 C4 C5 -2.7(12) . . . . ?
C3 C4 C5 C15 -175.1(8) . . . . ?
C3 C4 C5 N1 4.0(11) . . . . ?
C2 C1 C6 P1 165.9(6) . . . . ?
N1 C1 C6 P1 -24.2(9) . . . . ?
Cr3 C1 C6 P1 -137.4(5) . . . . ?
C2 C1 C6 Cr3 -56.7(6) . . . . ?
N1 C1 C6 Cr3 113.1(6) . . . . ?
N1 C5 C15 P2 -5.7(10) . . . . ?
C4 C5 C15 P2 173.5(6) . . . . ?
N2 C24 C25 C26 10.4(11) . . . . ?
C29 C24 C25 C26 179.3(7) . . . . ?
Cr3 C24 C25 C26 128.1(7) . . . . ?
N2 C24 C25 Cr3 -117.7(7) . . . . ?
C29 C24 C25 Cr3 51.1(6) . . . . ?
C24 C25 C26 C27 -6.0(12) . . . . ?
Cr3 C25 C26 C27 84.4(10) . . . . ?
C25 C26 C27 C28 -1.4(13) . . . . ?
C26 C27 C28 C38 -176.0(8) . . . . ?
C26 C27 C28 N2 4.8(12) . . . . ?
N2 C24 C29 P3 -22.6(9) . . . . ?
C25 C24 C29 P3 168.2(6) . . . . ?
Cr3 C24 C29 P3 -137.4(5) . . . . ?
N2 C24 C29 Cr3 114.7(6) . . . . ?
C25 C24 C29 Cr3 -54.4(6) . . . . ?
N2 C28 C38 P4 -1.3(11) . . . . ?
C27 C28 C38 P4 179.6(6) . . . . ?
C2 C1 N1 C5 -8.9(10) . . . . ?
C6 C1 N1 C5 -178.1(6) . . . . ?
Cr3 C1 N1 C5 -100.6(7) . . . . ?
C2 C1 N1 Cr1 174.7(5) . . . . ?
C6 C1 N1 Cr1 5.5(9) . . . . ?
Cr3 C1 N1 Cr1 83.0(6) . . . . ?
C15 C5 N1 C1 -179.2(7) . . . . ?
C4 C5 N1 C1 1.7(10) . . . . ?
C15 C5 N1 Cr1 -2.7(9) . . . . ?
C4 C5 N1 Cr1 178.1(5) . . . . ?
C25 C24 N2 C28 -6.9(10) . . . . ?
C29 C24 N2 C28 -175.7(7) . . . . ?
Cr3 C24 N2 C28 -96.4(7) . . . . ?
C25 C24 N2 Cr2 175.9(5) . . . . ?
C29 C24 N2 Cr2 7.1(9) . . . . ?
Cr3 C24 N2 Cr2 86.4(6) . . . . ?
C38 C28 N2 C24 -179.8(7) . . . . ?
C27 C28 N2 C24 -0.6(10) . . . . ?
C38 C28 N2 Cr2 -2.5(9) . . . . ?
C27 C28 N2 Cr2 176.7(5) . . . . ?
C1 C6 P1 C7 152.1(6) . . . . ?
Cr3 C6 P1 C7 56.4(7) . . . . ?
C1 C6 P1 C11 -87.0(6) . . . . ?
Cr3 C6 P1 C11 177.4(6) . . . . ?
C1 C6 P1 Cr1 26.8(6) . . . . ?
Cr3 C6 P1 Cr1 -68.8(6) . . . . ?
C8 C7 P1 C6 166.8(7) . . . . ?
C9 C7 P1 C6 -76.5(6) . . . . ?
C10 C7 P1 C6 42.3(7) . . . . ?
C8 C7 P1 C11 48.9(8) . . . . ?
C9 C7 P1 C11 165.5(6) . . . . ?
C10 C7 P1 C11 -75.7(7) . . . . ?
C8 C7 P1 Cr1 -81.9(7) . . . . ?
C9 C7 P1 Cr1 34.8(7) . . . . ?
C10 C7 P1 Cr1 153.5(5) . . . . ?
C12 C11 P1 C6 -71.0(8) . . . . ?
C13 C11 P1 C6 48.8(7) . . . . ?
C14 C11 P1 C6 162.8(6) . . . . ?
C12 C11 P1 C7 47.4(8) . . . . ?
C13 C11 P1 C7 167.1(7) . . . . ?
C14 C11 P1 C7 -78.9(7) . . . . ?
C12 C11 P1 Cr1 -176.8(6) . . . . ?
C13 C11 P1 Cr1 -57.0(7) . . . . ?
C14 C11 P1 Cr1 56.9(6) . . . . ?
C5 C15 P2 C16 -115.0(7) . . . . ?
C5 C15 P2 C20 124.8(7) . . . . ?
C5 C15 P2 Cr1 9.0(7) . . . . ?
C19 C16 P2 C15 47.9(8) . . . . ?
C17 C16 P2 C15 -72.9(7) . . . . ?
C18 C16 P2 C15 164.3(6) . . . . ?
C19 C16 P2 C20 164.9(6) . . . . ?
C17 C16 P2 C20 44.2(8) . . . . ?
C18 C16 P2 C20 -78.7(7) . . . . ?
C19 C16 P2 Cr1 -60.8(7) . . . . ?
C17 C16 P2 Cr1 178.4(6) . . . . ?
C18 C16 P2 Cr1 55.6(7) . . . . ?
C23 C20 P2 C15 168.8(7) . . . . ?
C22 C20 P2 C15 42.2(8) . . . . ?
C21 C20 P2 C15 -73.2(7) . . . . ?
C23 C20 P2 C16 51.3(8) . . . . ?
C22 C20 P2 C16 -75.3(8) . . . . ?
C21 C20 P2 C16 169.3(6) . . . . ?
