Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_f 

_database_code_CSD	167617


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name

'Brask, J. K.'
'Cummins, C.'
'Dura-Vila, V.'
'Fickes, M. G.'
'Odom, A. L.'
'Sangtrirutnugul, P.'

_publ_contact_author_name     	' Prof C Cummins'  
_publ_contact_author_address 
;
Department of Chemistry (Room 2-227)
Massachusetts Institute of Technology
Cambridge
MA
02139=4307
UNITED STATES OF AMERICA
;

_publ_contact_author_email       'ccummins@mit.edu '

_publ_section_title		
;
Niobium and vandium iminophosphinimide complexes
;

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C40 H63 N5 Nb P' 
_chemical_formula_weight          737.83 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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' 
'Nb'  'Nb'  -2.0727   0.6215 
'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                    10.584(7) 
_cell_length_b                    12.626(10) 
_cell_length_c                    17.968(13) 
_cell_angle_alpha                 106.92(4) 
_cell_angle_beta                  90.52(6) 
_cell_angle_gamma                 114.37(4) 
_cell_volume                      2069.4(26) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     183(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.13 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.184 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              788 
_exptl_absorpt_coefficient_mu     0.361 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.7070 
_exptl_absorpt_correction_T_max   0.9429 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       183(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        'Siemens P4' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             6162 
_diffrn_reflns_av_R_equivalents   0.0675 
_diffrn_reflns_av_sigmaI/netI     0.0932 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.20 
_diffrn_reflns_theta_max          20.00 
_reflns_number_total              3802 
_reflns_number_observed           2885 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 312 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.1256P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0016(4) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3490 
_refine_ls_number_parameters      425 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1122 
_refine_ls_R_factor_obs           0.0736 
_refine_ls_wR_factor_all          0.1678 
_refine_ls_wR_factor_obs          0.1301 
_refine_ls_goodness_of_fit_all    1.161 
_refine_ls_goodness_of_fit_obs    1.211 
_refine_ls_restrained_S_all       1.337 
_refine_ls_restrained_S_obs       1.211 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Nb Nb 0.61670(10) -0.01208(9) 0.27089(5) 0.0220(4) Uani 1 d . . 
P P 0.4595(3) 0.0260(2) 0.44022(15) 0.0267(7) Uani 1 d . . 
N1 N 0.8038(8) -0.0091(7) 0.2948(4) 0.027(2) Uani 1 d . . 
N2 N 0.4890(8) -0.1746(7) 0.1865(4) 0.024(2) Uani 1 d . . 
N3 N 0.6317(8) 0.1342(7) 0.2388(4) 0.024(2) Uani 1 d . . 
N4 N 0.5469(8) 0.0001(7) 0.3617(4) 0.023(2) Uani 1 d . . 
N5 N 0.4140(8) -0.0947(7) 0.4777(4) 0.024(2) Uani 1 d . . 
C11 C 0.9011(10) 0.0349(9) 0.2429(6) 0.028(3) Uani 1 d . . 
C12 C 0.9806(10) 0.1592(10) 0.2585(6) 0.031(3) Uani 1 d . . 
H12A H 0.9654(10) 0.2149(10) 0.3017(6) 0.037 Uiso 1 calc R . 
C13 C 1.0831(11) 0.2068(10) 0.2130(6) 0.038(3) Uani 1 d . . 
C14 C 1.0983(11) 0.1218(12) 0.1487(7) 0.045(3) Uani 1 d . . 
H14A H 1.1648(11) 0.1510(12) 0.1158(7) 0.054 Uiso 1 calc R . 
C15 C 1.0207(11) -0.0024(11) 0.1312(6) 0.035(3) Uani 1 d . . 
C16 C 0.9222(11) -0.0458(10) 0.1786(6) 0.035(3) Uani 1 d . . 
H16A H 0.8686(11) -0.1318(10) 0.1669(6) 0.042 Uiso 1 calc R . 
