Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Roesky, H. W.'
'Bai, Guangcai'
'Noltemeyer, Mathias'
'Schmidt, Hans-Georg'

_publ_contact_author_name     	'Prof H W Roesky'  
_publ_contact_author_address 
;
Institut fur Anorganische Chemie
Universitat Gottingen
Tammannstrasse 4
Gottingen
37077
GERMANY
;

_publ_contact_author_email       'HROESKY@GWDG.DE'

_publ_section_title		
;
The Formation of an Imido Zirconium Compound by Migration of the
Imido Group from Phosphorus to Zirconium
;

data_roe900y

_database_code_CSD	178315


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
compound 1 
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C32 H73 Cl N8 P4 Zr'
_chemical_formula_weight          820.53

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'
'Zr'  'Zr'  -2.9673   0.5597
'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'

_symmetry_cell_setting           monoclinic 
_symmetry_space_group_name_H-M    P21/n

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

_cell_length_a                    14.7679(16)
_cell_length_b                    19.227(3)
_cell_length_c                    15.448(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.732(12)
_cell_angle_gamma                 90.00
_cell_volume                      4384.4(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     203(2)
_cell_measurement_reflns_used     30
_cell_measurement_theta_min       10
_cell_measurement_theta_max       12.5

_exptl_crystal_description        blocks
_exptl_crystal_colour             'pale yellow'
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.40
_exptl_crystal_size_min           0.40
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.243
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1752
_exptl_absorpt_coefficient_mu     0.489
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   0.8285
_exptl_absorpt_correction_T_max   0.8285
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       203(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'STOE AED2'
_diffrn_measurement_method        'profile fit'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   '90 min'
_diffrn_standards_decay_%         none
_diffrn_reflns_number             7716
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0295
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          3.63
_diffrn_reflns_theta_max          25.02
_reflns_number_total              7716
_reflns_number_gt                 6482
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        DIF4
_computing_cell_refinement        DIF4
_computing_data_reduction         REDU4
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     SHELXTL
_computing_publication_material   SHELXTL