C23 C20 P2 Cr1 -86.4(7) . . . . ?
C22 C20 P2 Cr1 147.0(6) . . . . ?
C21 C20 P2 Cr1 31.6(6) . . . . ?
C24 C29 P3 C34 149.4(6) . . . . ?
Cr3 C29 P3 C34 51.4(7) . . . . ?
C24 C29 P3 C30 -90.4(6) . . . . ?
Cr3 C29 P3 C30 171.6(6) . . . . ?
C24 C29 P3 Cr2 23.1(6) . . . . ?
Cr3 C29 P3 Cr2 -74.9(6) . . . . ?
C36 C34 P3 C29 166.8(6) . . . . ?
C37 C34 P3 C29 42.2(6) . . . . ?
C35 C34 P3 C29 -77.1(6) . . . . ?
C36 C34 P3 C30 50.5(7) . . . . ?
C37 C34 P3 C30 -74.1(7) . . . . ?
C35 C34 P3 C30 166.6(5) . . . . ?
C36 C34 P3 Cr2 -82.8(6) . . . . ?
C37 C34 P3 Cr2 152.7(5) . . . . ?
C35 C34 P3 Cr2 33.3(6) . . . . ?
C33 C30 P3 C29 52.6(7) . . . . ?
C32 C30 P3 C29 -67.8(7) . . . . ?
C31 C30 P3 C29 167.6(6) . . . . ?
C33 C30 P3 C34 169.4(6) . . . . ?
C32 C30 P3 C34 49.1(8) . . . . ?
C31 C30 P3 C34 -75.6(7) . . . . ?
C33 C30 P3 Cr2 -52.0(6) . . . . ?
C32 C30 P3 Cr2 -172.3(6) . . . . ?
C31 C30 P3 Cr2 63.0(7) . . . . ?
C28 C38 P4 C43 122.7(7) . . . . ?
C28 C38 P4 C39 -118.5(7) . . . . ?
C28 C38 P4 Cr2 3.3(7) . . . . ?
C45 C43 P4 C38 -75.4(10) . . . . ?
C44 C43 P4 C38 49.5(11) . . . . ?
C46 C43 P4 C38 169.8(10) . . . . ?
C46B C43 P4 C38 -159(3) . . . . ?
C45B C43 P4 C38 -48.2(17) . . . . ?
C45 C43 P4 C39 168.4(9) . . . . ?
C44 C43 P4 C39 -66.7(11) . . . . ?
C46 C43 P4 C39 53.6(11) . . . . ?
C46B C43 P4 C39 85(3) . . . . ?
C45B C43 P4 C39 -164.4(16) . . . . ?
C45 C43 P4 Cr2 31.1(10) . . . . ?
C44 C43 P4 Cr2 156.1(8) . . . . ?
C46 C43 P4 Cr2 -83.7(11) . . . . ?
C46B C43 P4 Cr2 -52(3) . . . . ?
C45B C43 P4 Cr2 58.4(16) . . . . ?
C40 C39 P4 C38 -61.4(10) . . . . ?
C41 C39 P4 C38 159.5(10) . . . . ?
C42 C39 P4 C38 54.2(8) . . . . ?
C41B C39 P4 C38 -161.5(15) . . . . ?
C40 C39 P4 C43 54.6(10) . . . . ?
C41 C39 P4 C43 -84.5(11) . . . . ?
C42 C39 P4 C43 170.2(8) . . . . ?
C41B C39 P4 C43 -45.5(16) . . . . ?
C40 C39 P4 Cr2 -169.1(8) . . . . ?
C41 C39 P4 Cr2 51.7(11) . . . . ?
C42 C39 P4 Cr2 -53.6(8) . . . . ?
C41B C39 P4 Cr2 90.7(15) . . . . ?

_refine_diff_density_max         0.782
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.091

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.006 -0.126 0.140 218.4 35.5
2 0.006 0.374 0.360 218.3 35.7
3 0.506 0.126 0.640 218.3 35.0
4 0.494 0.626 0.860 218.4 35.5
_platon_squeeze_details          
;
 The residual electron density was assigned to a molecule of the
 pentane solvent [142/4 = 36 e per asymmetric unit; one molecule of
 C5H12 would give 42e].
;

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_pbts150721
_database_code_depnum_ccdc_archive 'CCDC 1427663'
_audit_update_record             
;
2015-09-25 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H41 Cl2 N P2 Zr'
_chemical_formula_sum            'C23 H41 Cl2 N P2 Zr'
_chemical_formula_weight         555.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   15.8964(13)
_cell_length_b                   21.1004(17)
_cell_length_c                   33.285(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11164.5(16)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9910
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.31

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_F_000             4640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.710
_shelx_estimated_absorpt_T_min   0.764
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            94787
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_av_R_equivalents  0.1179
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.717
_diffrn_reflns_theta_max         28.070
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13508
_reflns_number_gt                8100
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+52.3884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13508
_refine_ls_number_parameters     547
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0870
_refine_ls_wR_factor_ref         0.1408
_refine_ls_wR_factor_gt          0.1267
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.1728(4) 0.3808(3) 0.83664(17) 0.0326(14) Uani 1 1 d . . . . .
C2 C 0.1529(5) 0.3180(3) 0.8333(2) 0.0448(18) Uani 1 1 d . . . . .
H2 H 0.0994 0.3050 0.8236 0.054 Uiso 1 1 calc R U . . .
C3 C 0.2141(6) 0.2732(3) 0.8447(2) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.1997 0.2295 0.8445 0.064 Uiso 1 1 calc R U . . .
C4 C 0.2915(5) 0.2900(3) 0.85573(18) 0.0431(18) Uani 1 1 d . . . . .
H4 H 0.3305 0.2584 0.8639 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3168(4) 0.3558(3) 0.85548(17) 0.0334(15) Uani 1 1 d . . . . .