C17 C 0.8741(11) -0.0232(10) 0.3635(6) 0.037(3) Uani 1 d . . 
C18 C 0.9738(12) -0.0801(11) 0.3369(6) 0.060(4) Uani 1 d . . 
H18A H 1.0466(12) -0.0279(11) 0.3132(6) 0.090 Uiso 1 calc R . 
H18B H 0.9217(12) -0.1618(11) 0.2981(6) 0.090 Uiso 1 calc R . 
H18C H 1.0175(12) -0.0875(11) 0.3823(6) 0.090 Uiso 1 calc R . 
C19 C 0.9564(12) 0.1038(10) 0.4250(6) 0.051(3) Uani 1 d . . 
H19A H 0.8927(12) 0.1414(10) 0.4425(6) 0.076 Uiso 1 calc R . 
H19B H 1.0300(12) 0.1561(10) 0.4017(6) 0.076 Uiso 1 calc R . 
H19C H 0.9993(12) 0.0951(10) 0.4701(6) 0.076 Uiso 1 calc R . 
C21 C 0.5515(10) -0.2557(9) 0.1524(5) 0.025(3) Uani 1 d . . 
C22 C 0.5879(11) -0.2704(9) 0.0761(6) 0.033(3) Uani 1 d . . 
H22A H 0.5676(11) -0.2285(9) 0.0450(6) 0.040 Uiso 1 calc R . 
C23 C 0.6531(11) -0.3456(10) 0.0461(6) 0.039(3) Uani 1 d . . 
C24 C 0.6822(12) -0.4062(10) 0.0910(8) 0.051(3) Uani 1 d . . 
H24A H 0.7249(12) -0.4591(10) 0.0695(8) 0.062 Uiso 1 calc R . 
C25 C 0.6506(13) -0.3922(10) 0.1670(7) 0.047(3) Uani 1 d . . 
C26 C 0.5827(11) -0.3184(9) 0.1959(6) 0.038(3) Uani 1 d . . 
H26A H 0.5570(11) -0.3107(9) 0.2470(6) 0.045 Uiso 1 calc R . 
C27 C 0.3343(11) -0.2261(9) 0.1599(6) 0.030(3) Uani 1 d . . 
C28 C 0.2985(11) -0.2554(10) 0.0708(5) 0.044(3) Uani 1 d . . 
H28A H 0.3304(11) -0.3164(10) 0.0421(5) 0.066 Uiso 1 calc R . 
H28B H 0.3456(11) -0.1801(10) 0.0570(5) 0.066 Uiso 1 calc R . 
H28C H 0.1968(11) -0.2882(10) 0.0566(5) 0.066 Uiso 1 calc R . 
C29 C 0.2523(11) -0.3457(8) 0.1793(6) 0.036(3) Uani 1 d . . 
H29A H 0.2845(11) -0.4074(8) 0.1522(6) 0.054 Uiso 1 calc R . 
H29B H 0.1519(11) -0.3768(8) 0.1618(6) 0.054 Uiso 1 calc R . 
H29C H 0.2686(11) -0.3289(8) 0.2362(6) 0.054 Uiso 1 calc R . 
C31 C 0.6183(10) 0.2364(9) 0.2961(5) 0.021(2) Uani 1 d . . 
C32 C 0.7325(10) 0.3489(9) 0.3320(5) 0.024(3) Uani 1 d . . 
H32A H 0.8235(10) 0.3586(9) 0.3210(5) 0.028 Uiso 1 calc R . 
C33 C 0.7177(11) 0.4480(9) 0.3836(6) 0.031(3) Uani 1 d . . 
C34 C 0.5843(12) 0.4296(10) 0.3990(6) 0.034(3) Uani 1 d . . 
H34A H 0.5716(12) 0.4973(10) 0.4321(6) 0.041 Uiso 1 calc R . 