_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+5.1700P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7716
_refine_ls_number_parameters      439
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0495
_refine_ls_R_factor_gt            0.0372
_refine_ls_wR_factor_ref          0.0873
_refine_ls_wR_factor_gt           0.0792
_refine_ls_goodness_of_fit_ref    1.076
_refine_ls_restrained_S_all       1.076
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.308919(17) 0.061082(13) 0.247549(16) 0.02084(8) Uani 1 1 d . . .
Cl1 Cl 0.30821(5) -0.06734(3) 0.23957(5) 0.03545(17) Uani 1 1 d . . .
P1 P 0.14418(5) 0.10138(4) 0.34518(5) 0.02723(16) Uani 1 1 d . . .
P2 P 0.12830(5) 0.10661(4) 0.17336(5) 0.02724(16) Uani 1 1 d . . .
P3 P 0.45158(5) 0.14680(4) 0.24428(4) 0.02257(15) Uani 1 1 d . . .
P4 P 0.57027(5) 0.24782(4) 0.24047(5) 0.02877(17) Uani 1 1 d . . .
N1 N 0.24103(15) 0.05579(12) 0.36517(14) 0.0260(5) Uani 1 1 d . . .
N2 N 0.19419(14) 0.14702(11) 0.25806(14) 0.0234(5) Uani 1 1 d . . .
N3 N 0.08070(15) 0.06513(12) 0.26074(15) 0.0302(5) Uani 1 1 d . . .
N4 N 0.22026(15) 0.06306(12) 0.13845(14) 0.0268(5) Uani 1 1 d . . .
N5 N 0.50989(15) 0.19409(12) 0.16998(14) 0.0277(5) Uani 1 1 d . . .
N6 N 0.45826(15) 0.06226(11) 0.24184(14) 0.0248(5) Uani 1 1 d . . .
N7 N 0.67861(16) 0.22446(13) 0.23341(17) 0.0369(6) Uani 1 1 d . . .
H7A H 0.6885 0.1800 0.2300 0.044 Uiso 1 1 calc R . .
N8 N 0.52282(15) 0.19159(12) 0.31446(14) 0.0262(5) Uani 1 1 d . . .
C11 C 0.2492(2) 0.01525(15) 0.44791(18) 0.0315(7) Uani 1 1 d . . .
C12 C 0.1806(2) -0.04437(18) 0.4479(2) 0.0462(8) Uani 1 1 d . . .
H12A H 0.1879 -0.0729 0.3967 0.069 Uiso 1 1 calc R . .
H12B H 0.1197 -0.0255 0.4475 0.069 Uiso 1 1 calc R . .
H12C H 0.1906 -0.0726 0.4993 0.069 Uiso 1 1 calc R . .
C13 C 0.3440(2) -0.01563(17) 0.4567(2) 0.0412(8) Uani 1 1 d . . .
H13A H 0.3530 -0.0484 0.4101 0.062 Uiso 1 1 calc R . .
H13B H 0.3508 -0.0395 0.5119 0.062 Uiso 1 1 calc R . .
H13C H 0.3885 0.0213 0.4539 0.062 Uiso 1 1 calc R . .
C14 C 0.2341(3) 0.06340(18) 0.52518(19) 0.0462(8) Uani 1 1 d . . .
H14A H 0.1729 0.0817 0.5217 0.069 Uiso 1 1 calc R . .
H14B H 0.2771 0.1015 0.5242 0.069 Uiso 1 1 calc R . .
H14C H 0.2428 0.0374 0.5786 0.069 Uiso 1 1 calc R . .
C21 C 0.19110(19) 0.22554(14) 0.26193(19) 0.0300(6) Uani 1 1 d . . .
C22 C 0.0929(2) 0.25090(16) 0.2642(2) 0.0418(8) Uani 1 1 d . . .
H22A H 0.0608 0.2372 0.2112 0.063 Uiso 1 1 calc R . .
H22B H 0.0921 0.3012 0.2694 0.063 Uiso 1 1 calc R . .
H22C H 0.0636 0.2304 0.3134 0.063 Uiso 1 1 calc R . .
C23 C 0.2367(2) 0.25394(15) 0.1820(2) 0.0394(7) Uani 1 1 d . . .
H23A H 0.3001 0.2407 0.1837 0.059 Uiso 1 1 calc R . .
H23B H 0.2319 0.3042 0.1812 0.059 Uiso 1 1 calc R . .
H23C H 0.2071 0.2350 0.1303 0.059 Uiso 1 1 calc R . .
C24 C 0.2432(2) 0.24848(16) 0.3436(2) 0.0401(7) Uani 1 1 d . . .
H24A H 0.3051 0.2318 0.3417 0.060 Uiso 1 1 calc R . .
H24B H 0.2146 0.2294 0.3940 0.060 Uiso 1 1 calc R . .
H24C H 0.2432 0.2989 0.3470 0.060 Uiso 1 1 calc R . .
C31 C -0.0056(2) 0.02618(19) 0.2644(2) 0.0462(8) Uani 1 1 d . . .
C32 C -0.0507(2) 0.0429(3) 0.3496(2) 0.0655(12) Uani 1 1 d . . .
H32A H -0.0125 0.0266 0.3977 0.098 Uiso 1 1 calc R . .
H32B H -0.1091 0.0200 0.3509 0.098 Uiso 1 1 calc R . .
H32C H -0.0589 0.0928 0.3544 0.098 Uiso 1 1 calc R . .
C33 C -0.0685(2) 0.0503(2) 0.1894(3) 0.0649(12) Uani 1 1 d . . .
H33A H -0.0784 0.1001 0.1939 0.097 Uiso 1 1 calc R . .
H33B H -0.1260 0.0262 0.1921 0.097 Uiso 1 1 calc R . .
H33C H -0.0407 0.0400 0.1347 0.097 Uiso 1 1 calc R . .
C34 C 0.0115(3) -0.0516(2) 0.2578(3) 0.0670(12) Uani 1 1 d . . .
H34A H 0.0515 -0.0662 0.3054 0.101 Uiso 1 1 calc R . .
H34B H 0.0396 -0.0618 0.2033 0.101 Uiso 1 1 calc R . .
H34C H -0.0455 -0.0763 0.2606 0.101 Uiso 1 1 calc R . .
C41 C 0.2114(2) 0.02808(16) 0.05127(18) 0.0357(7) Uani 1 1 d . . .
C42 C 0.1424(3) -0.03099(19) 0.0541(2) 0.0512(9) Uani 1 1 d . . .
H42A H 0.1596 -0.0630 0.1003 0.077 Uiso 1 1 calc R . .
H42B H 0.1409 -0.0555 -0.0008 0.077 Uiso 1 1 calc R . .
H42C H 0.0829 -0.0120 0.0648 0.077 Uiso 1 1 calc R . .
C43 C 0.3023(3) -0.0026(2) 0.0280(2) 0.0555(10) Uani 1 1 d . . .
H43A H 0.3199 -0.0379 0.0702 0.083 Uiso 1 1 calc R . .
H43B H 0.3476 0.0339 0.0280 0.083 Uiso 1 1 calc R . .
H43C H 0.2973 -0.0235 -0.0291 0.083 Uiso 1 1 calc R . .
C44 C 0.1825(3) 0.0817(2) -0.0179(2) 0.0566(10) Uani 1 1 d . . .
H44A H 0.1232 0.1001 -0.0048 0.085 Uiso 1 1 calc R . .
H44B H 0.1797 0.0596 -0.0743 0.085 Uiso 1 1 calc R . .
H44C H 0.2261 0.1194 -0.0181 0.085 Uiso 1 1 calc R . .
C51 C 0.4973(2) 0.20544(16) 0.07510(18) 0.0349(7) Uani 1 1 d . . .
C52 C 0.4880(6) 0.2809(2) 0.0561(3) 0.139(3) Uani 1 1 d . . .
H52A H 0.4385 0.3000 0.0884 0.209 Uiso 1 1 calc R . .
H52B H 0.4757 0.2874 -0.0054 0.209 Uiso 1 1 calc R . .
H52C H 0.5439 0.3046 0.0728 0.209 Uiso 1 1 calc R . .
C53 C 0.4160(3) 0.1677(3) 0.0412(2) 0.098(2) Uani 1 1 d . . .
H53A H 0.3618 0.1903 0.0615 0.147 Uiso 1 1 calc R . .
H53B H 0.4178 0.1200 0.0615 0.147 Uiso 1 1 calc R . .
H53C H 0.4151 0.1682 -0.0216 0.147 Uiso 1 1 calc R . .
C54 C 0.5778(3) 0.1752(4) 0.0304(3) 0.118(3) Uani 1 1 d . . .
H54A H 0.6330 0.1958 0.0543 0.176 Uiso 1 1 calc R . .
H54B H 0.5726 0.1850 -0.0311 0.176 Uiso 1 1 calc R . .
H54C H 0.5795 0.1253 0.0394 0.176 Uiso 1 1 calc R . .
C61 C 0.53576(19) 0.01177(15) 0.23749(19) 0.0305(6) Uani 1 1 d . . .
C62 C 0.5338(2) -0.03685(17) 0.3157(2) 0.0410(8) Uani 1 1 d . . .
H62A H 0.4779 -0.0634 0.3137 0.062 Uiso 1 1 calc R . .
H62B H 0.5372 -0.0096 0.3685 0.062 Uiso 1 1 calc R . .
H62C H 0.5850 -0.0684 0.3144 0.062 Uiso 1 1 calc R . .
C63 C 0.6271(2) 0.04946(17) 0.2379(2) 0.0411(8) Uani 1 1 d . . .
H63A H 0.6291 0.0802 0.1882 0.062 Uiso 1 1 calc R . .
H63B H 0.6756 0.0156 0.2351 0.062 Uiso 1 1 calc R . .
H63C H 0.6344 0.0765 0.2907 0.062 Uiso 1 1 calc R . .
C64 C 0.5257(2) -0.03074(17) 0.1542(2) 0.0397(7) Uani 1 1 d . . .
H64A H 0.4698 -0.0572 0.1548 0.060 Uiso 1 1 calc R . .
H64B H 0.5766 -0.0623 0.1501 0.060 Uiso 1 1 calc R . .
H64C H 0.5243 0.0004 0.1047 0.060 Uiso 1 1 calc R . .
C71 C 0.7602(2) 0.26921(18) 0.2321(2) 0.0427(8) Uani 1 1 d . . .
C72 C 0.8067(3) 0.2588(2) 0.1460(3) 0.0632(11) Uani 1 1 d . . .
H72A H 0.8226 0.2102 0.1394 0.095 Uiso 1 1 calc R . .
H72B H 0.8611 0.2870 0.1451 0.095 Uiso 1 1 calc R . .
H72C H 0.7658 0.2726 0.0987 0.095 Uiso 1 1 calc R . .
C73 C 0.8250(2) 0.2471(3) 0.3056(3) 0.0747(13) Uani 1 1 d . . .
H73A H 0.8384 0.1979 0.3003 0.112 Uiso 1 1 calc R . .
H73B H 0.7972 0.2556 0.3607 0.112 Uiso 1 1 calc R . .
H73C H 0.8807 0.2736 0.3028 0.112 Uiso 1 1 calc R . .
C74 C 0.7330(3) 0.34486(19) 0.2419(3) 0.0609(11) Uani 1 1 d . . .
H74A H 0.7035 0.3511 0.2967 0.091 Uiso 1 1 calc R . .
H74B H 0.6916 0.3578 0.1948 0.091 Uiso 1 1 calc R . .
H74C H 0.7866 0.3740 0.2407 0.091 Uiso 1 1 calc R . .
C81 C 0.5208(2) 0.20571(16) 0.40892(18) 0.0338(7) Uani 1 1 d . . .
C82 C 0.4817(2) 0.27758(18) 0.4277(2) 0.0477(9) Uani 1 1 d . . .
H82A H 0.4191 0.2795 0.4070 0.072 Uiso 1 1 calc R . .
H82B H 0.5165 0.3128 0.3984 0.072 Uiso 1 1 calc R . .
H82C H 0.4847 0.2861 0.4896 0.072 Uiso 1 1 calc R . .
C83 C 0.4663(2) 0.14943(18) 0.45209(19) 0.0409(8) Uani 1 1 d . . .
H83A H 0.4046 0.1500 0.4287 0.061 Uiso 1 1 calc R . .
H83B H 0.4660 0.1578 0.5140 0.061 Uiso 1 1 calc R . .
H83C H 0.4933 0.1044 0.4412 0.061 Uiso 1 1 calc R . .
C84 C 0.6189(2) 0.2033(2) 0.4451(2) 0.0490(9) Uani 1 1 d . . .
H84A H 0.6461 0.1591 0.4303 0.073 Uiso 1 1 calc R . .
H84B H 0.6191 0.2084 0.5076 0.073 Uiso 1 1 calc R . .
H84C H 0.6533 0.2409 0.4202 0.073 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.02526(14) 0.01716(13) 0.02019(13) 0.00022(10) 0.00235(10) -0.00047(11)
Cl1 0.0463(4) 0.0182(3) 0.0419(4) -0.0003(3) 0.0016(3) -0.0011(3)
P1 0.0285(4) 0.0270(4) 0.0265(4) -0.0024(3) 0.0057(3) -0.0016(3)
P2 0.0287(4) 0.0254(4) 0.0274(4) -0.0011(3) -0.0023(3) 0.0001(3)
P3 0.0250(3) 0.0202(4) 0.0225(3) 0.0001(3) 0.0025(3) -0.0003(3)
P4 0.0305(4) 0.0247(4) 0.0312(4) 0.0010(3) 0.0040(3) -0.0037(3)
N1 0.0306(12) 0.0253(12) 0.0224(11) 0.0038(10) 0.0034(9) -0.0030(10)
N2 0.0287(12) 0.0178(11) 0.0237(11) -0.0006(9) 0.0002(9) -0.0021(10)
N3 0.0282(12) 0.0312(13) 0.0314(13) -0.0008(11) 0.0024(10) -0.0077(11)
N4 0.0330(12) 0.0249(12) 0.0224(11) -0.0020(10) -0.0003(9) -0.0003(10)
N5 0.0306(12) 0.0278(13) 0.0250(12) 0.0028(10) 0.0035(10) -0.0049(10)
N6 0.0274(12) 0.0208(12) 0.0262(12) -0.0022(10) 0.0035(9) 0.0016(10)
N7 0.0325(13) 0.0265(13) 0.0522(16) 0.0029(12) 0.0058(12) -0.0034(11)
N8 0.0299(12) 0.0255(12) 0.0232(11) -0.0005(10) 0.0031(9) -0.0058(10)
C11 0.0416(17) 0.0303(16) 0.0228(14) 0.0056(12) 0.0037(12) -0.0055(13)
C12 0.056(2) 0.043(2) 0.0404(18) 0.0133(16) 0.0092(16) -0.0112(17)
C13 0.0461(19) 0.0411(19) 0.0363(17) 0.0131(15) -0.0033(14) -0.0009(15)
C14 0.067(2) 0.049(2) 0.0231(15) 0.0011(15) 0.0047(15) -0.0053(18)
C21 0.0337(15) 0.0163(13) 0.0402(17) -0.0032(12) 0.0020(13) 0.0038(12)
C22 0.0385(17) 0.0290(16) 0.058(2) -0.0049(15) 0.0021(15) 0.0082(14)
C23 0.0472(18) 0.0230(15) 0.0482(19) 0.0071(14) 0.0065(15) 0.0042(14)
C24 0.0461(18) 0.0272(16) 0.0465(19) -0.0072(14) -0.0045(15) 0.0009(14)
C31 0.0338(17) 0.055(2) 0.050(2) -0.0039(17) 0.0053(15) -0.0205(16)
C32 0.0355(19) 0.104(4) 0.058(2) 0.000(2) 0.0153(17) -0.023(2)
C33 0.037(2) 0.096(3) 0.062(2) -0.001(2) -0.0090(17) -0.021(2)
C34 0.079(3) 0.052(2) 0.071(3) -0.003(2) 0.003(2) -0.037(2)
C41 0.0507(19) 0.0343(17) 0.0221(14) -0.0060(13) -0.0011(13) 0.0043(15)
C42 0.068(2) 0.045(2) 0.0397(19) -0.0154(17) -0.0078(17) -0.0066(18)
C43 0.069(2) 0.065(3) 0.0331(18) -0.0147(18) 0.0104(17) 0.013(2)
C44 0.088(3) 0.056(2) 0.0252(16) -0.0019(16) -0.0074(17) 0.008(2)
C51 0.0432(17) 0.0372(17) 0.0245(14) 0.0053(13) 0.0057(13) -0.0032(14)
C52 0.330(10) 0.044(3) 0.042(3) 0.018(2) -0.035(4) -0.006(4)
C53 0.086(3) 0.178(6) 0.029(2) 0.008(3) -0.009(2) -0.062(4)
C54 0.089(4) 0.230(8) 0.035(2) -0.004(3) 0.018(2) 0.064(4)
C61 0.0288(15) 0.0244(15) 0.0383(16) -0.0007(13) 0.0026(12) 0.0083(12)
C62 0.0410(18) 0.0364(18) 0.0455(19) 0.0061(15) -0.0002(15) 0.0130(15)
C63 0.0289(16) 0.0350(18) 0.060(2) -0.0042(16) 0.0049(14) 0.0060(14)
C64 0.0423(18) 0.0315(17) 0.0457(19) -0.0079(15) 0.0090(15) 0.0070(14)
C71 0.0303(16) 0.048(2) 0.051(2) -0.0016(16) 0.0076(14) -0.0085(15)
C72 0.051(2) 0.067(3) 0.073(3) 0.000(2) 0.028(2) -0.010(2)
C73 0.037(2) 0.107(4) 0.079(3) 0.004(3) -0.0047(19) -0.013(2)
C74 0.048(2) 0.047(2) 0.089(3) -0.013(2) 0.021(2) -0.0236(18)
C81 0.0382(16) 0.0360(17) 0.0270(15) -0.0024(13) -0.0017(12) -0.0078(14)
C82 0.056(2) 0.043(2) 0.0445(19) -0.0185(16) 0.0046(16) -0.0072(17)
C83 0.0480(19) 0.049(2) 0.0256(15) -0.0013(14) 0.0042(13) -0.0114(16)
C84 0.0419(19) 0.067(2) 0.0371(18) 0.0023(17) -0.0071(15) -0.0110(18)