C6 C 0.1212(4) 0.4369(3) 0.82925(19) 0.0425(17) Uani 1 1 d . . . . .
H6 H 0.0836 0.4388 0.8052 0.051 Uiso 1 1 calc R U . . .
C7 C 0.0285(6) 0.5491(4) 0.8501(2) 0.074(3) Uani 1 1 d . . . . .
C8 C 0.0679(6) 0.5783(4) 0.8131(2) 0.073(3) Uani 1 1 d . . . . .
H8A H 0.0786 0.5452 0.7931 0.109 Uiso 1 1 calc R U . . .
H8B H 0.1212 0.5987 0.8204 0.109 Uiso 1 1 calc R U . . .
H8C H 0.0296 0.6100 0.8018 0.109 Uiso 1 1 calc R U . . .
C9 C 0.0159(11) 0.6008(5) 0.8814(3) 0.189(9) Uani 1 1 d . . . . .
H9A H -0.0188 0.6348 0.8700 0.283 Uiso 1 1 calc R U . . .
H9B H 0.0707 0.6181 0.8893 0.283 Uiso 1 1 calc R U . . .
H9C H -0.0123 0.5830 0.9050 0.283 Uiso 1 1 calc R U . . .
C10 C -0.0563(6) 0.5188(6) 0.8384(3) 0.135(6) Uani 1 1 d . . . . .
H10A H -0.0831 0.5010 0.8624 0.202 Uiso 1 1 calc R U . . .
H10B H -0.0466 0.4850 0.8187 0.202 Uiso 1 1 calc R U . . .
H10C H -0.0930 0.5512 0.8266 0.202 Uiso 1 1 calc R U . . .
C11 C 0.0691(4) 0.4500(3) 0.9179(2) 0.0416(16) Uani 1 1 d . . . . .
C12 C 0.0629(8) 0.4977(4) 0.9508(2) 0.099(4) Uani 1 1 d . . . . .
H12A H 0.0446 0.4768 0.9756 0.149 Uiso 1 1 calc R U . . .
H12B H 0.0221 0.5304 0.9433 0.149 Uiso 1 1 calc R U . . .
H12C H 0.1181 0.5173 0.9551 0.149 Uiso 1 1 calc R U . . .
C13 C -0.0142(6) 0.4176(6) 0.9119(4) 0.142(6) Uani 1 1 d . . . . .
H13A H -0.0349 0.4017 0.9377 0.213 Uiso 1 1 calc R U . . .
H13B H -0.0072 0.3821 0.8932 0.213 Uiso 1 1 calc R U . . .
H13C H -0.0547 0.4478 0.9007 0.213 Uiso 1 1 calc R U . . .
C14 C 0.1337(6) 0.4015(4) 0.9298(2) 0.067(3) Uani 1 1 d . . . . .
H14A H 0.1884 0.4223 0.9334 0.101 Uiso 1 1 calc R U . . .
H14B H 0.1381 0.3693 0.9088 0.101 Uiso 1 1 calc R U . . .
H14C H 0.1168 0.3814 0.9551 0.101 Uiso 1 1 calc R U . . .
C15 C 0.3963(4) 0.3774(3) 0.86137(18) 0.0356(15) Uani 1 1 d . . . . .
H15 H 0.4407 0.3502 0.8697 0.043 Uiso 1 1 calc R U . . .
C16 C 0.4942(5) 0.4640(4) 0.8125(2) 0.057(2) Uani 1 1 d . . . . .
C17 C 0.4678(5) 0.4199(4) 0.7788(2) 0.061(2) Uani 1 1 d . . . . .
H17A H 0.4120 0.4321 0.7691 0.092 Uiso 1 1 calc R U . . .
H17B H 0.4660 0.3762 0.7889 0.092 Uiso 1 1 calc R U . . .
H17C H 0.5085 0.4227 0.7568 0.092 Uiso 1 1 calc R U . . .
C18 C 0.5827(5) 0.4447(5) 0.8275(3) 0.081(3) Uani 1 1 d . . . . .
H18A H 0.5799 0.4027 0.8400 0.122 Uiso 1 1 calc R U . . .
H18B H 0.6025 0.4758 0.8473 0.122 Uiso 1 1 calc R U . . .
H18C H 0.6217 0.4435 0.8047 0.122 Uiso 1 1 calc R U . . .
C19 C 0.4952(6) 0.5319(4) 0.7961(3) 0.090(3) Uani 1 1 d . . . . .
H19A H 0.5419 0.5367 0.7771 0.135 Uiso 1 1 calc R U . . .
H19B H 0.5025 0.5618 0.8184 0.135 Uiso 1 1 calc R U . . .
H19C H 0.4420 0.5407 0.7823 0.135 Uiso 1 1 calc R U . . .
C20 C 0.4488(4) 0.4922(3) 0.9023(2) 0.0434(16) Uani 1 1 d . . . . .
C21 C 0.5149(5) 0.4493(4) 0.9228(2) 0.062(2) Uani 1 1 d . . . . .
H21A H 0.5675 0.4506 0.9075 0.093 Uiso 1 1 calc R U . . .
H21B H 0.4940 0.4057 0.9238 0.093 Uiso 1 1 calc R U . . .
H21C H 0.5253 0.4645 0.9502 0.093 Uiso 1 1 calc R U . . .
C22 C 0.4827(5) 0.5598(4) 0.8990(2) 0.065(2) Uani 1 1 d . . . . .
H22A H 0.4433 0.5857 0.8834 0.098 Uiso 1 1 calc R U . . .
H22B H 0.5375 0.5591 0.8855 0.098 Uiso 1 1 calc R U . . .
H22C H 0.4890 0.5779 0.9260 0.098 Uiso 1 1 calc R U . . .
