#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:50:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178826 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/80/4108076.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4108076
loop_
_publ_author_name
'Nicholas A. Piro'
'Christopher C. Cummins'
_publ_contact_author_address
;Department of Chemistry
Massachusetts Institute of Technology
77 Massachusetts Avenue, Room 6-435
Cambridge, MA  02139-4307 (USA)
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_fax         617-258-5700
_publ_contact_author_name        'Christopher C. Cummins'
_publ_contact_author_phone       617-253-5332
_publ_section_title
;
 P2Addition to Terminal Phosphide M\\tbP Triple Bonds: A Rational
 Synthesis of cyclo-P3 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9524
_journal_page_last               9535
_journal_paper_doi               10.1021/ja802080m
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C59 H76 N3 Na Nb O11 P3 W2'
_chemical_formula_weight         1579.74
_chemical_name_common
'{Et2ONa}{[W(CO)5]2(cyclo-P3)Nb(N[Np]Ar)3} (C6H6)'
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.235(4)
_cell_angle_beta                 91.068(4)
_cell_angle_gamma                94.536(4)
_cell_formula_units_Z            2
_cell_length_a                   12.145(3)
_cell_length_b                   13.565(3)
_cell_length_c                   22.695(6)
_cell_measurement_reflns_used    7638
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     3575.3(15)
_computing_cell_refinement       'SAINT 7 (Bruker-AXS, 2005)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 7 (Bruker-AXS, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62023
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.5419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14086
_refine_ls_number_restraints     797
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0677P)²+2.6066P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                9270
_reflns_number_total             14086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802080m-file003.cif
_cod_data_source_block           06215
_cod_original_cell_volume        3575.5(15)
_cod_database_code               4108076
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
W1 W 0.44767(3) 0.33080(3) 0.406785(15) 0.02741(11) Uani 1 1 d . A .
Nb1 Nb 0.24432(5) 0.36460(6) 0.20884(3) 0.01959(16) Uani 1 1 d . A .
P1 P 0.25631(17) 0.48466(17) 0.31856(10) 0.0247(5) Uani 1 1 d . A .
N1 N 0.1219(5) 0.4228(5) 0.1723(3) 0.0241(15) Uani 1 1 d . . .
Na1 Na 0.2443(3) 0.6603(3) 0.43419(16) 0.0500(11) Uani 1 1 d . . .
W2 W 0.00824(3) 0.30760(3) 0.380927(15) 0.02746(11) Uani 1 1 d . B .
P2 P 0.16122(17) 0.33840(17) 0.30758(9) 0.0233(5) Uani 1 1 d . . .
N2 N 0.2371(7) 0.2121(6) 0.1707(3) 0.039(2) Uani 1 1 d . . .
P3 P 0.34070(17) 0.34528(18) 0.31101(10) 0.0257(5) Uani 1 1 d . A .
N3 N 0.3829(5) 0.4405(5) 0.1880(3) 0.0215(14) Uani 1 1 d . . .
C11 C 0.0388(6) 0.3649(6) 0.1282(3) 0.0267(19) Uani 1 1 d D . .
C12 C -0.0342(6) 0.2917(6) 0.1419(4) 0.0267(19) Uani 1 1 d D . .
H12 H -0.0293 0.2798 0.1812 0.032 Uiso 1 1 calc R . .
C13 C -0.1159(7) 0.2344(7) 0.0979(4) 0.037(2) Uani 1 1 d D . .
C131 C -0.1948(8) 0.1554(7) 0.1138(5) 0.051(3) Uani 1 1 d D . .
H13A H -0.2697 0.1779 0.1154 0.076 Uiso 1 1 calc R . .
H13B H -0.1724 0.1478 0.1539 0.076 Uiso 1 1 calc R . .
H13C H -0.1937 0.0891 0.0824 0.076 Uiso 1 1 calc R . .
C14 C -0.1196(7) 0.2527(7) 0.0417(4) 0.038(2) Uani 1 1 d D . .
H14 H -0.1740 0.2138 0.0118 0.045 Uiso 1 1 calc R . .
C15 C -0.0480(7) 0.3251(7) 0.0262(4) 0.037(2) Uani 1 1 d D . .
C151 C -0.0535(9) 0.3429(8) -0.0368(4) 0.053(3) Uani 1 1 d D . .
H15A H 0.0095 0.3902 -0.0406 0.080 Uiso 1 1 calc R . .
H15B H -0.1225 0.3728 -0.0422 0.080 Uiso 1 1 calc R . .
H15C H -0.0511 0.2770 -0.0685 0.080 Uiso 1 1 calc R . .
C16 C 0.0324(6) 0.3803(6) 0.0701(3) 0.0287(19) Uani 1 1 d D . .
H16 H 0.0838 0.4292 0.0603 0.034 Uiso 1 1 calc R . .
C17 C 0.1262(6) 0.5356(6) 0.1847(4) 0.0261(19) Uani 1 1 d D . .
H17A H 0.1353 0.5521 0.1451 0.031 Uiso 1 1 calc R . .
H17B H 0.1933 0.5661 0.2109 0.031 Uiso 1 1 calc R . .