_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 N4 2.103(2) . ?
Zr1 N1 2.104(2) . ?
Zr1 N6 2.210(2) . ?
Zr1 N2 2.376(2) . ?
Zr1 Cl1 2.4723(8) . ?
Zr1 P3 2.6766(8) . ?
Zr1 P2 3.0016(8) . ?
Zr1 P1 3.0027(8) . ?
P1 N1 1.698(2) . ?
P1 N3 1.730(2) . ?
P1 N2 1.785(2) . ?
P1 P2 2.6594(11) . ?
P2 N4 1.697(2) . ?
P2 N3 1.735(2) . ?
P2 N2 1.785(2) . ?
P3 N6 1.629(2) . ?
P3 N5 1.716(2) . ?
P3 N8 1.719(2) . ?
P3 P4 2.6181(10) . ?
P4 N7 1.668(2) . ?
P4 N5 1.729(2) . ?
P4 N8 1.736(2) . ?
N1 C11 1.499(3) . ?
N2 C21 1.512(3) . ?
N3 C31 1.481(4) . ?
N4 C41 1.508(3) . ?
N5 C51 1.488(3) . ?
N6 C61 1.504(3) . ?
N7 C71 1.481(4) . ?
N8 C81 1.485(3) . ?
C11 C13 1.523(4) . ?
C11 C12 1.530(4) . ?
C11 C14 1.532(4) . ?
C21 C24 1.523(4) . ?
C21 C23 1.525(4) . ?
C21 C22 1.531(4) . ?
C31 C34 1.520(5) . ?
C31 C32 1.527(5) . ?
C31 C33 1.534(5) . ?
C41 C43 1.520(5) . ?
C41 C42 1.527(5) . ?
C41 C44 1.536(4) . ?
C51 C53 1.485(5) . ?
C51 C52 1.486(5) . ?
C51 C54 1.509(5) . ?
C61 C64 1.528(4) . ?
C61 C62 1.528(4) . ?
C61 C63 1.531(4) . ?
C71 C74 1.518(5) . ?
C71 C73 1.523(5) . ?
C71 C72 1.529(5) . ?
C81 C83 1.515(4) . ?
C81 C82 1.529(4) . ?
C81 C84 1.537(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Zr1 N1 113.05(9) . . ?
N4 Zr1 N6 124.46(8) . . ?
N1 Zr1 N6 122.48(8) . . ?
N4 Zr1 N2 67.30(8) . . ?
N1 Zr1 N2 67.37(8) . . ?
N6 Zr1 N2 135.26(8) . . ?
N4 Zr1 Cl1 88.66(7) . . ?
N1 Zr1 Cl1 89.62(7) . . ?
N6 Zr1 Cl1 90.63(6) . . ?
N2 Zr1 Cl1 134.12(6) . . ?
N4 Zr1 P3 116.43(6) . . ?
N1 Zr1 P3 116.23(6) . . ?
N6 Zr1 P3 37.43(6) . . ?
N2 Zr1 P3 97.84(5) . . ?
Cl1 Zr1 P3 128.04(3) . . ?
N4 Zr1 P2 33.30(6) . . ?
N1 Zr1 P2 84.42(6) . . ?
N6 Zr1 P2 149.11(6) . . ?
N2 Zr1 P2 36.48(5) . . ?
Cl1 Zr1 P2 105.66(2) . . ?
P3 Zr1 P2 120.28(2) . . ?
N4 Zr1 P1 84.47(6) . . ?
N1 Zr1 P1 33.31(6) . . ?
N6 Zr1 P1 147.36(6) . . ?
N2 Zr1 P1 36.47(5) . . ?
Cl1 Zr1 P1 106.29(2) . . ?
P3 Zr1 P1 120.05(2) . . ?
P2 Zr1 P1 52.58(2) . . ?
N1 P1 N3 111.31(12) . . ?
N1 P1 N2 91.46(10) . . ?
N3 P1 N2 81.76(11) . . ?
N1 P1 P2 104.44(8) . . ?
N3 P1 P2 39.93(8) . . ?
N2 P1 P2 41.84(7) . . ?
N1 P1 Zr1 42.88(7) . . ?
N3 P1 Zr1 86.91(8) . . ?
N2 P1 Zr1 52.28(7) . . ?
P2 P1 Zr1 63.69(2) . . ?
N4 P2 N3 111.56(12) . . ?
N4 P2 N2 91.38(11) . . ?
N3 P2 N2 81.64(11) . . ?
N4 P2 P1 104.55(8) . . ?
N3 P2 P1 39.80(8) . . ?
N2 P2 P1 41.85(7) . . ?
N4 P2 Zr1 42.87(7) . . ?
N3 P2 Zr1 86.86(8) . . ?
N2 P2 Zr1 52.31(7) . . ?
P1 P2 Zr1 63.73(2) . . ?
N6 P3 N5 118.77(12) . . ?
N6 P3 N8 118.56(12) . . ?
N5 P3 N8 81.17(11) . . ?
N6 P3 P4 134.33(9) . . ?
N5 P3 P4 40.72(8) . . ?
N8 P3 P4 40.99(8) . . ?
N6 P3 Zr1 55.55(8) . . ?
N5 P3 Zr1 138.59(8) . . ?
N8 P3 Zr1 139.79(8) . . ?
P4 P3 Zr1 170.11(3) . . ?
N7 P4 N5 105.98(12) . . ?
N7 P4 N8 106.40(12) . . ?
N5 P4 N8 80.32(11) . . ?
N7 P4 P3 116.47(9) . . ?
N5 P4 P3 40.36(8) . . ?
N8 P4 P3 40.49(7) . . ?
C11 N1 P1 117.99(18) . . ?
C11 N1 Zr1 137.17(18) . . ?
P1 N1 Zr1 103.81(11) . . ?
C21 N2 P2 116.58(17) . . ?
C21 N2 P1 116.59(18) . . ?
P2 N2 P1 96.31(11) . . ?
C21 N2 Zr1 136.03(17) . . ?
P2 N2 Zr1 91.21(9) . . ?
P1 N2 Zr1 91.25(9) . . ?
C31 N3 P1 128.5(2) . . ?
C31 N3 P2 129.2(2) . . ?
P1 N3 P2 100.28(12) . . ?
C41 N4 P2 117.08(18) . . ?
C41 N4 Zr1 137.99(18) . . ?
P2 N4 Zr1 103.83(11) . . ?
C51 N5 P3 133.32(19) . . ?
C51 N5 P4 125.42(19) . . ?
P3 N5 P4 98.92(12) . . ?
C61 N6 P3 133.78(19) . . ?
C61 N6 Zr1 139.20(17) . . ?
P3 N6 Zr1 87.02(10) . . ?
C71 N7 P4 128.8(2) . . ?
C81 N8 P3 132.92(18) . . ?
C81 N8 P4 123.60(18) . . ?
P3 N8 P4 98.53(11) . . ?
N1 C11 C13 109.2(2) . . ?
N1 C11 C12 110.7(2) . . ?
C13 C11 C12 108.4(3) . . ?
N1 C11 C14 109.9(2) . . ?
C13 C11 C14 108.7(3) . . ?
C12 C11 C14 109.9(3) . . ?
N2 C21 C24 107.9(2) . . ?
N2 C21 C23 108.1(2) . . ?
C24 C21 C23 110.0(3) . . ?
N2 C21 C22 110.4(2) . . ?
C24 C21 C22 110.1(2) . . ?
C23 C21 C22 110.2(3) . . ?
N3 C31 C34 110.4(3) . . ?
N3 C31 C32 108.9(3) . . ?
C34 C31 C32 110.0(3) . . ?
N3 C31 C33 108.7(3) . . ?
C34 C31 C33 110.2(3) . . ?
C32 C31 C33 108.6(3) . . ?
N4 C41 C43 109.4(2) . . ?
N4 C41 C42 110.2(2) . . ?
C43 C41 C42 108.2(3) . . ?
N4 C41 C44 109.7(3) . . ?
C43 C41 C44 109.0(3) . . ?
C42 C41 C44 110.4(3) . . ?
C53 C51 C52 109.8(4) . . ?
C53 C51 N5 110.6(3) . . ?
C52 C51 N5 110.3(3) . . ?
C53 C51 C54 106.9(4) . . ?
C52 C51 C54 110.8(5) . . ?
N5 C51 C54 108.5(3) . . ?
N6 C61 C64 109.1(2) . . ?
N6 C61 C62 109.1(2) . . ?
C64 C61 C62 109.6(3) . . ?
N6 C61 C63 111.5(2) . . ?
C64 C61 C63 108.7(2) . . ?
C62 C61 C63 108.9(3) . . ?
N7 C71 C74 109.7(3) . . ?
N7 C71 C73 108.7(3) . . ?
C74 C71 C73 110.8(3) . . ?
N7 C71 C72 108.8(3) . . ?
C74 C71 C72 109.8(3) . . ?
C73 C71 C72 108.9(3) . . ?
N8 C81 C83 109.2(2) . . ?
N8 C81 C82 111.8(2) . . ?
C83 C81 C82 110.7(3) . . ?
N8 C81 C84 107.8(2) . . ?
C83 C81 C84 109.0(3) . . ?
C82 C81 C84 108.4(3) . . ?