C23 C 0.3696(5) 0.4913(3) 0.92861(19) 0.0513(19) Uani 1 1 d . . . . .
H23A H 0.3838 0.5055 0.9558 0.077 Uiso 1 1 calc R U . . .
H23B H 0.3471 0.4480 0.9297 0.077 Uiso 1 1 calc R U . . .
H23C H 0.3272 0.5196 0.9171 0.077 Uiso 1 1 calc R U . . .
C24 C 0.2128(4) 0.3528(3) 1.05653(16) 0.0265(12) Uani 1 1 d . . . . .
C25 C 0.1989(4) 0.4144(3) 1.04608(18) 0.0373(15) Uani 1 1 d . . . . .
H25 H 0.1733 0.4250 1.0212 0.045 Uiso 1 1 calc R U . . .
C26 C 0.2239(4) 0.4618(3) 1.07349(18) 0.0362(15) Uani 1 1 d . . . . .
H26 H 0.2166 0.5050 1.0662 0.043 Uiso 1 1 calc R U . . .
C27 C 0.2578(4) 0.4482(2) 1.10955(18) 0.0313(14) Uani 1 1 d . . . . .
H27 H 0.2754 0.4817 1.1266 0.038 Uiso 1 1 calc R U . . .
C28 C 0.2675(4) 0.3837(2) 1.12254(17) 0.0285(14) Uani 1 1 d . . . . .
C29 C 0.1935(4) 0.2950(3) 1.03396(17) 0.0296(14) Uani 1 1 d . . . . .
H29 H 0.1384 0.2915 1.0196 0.035 Uiso 1 1 calc R U . . .
C30 C 0.2222(4) 0.1783(3) 0.99123(18) 0.0396(16) Uani 1 1 d . . . . .
C31 C 0.1488(4) 0.1511(3) 1.01552(19) 0.0373(15) Uani 1 1 d . . . . .
H31A H 0.1203 0.1183 0.9997 0.056 Uiso 1 1 calc R U . . .
H31B H 0.1090 0.1850 1.0219 0.056 Uiso 1 1 calc R U . . .
H31C H 0.1702 0.1325 1.0405 0.056 Uiso 1 1 calc R U . . .
C32 C 0.2832(5) 0.1237(4) 0.9834(3) 0.089(3) Uani 1 1 d . . . . .
H32A H 0.3070 0.1092 1.0090 0.134 Uiso 1 1 calc R U . . .
H32B H 0.3287 0.1382 0.9658 0.134 Uiso 1 1 calc R U . . .
H32C H 0.2531 0.0886 0.9705 0.134 Uiso 1 1 calc R U . . .
C33 C 0.1863(6) 0.2049(4) 0.9517(2) 0.078(3) Uani 1 1 d . . . . .
H33A H 0.2326 0.2182 0.9342 0.117 Uiso 1 1 calc R U . . .
H33B H 0.1503 0.2415 0.9576 0.117 Uiso 1 1 calc R U . . .
H33C H 0.1532 0.1721 0.9382 0.117 Uiso 1 1 calc R U . . .
C34 C 0.3722(4) 0.2730(3) 0.99949(17) 0.0351(15) Uani 1 1 d . . . . .
C35 C 0.4405(5) 0.2240(4) 1.0003(4) 0.120(5) Uani 1 1 d . . . . .
H35A H 0.4267 0.1898 0.9815 0.180 Uiso 1 1 calc R U . . .
H35B H 0.4456 0.2067 1.0275 0.180 Uiso 1 1 calc R U . . .
H35C H 0.4940 0.2435 0.9924 0.180 Uiso 1 1 calc R U . . .
C36 C 0.3578(6) 0.2946(6) 0.9576(3) 0.130(5) Uani 1 1 d . . . . .
H36A H 0.4113 0.3084 0.9459 0.195 Uiso 1 1 calc R U . . .
H36B H 0.3180 0.3300 0.9576 0.195 Uiso 1 1 calc R U . . .
H36C H 0.3348 0.2596 0.9417 0.195 Uiso 1 1 calc R U . . .
C37 C 0.4010(5) 0.3282(4) 1.0244(3) 0.087(3) Uani 1 1 d . . . . .
H37A H 0.4510 0.3472 1.0121 0.130 Uiso 1 1 calc R U . . .
H37B H 0.4147 0.3136 1.0516 0.130 Uiso 1 1 calc R U . . .
H37C H 0.3560 0.3599 1.0258 0.130 Uiso 1 1 calc R U . . .
C38 C 0.2895(4) 0.3639(3) 1.15953(17) 0.0362(15) Uani 1 1 d . . . . .
H38 H 0.3088 0.3928 1.1794 0.043 Uiso 1 1 calc R U . . .
C39 C 0.2162(6) 0.2738(3) 1.21617(19) 0.061(2) Uani 1 1 d . . . . .
C40 C 0.1369(6) 0.3137(4) 1.2096(2) 0.073(3) Uani 1 1 d . . . . .
H40A H 0.0989 0.3083 1.2326 0.109 Uiso 1 1 calc R U . . .
H40B H 0.1086 0.2998 1.1850 0.109 Uiso 1 1 calc R U . . .
H40C H 0.1525 0.3584 1.2071 0.109 Uiso 1 1 calc R U . . .
C41 C 0.2616(7) 0.2980(4) 1.2533(2) 0.092(4) Uani 1 1 d . . . . .
H41A H 0.2824 0.3410 1.2483 0.138 Uiso 1 1 calc R U . . .
H41B H 0.3090 0.2700 1.2595 0.138 Uiso 1 1 calc R U . . .
H41C H 0.2225 0.2986 1.2761 0.138 Uiso 1 1 calc R U . . .
C42 C 0.1891(6) 0.2039(4) 1.2218(2) 0.076(3) Uani 1 1 d . . . . .