C35 C 0.4667(11) 0.3166(11) 0.3686(6) 0.034(3) Uani 1 d . . 
C36 C 0.4859(11) 0.2206(9) 0.3153(5) 0.024(3) Uani 1 d . . 
H36A H 0.4075(11) 0.1435(9) 0.2919(5) 0.029 Uiso 1 calc R . 
C37 C 0.6481(11) 0.1512(9) 0.1591(5) 0.031(3) Uani 1 d . . 
C38 C 0.6615(12) 0.0418(9) 0.1036(5) 0.043(3) Uani 1 d . . 
H38A H 0.5790(12) -0.0337(9) 0.1011(5) 0.064 Uiso 1 calc R . 
H38B H 0.7461(12) 0.0382(9) 0.1227(5) 0.064 Uiso 1 calc R . 
H38C H 0.6680(12) 0.0501(9) 0.0510(5) 0.064 Uiso 1 calc R . 
C39 C 0.5148(11) 0.1575(10) 0.1274(6) 0.045(3) Uani 1 d . . 
H39A H 0.5054(11) 0.2282(10) 0.1631(6) 0.068 Uiso 1 calc R . 
H39B H 0.4317(11) 0.0819(10) 0.1240(6) 0.068 Uiso 1 calc R . 
H39C H 0.5233(11) 0.1663(10) 0.0750(6) 0.068 Uiso 1 calc R . 
C48 C 0.2831(11) -0.1310(9) 0.2026(6) 0.038(3) Uani 1 d . . 
H48A H 0.3046(11) -0.1109(9) 0.2595(6) 0.058 Uiso 1 calc R . 
H48B H 0.1815(11) -0.1646(9) 0.1875(6) 0.058 Uiso 1 calc R . 
H48C H 0.3303(11) -0.0564(9) 0.1881(6) 0.058 Uiso 1 calc R . 
C51 C 0.3224(9) -0.2268(8) 0.4387(5) 0.022(2) Uani 1 d . . 
C52 C 0.4045(10) -0.2880(9) 0.3891(6) 0.041(3) Uani 1 d . . 
H52A H 0.4838(10) -0.2791(9) 0.4229(6) 0.062 Uiso 1 calc R . 
H52B H 0.4395(10) -0.2488(9) 0.3490(6) 0.062 Uiso 1 calc R . 
H52C H 0.3431(10) -0.3754(9) 0.3633(6) 0.062 Uiso 1 calc R . 
C53 C 0.2726(11) -0.2883(9) 0.5012(6) 0.041(3) Uani 1 d . . 
H53A H 0.3539(11) -0.2784(9) 0.5339(6) 0.062 Uiso 1 calc R . 
H53B H 0.2121(11) -0.3760(9) 0.4757(6) 0.062 Uiso 1 calc R . 
H53C H 0.2198(11) -0.2500(9) 0.5343(6) 0.062 Uiso 1 calc R . 
C54 C 0.1993(11) -0.2402(9) 0.3868(6) 0.040(3) Uani 1 d . . 
H54A H 0.1468(11) -0.2007(9) 0.4191(6) 0.061 Uiso 1 calc R . 
H54B H 0.1377(11) -0.3276(9) 0.3611(6) 0.061 Uiso 1 calc R . 
H54C H 0.2338(11) -0.2010(9) 0.3468(6) 0.061 Uiso 1 calc R . 
C58 C 0.7628(11) -0.1058(10) 0.3999(6) 0.048(3) Uani 1 d . . 
H58A H 0.6972(11) -0.0704(10) 0.4175(6) 0.072 Uiso 1 calc R . 
H58B H 0.8076(11) -0.1129(10) 0.4450(6) 0.072 Uiso 1 calc R . 
H58C H 0.7118(11) -0.1874(10) 0.3608(6) 0.072 Uiso 1 calc R . 
C131 C 1.1693(13) 0.3440(10) 0.2305(7) 0.064(4) Uani 1 d . . 