C18 C 0.0258(6) 0.5906(6) 0.2161(4) 0.029(2) Uani 1 1 d D . .
C181 C 0.0618(9) 0.7053(6) 0.2329(5) 0.055(3) Uani 1 1 d D . .
H18A H 0.0020 0.7443 0.2535 0.082 Uiso 1 1 calc R . .
H18B H 0.0787 0.7251 0.1955 0.082 Uiso 1 1 calc R . .
H18C H 0.1278 0.7204 0.2605 0.082 Uiso 1 1 calc R . .
C182 C -0.0751(6) 0.5714(7) 0.1721(4) 0.035(2) Uani 1 1 d D . .
H18D H -0.1016 0.4981 0.1609 0.053 Uiso 1 1 calc R . .
H18E H -0.0548 0.5908 0.1350 0.053 Uiso 1 1 calc R . .
H18F H -0.1337 0.6128 0.1921 0.053 Uiso 1 1 calc R . .
C183 C -0.0027(7) 0.5578(7) 0.2729(4) 0.039(2) Uani 1 1 d D . .
H18G H 0.0587 0.5807 0.3036 0.058 Uiso 1 1 calc R . .
H18H H -0.0158 0.4825 0.2619 0.058 Uiso 1 1 calc R . .
H18I H -0.0695 0.5888 0.2900 0.058 Uiso 1 1 calc R . .
C21 C 0.2760(10) 0.1830(13) 0.1073(5) 0.026(3) Uani 0.711(9) 1 d PDU A 1
C22 C 0.1959(10) 0.1719(11) 0.0607(5) 0.030(3) Uani 0.711(9) 1 d PDU A 1
H22 H 0.1217 0.1844 0.0708 0.036 Uiso 0.711(9) 1 calc PR A 1
C23 C 0.2242(10) 0.1421(10) -0.0014(5) 0.028(3) Uani 0.711(9) 1 d PDU A 1
C231 C 0.1352(11) 0.1259(12) -0.0516(6) 0.046(4) Uani 0.711(9) 1 d PDU A 1
H23A H 0.1695 0.1276 -0.0901 0.069 Uiso 0.711(9) 1 calc PR A 1
H23B H 0.0851 0.1807 -0.0401 0.069 Uiso 0.711(9) 1 calc PR A 1
H23C H 0.0934 0.0589 -0.0572 0.069 Uiso 0.711(9) 1 calc PR A 1
C24 C 0.3330(9) 0.1244(11) -0.0137(5) 0.029(3) Uani 0.711(9) 1 d PDU A 1
H24 H 0.3530 0.1045 -0.0554 0.035 Uiso 0.711(9) 1 calc PR A 1
C25 C 0.4148(9) 0.1341(10) 0.0316(5) 0.032(3) Uani 0.711(9) 1 d PDU A 1
C251 C 0.5350(10) 0.1233(12) 0.0175(7) 0.050(4) Uani 0.711(9) 1 d PDU A 1
H25A H 0.5414 0.0921 -0.0266 0.075 Uiso 0.711(9) 1 calc PR A 1
H25B H 0.5656 0.0792 0.0402 0.075 Uiso 0.711(9) 1 calc PR A 1
H25C H 0.5762 0.1915 0.0298 0.075 Uiso 0.711(9) 1 calc PR A 1
C26 C 0.3837(10) 0.1626(10) 0.0926(5) 0.029(3) Uani 0.711(9) 1 d PDU A 1
H26 H 0.4374 0.1681 0.1246 0.034 Uiso 0.711(9) 1 calc PR A 1
C27 C 0.2606(10) 0.1299(9) 0.2017(6) 0.037(3) Uani 0.711(9) 1 d PDU A 1
H27A H 0.2585 0.1597 0.2467 0.044 Uiso 0.711(9) 1 calc PR A 1
H27B H 0.3362 0.1096 0.1923 0.044 Uiso 0.711(9) 1 calc PR A 1
C28 C 0.1789(10) 0.0329(9) 0.1820(6) 0.039(3) Uani 0.711(9) 1 d PDU A 1
C281 C 0.0614(9) 0.0644(10) 0.1868(6) 0.045(3) Uani 0.711(9) 1 d PDU A 1
H28A H 0.0096 0.0033 0.1824 0.068 Uiso 0.711(9) 1 calc PR A 1
H28B H 0.0452 0.0962 0.1542 0.068 Uiso 0.711(9) 1 calc PR A 1
H28C H 0.0535 0.1139 0.2269 0.068 Uiso 0.711(9) 1 calc PR A 1
C282 C 0.1998(14) -0.0290(17) 0.2281(11) 0.046(4) Uani 0.711(9) 1 d PDU A 1
H28D H 0.1925 0.0148 0.2700 0.069 Uiso 0.711(9) 1 calc PR A 1
H28E H 0.2746 -0.0518 0.2238 0.069 Uiso 0.711(9) 1 calc PR A 1
H28F H 0.1457 -0.0892 0.2199 0.069 Uiso 0.711(9) 1 calc PR A 1
C283 C 0.196(2) -0.038(2) 0.1171(9) 0.059(5) Uani 0.711(9) 1 d PDU A 1