H42A H 0.2381 0.1783 1.2292 0.114 Uiso 1 1 calc R U . . .
H42B H 0.1653 0.1879 1.1966 0.114 Uiso 1 1 calc R U . . .
H42C H 0.1466 0.2012 1.2431 0.114 Uiso 1 1 calc R U . . .
C43 C 0.3915(4) 0.2519(3) 1.1759(2) 0.0487(18) Uani 1 1 d . . . . .
C44 C 0.4449(5) 0.2954(4) 1.2024(3) 0.075(3) Uani 1 1 d . . . . .
H44A H 0.5033 0.2806 1.2024 0.112 Uiso 1 1 calc R U . . .
H44B H 0.4230 0.2948 1.2300 0.112 Uiso 1 1 calc R U . . .
H44C H 0.4426 0.3388 1.1919 0.112 Uiso 1 1 calc R U . . .
C45 C 0.3949(5) 0.1840(3) 1.1934(2) 0.061(2) Uani 1 1 d . . . . .
H45A H 0.3554 0.1568 1.1788 0.091 Uiso 1 1 calc R U . . .
H45B H 0.3795 0.1852 1.2219 0.091 Uiso 1 1 calc R U . . .
H45C H 0.4520 0.1671 1.1906 0.091 Uiso 1 1 calc R U . . .
C46 C 0.4279(4) 0.2528(3) 1.1335(2) 0.0520(19) Uani 1 1 d . . . . .
H46A H 0.4221 0.2954 1.1221 0.078 Uiso 1 1 calc R U . . .
H46B H 0.3974 0.2223 1.1167 0.078 Uiso 1 1 calc R U . . .
H46C H 0.4875 0.2411 1.1345 0.078 Uiso 1 1 calc R U . . .
N1 N 0.2534(3) 0.3990(2) 0.84757(13) 0.0265(11) Uani 1 1 d . . . . .
N2 N 0.2473(3) 0.33731(19) 1.09353(13) 0.0242(10) Uani 1 1 d . . . . .
P1 P 0.10526(12) 0.48964(8) 0.87012(5) 0.0415(4) Uani 1 1 d . . . . .
P2 P 0.41241(11) 0.45867(8) 0.85271(5) 0.0345(4) Uani 1 1 d . . . . .
P3 P 0.27490(10) 0.23941(7) 1.02341(4) 0.0291(3) Uani 1 1 d . . . . .
P4 P 0.28073(12) 0.28182(7) 1.16951(5) 0.0370(4) Uani 1 1 d . . . . .
Cl1 Cl 0.28565(16) 0.60225(7) 0.85191(6) 0.0687(6) Uani 1 1 d . . . . .
Cl2 Cl 0.25661(16) 0.50437(9) 0.75916(5) 0.0638(5) Uani 1 1 d . . . . .
Cl3 Cl 0.06683(10) 0.23428(7) 1.10989(5) 0.0429(4) Uani 1 1 d . . . . .
Cl4 Cl 0.25571(11) 0.13210(6) 1.11380(5) 0.0404(4) Uani 1 1 d . . . . .
Zr1 Zr 0.24906(5) 0.49573(2) 0.83043(2) 0.03601(15) Uani 1 1 d . . . . .
Zr2 Zr 0.21357(4) 0.23954(2) 1.09653(2) 0.02532(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.367(8) . ?
C1 N1 1.385(7) . ?
C1 C6 1.460(8) . ?
C1 Zr1 2.718(6) . ?
C2 C3 1.409(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.332(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.445(8) . ?
C4 H4 0.9500 . ?
C5 C15 1.358(9) . ?
C5 N1 1.386(7) . ?
C6 P1 1.776(6) . ?
C6 Zr1 2.382(7) . ?
C6 H6 1.0000 . ?
C7 C8 1.513(11) . ?
C7 C9 1.522(12) . ?
C7 C10 1.542(14) . ?
C7 P1 1.873(8) . ?
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 1.489(10) . ?
C11 C14 1.503(9) . ?
C11 C13 1.504(10) . ?
C11 P1 1.887(7) . ?
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 P2 1.757(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.515(10) . ?
C16 C19 1.534(11) . ?
C16 C18 1.547(11) . ?
C16 P2 1.870(7) . ?
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 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.528(9) . ?
C20 C23 1.533(9) . ?
C20 C21 1.545(9) . ?
C20 P2 1.888(7) . ?
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 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.362(8) . ?
C24 N2 1.387(7) . ?
C24 C29 1.465(7) . ?
C24 Zr2 2.736(5) . ?
C25 C26 1.412(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.346(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.438(7) . ?
C27 H27 0.9500 . ?
C28 C38 1.346(8) . ?
C28 N2 1.411(6) . ?
C29 P3 1.782(6) . ?
C29 Zr2 2.411(6) . ?
C29 H29 1.0000 . ?
C30 C32 1.528(10) . ?
C30 C31 1.531(9) . ?
C30 C33 1.540(10) . ?
C30 P3 1.874(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.484(10) . ?
C34 C35 1.501(10) . ?
C34 C37 1.502(9) . ?
C34 P3 1.878(6) . ?
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 P4 1.770(6) . ?
C38 H38 0.9500 . ?
C39 C41 1.519(11) . ?
C39 C40 1.530(11) . ?
C39 C42 1.549(10) . ?
C39 P4 1.869(8) . ?
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 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C46 1.526(10) . ?
C43 C44 1.530(9) . ?
C43 C45 1.547(9) . ?
C43 P4 1.883(7) . ?
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 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N1 Zr1 2.120(4) . ?
N2 Zr2 2.134(4) . ?
P1 Zr1 2.643(2) . ?
P2 Zr1 2.8113(19) . ?
P3 Zr2 2.6220(15) . ?
P4 Zr2 2.7994(17) . ?
Cl1 Zr1 2.4293(17) . ?