_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.504
_refine_diff_density_min   -0.424
_refine_diff_density_rms    0.061

data_roe912x

_database_code_CSD	178316


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
compound 2 
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C42.50 H85  K N8 P4 Zr incl. 1.5 toluene'
_chemical_formula_weight          962.39

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'
'Zr'  'Zr'  -2.9673   0.5597
'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'
'K'  'K'   0.2009   0.2494
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1

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

_cell_length_a                    11.070(6)
_cell_length_b                    13.937(12)
_cell_length_c                    18.628(15)
_cell_angle_alpha                 72.35(6)
_cell_angle_beta                  85.56(5)
_cell_angle_gamma                 82.79(6)
_cell_volume                      2715(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     200(2)
_cell_measurement_reflns_used     29
_cell_measurement_theta_min       10
_cell_measurement_theta_max       12.5

_exptl_crystal_description        blocks
_exptl_crystal_colour             none
_exptl_crystal_size_max           1.20
_exptl_crystal_size_mid           0.30
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.177
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1030
_exptl_absorpt_coefficient_mu     0.432
_exptl_absorpt_correction_type    'azimuthal scans'
_exptl_absorpt_correction_T_min   0.6254
_exptl_absorpt_correction_T_max   0.9186
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       200(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             16403
_diffrn_reflns_av_R_equivalents   0.0511
_diffrn_reflns_av_sigmaI/netI     0.0579
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          3.53
_diffrn_reflns_theta_max          25.00
_reflns_number_total              9538
_reflns_number_gt                 7557
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        DIF4
_computing_cell_refinement        DIF4
_computing_data_reduction         REDU4
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     SHELXTL
_computing_publication_material   SHELXTL