H28G H 0.2728 -0.0555 0.1141 0.088 Uiso 0.711(9) 1 calc PR A 1
H28H H 0.1790 -0.0028 0.0863 0.088 Uiso 0.711(9) 1 calc PR A 1
H28I H 0.1465 -0.1017 0.1098 0.088 Uiso 0.711(9) 1 calc PR A 1
C61 C 0.239(2) 0.187(4) 0.1060(11) 0.031(5) Uani 0.289(9) 1 d PDU A 2
C62 C 0.347(2) 0.184(3) 0.0874(11) 0.033(5) Uani 0.289(9) 1 d PDU A 2
H62 H 0.4063 0.2003 0.1171 0.039 Uiso 0.289(9) 1 calc PR A 2
C63 C 0.3678(19) 0.157(3) 0.0240(12) 0.040(5) Uani 0.289(9) 1 d PDU A 2
C631 C 0.485(2) 0.168(4) 0.0037(17) 0.071(10) Uani 0.289(9) 1 d PDU A 2
H63A H 0.4837 0.1786 -0.0373 0.107 Uiso 0.289(9) 1 calc PR A 2
H63B H 0.5213 0.1055 0.0024 0.107 Uiso 0.289(9) 1 calc PR A 2
H63C H 0.5261 0.2275 0.0328 0.107 Uiso 0.289(9) 1 calc PR A 2
C64 C 0.2785(19) 0.126(3) -0.0169(11) 0.033(5) Uani 0.289(9) 1 d PDU A 2
H64 H 0.2921 0.1073 -0.0595 0.039 Uiso 0.289(9) 1 calc PR A 2
C65 C 0.1702(19) 0.120(3) 0.0002(11) 0.035(5) Uani 0.289(9) 1 d PDU A 2
C651 C 0.072(2) 0.087(3) -0.0446(13) 0.042(8) Uani 0.289(9) 1 d PDU A 2
H65A H 0.0962 0.0773 -0.0866 0.062 Uiso 0.289(9) 1 calc PR A 2
H65B H 0.0195 0.1405 -0.0354 0.062 Uiso 0.289(9) 1 calc PR A 2
H65C H 0.0348 0.0222 -0.0409 0.062 Uiso 0.289(9) 1 calc PR A 2
C66 C 0.152(2) 0.151(3) 0.0629(11) 0.034(5) Uani 0.289(9) 1 d PDU A 2
H66 H 0.0782 0.1463 0.0763 0.040 Uiso 0.289(9) 1 calc PR A 2
C67 C 0.160(2) 0.1261(19) 0.1887(13) 0.038(5) Uani 0.289(9) 1 d PDU A 2
H67A H 0.1344 0.1538 0.2308 0.045 Uiso 0.289(9) 1 calc PR A 2
H67B H 0.0945 0.1052 0.1601 0.045 Uiso 0.289(9) 1 calc PR A 2
C68 C 0.226(2) 0.0317(19) 0.1856(14) 0.042(5) Uani 0.289(9) 1 d PDU A 2
C681 C 0.166(3) -0.025(4) 0.226(3) 0.051(8) Uani 0.289(9) 1 d PDU A 2
H68A H 0.2073 -0.0829 0.2294 0.077 Uiso 0.289(9) 1 calc PR A 2
H68B H 0.0916 -0.0519 0.2084 0.077 Uiso 0.289(9) 1 calc PR A 2
H68C H 0.1599 0.0220 0.2673 0.077 Uiso 0.289(9) 1 calc PR A 2
C682 C 0.226(4) -0.039(4) 0.120(2) 0.046(9) Uani 0.289(9) 1 d PDU A 2
H68D H 0.2093 -0.1112 0.1201 0.068 Uiso 0.289(9) 1 calc PR A 2
H68E H 0.2982 -0.0314 0.1028 0.068 Uiso 0.289(9) 1 calc PR A 2
H68F H 0.1689 -0.0211 0.0943 0.068 Uiso 0.289(9) 1 calc PR A 2
C683 C 0.3460(19) 0.062(2) 0.2088(14) 0.042(7) Uani 0.289(9) 1 d PDU A 2
H68G H 0.3484 0.1056 0.2513 0.064 Uiso 0.289(9) 1 calc PR A 2
H68H H 0.3841 0.0990 0.1829 0.064 Uiso 0.289(9) 1 calc PR A 2
H68I H 0.3827 -0.0009 0.2073 0.064 Uiso 0.289(9) 1 calc PR A 2
C31 C 0.3692(6) 0.4820(6) 0.1364(4) 0.029(2) Uani 1 1 d D A .
C32 C 0.3442(7) 0.4182(6) 0.0777(3) 0.031(2) Uani 1 1 d D . .
H32 H 0.3365 0.3457 0.0711 0.037 Uiso 1 1 calc R A .
C33 C 0.3301(8) 0.4582(7) 0.0276(4) 0.038(2) Uani 1 1 d D A .
C331 C 0.3072(12) 0.3866(9) -0.0364(4) 0.078(4) Uani 1 1 d D . .
H33A H 0.2577 0.4173 -0.0595 0.117 Uiso 1 1 calc R A .
H33B H 0.2723 0.3204 -0.0339 0.117 Uiso 1 1 calc R . .