Cl2 Zr1 2.3821(17) . ?
Cl3 Zr2 2.3772(17) . ?
Cl4 Zr2 2.4327(15) . ?

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
C2 C1 N1 120.3(6) . . ?
C2 C1 C6 129.9(7) . . ?
N1 C1 C6 109.8(5) . . ?
C2 C1 Zr1 164.1(5) . . ?
N1 C1 Zr1 50.3(3) . . ?
C6 C1 Zr1 61.0(3) . . ?
C1 C2 C3 117.9(7) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 122.3(6) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 120.7(6) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C15 C5 N1 118.9(5) . . ?
C15 C5 C4 125.6(6) . . ?
N1 C5 C4 115.5(6) . . ?
C1 C6 P1 117.3(5) . . ?
C1 C6 Zr1 86.6(4) . . ?
P1 C6 Zr1 77.4(3) . . ?
C1 C6 H6 120.2 . . ?
P1 C6 H6 120.2 . . ?
Zr1 C6 H6 120.2 . . ?
C8 C7 C9 108.7(9) . . ?
C8 C7 C10 109.0(8) . . ?
C9 C7 C10 110.8(10) . . ?
C8 C7 P1 107.0(6) . . ?
C9 C7 P1 108.8(6) . . ?
C10 C7 P1 112.4(7) . . ?
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 108.1(7) . . ?
C12 C11 C13 110.4(8) . . ?
C14 C11 C13 109.1(7) . . ?
C12 C11 P1 109.9(5) . . ?
C14 C11 P1 108.4(5) . . ?
C13 C11 P1 110.9(6) . . ?
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 . . ?
C5 C15 P2 116.1(5) . . ?
C5 C15 H15 121.9 . . ?
P2 C15 H15 121.9 . . ?
C17 C16 C19 108.3(7) . . ?
C17 C16 C18 109.2(7) . . ?
C19 C16 C18 110.5(7) . . ?
C17 C16 P2 107.5(5) . . ?
C19 C16 P2 108.5(6) . . ?
C18 C16 P2 112.7(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 C23 110.1(6) . . ?
C22 C20 C21 109.8(6) . . ?
C23 C20 C21 107.4(6) . . ?
C22 C20 P2 113.2(5) . . ?
C23 C20 P2 104.0(4) . . ?
C21 C20 P2 112.0(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 N2 121.0(5) . . ?
C25 C24 C29 129.0(5) . . ?
N2 C24 C29 110.0(5) . . ?
C25 C24 Zr2 163.3(4) . . ?
N2 C24 Zr2 50.2(2) . . ?
C29 C24 Zr2 61.5(3) . . ?
C24 C25 C26 117.8(5) . . ?
C24 C25 H25 121.1 . . ?
C26 C25 H25 121.1 . . ?
C27 C26 C25 122.5(5) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C26 C27 C28 120.9(5) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C38 C28 N2 118.1(5) . . ?
C38 C28 C27 126.6(5) . . ?
N2 C28 C27 115.2(5) . . ?
C24 C29 P3 119.8(4) . . ?
C24 C29 Zr2 86.2(3) . . ?
P3 C29 Zr2 75.8(2) . . ?
C24 C29 H29 119.4 . . ?
P3 C29 H29 119.4 . . ?
Zr2 C29 H29 119.4 . . ?
C32 C30 C31 106.9(6) . . ?
C32 C30 C33 111.5(6) . . ?
C31 C30 C33 107.8(6) . . ?
C32 C30 P3 109.4(5) . . ?
C31 C30 P3 107.3(4) . . ?
C33 C30 P3 113.7(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 109.9(8) . . ?
C36 C34 C37 109.1(7) . . ?
C35 C34 C37 107.7(7) . . ?
C36 C34 P3 112.8(5) . . ?
C35 C34 P3 109.2(5) . . ?
C37 C34 P3 108.1(4) . . ?
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 . . ?
C28 C38 P4 117.0(4) . . ?
C28 C38 H38 121.5 . . ?
P4 C38 H38 121.5 . . ?
C41 C39 C40 108.8(7) . . ?
C41 C39 C42 110.7(6) . . ?
C40 C39 C42 108.1(8) . . ?
C41 C39 P4 112.7(7) . . ?
C40 C39 P4 106.5(5) . . ?
C42 C39 P4 109.8(5) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C46 C43 C44 108.4(7) . . ?
C46 C43 C45 110.3(6) . . ?
C44 C43 C45 108.6(6) . . ?
C46 C43 P4 104.2(4) . . ?
C44 C43 P4 112.5(5) . . ?
C45 C43 P4 112.7(5) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C1 N1 C5 122.7(5) . . ?
C1 N1 Zr1 99.6(4) . . ?
C5 N1 Zr1 135.1(4) . . ?
C24 N2 C28 122.3(4) . . ?
C24 N2 Zr2 99.8(3) . . ?
C28 N2 Zr2 134.0(4) . . ?
C6 P1 C7 103.9(3) . . ?
C6 P1 C11 114.3(3) . . ?
C7 P1 C11 113.5(4) . . ?
C6 P1 Zr1 61.6(2) . . ?
C7 P1 Zr1 110.7(3) . . ?
C11 P1 Zr1 134.9(2) . . ?
C15 P2 C16 106.1(3) . . ?
C15 P2 C20 105.5(3) . . ?
C16 P2 C20 113.0(3) . . ?
C15 P2 Zr1 100.4(2) . . ?
C16 P2 Zr1 115.9(3) . . ?
C20 P2 Zr1 114.2(2) . . ?
C29 P3 C30 104.0(3) . . ?
C29 P3 C34 115.6(3) . . ?
C30 P3 C34 112.7(3) . . ?
C29 P3 Zr2 63.02(19) . . ?
C30 P3 Zr2 111.4(2) . . ?
C34 P3 Zr2 134.4(2) . . ?