_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+2.7600P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          9538
_refine_ls_number_parameters      546
_refine_ls_number_restraints      624
_refine_ls_R_factor_all           0.0647
_refine_ls_R_factor_gt            0.0453
_refine_ls_wR_factor_ref          0.1135
_refine_ls_wR_factor_gt           0.1018
_refine_ls_goodness_of_fit_ref    1.061
_refine_ls_restrained_S_all       1.044
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.25856(3) 0.34818(2) 0.305715(17) 0.02846(9) Uani 1 1 d U . .
P1 P 0.13578(8) 0.56035(6) 0.24078(5) 0.0350(2) Uani 1 1 d U . .
P2 P 0.23634(9) 0.50243(7) 0.15092(5) 0.0383(2) Uani 1 1 d U . .
N1 N 0.2010(2) 0.49441(19) 0.32280(14) 0.0323(6) Uani 1 1 d U . .
C1 C 0.6095(4) 0.7390(3) 0.2032(3) 0.0667(11) Uani 1 1 d U . .
H1A H 0.5725 0.7913 0.1629 0.080 Uiso 1 1 calc R . .
N2 N 0.3453(3) 0.4120(2) 0.19419(15) 0.0387(6) Uani 1 1 d U . .
C2 C 0.5706(4) 0.7314(3) 0.2771(3) 0.0700(12) Uani 1 1 d U . .
H2A H 0.5068 0.7785 0.2873 0.084 Uiso 1 1 calc R . .
P3 P 0.13149(7) 0.20968(6) 0.27167(5) 0.02936(18) Uani 1 1 d U . .
N3 N 0.2561(3) 0.61098(19) 0.17754(15) 0.0355(6) Uani 1 1 d U . .
C3 C 0.6240(4) 0.6558(4) 0.3359(3) 0.0699(12) Uani 1 1 d U . .
H3A H 0.5972 0.6505 0.3865 0.084 Uiso 1 1 calc R . .
P4 P 0.03910(8) 0.07512(7) 0.22559(5) 0.0391(2) Uani 1 1 d U . .
N4 N 0.3872(3) 0.2924(2) 0.36966(17) 0.0415(6) Uani 1 1 d U . .
C4 C 0.7145(4) 0.5896(4) 0.3210(3) 0.0644(11) Uani 1 1 d U . .
H4A H 0.7510 0.5373 0.3615 0.077 Uiso 1 1 calc R . .
N5 N 0.0947(2) 0.25973(19) 0.33920(14) 0.0303(6) Uani 1 1 d U . .
C5 C 0.7547(4) 0.5963(3) 0.2486(3) 0.0612(10) Uani 1 1 d U . .
H5A H 0.8195 0.5493 0.2396 0.073 Uiso 1 1 calc R . .
K1 K 0.46731(8) 0.52404(6) 0.26666(5) 0.0505(2) Uani 1 1 d U . .
N6 N 0.1330(2) 0.07928(19) 0.29463(16) 0.0353(6) Uani 1 1 d U . .
C6 C 0.7021(4) 0.6708(3) 0.1880(3) 0.0591(10) Uani 1 1 d U . .
N7 N 0.0123(2) 0.2032(2) 0.21783(15) 0.0356(6) Uani 1 1 d U . .
C7 C 0.7478(6) 0.6777(5) 0.1087(3) 0.0992(18) Uani 1 1 d U . .
H7A H 0.8368 0.6759 0.1054 0.149 Uiso 1 1 calc R . .
H7B H 0.7121 0.7413 0.0741 0.149 Uiso 1 1 calc R . .
H7C H 0.7244 0.6204 0.0947 0.149 Uiso 1 1 calc R . .
N8 N -0.0849(3) 0.0252(2) 0.27126(19) 0.0500(8) Uani 1 1 d U . .
H8A H -0.1113 0.0470 0.3099 0.060 Uiso 1 1 calc R . .
C11 C 0.1880(3) 0.5425(2) 0.38580(19) 0.0390(8) Uani 1 1 d U . .
C12 C 0.2939(4) 0.6053(3) 0.3816(2) 0.0571(11) Uani 1 1 d U . .
H12A H 0.3702 0.5603 0.3908 0.086 Uiso 1 1 calc R . .
H12B H 0.2799 0.6412 0.4198 0.086 Uiso 1 1 calc R . .
H12C H 0.2992 0.6545 0.3314 0.086 Uiso 1 1 calc R . .
C13 C 0.0677(4) 0.6118(3) 0.3827(2) 0.0586(11) Uani 1 1 d U . .
H13A H -0.0004 0.5744 0.3805 0.088 Uiso 1 1 calc R . .
H13B H 0.0699 0.6708 0.3378 0.088 Uiso 1 1 calc R . .
H13C H 0.0571 0.6346 0.4279 0.088 Uiso 1 1 calc R . .
C14 C 0.1915(4) 0.4583(3) 0.4604(2) 0.0544(10) Uani 1 1 d U . .
H14A H 0.2655 0.4115 0.4609 0.082 Uiso 1 1 calc R . .
H14B H 0.1197 0.4216 0.4663 0.082 Uiso 1 1 calc R . .
H14C H 0.1916 0.4877 0.5020 0.082 Uiso 1 1 calc R . .
C21 C 0.4410(4) 0.3715(3) 0.1464(2) 0.0473(9) Uani 1 1 d U . .
C22 C 0.3888(5) 0.3542(9) 0.0809(5) 0.187(4) Uani 1 1 d U . .
H22A H 0.4546 0.3316 0.0495 0.280 Uiso 1 1 calc R . .
H22B H 0.3447 0.4174 0.0510 0.280 Uiso 1 1 calc R . .
H22C H 0.3325 0.3021 0.0989 0.280 Uiso 1 1 calc R . .
C23 C 0.5374(5) 0.4409(4) 0.1188(4) 0.099(2) Uani 1 1 d U . .
H23A H 0.5989 0.4124 0.0880 0.148 Uiso 1 1 calc R . .
H23B H 0.5759 0.4490 0.1619 0.148 Uiso 1 1 calc R . .
H23C H 0.5009 0.5070 0.0883 0.148 Uiso 1 1 calc R . .
C24 C 0.5028(9) 0.2737(5) 0.1937(4) 0.195(5) Uani 1 1 d U . .
H24A H 0.5721 0.2508 0.1648 0.293 Uiso 1 1 calc R . .
H24B H 0.4449 0.2227 0.2083 0.293 Uiso 1 1 calc R . .
H24C H 0.5318 0.2837 0.2391 0.293 Uiso 1 1 calc R . .
C31 C 0.2395(4) 0.7157(3) 0.12257(19) 0.0438(8) Uani 1 1 d U . .
C32 C 0.2495(4) 0.7898(3) 0.1669(2) 0.0539(10) Uani 1 1 d U . .
H32A H 0.3294 0.7759 0.1893 0.081 Uiso 1 1 calc R . .
H32B H 0.1853 0.7819 0.2069 0.081 Uiso 1 1 calc R . .
H32C H 0.2401 0.8592 0.1329 0.081 Uiso 1 1 calc R . .
C33 C 0.1149(4) 0.7391(3) 0.0854(2) 0.0597(11) Uani 1 1 d U . .
H33A H 0.1062 0.6885 0.0600 0.090 Uiso 1 1 calc R . .
H33B H 0.1099 0.8066 0.0485 0.090 Uiso 1 1 calc R . .
H33C H 0.0494 0.7372 0.1242 0.090 Uiso 1 1 calc R . .
C34 C 0.3422(4) 0.7220(3) 0.0631(2) 0.0609(11) Uani 1 1 d U . .
H34A H 0.4206 0.7090 0.0872 0.091 Uiso 1 1 calc R . .
H34B H 0.3353 0.7898 0.0266 0.091 Uiso 1 1 calc R . .
H34C H 0.3369 0.6714 0.0370 0.091 Uiso 1 1 calc R . .
C41 C 0.4802(3) 0.2436(3) 0.4252(2) 0.0511(9) Uani 1 1 d U . .
C42 C 0.5594(5) 0.3220(4) 0.4337(3) 0.0814(15) Uani 1 1 d U . .
H42A H 0.5081 0.3738 0.4511 0.122 Uiso 1 1 calc R . .
H42B H 0.5991 0.3540 0.3848 0.122 Uiso 1 1 calc R . .
H42C H 0.6216 0.2884 0.4705 0.122 Uiso 1 1 calc R . .
C43 C 0.4205(4) 0.1929(3) 0.5017(2) 0.0643(11) Uani 1 1 d U . .
H43A H 0.3683 0.2440 0.5194 0.097 Uiso 1 1 calc R . .
H43B H 0.4837 0.1603 0.5379 0.097 Uiso 1 1 calc R . .
H43C H 0.3711 0.1418 0.4967 0.097 Uiso 1 1 calc R . .
C44 C 0.5637(4) 0.1615(4) 0.3998(3) 0.0738(13) Uani 1 1 d U . .
H44A H 0.6074 0.1931 0.3524 0.111 Uiso 1 1 calc R . .
H44B H 0.5143 0.1119 0.3924 0.111 Uiso 1 1 calc R . .
H44C H 0.6226 0.1273 0.4386 0.111 Uiso 1 1 calc R . .
C51 C -0.0006(3) 0.2440(3) 0.40090(19) 0.0381(8) Uani 1 1 d U . .
C52 C 0.0635(4) 0.2093(3) 0.47623(19) 0.0486(9) Uani 1 1 d U . .
H52A H 0.1050 0.1408 0.4837 0.073 Uiso 1 1 calc R . .
H52B H 0.0031 0.2091 0.5176 0.073 Uiso 1 1 calc R . .
H52C H 0.1235 0.2558 0.4754 0.073 Uiso 1 1 calc R . .
C53 C -0.0786(3) 0.3452(3) 0.3922(2) 0.0477(9) Uani 1 1 d U . .
H53A H -0.0260 0.3976 0.3899 0.072 Uiso 1 1 calc R . .
H53B H -0.1367 0.3388 0.4354 0.072 Uiso 1 1 calc R . .
H53C H -0.1232 0.3638 0.3456 0.072 Uiso 1 1 calc R . .
C54 C -0.0841(3) 0.1649(3) 0.3995(2) 0.0506(9) Uani 1 1 d U . .
H54A H -0.0351 0.1000 0.4034 0.076 Uiso 1 1 calc R . .
H54B H -0.1267 0.1874 0.3521 0.076 Uiso 1 1 calc R . .
H54C H -0.1438 0.1568 0.4420 0.076 Uiso 1 1 calc R . .
C61 C 0.2372(3) 0.0033(2) 0.3263(2) 0.0433(8) Uani 1 1 d U . .
C62 C 0.3444(4) 0.0101(4) 0.2697(3) 0.0798(15) Uani 1 1 d U . .
H62A H 0.3724 0.0774 0.2569 0.120 Uiso 1 1 calc R . .
H62B H 0.3190 -0.0014 0.2239 0.120 Uiso 1 1 calc R . .
H62C H 0.4108 -0.0415 0.2916 0.120 Uiso 1 1 calc R . .
C63 C 0.2741(5) 0.0210(3) 0.3979(3) 0.0728(14) Uani 1 1 d U . .
H63A H 0.2977 0.0898 0.3861 0.109 Uiso 1 1 calc R . .
H63B H 0.3432 -0.0282 0.4189 0.109 Uiso 1 1 calc R . .
H63C H 0.2053 0.0129 0.4349 0.109 Uiso 1 1 calc R . .