H13A H 1.1442(13) 0.3888(10) 0.2777(7) 0.096 Uiso 1 calc R . 
H13B H 1.1500(13) 0.3676(10) 0.1858(7) 0.096 Uiso 1 calc R . 
H13C H 1.2692(13) 0.3641(10) 0.2391(7) 0.096 Uiso 1 calc R . 
C151 C 1.0422(12) -0.0935(11) 0.0614(6) 0.054(3) Uani 1 d . . 
H15A H 0.9778(12) -0.1775(11) 0.0582(6) 0.081 Uiso 1 calc R . 
H15B H 1.1391(12) -0.0828(11) 0.0683(6) 0.081 Uiso 1 calc R . 
H15C H 1.0234(12) -0.0786(11) 0.0128(6) 0.081 Uiso 1 calc R . 
C231 C 0.6856(12) -0.3668(10) -0.0375(6) 0.056(4) Uani 1 d . . 
H23A H 0.6588(12) -0.3169(10) -0.0613(6) 0.084 Uiso 1 calc R . 
H23B H 0.6326(12) -0.4539(10) -0.0682(6) 0.084 Uiso 1 calc R . 
H23C H 0.7862(12) -0.3433(10) -0.0371(6) 0.084 Uiso 1 calc R . 
C251 C 0.6801(15) -0.4587(11) 0.2184(7) 0.077(4) Uani 1 d . . 
H25A H 0.6496(15) -0.4355(11) 0.2696(7) 0.115 Uiso 1 calc R . 
H25B H 0.7809(15) -0.4359(11) 0.2261(7) 0.115 Uiso 1 calc R . 
H25C H 0.6287(15) -0.5477(11) 0.1927(7) 0.115 Uiso 1 calc R . 
C310 C 0.7794(11) 0.2665(9) 0.1608(6) 0.040(3) Uani 1 d . . 
H31A H 0.7741(11) 0.3394(9) 0.1964(6) 0.061 Uiso 1 calc R . 
H31B H 0.7848(11) 0.2728(9) 0.1077(6) 0.061 Uiso 1 calc R . 
H31C H 0.8630(11) 0.2610(9) 0.1794(6) 0.061 Uiso 1 calc R . 
C331 C 0.8418(11) 0.5684(9) 0.4213(6) 0.050(3) Uani 1 d . . 
H33A H 0.9267(11) 0.5632(9) 0.4030(6) 0.075 Uiso 1 calc R . 
H33B H 0.8510(11) 0.5879(9) 0.4786(6) 0.075 Uiso 1 calc R . 
H33C H 0.8291(11) 0.6329(9) 0.4070(6) 0.075 Uiso 1 calc R . 
C351 C 0.3251(11) 0.2957(10) 0.3943(6) 0.052(3) Uani 1 d . . 
H35A H 0.2569(11) 0.2110(10) 0.3664(6) 0.079 Uiso 1 calc R . 
H35B H 0.2942(11) 0.3528(10) 0.3822(6) 0.079 Uiso 1 calc R . 