C38 P4 C39 106.7(3) . . ?
C38 P4 C43 106.0(3) . . ?
C39 P4 C43 112.9(4) . . ?
C38 P4 Zr2 100.3(2) . . ?
C39 P4 Zr2 118.9(3) . . ?
C43 P4 Zr2 110.4(2) . . ?
N1 Zr1 C6 62.0(2) . . ?
N1 Zr1 Cl2 109.88(13) . . ?
C6 Zr1 Cl2 93.81(16) . . ?
N1 Zr1 Cl1 143.48(13) . . ?
C6 Zr1 Cl1 133.74(16) . . ?
Cl2 Zr1 Cl1 102.14(7) . . ?
N1 Zr1 P1 81.17(14) . . ?
C6 Zr1 P1 40.97(15) . . ?
Cl2 Zr1 P1 123.02(8) . . ?
Cl1 Zr1 P1 96.02(7) . . ?
N1 Zr1 C1 30.16(18) . . ?
C6 Zr1 C1 32.4(2) . . ?
Cl2 Zr1 C1 99.58(13) . . ?
Cl1 Zr1 C1 155.44(13) . . ?
P1 Zr1 C1 62.17(13) . . ?
N1 Zr1 P2 68.38(14) . . ?
C6 Zr1 P2 130.35(16) . . ?
Cl2 Zr1 P2 103.74(7) . . ?
Cl1 Zr1 P2 87.62(7) . . ?
P1 Zr1 P2 130.79(6) . . ?
C1 Zr1 P2 98.26(14) . . ?
N2 Zr2 Cl3 107.48(13) . . ?
N2 Zr2 C29 61.51(17) . . ?
Cl3 Zr2 C29 93.12(15) . . ?
N2 Zr2 Cl4 147.44(13) . . ?
Cl3 Zr2 Cl4 100.51(6) . . ?
C29 Zr2 Cl4 133.90(14) . . ?
N2 Zr2 P3 82.19(12) . . ?
Cl3 Zr2 P3 122.58(6) . . ?
C29 Zr2 P3 41.21(14) . . ?
Cl4 Zr2 P3 96.66(5) . . ?
N2 Zr2 C24 29.97(16) . . ?
Cl3 Zr2 C24 97.32(13) . . ?
C29 Zr2 C24 32.28(17) . . ?
Cl4 Zr2 C24 158.48(13) . . ?
P3 Zr2 C24 63.31(12) . . ?
N2 Zr2 P4 68.70(12) . . ?
Cl3 Zr2 P4 103.11(6) . . ?
C29 Zr2 P4 130.19(14) . . ?
Cl4 Zr2 P4 89.25(5) . . ?
P3 Zr2 P4 131.61(6) . . ?
C24 Zr2 P4 98.36(12) . . ?

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 C1 C2 C3 5.5(9) . . . . ?
C6 C1 C2 C3 -176.4(6) . . . . ?
Zr1 C1 C2 C3 55(2) . . . . ?
C1 C2 C3 C4 -4.7(10) . . . . ?
C2 C3 C4 C5 -1.6(10) . . . . ?
C3 C4 C5 C15 -171.5(6) . . . . ?
C3 C4 C5 N1 6.9(9) . . . . ?
C2 C1 C6 P1 120.1(7) . . . . ?
N1 C1 C6 P1 -61.5(6) . . . . ?
Zr1 C1 C6 P1 -74.0(4) . . . . ?
C2 C1 C6 Zr1 -165.9(6) . . . . ?
N1 C1 C6 Zr1 12.4(4) . . . . ?
N1 C5 C15 P2 -6.9(8) . . . . ?
C4 C5 C15 P2 171.5(5) . . . . ?
N2 C24 C25 C26 2.5(9) . . . . ?
C29 C24 C25 C26 -179.8(6) . . . . ?
Zr2 C24 C25 C26 56.2(19) . . . . ?
C24 C25 C26 C27 -2.4(10) . . . . ?
C25 C26 C27 C28 -2.1(10) . . . . ?
C26 C27 C28 C38 -170.4(7) . . . . ?
C26 C27 C28 N2 6.1(9) . . . . ?
C25 C24 C29 P3 124.5(6) . . . . ?
N2 C24 C29 P3 -57.6(6) . . . . ?
Zr2 C24 C29 P3 -71.2(3) . . . . ?
C25 C24 C29 Zr2 -164.3(6) . . . . ?
N2 C24 C29 Zr2 13.6(4) . . . . ?
N2 C28 C38 P4 -6.1(8) . . . . ?
C27 C28 C38 P4 170.3(5) . . . . ?
C2 C1 N1 C5 0.1(8) . . . . ?
C6 C1 N1 C5 -178.4(5) . . . . ?
Zr1 C1 N1 C5 -164.2(6) . . . . ?
C2 C1 N1 Zr1 164.3(5) . . . . ?
C6 C1 N1 Zr1 -14.2(5) . . . . ?
C15 C5 N1 C1 172.3(5) . . . . ?
C4 C5 N1 C1 -6.2(8) . . . . ?
C15 C5 N1 Zr1 14.7(8) . . . . ?
C4 C5 N1 Zr1 -163.9(4) . . . . ?
C25 C24 N2 C28 1.8(9) . . . . ?
C29 C24 N2 C28 -176.3(5) . . . . ?
Zr2 C24 N2 C28 -160.6(6) . . . . ?
C25 C24 N2 Zr2 162.4(5) . . . . ?
C29 C24 N2 Zr2 -15.7(5) . . . . ?
C38 C28 N2 C24 170.8(6) . . . . ?
C27 C28 N2 C24 -5.9(8) . . . . ?
C38 C28 N2 Zr2 17.8(9) . . . . ?
C27 C28 N2 Zr2 -158.9(4) . . . . ?