H33C H 0.3769 0.3757 -0.0574 0.117 Uiso 1 1 calc R . .
C34 C 0.3410(8) 0.5616(7) 0.0364(4) 0.048(3) Uani 1 1 d D . .
H34 H 0.3330 0.5885 0.0022 0.058 Uiso 1 1 calc R A .
C35 C 0.3638(10) 0.6286(7) 0.0946(5) 0.059(3) Uani 1 1 d D A .
C351 C 0.3666(17) 0.7419(8) 0.1041(6) 0.129(8) Uani 1 1 d D . .
H35A H 0.4407 0.7685 0.0964 0.193 Uiso 1 1 calc R A .
H35B H 0.3485 0.7755 0.1465 0.193 Uiso 1 1 calc R . .
H35C H 0.3125 0.7563 0.0757 0.193 Uiso 1 1 calc R . .
C36 C 0.3782(8) 0.5876(7) 0.1438(4) 0.044(2) Uani 1 1 d D . .
H36 H 0.3948 0.6333 0.1836 0.053 Uiso 1 1 calc R A .
C37 C 0.4840(6) 0.4847(7) 0.2266(4) 0.031(2) Uani 1 1 d D A .
H37A H 0.4692 0.4846 0.2694 0.037 Uiso 1 1 calc R . .
H37B H 0.4984 0.5575 0.2265 0.037 Uiso 1 1 calc R . .
C38 C 0.5902(6) 0.4299(7) 0.2078(4) 0.041(3) Uani 1 1 d D . .
C381 C 0.6836(7) 0.4997(9) 0.2479(4) 0.057(3) Uani 1 1 d D A .
H38A H 0.6647 0.5148 0.2911 0.086 Uiso 1 1 calc R . .
H38B H 0.6941 0.5642 0.2364 0.086 Uiso 1 1 calc R . .
H38C H 0.7520 0.4650 0.2419 0.086 Uiso 1 1 calc R . .
C382 C 0.5800(8) 0.3252(8) 0.2194(5) 0.052(3) Uani 1 1 d D A .
H38D H 0.5116 0.2863 0.1993 0.078 Uiso 1 1 calc R . .
H38E H 0.5785 0.3339 0.2637 0.078 Uiso 1 1 calc R . .
H38F H 0.6435 0.2877 0.2028 0.078 Uiso 1 1 calc R . .
C383 C 0.6126(7) 0.4189(9) 0.1402(4) 0.050(3) Uani 1 1 d D A .
H38G H 0.6829 0.3885 0.1302 0.076 Uiso 1 1 calc R . .
H38H H 0.6167 0.4870 0.1329 0.076 Uiso 1 1 calc R . .
H38I H 0.5527 0.3742 0.1141 0.076 Uiso 1 1 calc R . .
O41 O 0.5726(5) 0.3162(5) 0.5257(3) 0.0388(16) Uani 1 1 d . . .
C41 C 0.5247(7) 0.3202(7) 0.4810(4) 0.032(2) Uani 1 1 d . . .
O42 O 0.2815(5) 0.4912(5) 0.4749(3) 0.0392(16) Uani 1 1 d . B .
C42 C 0.3405(7) 0.4305(7) 0.4527(4) 0.033(2) Uani 1 1 d . . .
O43 O 0.2842(6) 0.1313(6) 0.3972(3) 0.0533(19) Uani 1 1 d . B .
C43 C 0.3421(8) 0.2046(7) 0.4020(4) 0.034(2) Uani 1 1 d . . .
O44 O 0.6227(7) 0.1894(7) 0.3318(4) 0.068(2) Uani 1 1 d . B .
C44 C 0.5572(9) 0.2399(8) 0.3576(4) 0.047(3) Uani 1 1 d . . .
O45 O 0.6071(6) 0.5269(6) 0.4025(3) 0.0485(18) Uani 1 1 d . B .
C45 C 0.5502(7) 0.4570(8) 0.4042(4) 0.034(2) Uani 1 1 d . . .
O51 O -0.1922(5) 0.2920(5) 0.4631(3) 0.0414(16) Uani 1 1 d . . .
C51 C -0.1149(8) 0.2981(8) 0.4329(4) 0.041(2) Uani 1 1 d . . .
O52 O 0.1531(5) 0.2970(6) 0.4972(3) 0.053(2) Uani 1 1 d . B .
C52 C 0.1061(8) 0.3034(8) 0.4546(5) 0.041(2) Uani 1 1 d . . .
O53 O 0.0370(6) 0.5507(6) 0.4310(3) 0.0458(17) Uani 1 1 d . B .
C53 C 0.0217(7) 0.4625(8) 0.4122(4) 0.036(2) Uani 1 1 d . . .
C54 C -0.1025(8) 0.3031(9) 0.3128(5) 0.048(3) Uani 1 1 d . . .
O54 O -0.1702(6) 0.2947(7) 0.2746(3) 0.066(2) Uani 1 1 d . B .
O55 O 0.0064(7) 0.0628(6) 0.3419(4) 0.078(3) Uani 1 1 d . B .
C55 C 0.0088(9) 0.1514(9) 0.3544(5) 0.052(3) Uani 1 1 d . . .