H35C H 0.3325(11) 0.3097(10) 0.4511(6) 0.079 Uiso 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 
Nb 0.0317(6) 0.0234(6) 0.0153(6) 0.0097(4) 0.0060(4) 0.0137(5) 
P 0.038(2) 0.026(2) 0.020(2) 0.0099(13) 0.0107(14) 0.0155(15) 
N1 0.035(5) 0.021(5) 0.014(5) 0.009(4) 0.010(4) -0.001(4) 
N2 0.033(6) 0.025(5) 0.021(5) 0.010(4) 0.008(4) 0.016(5) 
N3 0.036(5) 0.026(5) 0.013(5) 0.002(4) 0.006(4) 0.020(4) 
N4 0.024(5) 0.028(5) 0.020(5) 0.010(4) -0.006(4) 0.012(4) 
N5 0.032(5) 0.021(5) 0.013(5) 0.007(4) -0.001(4) 0.004(4) 
C11 0.028(7) 0.022(7) 0.024(7) 0.006(6) -0.013(6) 0.002(6) 
C12 0.036(7) 0.044(8) 0.016(6) 0.016(6) 0.004(6) 0.017(6) 
C13 0.041(8) 0.047(8) 0.023(7) 0.020(7) -0.002(6) 0.009(7) 
C14 0.031(7) 0.068(10) 0.035(8) 0.035(8) 0.016(6) 0.010(7) 
C15 0.033(7) 0.059(9) 0.025(7) 0.023(7) 0.008(6) 0.024(7) 
C16 0.034(7) 0.041(7) 0.035(7) 0.019(7) 0.007(6) 0.017(6) 
C17 0.044(7) 0.070(9) 0.016(6) 0.024(6) 0.013(6) 0.037(7) 
C18 0.071(9) 0.092(10) 0.048(8) 0.042(8) 0.024(7) 0.052(9) 
C19 0.062(9) 0.067(9) 0.029(7) 0.021(7) -0.007(6) 0.030(7) 
C21 0.034(7) 0.022(6) 0.010(6) 0.003(5) 0.001(5) 0.005(6) 
C22 0.051(8) 0.016(6) 0.028(7) 0.008(5) 0.000(6) 0.010(6) 
C23 0.046(8) 0.026(7) 0.035(8) 0.005(6) 0.014(6) 0.009(6) 
C24 0.065(9) 0.030(7) 0.061(10) 0.001(7) 0.029(7) 0.031(7) 
C25 0.068(9) 0.032(7) 0.040(8) 0.001(6) -0.004(7) 0.029(7) 
C26 0.066(9) 0.038(7) 0.014(6) 0.006(6) 0.011(6) 0.029(7) 
C27 0.036(7) 0.026(6) 0.035(7) 0.012(5) 0.018(6) 0.019(6) 
C28 0.045(8) 0.060(8) 0.022(7) 0.001(6) -0.002(6) 0.027(7) 
C29 0.042(7) 0.030(7) 0.034(7) 0.007(5) 0.001(6) 0.016(6) 
C31 0.022(7) 0.032(7) 0.014(6) 0.020(6) 0.006(5) 0.009(6) 
C32 0.021(6) 0.030(7) 0.020(6) 0.015(6) 0.009(5) 0.006(6) 
C33 0.044(8) 0.022(7) 0.024(7) 0.003(5) 0.006(6) 0.015(6) 
C34 0.050(9) 0.030(7) 0.026(7) 0.003(6) 0.010(6) 0.025(7) 
C35 0.036(8) 0.047(8) 0.029(7) 0.008(6) 0.008(6) 0.031(7) 
C36 0.036(8) 0.023(6) 0.016(6) 0.011(5) -0.005(5) 0.012(6) 
C37 0.061(8) 0.035(7) 0.009(6) 0.014(5) 0.015(5) 0.027(6) 
C38 0.077(9) 0.038(7) 0.020(6) 0.008(6) 0.022(6) 0.032(7) 
C39 0.059(8) 0.055(8) 0.026(7) 0.020(6) 0.007(6) 0.024(7) 
C48 0.042(7) 0.040(7) 0.036(7) 0.013(6) 0.004(6) 0.020(6) 
C51 0.016(6) 0.025(7) 0.017(6) 0.003(5) -0.005(5) 0.006(5) 
C52 0.030(7) 0.038(7) 0.042(7) 0.010(6) 0.004(6) 0.003(6) 
C53 0.047(8) 0.050(8) 0.034(7) 0.025(6) 0.015(6) 0.020(6) 
C54 0.053(8) 0.033(7) 0.026(7) 0.013(5) 0.003(6) 0.006(6) 
C58 0.048(8) 0.081(9) 0.042(7) 0.047(7) 0.013(6) 0.035(7) 
C131 0.064(9) 0.056(9) 0.067(9) 0.042(7) 0.013(7) 0.005(8) 
C151 0.064(9) 0.077(9) 0.038(8) 0.026(7) 0.020(7) 0.042(8) 
C231 0.071(9) 0.041(8) 0.040(8) -0.001(6) 0.026(7) 0.018(7) 
C251 0.131(13) 0.074(10) 0.074(10) 0.046(8) 0.027(9) 0.076(10) 
C310 0.068(9) 0.032(7) 0.027(7) 0.015(6) 0.022(6) 0.024(7) 
C331 0.049(8) 0.028(7) 0.048(8) -0.005(6) 0.005(6) 0.004(7) 
C351 0.040(8) 0.058(8) 0.048(8) -0.009(6) -0.003(6) 0.029(7) 

_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 
Nb N4 1.790(7) . ? 