C1 C6 P1 C7 -174.4(6) . . . . ?
Zr1 C6 P1 C7 106.2(4) . . . . ?
C1 C6 P1 C11 -50.2(6) . . . . ?
Zr1 C6 P1 C11 -129.6(3) . . . . ?
C1 C6 P1 Zr1 79.4(5) . . . . ?
C8 C7 P1 C6 -57.5(7) . . . . ?
C9 C7 P1 C6 -174.8(9) . . . . ?
C10 C7 P1 C6 62.0(7) . . . . ?
C8 C7 P1 C11 177.7(6) . . . . ?
C9 C7 P1 C11 60.4(10) . . . . ?
C10 C7 P1 C11 -62.7(7) . . . . ?
C8 C7 P1 Zr1 7.0(7) . . . . ?
C9 C7 P1 Zr1 -110.3(8) . . . . ?
C10 C7 P1 Zr1 126.5(6) . . . . ?
C12 C11 P1 C6 176.4(6) . . . . ?
C14 C11 P1 C6 58.4(6) . . . . ?
C13 C11 P1 C6 -61.3(8) . . . . ?
C12 C11 P1 C7 -64.6(7) . . . . ?
C14 C11 P1 C7 177.4(6) . . . . ?
C13 C11 P1 C7 57.7(8) . . . . ?
C12 C11 P1 Zr1 103.1(6) . . . . ?
C14 C11 P1 Zr1 -14.9(7) . . . . ?
C13 C11 P1 Zr1 -134.6(6) . . . . ?
C5 C15 P2 C16 -120.8(5) . . . . ?
C5 C15 P2 C20 119.1(5) . . . . ?
C5 C15 P2 Zr1 0.2(5) . . . . ?
C17 C16 P2 C15 49.0(6) . . . . ?
C19 C16 P2 C15 165.9(6) . . . . ?
C18 C16 P2 C15 -71.3(6) . . . . ?
C17 C16 P2 C20 164.1(5) . . . . ?
C19 C16 P2 C20 -79.0(7) . . . . ?
C18 C16 P2 C20 43.7(7) . . . . ?
C17 C16 P2 Zr1 -61.4(6) . . . . ?
C19 C16 P2 Zr1 55.6(6) . . . . ?
C18 C16 P2 Zr1 178.3(5) . . . . ?
C22 C20 P2 C15 168.6(5) . . . . ?
C23 C20 P2 C15 -71.9(5) . . . . ?
C21 C20 P2 C15 43.8(6) . . . . ?
C22 C20 P2 C16 53.2(6) . . . . ?
C23 C20 P2 C16 172.6(5) . . . . ?
C21 C20 P2 C16 -71.7(6) . . . . ?
C22 C20 P2 Zr1 -82.1(5) . . . . ?
C23 C20 P2 Zr1 37.3(5) . . . . ?
C21 C20 P2 Zr1 153.0(5) . . . . ?
C24 C29 P3 C30 -175.8(4) . . . . ?
Zr2 C29 P3 C30 107.2(2) . . . . ?
C24 C29 P3 C34 -51.7(5) . . . . ?
Zr2 C29 P3 C34 -128.8(2) . . . . ?
C24 C29 P3 Zr2 77.0(4) . . . . ?
C32 C30 P3 C29 -174.2(5) . . . . ?
C31 C30 P3 C29 -58.7(5) . . . . ?
C33 C30 P3 C29 60.4(6) . . . . ?
C32 C30 P3 C34 59.8(6) . . . . ?
C31 C30 P3 C34 175.4(4) . . . . ?
C33 C30 P3 C34 -65.6(6) . . . . ?
C32 C30 P3 Zr2 -108.1(5) . . . . ?
C31 C30 P3 Zr2 7.5(5) . . . . ?
C33 C30 P3 Zr2 126.5(5) . . . . ?
C36 C34 P3 C29 -69.1(7) . . . . ?
C35 C34 P3 C29 168.4(6) . . . . ?
C37 C34 P3 C29 51.6(6) . . . . ?
C36 C34 P3 C30 50.3(8) . . . . ?
C35 C34 P3 C30 -72.2(7) . . . . ?
C37 C34 P3 C30 171.0(6) . . . . ?
C36 C34 P3 Zr2 -145.6(6) . . . . ?
C35 C34 P3 Zr2 92.0(6) . . . . ?
C37 C34 P3 Zr2 -24.9(7) . . . . ?
C28 C38 P4 C39 -127.1(6) . . . . ?
C28 C38 P4 C43 112.3(6) . . . . ?
C28 C38 P4 Zr2 -2.6(6) . . . . ?
C41 C39 P4 C38 -68.5(6) . . . . ?
C40 C39 P4 C38 50.7(6) . . . . ?
C42 C39 P4 C38 167.6(6) . . . . ?
C41 C39 P4 C43 47.5(6) . . . . ?
C40 C39 P4 C43 166.8(5) . . . . ?
C42 C39 P4 C43 -76.4(7) . . . . ?
C41 C39 P4 Zr2 179.2(4) . . . . ?
C40 C39 P4 Zr2 -61.6(6) . . . . ?
C42 C39 P4 Zr2 55.3(7) . . . . ?
C46 C43 P4 C38 -72.3(5) . . . . ?
C44 C43 P4 C38 44.9(6) . . . . ?
C45 C43 P4 C38 168.1(5) . . . . ?
C46 C43 P4 C39 171.2(4) . . . . ?
C44 C43 P4 C39 -71.5(6) . . . . ?
C45 C43 P4 C39 51.7(6) . . . . ?
C46 C43 P4 Zr2 35.5(5) . . . . ?
C44 C43 P4 Zr2 152.7(5) . . . . ?
C45 C43 P4 Zr2 -84.1(5) . . . . ?

_refine_diff_density_max         0.743
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.099

_shelxl_version_number           2013-4