C64 C 0.1943(4) -0.1021(3) 0.3465(3) 0.0659(12) Uani 1 1 d U . .
H64A H 0.1222 -0.1054 0.3809 0.099 Uiso 1 1 calc R . .
H64B H 0.2596 -0.1530 0.3711 0.099 Uiso 1 1 calc R . .
H64C H 0.1737 -0.1155 0.3005 0.099 Uiso 1 1 calc R . .
C71 C -0.0383(3) 0.2825(3) 0.15125(19) 0.0407(8) Uani 1 1 d U . .
C72 C 0.0581(4) 0.3104(4) 0.0877(2) 0.0623(11) Uani 1 1 d U . .
H72A H 0.1246 0.3369 0.1049 0.093 Uiso 1 1 calc R . .
H72B H 0.0214 0.3621 0.0443 0.093 Uiso 1 1 calc R . .
H72C H 0.0901 0.2500 0.0728 0.093 Uiso 1 1 calc R . .
C73 C -0.0867(4) 0.3767(3) 0.1749(2) 0.0580(11) Uani 1 1 d U . .
H73A H -0.0196 0.4019 0.1927 0.087 Uiso 1 1 calc R . .
H73B H -0.1492 0.3592 0.2155 0.087 Uiso 1 1 calc R . .
H73C H -0.1222 0.4292 0.1316 0.087 Uiso 1 1 calc R . .
C74 C -0.1449(4) 0.2435(3) 0.1243(2) 0.0562(10) Uani 1 1 d U . .
H74A H -0.2052 0.2238 0.1661 0.084 Uiso 1 1 calc R . .
H74B H -0.1146 0.1848 0.1071 0.084 Uiso 1 1 calc R . .
H74C H -0.1831 0.2972 0.0826 0.084 Uiso 1 1 calc R . .
C81 C -0.1584(3) -0.0496(3) 0.2580(2) 0.0527(10) Uani 1 1 d U . .
C82 C -0.2880(4) -0.0019(4) 0.2428(4) 0.0834(16) Uani 1 1 d U . .
H82A H -0.2887 0.0553 0.1966 0.125 Uiso 1 1 calc R . .
H82B H -0.3219 0.0220 0.2852 0.125 Uiso 1 1 calc R . .
H82C H -0.3374 -0.0523 0.2366 0.125 Uiso 1 1 calc R . .
C83 C -0.1046(5) -0.0819(5) 0.1914(4) 0.111(2) Uani 1 1 d U . .
H83A H -0.1056 -0.0229 0.1465 0.166 Uiso 1 1 calc R . .
H83B H -0.1528 -0.1318 0.1833 0.166 Uiso 1 1 calc R . .
H83C H -0.0205 -0.1123 0.2011 0.166 Uiso 1 1 calc R . .
C84 C -0.1550(6) -0.1410(4) 0.3269(4) 0.123(3) Uani 1 1 d U . .
H84A H -0.0701 -0.1674 0.3382 0.184 Uiso 1 1 calc R . .
H84B H -0.1971 -0.1934 0.3172 0.184 Uiso 1 1 calc R . .
H84C H -0.1955 -0.1217 0.3698 0.184 Uiso 1 1 calc R . .
C91 C 0.4055(15) 1.0396(11) 0.0315(8) 0.185(6) Uani 0.50 1 d PGU A -1
C97 C 0.2905(15) 1.0785(14) 0.0532(12) 0.292(16) Uiso 0.50 1 d PGU A -1
H97A H 0.2309 1.0734 0.0200 0.438 Uiso 0.50 1 d PG A -1
H97B H 0.2696 1.0405 0.1040 0.438 Uiso 0.50 1 d PG A -1
H97C H 0.2919 1.1483 0.0504 0.438 Uiso 0.50 1 d PG A -1
C92 C 0.4185(19) 1.0016(11) -0.0299(7) 0.215(8) Uani 0.50 1 d PGU A -1
H92A H 0.3485 1.0021 -0.0575 0.258 Uiso 0.50 1 d PG A -1
C93 C 0.533(2) 0.9630(10) -0.0514(6) 0.228(9) Uani 0.50 1 d PGU A -1
H93A H 0.5417 0.9367 -0.0939 0.274 Uiso 0.50 1 d PG A -1
C94 C 0.6340(18) 0.9623(11) -0.0115(8) 0.193(7) Uani 0.50 1 d PGU A -1
H94B H 0.7129 0.9356 -0.0264 0.232 Uiso 0.50 1 d PG A -1
C95 C 0.6211(15) 1.0002(12) 0.0499(8) 0.143(6) Uani 0.50 1 d PGU A -1
H92B H 0.6911 0.9997 0.0774 0.172 Uiso 0.50 1 d PG A -1
C96 C 0.5068(15) 1.0389(11) 0.0714(7) 0.134(5) Uani 0.50 1 d PGU A -1
H93B H 0.4979 1.0651 0.1138 0.161 Uiso 0.50 1 d PG A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.02690(16) 0.03033(16) 0.03126(17) -0.01338(12) 0.00500(12) -0.00779(12)
P1 0.0340(5) 0.0377(4) 0.0364(5) -0.0162(4) 0.0031(4) -0.0052(4)
P2 0.0468(5) 0.0403(5) 0.0329(4) -0.0168(4) 0.0070(4) -0.0135(4)
N1 0.0381(14) 0.0322(13) 0.0307(13) -0.0160(11) 0.0054(11) -0.0058(11)
C1 0.054(2) 0.041(2) 0.102(3) -0.010(2) -0.018(2) -0.0141(17)
N2 0.0454(16) 0.0319(14) 0.0412(15) -0.0167(12) 0.0171(12) -0.0104(11)
C2 0.046(2) 0.053(2) 0.130(4) -0.053(3) 0.003(2) -0.0111(18)
P3 0.0261(4) 0.0303(4) 0.0351(4) -0.0141(3) -0.0001(3) -0.0053(3)
N3 0.0412(15) 0.0330(13) 0.0348(14) -0.0133(11) 0.0044(12) -0.0091(12)
C3 0.066(3) 0.077(3) 0.087(3) -0.049(2) 0.001(2) -0.027(2)
P4 0.0357(5) 0.0404(5) 0.0499(5) -0.0251(4) -0.0013(4) -0.0080(4)
N4 0.0295(15) 0.0466(15) 0.0531(17) -0.0217(13) -0.0036(13) -0.0032(12)
C4 0.057(2) 0.067(3) 0.076(3) -0.026(2) -0.020(2) -0.0087(19)
N5 0.0289(14) 0.0337(13) 0.0317(13) -0.0145(11) 0.0013(11) -0.0062(11)
C5 0.044(2) 0.057(2) 0.088(3) -0.031(2) -0.005(2) -0.0026(17)
K1 0.0491(5) 0.0529(5) 0.0589(5) -0.0259(4) 0.0017(4) -0.0194(4)
N6 0.0304(14) 0.0315(13) 0.0478(16) -0.0170(12) -0.0033(12) -0.0040(11)
C6 0.053(2) 0.057(2) 0.071(2) -0.019(2) 0.002(2) -0.0222(18)
N7 0.0334(15) 0.0383(14) 0.0400(15) -0.0168(12) -0.0047(12) -0.0071(12)
C7 0.100(4) 0.116(5) 0.081(3) -0.021(3) 0.015(3) -0.045(4)
N8 0.0445(18) 0.0513(18) 0.069(2) -0.0358(16) 0.0072(16) -0.0221(14)
C11 0.050(2) 0.0386(18) 0.0354(17) -0.0218(14) 0.0069(15) -0.0084(15)
C12 0.070(3) 0.063(2) 0.052(2) -0.032(2) 0.008(2) -0.028(2)
C13 0.067(3) 0.059(2) 0.060(3) -0.039(2) 0.007(2) 0.003(2)
C14 0.080(3) 0.054(2) 0.0355(19) -0.0227(17) 0.0058(19) -0.013(2)
C21 0.051(2) 0.0440(19) 0.050(2) -0.0214(16) 0.0236(17) -0.0114(16)
C22 0.059(4) 0.402(13) 0.214(7) -0.273(9) 0.026(4) -0.017(5)
C23 0.057(3) 0.094(4) 0.169(6) -0.080(4) 0.058(3) -0.033(3)
C24 0.263(10) 0.081(4) 0.143(5) 0.033(4) 0.143(5) 0.094(5)
C31 0.057(2) 0.0352(17) 0.0367(18) -0.0072(14) 0.0012(16) -0.0047(16)
C32 0.069(3) 0.0342(19) 0.058(2) -0.0133(17) -0.004(2) -0.0041(18)
C33 0.070(3) 0.057(2) 0.048(2) -0.0110(19) -0.017(2) 0.005(2)
C34 0.077(3) 0.047(2) 0.049(2) -0.0028(18) 0.014(2) -0.011(2)
C41 0.033(2) 0.054(2) 0.068(3) -0.0214(19) -0.0146(18) 0.0004(16)
C42 0.062(3) 0.083(3) 0.106(4) -0.026(3) -0.040(3) -0.014(2)
C43 0.064(3) 0.069(3) 0.059(2) -0.016(2) -0.023(2) 0.006(2)
C44 0.041(2) 0.084(3) 0.099(4) -0.035(3) -0.019(2) 0.017(2)
C51 0.0334(18) 0.0457(19) 0.0402(18) -0.0194(15) 0.0094(14) -0.0133(15)
C52 0.054(2) 0.059(2) 0.0354(18) -0.0166(17) 0.0079(16) -0.0133(18)
C53 0.0351(19) 0.062(2) 0.052(2) -0.0300(19) 0.0075(17) -0.0020(17)
C54 0.043(2) 0.063(2) 0.054(2) -0.0270(19) 0.0185(18) -0.0274(18)
C61 0.0361(19) 0.0281(16) 0.067(2) -0.0161(16) -0.0063(17) -0.0010(14)
C62 0.045(2) 0.059(3) 0.122(4) -0.016(3) 0.018(3) 0.007(2)
C63 0.082(3) 0.046(2) 0.093(3) -0.022(2) -0.048(3) 0.013(2)
C64 0.063(3) 0.033(2) 0.101(4) -0.016(2) -0.013(3) -0.0068(19)
C71 0.0401(19) 0.0469(19) 0.0393(18) -0.0167(15) -0.0089(15) -0.0059(15)
C72 0.063(3) 0.076(3) 0.047(2) -0.013(2) 0.000(2) -0.019(2)
C73 0.063(3) 0.048(2) 0.064(3) -0.0199(19) -0.022(2) 0.0079(19)
C74 0.054(2) 0.067(3) 0.051(2) -0.018(2) -0.0219(19) -0.010(2)
C81 0.041(2) 0.050(2) 0.078(3) -0.030(2) -0.010(2) -0.0140(17)
C82 0.047(2) 0.072(3) 0.149(5) -0.055(3) -0.013(3) -0.011(2)
C83 0.076(3) 0.134(5) 0.181(6) -0.128(5) 0.030(4) -0.049(4)
C84 0.127(5) 0.075(4) 0.157(5) 0.015(4) -0.066(5) -0.063(4)
C91 0.279(15) 0.156(15) 0.111(15) 0.044(11) -0.108(10) -0.142(12)
C92 0.45(2) 0.133(16) 0.074(12) 0.048(8) -0.135(14) -0.195(16)
C93 0.52(3) 0.118(14) 0.065(10) 0.025(8) -0.093(16) -0.177(19)
C94 0.43(2) 0.071(10) 0.061(10) 0.027(7) -0.041(13) -0.062(13)
C95 0.272(16) 0.085(10) 0.072(10) -0.001(7) -0.065(12) -0.040(12)
C96 0.216(15) 0.104(11) 0.086(11) 0.007(8) -0.075(10) -0.080(11)