Nb N1 2.005(8) . ? 
Nb N3 2.037(7) . ? 
Nb N2 2.050(8) . ? 
P N4 1.719(8) . ? 
P N5 1.727(8) 2_656 ? 
P N5 1.734(7) . ? 
P P 2.653(5) 2_656 ? 
N1 C11 1.445(12) . ? 
N1 C17 1.526(12) . ? 
N2 C21 1.436(11) . ? 
N2 C27 1.503(12) . ? 
N3 C31 1.459(11) . ? 
N3 C37 1.510(11) . ? 
N5 C51 1.479(11) . ? 
N5 P 1.727(8) 2_656 ? 
C11 C12 1.378(13) . ? 
C11 C16 1.388(13) . ? 
C12 C13 1.403(13) . ? 
C13 C14 1.390(14) . ? 
C13 C131 1.518(14) . ? 
C14 C15 1.370(14) . ? 
C15 C16 1.389(13) . ? 
C15 C151 1.526(14) . ? 
C17 C18 1.515(14) . ? 
C17 C58 1.517(13) . ? 
C17 C19 1.532(14) . ? 
C21 C26 1.385(13) . ? 
C21 C22 1.408(13) . ? 
C22 C23 1.386(14) . ? 
C23 C24 1.37(2) . ? 
C23 C231 1.516(14) . ? 
C24 C25 1.387(15) . ? 
C25 C26 1.390(14) . ? 
C25 C251 1.524(15) . ? 
C27 C48 1.527(13) . ? 
C27 C28 1.540(13) . ? 
C27 C29 1.545(13) . ? 
C31 C32 1.389(12) . ? 
C31 C36 1.393(12) . ? 
C32 C33 1.392(13) . ? 
C33 C34 1.377(13) . ? 
C33 C331 1.494(13) . ? 
C34 C35 1.397(14) . ? 
C35 C36 1.399(13) . ? 
C35 C351 1.512(14) . ? 
C37 C38 1.511(12) . ? 
C37 C310 1.535(13) . ? 
C37 C39 1.558(14) . ? 
C51 C54 1.516(13) . ? 
C51 C52 1.521(13) . ? 
C51 C53 1.525(12) . ? 

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 Nb N1 105.1(3) . . ? 
N4 Nb N3 107.2(3) . . ? 
N1 Nb N3 112.9(3) . . ? 
N4 Nb N2 110.4(3) . . ? 
N1 Nb N2 110.0(3) . . ? 
N3 Nb N2 111.0(3) . . ? 
N4 P N5 105.1(4) . 2_656 ? 
N4 P N5 108.7(4) . . ? 
N5 P N5 79.9(4) 2_656 . ? 
N4 P P 112.2(3) . 2_656 ? 
N5 P P 40.1(2) 2_656 2_656 ? 
N5 P P 39.8(2) . 2_656 ? 
C11 N1 C17 112.1(7) . . ? 
C11 N1 Nb 113.2(6) . . ? 