C1T C 0.4082(18) 0.7591(15) 0.3337(9) 0.086(5) Uani 0.646(9) 1 d PDU B 1
H1T1 H 0.4700 0.7836 0.3128 0.130 Uiso 0.646(9) 1 calc PR B 1
H1T2 H 0.3650 0.7011 0.3046 0.130 Uiso 0.646(9) 1 calc PR B 1
H1T3 H 0.4370 0.7365 0.3680 0.130 Uiso 0.646(9) 1 calc PR B 1
C2T C 0.3280(17) 0.8539(15) 0.3603(11) 0.086(4) Uani 0.646(9) 1 d PDU B 1
H2T1 H 0.3678 0.9129 0.3913 0.104 Uiso 0.646(9) 1 calc PR B 1
H2T2 H 0.2961 0.8781 0.3269 0.104 Uiso 0.646(9) 1 calc PR B 1
O1T O 0.2369(11) 0.7948(11) 0.3900(7) 0.086(3) Uani 0.646(9) 1 d PDU B 1
C3T C 0.1553(17) 0.8838(15) 0.4079(11) 0.089(4) Uani 0.646(9) 1 d PDU B 1
H3T1 H 0.1292 0.9043 0.3718 0.107 Uiso 0.646(9) 1 calc PR B 1
H3T2 H 0.1881 0.9452 0.4400 0.107 Uiso 0.646(9) 1 calc PR B 1
C4T C 0.0589(18) 0.8182(18) 0.4338(11) 0.091(5) Uani 0.646(9) 1 d PDU B 1
H4T1 H -0.0016 0.8615 0.4482 0.136 Uiso 0.646(9) 1 calc PR B 1
H4T2 H 0.0897 0.7965 0.4679 0.136 Uiso 0.646(9) 1 calc PR B 1
H4T3 H 0.0307 0.7573 0.4008 0.136 Uiso 0.646(9) 1 calc PR B 1
C1TA C 0.330(3) 0.787(3) 0.3689(19) 0.088(4) Uani 0.354(9) 1 d PDU B 2
H1T4 H 0.3845 0.8221 0.3482 0.132 Uiso 0.354(9) 1 calc PR B 2
H1T5 H 0.3007 0.7217 0.3404 0.132 Uiso 0.354(9) 1 calc PR B 2
H1T6 H 0.3662 0.7745 0.4047 0.132 Uiso 0.354(9) 1 calc PR B 2
C2TA C 0.228(3) 0.862(3) 0.391(2) 0.090(4) Uani 0.354(9) 1 d PDU B 2
H2T3 H 0.2530 0.9264 0.4232 0.108 Uiso 0.354(9) 1 calc PR B 2
H2T4 H 0.1896 0.8772 0.3567 0.108 Uiso 0.354(9) 1 calc PR B 2
O1TA O 0.156(2) 0.7837(19) 0.4183(12) 0.089(4) Uani 0.354(9) 1 d PDU B 2
C3TA C 0.037(2) 0.817(3) 0.4130(18) 0.090(5) Uani 0.354(9) 1 d PDU B 2
H3T3 H -0.0207 0.7625 0.4146 0.108 Uiso 0.354(9) 1 calc PR B 2
H3T4 H 0.0251 0.8395 0.3756 0.108 Uiso 0.354(9) 1 calc PR B 2
C4TA C 0.046(4) 0.914(3) 0.4760(17) 0.105(8) Uani 0.354(9) 1 d PDU B 2
H4T4 H -0.0254 0.9431 0.4829 0.157 Uiso 0.354(9) 1 calc PR B 2
H4T5 H 0.1022 0.9678 0.4716 0.157 Uiso 0.354(9) 1 calc PR B 2
H4T6 H 0.0677 0.8902 0.5111 0.157 Uiso 0.354(9) 1 calc PR B 2
C1S C 0.8098(9) -0.0957(11) 0.2247(7) 0.063(4) Uani 0.50 1 d PGU . .
H1S H 0.8845 -0.1006 0.2359 0.075 Uiso 0.50 1 calc PR . .
C2S C 0.7383(11) -0.1845(8) 0.2034(7) 0.056(4) Uani 0.50 1 d PGU . .
H2S H 0.7641 -0.2500 0.2000 0.068 Uiso 0.50 1 calc PR . .
C3S C 0.6290(10) -0.1773(7) 0.1870(6) 0.047(3) Uani 0.50 1 d PGU . .
H3S H 0.5801 -0.2380 0.1724 0.056 Uiso 0.50 1 calc PR . .
C4S C 0.5912(8) -0.0814(9) 0.1919(6) 0.043(3) Uani 0.50 1 d PGU . .
H4S H 0.5165 -0.0765 0.1807 0.051 Uiso 0.50 1 calc PR . .
C5S C 0.6627(11) 0.0074(7) 0.2132(6) 0.044(3) Uani 0.50 1 d PGU . .
H5S H 0.6368 0.0730 0.2166 0.052 Uiso 0.50 1 calc PR . .
C6S C 0.7720(10) 0.0003(8) 0.2296(6) 0.056(4) Uani 0.50 1 d PGU . .
H6S H 0.8208 0.0609 0.2442 0.067 Uiso 0.50 1 calc PR . .