_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 N4 1.864(3) . ?
Zr1 N1 2.167(3) . ?
Zr1 N2 2.194(3) . ?
Zr1 N5 2.263(3) . ?
Zr1 P3 2.769(2) . ?
Zr1 P1 3.022(3) . ?
Zr1 P2 3.035(3) . ?
Zr1 K1 3.458(3) . ?
P1 N1 1.689(3) . ?
P1 N3 1.774(3) . ?
P1 P2 2.236(2) . ?
P1 K1 3.690(2) . ?
P2 N2 1.687(3) . ?
P2 N3 1.771(3) . ?
P2 K1 3.566(2) . ?
N1 C11 1.508(4) . ?
N1 K1 3.086(3) . ?
C1 C6 1.381(6) . ?
C1 C2 1.388(7) . ?
C1 K1 3.406(5) . ?
N2 C21 1.498(4) . ?
N2 K1 2.859(3) . ?
C2 C3 1.380(7) . ?
C2 K1 3.302(5) . ?
P3 N5 1.618(3) . ?
P3 N6 1.734(3) . ?
P3 N7 1.745(3) . ?
P3 P4 2.626(2) . ?
N3 C31 1.505(4) . ?
N3 K1 2.892(4) . ?
C3 C4 1.346(6) . ?
C3 K1 3.260(5) . ?
P4 N8 1.671(3) . ?
P4 N6 1.734(3) . ?
P4 N7 1.735(3) . ?
N4 C41 1.467(5) . ?
N4 K1 3.404(4) . ?
C4 C5 1.366(6) . ?
C4 K1 3.311(5) . ?
N5 C51 1.483(4) . ?
C5 C6 1.390(6) . ?
C5 K1 3.417(5) . ?
K1 C6 3.466(5) . ?
N6 C61 1.489(4) . ?
C6 C7 1.502(7) . ?
N7 C71 1.482(5) . ?
N8 C81 1.486(4) . ?
C11 C14 1.521(5) . ?
C11 C12 1.532(5) . ?
C11 C13 1.538(5) . ?
C21 C22 1.483(7) . ?
C21 C23 1.487(6) . ?
C21 C24 1.494(7) . ?
C31 C34 1.516(5) . ?
C31 C32 1.523(5) . ?
C31 C33 1.545(6) . ?
C41 C43 1.526(6) . ?
C41 C42 1.535(6) . ?
C41 C44 1.544(6) . ?
C51 C53 1.529(5) . ?
C51 C54 1.533(5) . ?
C51 C52 1.537(5) . ?
C61 C62 1.518(6) . ?
C61 C63 1.522(6) . ?
C61 C64 1.529(5) . ?
C71 C72 1.524(5) . ?
C71 C73 1.530(5) . ?
C71 C74 1.536(5) . ?
C81 C83 1.501(7) . ?
C81 C84 1.508(7) . ?
C81 C82 1.514(6) . ?
C91 C92 1.3898 . ?
C91 C96 1.3901 . ?
C91 C97 1.3999 . ?
C92 C93 1.3901 . ?
C93 C94 1.3901 . ?
C94 C95 1.3901 . ?
C95 C96 1.3899 . ?