C17 N1 Nb 133.7(6) . . ? 
C21 N2 C27 114.8(7) . . ? 
C21 N2 Nb 116.4(6) . . ? 
C27 N2 Nb 128.6(6) . . ? 
C31 N3 C37 112.2(7) . . ? 
C31 N3 Nb 119.3(5) . . ? 
C37 N3 Nb 128.4(5) . . ? 
P N4 Nb 167.0(5) . . ? 
C51 N5 P 128.7(6) . 2_656 ? 
C51 N5 P 129.0(6) . . ? 
P N5 P 100.1(4) 2_656 . ? 
C12 C11 C16 118.3(10) . . ? 
C12 C11 N1 120.2(9) . . ? 
C16 C11 N1 121.5(9) . . ? 
C11 C12 C13 122.6(10) . . ? 
C14 C13 C12 116.6(10) . . ? 
C14 C13 C131 121.3(10) . . ? 
C12 C13 C131 122.1(10) . . ? 
C15 C14 C13 122.4(10) . . ? 
C14 C15 C16 119.2(10) . . ? 
C14 C15 C151 121.2(10) . . ? 
C16 C15 C151 119.6(10) . . ? 
C11 C16 C15 120.9(10) . . ? 
C18 C17 C58 108.3(9) . . ? 
C18 C17 N1 111.5(8) . . ? 
C58 C17 N1 109.4(8) . . ? 
C18 C17 C19 108.9(9) . . ? 
C58 C17 C19 109.7(8) . . ? 
N1 C17 C19 109.0(8) . . ? 
C26 C21 C22 118.1(10) . . ? 
C26 C21 N2 120.0(9) . . ? 
C22 C21 N2 121.9(9) . . ? 
C23 C22 C21 120.4(10) . . ? 
C24 C23 C22 119.8(10) . . ? 
C24 C23 C231 119.7(11) . . ? 
C22 C23 C231 120.5(11) . . ? 
C23 C24 C25 121.6(10) . . ? 
C24 C25 C26 118.1(10) . . ? 
C24 C25 C251 123.1(11) . . ? 
C26 C25 C251 118.7(11) . . ? 
C21 C26 C25 122.0(10) . . ? 
N2 C27 C48 108.5(8) . . ? 
N2 C27 C28 112.7(8) . . ? 
C48 C27 C28 108.0(8) . . ? 
N2 C27 C29 111.2(8) . . ? 
C48 C27 C29 108.8(8) . . ? 
C28 C27 C29 107.5(8) . . ? 
C32 C31 C36 118.9(9) . . ? 
C32 C31 N3 122.4(8) . . ? 
C36 C31 N3 118.7(8) . . ? 
C31 C32 C33 122.0(9) . . ? 
C34 C33 C32 117.2(9) . . ? 
C34 C33 C331 121.7(9) . . ? 
C32 C33 C331 121.1(10) . . ? 
C33 C34 C35 123.5(9) . . ? 
C34 C35 C36 117.3(9) . . ? 
C34 C35 C351 122.0(9) . . ? 
C36 C35 C351 120.7(10) . . ? 
C31 C36 C35 121.0(9) . . ? 
N3 C37 C38 108.8(7) . . ? 
N3 C37 C310 113.0(8) . . ? 
C38 C37 C310 107.3(8) . . ? 
N3 C37 C39 108.8(8) . . ? 
C38 C37 C39 109.0(9) . . ? 
C310 C37 C39 109.8(8) . . ? 
N5 C51 C54 109.0(8) . . ? 
N5 C51 C52 110.0(7) . . ? 
C54 C51 C52 109.9(8) . . ? 
N5 C51 C53 109.1(7) . . ? 
C54 C51 C53 111.0(8) . . ? 
C52 C51 C53 107.9(8) . . ? 

_refine_diff_density_max    0.496 
_refine_diff_density_min   -0.402 
_refine_diff_density_rms    0.089