C1R C 0.2481(16) 0.0963(16) 0.6310(8) 0.106(6) Uani 0.50 1 d PGU . .
H1R H 0.2017 0.1035 0.6649 0.127 Uiso 0.50 1 calc PR . .
C2R C 0.2939(17) 0.0037(13) 0.6060(9) 0.106(6) Uani 0.50 1 d PGU . .
H2R H 0.2789 -0.0523 0.6229 0.127 Uiso 0.50 1 calc PR . .
C3R C 0.3616(17) -0.0069(12) 0.5563(9) 0.107(6) Uani 0.50 1 d PGU . .
H3R H 0.3930 -0.0701 0.5393 0.129 Uiso 0.50 1 calc PR . .
C4R C 0.3836(15) 0.0752(16) 0.5316(7) 0.100(6) Uani 0.50 1 d PGU . .
H4R H 0.4299 0.0679 0.4977 0.120 Uiso 0.50 1 calc PR . .
C5R C 0.3378(16) 0.1677(13) 0.5565(8) 0.094(5) Uani 0.50 1 d PGU . .
H5R H 0.3528 0.2238 0.5396 0.112 Uiso 0.50 1 calc PR . .
C6R C 0.2700(16) 0.1783(12) 0.6062(8) 0.099(6) Uani 0.50 1 d PGU . .
H6R H 0.2387 0.2416 0.6233 0.119 Uiso 0.50 1 calc PR . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C41 W1 C44 87.6(4) . .
C41 W1 C43 92.6(4) . .
C44 W1 C43 90.2(4) . .
C41 W1 C42 95.0(3) . .
C44 W1 C42 175.5(4) . .
C43 W1 C42 93.3(4) . .
C41 W1 C45 92.0(3) . .
C44 W1 C45 88.7(4) . .
C43 W1 C45 175.2(3) . .
C42 W1 C45 87.6(4) . .
C41 W1 P3 178.2(2) . .
C44 W1 P3 93.9(3) . .
C43 W1 P3 86.5(2) . .
C42 W1 P3 83.5(2) . .
C45 W1 P3 89.0(2) . .
N2 Nb1 N1 109.4(3) . .
N2 Nb1 N3 112.9(3) . .
N1 Nb1 N3 103.1(3) . .
N2 Nb1 P1 135.6(2) . .
N1 Nb1 P1 100.2(2) . .
N3 Nb1 P1 90.68(19) . .
N2 Nb1 P2 91.0(2) . .
N1 Nb1 P2 102.8(2) . .
N3 Nb1 P2 135.88(18) . .
P1 Nb1 P2 49.82(7) . .
N2 Nb1 P3 90.8(2) . .
N1 Nb1 P3 146.6(2) . .
N3 Nb1 P3 92.33(18) . .
P1 Nb1 P3 49.45(7) . .
P2 Nb1 P3 48.96(7) . .
P2 P1 P3 59.92(10) . .
P2 P1 Nb1 65.48(8) . .
P3 P1 Nb1 67.76(8) . .
P2 P1 Na1 120.68(13) . .
P3 P1 Na1 125.76(12) . .
Nb1 P1 Na1 166.40(12) . .
C11 N1 C17 115.7(6) . .
C11 N1 Nb1 125.9(5) . .
C17 N1 Nb1 117.8(5) . .
O1TA Na1 O1T 30.9(6) . .
O1TA Na1 O51 89.2(7) . 2_566
O1T Na1 O51 111.7(4) . 2_566
O1TA Na1 O41 123.4(7) . 2_666
O1T Na1 O41 102.5(4) . 2_666
O51 Na1 O41 86.2(2) 2_566 2_666
O1TA Na1 O42 158.0(7) . .
O1T Na1 O42 170.8(4) . .
O51 Na1 O42 76.0(2) 2_566 .
O41 Na1 O42 72.4(2) 2_666 .
O1TA Na1 O53 87.1(7) . .
O1T Na1 O53 112.4(4) . .
O51 Na1 O53 75.9(2) 2_566 .
O41 Na1 O53 144.5(3) 2_666 .
O42 Na1 O53 73.7(2) . .
O1TA Na1 P1 112.3(7) . .
O1T Na1 P1 99.0(4) . .
O51 Na1 P1 145.8(2) 2_566 .
O41 Na1 P1 101.9(2) 2_666 .
C1TA Na1 P1 86.9(9) . .
O42 Na1 P1 74.97(16) . .
O53 Na1 P1 78.82(18) . .
C51 W2 C53 91.2(4) . .
C51 W2 C54 88.2(4) . .
C53 W2 C54 93.9(4) . .
C51 W2 C55 90.5(4) . .
C53 W2 C55 174.2(4) . .
C54 W2 C55 91.6(5) . .
C51 W2 C52 85.5(4) . .
C53 W2 C52 89.0(4) . .
C54 W2 C52 173.2(4) . .
C55 W2 C52 85.7(4) . .
C51 W2 P2 172.9(3) . .
C53 W2 P2 83.8(3) . .
C54 W2 P2 87.1(3) . .
C55 W2 P2 94.9(3) . .
C52 W2 P2 99.4(3) . .