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
N4 Zr1 N1 105.06(13) . . ?
N4 Zr1 N2 105.04(14) . . ?
N1 Zr1 N2 94.33(12) . . ?
N4 Zr1 N5 112.54(13) . . ?
N1 Zr1 N5 105.75(11) . . ?
N2 Zr1 N5 130.17(11) . . ?
N4 Zr1 P3 115.39(11) . . ?
N1 Zr1 P3 132.13(9) . . ?
N2 Zr1 P3 98.66(10) . . ?
N5 Zr1 P3 35.74(7) . . ?
N4 Zr1 P1 134.09(10) . . ?
N1 Zr1 P1 33.07(8) . . ?
N2 Zr1 P1 72.62(10) . . ?
N5 Zr1 P1 100.80(9) . . ?
P3 Zr1 P1 110.16(6) . . ?
N4 Zr1 P2 134.02(10) . . ?
N1 Zr1 P2 72.78(10) . . ?
N2 Zr1 P2 32.93(9) . . ?
N5 Zr1 P2 112.03(9) . . ?
P3 Zr1 P2 94.74(7) . . ?
P1 Zr1 P2 43.32(5) . . ?
N4 Zr1 K1 72.65(11) . . ?
N1 Zr1 K1 61.60(9) . . ?
N2 Zr1 K1 55.50(9) . . ?
N5 Zr1 K1 167.34(7) . . ?
P3 Zr1 K1 153.81(4) . . ?
P1 Zr1 K1 69.06(6) . . ?
P2 Zr1 K1 66.25(6) . . ?
N1 P1 N3 106.08(15) . . ?
N1 P1 P2 106.67(11) . . ?
N3 P1 P2 50.84(10) . . ?
N1 P1 Zr1 44.45(9) . . ?
N3 P1 Zr1 98.14(11) . . ?
P2 P1 Zr1 68.66(7) . . ?
N1 P1 K1 56.14(11) . . ?
N3 P1 K1 50.07(10) . . ?
P2 P1 K1 69.05(6) . . ?
Zr1 P1 K1 61.06(6) . . ?
N2 P2 N3 105.71(15) . . ?
N2 P2 P1 106.46(12) . . ?
N3 P2 P1 50.97(10) . . ?
N2 P2 Zr1 44.97(10) . . ?
N3 P2 Zr1 97.73(11) . . ?
P1 P2 Zr1 68.01(7) . . ?
N2 P2 K1 52.12(11) . . ?
N3 P2 K1 53.62(11) . . ?
P1 P2 K1 75.11(6) . . ?
Zr1 P2 K1 62.57(6) . . ?
C11 N1 P1 117.7(2) . . ?
C11 N1 Zr1 139.1(2) . . ?
P1 N1 Zr1 102.48(13) . . ?
C11 N1 K1 101.40(19) . . ?
P1 N1 K1 96.84(12) . . ?
Zr1 N1 K1 80.25(10) . . ?
C6 C1 C2 120.2(4) . . ?
C6 C1 K1 80.9(2) . . ?
C2 C1 K1 73.9(2) . . ?
C21 N2 P2 118.4(2) . . ?
C21 N2 Zr1 134.3(2) . . ?
P2 N2 Zr1 102.10(14) . . ?
C21 N2 K1 106.0(2) . . ?
P2 N2 K1 100.11(13) . . ?
Zr1 N2 K1 85.28(11) . . ?
C3 C2 C1 120.3(4) . . ?
C3 C2 K1 76.2(2) . . ?
C1 C2 K1 82.3(2) . . ?
N5 P3 N6 116.61(15) . . ?
N5 P3 N7 116.10(14) . . ?
N6 P3 N7 80.30(14) . . ?
N5 P3 P4 133.70(11) . . ?
N6 P3 P4 40.79(10) . . ?
N7 P3 P4 40.89(10) . . ?
N5 P3 Zr1 54.79(10) . . ?
N6 P3 Zr1 138.21(11) . . ?
N7 P3 Zr1 141.49(10) . . ?
P4 P3 Zr1 171.38(4) . . ?
C31 N3 P2 121.4(2) . . ?
C31 N3 P1 121.3(2) . . ?
P2 N3 P1 78.19(13) . . ?
C31 N3 K1 125.7(2) . . ?
P2 N3 K1 96.83(13) . . ?
P1 N3 K1 101.85(13) . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 K1 80.3(3) . . ?
C2 C3 K1 79.6(3) . . ?
N8 P4 N6 106.00(16) . . ?
N8 P4 N7 105.02(16) . . ?
N6 P4 N7 80.58(14) . . ?
N8 P4 P3 118.77(12) . . ?
N6 P4 P3 40.80(10) . . ?
N7 P4 P3 41.16(10) . . ?
C41 N4 Zr1 174.7(3) . . ?
C41 N4 K1 108.7(2) . . ?
Zr1 N4 K1 75.83(11) . . ?
C3 C4 C5 121.1(5) . . ?
C3 C4 K1 76.1(3) . . ?
C5 C4 K1 82.7(3) . . ?
C51 N5 P3 133.9(2) . . ?
C51 N5 Zr1 136.39(19) . . ?
P3 N5 Zr1 89.47(12) . . ?
C4 C5 C6 121.0(4) . . ?
C4 C5 K1 74.0(3) . . ?
C6 C5 K1 80.3(2) . . ?
N2 K1 N3 57.30(9) . . ?
N2 K1 N1 64.96(9) . . ?
N3 K1 N1 55.05(9) . . ?
N2 K1 C3 174.73(11) . . ?
N3 K1 C3 123.15(12) . . ?
N1 K1 C3 119.97(11) . . ?
N2 K1 C2 153.50(12) . . ?
N3 K1 C2 100.46(12) . . ?
N1 K1 C2 116.51(11) . . ?
C3 K1 C2 24.27(12) . . ?
N2 K1 C4 152.85(11) . . ?
N3 K1 C4 141.06(11) . . ?
N1 K1 C4 139.01(11) . . ?
C3 K1 C4 23.63(11) . . ?
C2 K1 C4 41.73(12) . . ?
N2 K1 N4 61.30(9) . . ?
N3 K1 N4 102.41(10) . . ?
N1 K1 N4 58.95(9) . . ?
C3 K1 N4 122.25(13) . . ?
C2 K1 N4 144.13(12) . . ?
C4 K1 N4 115.00(12) . . ?
N2 K1 C1 133.73(12) . . ?
N3 K1 C1 93.83(11) . . ?
N1 K1 C1 130.38(11) . . ?
C3 K1 C1 42.14(14) . . ?
C2 K1 C1 23.81(12) . . ?
C4 K1 C1 48.17(13) . . ?
N4 K1 C1 163.08(10) . . ?
N2 K1 C5 133.77(10) . . ?
N3 K1 C5 130.74(11) . . ?
N1 K1 C5 161.27(9) . . ?
C3 K1 C5 41.34(12) . . ?
C2 K1 C5 47.92(11) . . ?
C4 K1 C5 23.36(11) . . ?
N4 K1 C5 125.20(11) . . ?
C1 K1 C5 40.74(11) . . ?
N2 K1 Zr1 39.23(7) . . ?
N3 K1 Zr1 70.97(8) . . ?
N1 K1 Zr1 38.15(6) . . ?
C3 K1 Zr1 145.80(10) . . ?
C2 K1 Zr1 153.87(9) . . ?
C4 K1 Zr1 146.16(10) . . ?
N4 K1 Zr1 31.52(6) . . ?
C1 K1 Zr1 164.61(8) . . ?
C5 K1 Zr1 154.02(8) . . ?
N2 K1 C6 126.12(11) . . ?
N3 K1 C6 107.46(11) . . ?
N1 K1 C6 153.29(10) . . ?
C3 K1 C6 48.66(13) . . ?
C2 K1 C6 41.45(12) . . ?
C4 K1 C6 41.38(12) . . ?
N4 K1 C6 146.94(10) . . ?
C1 K1 C6 23.17(11) . . ?
C5 K1 C6 23.29(11) . . ?
Zr1 K1 C6 164.14(8) . . ?
N2 K1 P2 27.76(6) . . ?
N3 K1 P2 29.55(6) . . ?
N1 K1 P2 56.26(7) . . ?
C3 K1 P2 152.24(11) . . ?
C2 K1 P2 128.43(11) . . ?
C4 K1 P2 161.50(10) . . ?
N4 K1 P2 81.12(8) . . ?
C1 K1 P2 115.75(10) . . ?
C5 K1 P2 139.36(9) . . ?
Zr1 K1 P2 51.18(5) . . ?
C6 K1 P2 120.12(10) . . ?
C61 N6 P4 126.3(2) . . ?
C61 N6 P3 125.7(2) . . ?
P4 N6 P3 98.41(15) . . ?
C1 C6 C5 118.0(4) . . ?
C1 C6 C7 121.6(5) . . ?
C5 C6 C7 120.4(5) . . ?
C1 C6 K1 76.0(2) . . ?
C5 C6 K1 76.4(2) . . ?
C7 C6 K1 119.0(3) . . ?
C71 N7 P4 124.8(2) . . ?
C71 N7 P3 127.5(2) . . ?
P4 N7 P3 97.95(15) . . ?
C81 N8 P4 131.3(3) . . ?
N1 C11 C14 108.2(3) . . ?
N1 C11 C12 110.6(3) . . ?
C14 C11 C12 108.4(3) . . ?
N1 C11 C13 111.6(3) . . ?
C14 C11 C13 109.5(3) . . ?
C12 C11 C13 108.5(3) . . ?
C22 C21 C23 109.2(5) . . ?
C22 C21 C24 109.2(6) . . ?
C23 C21 C24 106.3(5) . . ?
C22 C21 N2 112.0(4) . . ?
C23 C21 N2 111.2(3) . . ?
C24 C21 N2 108.8(3) . . ?
N3 C31 C34 107.0(3) . . ?
N3 C31 C32 106.8(3) . . ?
C34 C31 C32 110.5(3) . . ?
N3 C31 C33 112.5(3) . . ?
C34 C31 C33 110.3(3) . . ?
C32 C31 C33 109.6(3) . . ?
N4 C41 C43 110.5(3) . . ?
N4 C41 C42 110.3(3) . . ?
C43 C41 C42 109.2(4) . . ?
N4 C41 C44 110.4(3) . . ?
C43 C41 C44 108.0(4) . . ?
C42 C41 C44 108.3(4) . . ?
N5 C51 C53 107.8(3) . . ?
N5 C51 C54 113.2(3) . . ?
C53 C51 C54 108.4(3) . . ?
N5 C51 C52 107.9(3) . . ?
C53 C51 C52 110.5(3) . . ?
C54 C51 C52 109.0(3) . . ?
N6 C61 C62 111.2(3) . . ?
N6 C61 C63 108.9(3) . . ?
C62 C61 C63 110.5(4) . . ?
N6 C61 C64 108.1(3) . . ?
C62 C61 C64 109.3(3) . . ?
C63 C61 C64 108.8(4) . . ?
N7 C71 C72 111.5(3) . . ?
N7 C71 C73 108.7(3) . . ?
C72 C71 C73 109.2(3) . . ?
N7 C71 C74 108.7(3) . . ?
C72 C71 C74 110.1(3) . . ?
C73 C71 C74 108.6(3) . . ?
N8 C81 C83 109.7(4) . . ?
N8 C81 C84 108.6(4) . . ?
C83 C81 C84 108.8(5) . . ?
N8 C81 C82 109.5(3) . . ?
C83 C81 C82 109.4(4) . . ?
C84 C81 C82 110.7(5) . . ?
C92 C91 C96 120.0 . . ?
C92 C91 C97 120.0 . . ?
C96 C91 C97 120.0 . . ?
C91 C92 C93 120.0 . . ?
C94 C93 C92 120.0 . . ?
C95 C94 C93 120.0 . . ?
C96 C95 C94 120.0 . . ?
C95 C96 C91 120.0 . . ?

_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.661
_refine_diff_density_min   -0.568
_refine_diff_density_rms    0.063