P1 P2 P3 60.58(10) . .
P1 P2 Nb1 64.70(8) . .
P3 P2 Nb1 67.64(8) . .
P1 P2 W2 124.01(11) . .
P3 P2 W2 134.59(10) . .
Nb1 P2 W2 157.64(9) . .
C21 N2 C27 109.7(9) . .
C61 N2 C67 108.8(18) . .
C61 N2 Nb1 111.4(19) . .
C21 N2 Nb1 113.4(8) . .
C27 N2 Nb1 127.7(6) . .
C67 N2 Nb1 127.3(10) . .
P2 P3 P1 59.49(10) . .
P2 P3 W1 120.80(11) . .
P1 P3 W1 117.99(11) . .
P2 P3 Nb1 63.40(7) . .
P1 P3 Nb1 62.78(8) . .
W1 P3 Nb1 175.72(9) . .
C31 N3 C37 113.5(6) . .
C31 N3 Nb1 114.9(5) . .
C37 N3 Nb1 129.2(5) . .
C12 C11 C16 119.4(7) . .
C12 C11 N1 120.7(7) . .
C16 C11 N1 119.9(7) . .
C11 C12 C13 120.4(7) . .
C14 C13 C12 118.1(7) . .
C14 C13 C131 122.2(8) . .
C12 C13 C131 119.6(8) . .
C13 C14 C15 123.2(8) . .
C14 C15 C16 117.8(7) . .
C14 C15 C151 121.9(8) . .
C16 C15 C151 120.4(8) . .
C15 C16 C11 121.2(7) . .
N1 C17 C18 117.6(6) . .
C183 C18 C181 110.8(7) . .
C183 C18 C182 110.4(7) . .
C181 C18 C182 107.1(7) . .
C183 C18 C17 110.9(6) . .
C181 C18 C17 105.6(7) . .
C182 C18 C17 111.9(7) . .
C26 C21 C22 119.9(10) . .
C26 C21 N2 124.1(10) . .
C22 C21 N2 116.0(9) . .
C21 C22 C23 120.3(10) . .
C24 C23 C22 117.6(9) . .
C24 C23 C231 122.6(10) . .
C22 C23 C231 119.7(10) . .
C23 C24 C25 123.6(10) . .
C24 C25 C26 117.4(9) . .
C24 C25 C251 122.7(10) . .
C26 C25 C251 119.8(10) . .
C21 C26 C25 121.2(10) . .
N2 C27 C28 114.0(9) . .
C281 C28 C27 109.4(10) . .
C281 C28 C282 109.6(11) . .
C27 C28 C282 105.9(11) . .
C281 C28 C283 110.3(12) . .
C27 C28 C283 114.4(13) . .
C282 C28 C283 107.2(12) . .
C62 C61 C66 119.9(18) . .
C62 C61 N2 110.4(19) . .
C66 C61 N2 128.6(19) . .
C61 C62 C63 120.0(17) . .
C64 C63 C62 117.5(16) . .
C64 C63 C631 122.6(18) . .
C62 C63 C631 119.8(18) . .
C63 C64 C65 124.0(17) . .
C64 C65 C66 117.2(16) . .
C64 C65 C651 124.2(18) . .
C66 C65 C651 118.5(17) . .
C61 C66 C65 121.0(17) . .
C68 C67 N2 109.4(18) . .
C681 C68 C683 109.7(19) . .
C681 C68 C682 110(2) . .
C683 C68 C682 107.9(19) . .
C681 C68 C67 105.3(18) . .
C683 C68 C67 113.0(18) . .
C682 C68 C67 111(2) . .
C32 C31 C36 117.0(7) . .
C32 C31 N3 121.3(7) . .
C36 C31 N3 121.6(7) . .
C31 C32 C33 121.5(8) . .
C34 C33 C32 119.8(8) . .
C34 C33 C331 119.8(8) . .
C32 C33 C331 120.4(8) . .
C33 C34 C35 120.7(8) . .
C34 C35 C36 118.7(9) . .
C34 C35 C351 120.0(9) . .
C36 C35 C351 121.2(10) . .
C31 C36 C35 122.2(8) . .
N3 C37 C38 116.4(6) . .
C382 C38 C381 110.8(8) . .
C382 C38 C383 110.2(8) . .
C381 C38 C383 109.1(7) . .
C382 C38 C37 110.0(7) . .
C381 C38 C37 105.5(7) . .
C383 C38 C37 111.1(7) . .
C41 O41 Na1 138.3(6) . 2_666
O41 C41 W1 178.3(8) . .
C42 O42 Na1 124.1(6) . .
O42 C42 W1 174.3(8) . .
O43 C43 W1 177.3(8) . .
O44 C44 W1 177.0(9) . .
O45 C45 W1 179.7(8) . .
C51 O51 Na1 140.9(6) . 2_566
O51 C51 W2 177.9(8) . .
O52 C52 W2 174.3(8) . .
C53 O53 Na1 123.7(6) . .
O53 C53 W2 175.3(8) . .
O54 C54 W2 175.1(9) . .
O55 C55 W2 176.6(9) . .
O1T C2T C1T 99.2(13) . .
C2T O1T C3T 97.5(12) . .
C2T O1T Na1 132.3(10) . .
C3T O1T Na1 125.6(10) . .
O1T C3T C4T 96.4(13) . .
C2TA C1TA Na1 88.6(16) . .
O1TA C2TA C1TA 96.6(17) . .
C3TA O1TA C2TA 102(2) . .
C3TA O1TA Na1 142(2) . .
C2TA O1TA Na1 114.5(15) . .
O1TA C3TA C4TA 97.0(18) . .
C2S C1S C6S 120.0 . .
C3S C2S C1S 120.0 . .
C2S C3S C4S 120.0 . .
C5S C4S C3S 120.0 . .
C6S C5S C4S 120.0 . .
C5S C6S C1S 120.0 . .
C2R C1R C6R 120.0 . .
C3R C2R C1R 120.0 . .
C2R C3R C4R 120.0 . .
C5R C4R C3R 120.0 . .
C4R C5R C6R 120.0 . .
C5R C6R C1R 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C41 1.957(9) .
W1 C44 2.020(10) .
W1 C43 2.032(10) .
W1 C42 2.037(10) .
W1 C45 2.051(10) .
W1 P3 2.574(2) .
Nb1 N2 2.001(7) .
Nb1 N1 2.006(6) .
Nb1 N3 2.036(6) .
Nb1 P1 2.560(2) .
Nb1 P2 2.577(2) .
Nb1 P3 2.665(2) .
P1 P2 2.164(3) .
P1 P3 2.188(3) .
P1 Na1 3.026(4) .
N1 C11 1.427(9) .
N1 C17 1.474(10) .
Na1 O1TA 2.16(2) .
Na1 O1T 2.320(15) .
Na1 O51 2.351(7) 2_566
Na1 O41 2.351(7) 2_666
Na1 O42 2.768(8) .
Na1 O53 2.810(8) .
W2 C51 1.941(10) .
W2 C53 2.013(11) .
W2 C54 2.015(10) .
W2 C55 2.035(12) .
W2 C52 2.050(11) .
W2 P2 2.604(2) .
P2 P3 2.174(3) .
N2 C61 1.41(2) .
N2 C21 1.479(13) .
N2 C27 1.518(13) .
N2 C67 1.58(3) .
N3 C31 1.446(9) .
N3 C37 1.478(9) .
C11 C12 1.383(9) .
C11 C16 1.393(9) .
C12 C13 1.412(10) .
C13 C14 1.368(10) .
C13 C131 1.503(10) .
C14 C15 1.384(10) .
C15 C16 1.391(10) .
C15 C151 1.517(10) .
C17 C18 1.559(9) .
C18 C183 1.514(10) .
C18 C181 1.520(10) .
C18 C182 1.525(10) .
C21 C26 1.386(12) .
C21 C22 1.391(12) .
C22 C23 1.411(12) .
C23 C24 1.382(12) .
C23 C231 1.514(12) .
C24 C25 1.387(12) .
C25 C26 1.396(12) .
C25 C251 1.510(13) .
C27 C28 1.537(12) .
C28 C281 1.519(13) .
C28 C282 1.542(14) .
C28 C283 1.547(13) .
C61 C62 1.381(16) .
C61 C66 1.393(16) .
C62 C63 1.416(16) .
C63 C64 1.373(16) .
C63 C631 1.515(16) .
C64 C65 1.381(16) .
C65 C66 1.394(16) .
C65 C651 1.512(16) .
C67 C68 1.547(16) .
C68 C681 1.524(17) .
C68 C683 1.528(16) .
C68 C682 1.535(17) .
C31 C32 1.385(10) .
C31 C36 1.389(10) .
C32 C33 1.402(10) .
C33 C34 1.357(11) .
C33 C331 1.511(11) .
C34 C35 1.386(11) .
C35 C36 1.394(11) .
C35 C351 1.488(12) .
C37 C38 1.547(10) .
C38 C382 1.511(11) .
C38 C381 1.524(10) .
C38 C383 1.531(10) .
O41 C41 1.176(10) .
O41 Na1 2.351(6) 2_666
O42 C42 1.149(10) .
O43 C43 1.149(11) .
O44 C44 1.150(11) .
O45 C45 1.138(10) .
O51 C51 1.184(10) .
O51 Na1 2.351(7) 2_566
O52 C52 1.141(11) .
O53 C53 1.151(11) .
C54 O54 1.159(11) .
O55 C55 1.153(12) .
C1T C2T 1.66(2) .
C2T O1T 1.584(18) .
O1T C3T 1.592(17) .
C3T C4T 1.63(2) .
C1TA C2TA 1.66(2) .
C2TA O1TA 1.58(2) .
O1TA C3TA 1.56(2) .
C3TA C4TA 1.65(2) .
C1S C2S 1.3900 .
C1S C6S 1.3900 .
C2S C3S 1.3900 .
C3S C4S 1.3900 .
C4S C5S 1.3900 .
C5S C6S 1.3900 .
C1R C2R 1.3900 .
C1R C6R 1.3900 .
C2R C3R 1.3900 .
C3R C4R 1.3900 .
C4R C5R 1.3900 .
C5R C6R 1.3900 .
