#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:48:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179765 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/61/7006185.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_7006185
loop_
_publ_author_name
'Errington, R. John'
'Petkar, Sagar S.'
'Middleton, Paul S.'
'McFarlane, William'
'Clegg, William'
'Coxall, Robert A.'
'Harrington, Ross W.'
_publ_section_title
;
 Non-aqueous synthetic methodology for TiW(5) polyoxometalates:
 protonolysis of [(MeO)TiW(5)O(18)](3-) with alcohols, water and
 phenols.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5211
_journal_page_last               5222
_journal_paper_doi               10.1039/b709732h
_journal_year                    2007
_chemical_formula_moiety         '3 C16 H36 N +,C3 H7 O19 Ti W5 3-'
_chemical_formula_sum            'C51 H115 N3 O19 Ti W5'
_chemical_formula_weight         2041.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.487(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.276(2)
_cell_length_b                   16.240(3)
_cell_length_c                   23.808(4)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     7033.9(19)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    SIR2002
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39201
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.314
_exptl_absorpt_correction_T_max  0.136
_exptl_absorpt_correction_T_min  0.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.565
_refine_diff_density_min         -2.459
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         10797
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0521P)²+184.6787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                7093
_reflns_number_total             10797
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b709732h.txt
_cod_data_source_block           rje384_(TBA)3[3]
_cod_original_cell_volume        7033.9(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7006185
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.65383(3) 0.20553(4) 0.18369(3) 0.0430(2) Uani 1 1 d . . .
W2 W 0.83399(4) 0.21758(7) 0.18981(3) 0.0706(3) Uani 1 1 d . . .
W3 W 0.84941(4) 0.11716(5) 0.31050(3) 0.0566(2) Uani 1 1 d . . .
W4 W 0.66909(4) 0.10382(5) 0.30410(4) 0.0643(3) Uani 1 1 d . . .
W5 W 0.74816(4) 0.28632(4) 0.29657(3) 0.0508(2) Uani 1 1 d . . .
Ti1 Ti 0.7530(2) 0.0412(2) 0.20248(18) 0.0721(12) Uani 1 1 d . . .
O1 O 0.7586(13) -0.0501(11) 0.1626(10) 0.165(11) Uani 1 1 d . . .
O2 O 0.8937(8) 0.2667(16) 0.1492(7) 0.140(9) Uani 1 1 d . . .
O3 O 0.5828(7) 0.2415(8) 0.1375(5) 0.066(4) Uani 1 1 d . . .
O4 O 0.6102(8) 0.0622(11) 0.3480(8) 0.113(7) Uani 1 1 d . . .
O5 O 0.9202(7) 0.0847(10) 0.3579(6) 0.087(5) Uani 1 1 d . . .
O6 O 0.7453(11) 0.3775(9) 0.3315(7) 0.113(7) Uani 1 1 d . . .
O7 O 0.8341(8) 0.0278(8) 0.2605(6) 0.087(5) Uani 1 1 d . . .
O8 O 0.8200(9) 0.1083(10) 0.1628(6) 0.104(7) Uani 1 1 d . . .
O9 O 0.6751(7) 0.1007(8) 0.1567(6) 0.074(4) Uani 1 1 d . . .
O10 O 0.6877(8) 0.0178(7) 0.2537(8) 0.092(5) Uani 1 1 d . . .
O11 O 0.6819(6) 0.2153(8) 0.3329(5) 0.057(3) Uani 1 1 d . . .
O12 O 0.6705(6) 0.2979(6) 0.2366(5) 0.050(3) Uani 1 1 d . . .
O13 O 0.8139(6) 0.3094(8) 0.2418(5) 0.062(4) Uani 1 1 d . . .
O14 O 0.8269(6) 0.2270(7) 0.3384(5) 0.051(3) Uani 1 1 d . . .
O15 O 0.8978(6) 0.1751(9) 0.2535(5) 0.071(4) Uani 1 1 d . . .
O16 O 0.7398(6) 0.2477(8) 0.1514(5) 0.060(3) Uani 1 1 d . . .
O17 O 0.6055(6) 0.1538(7) 0.2436(6) 0.061(3) Uani 1 1 d . . .
O18 O 0.7637(7) 0.0815(8) 0.3453(6) 0.066(4) Uani 1 1 d . . .
O19 O 0.7513(5) 0.1628(6) 0.2467(4) 0.036(2) Uani 1 1 d . . .
N1 N 0.7480(11) 0.1148(11) 0.5121(8) 0.081(5) Uani 1 1 d . . .
C1 C 0.8250(14) 0.119(2) 0.5401(12) 0.122(10) Uani 1 1 d U . .
H1A H 0.8345 0.0695 0.5627 0.146 Uiso 1 1 calc R . .
H1B H 0.8290 0.1657 0.5654 0.146 Uiso 1 1 calc R . .
C2 C 0.8835(17) 0.126(3) 0.4994(16) 0.186(12) Uani 1 1 d U . .
H2A H 0.8818 0.1793 0.4808 0.224 Uiso 1 1 calc R . .
H2B H 0.8791 0.0828 0.4712 0.224 Uiso 1 1 calc R . .
C3 C 1.016(3) 0.140(5) 0.508(3) 0.35(3) Uani 1 1 d U . .
H3A H 1.0631 0.1378 0.5293 0.518 Uiso 1 1 calc R . .
H3B H 1.0065 0.1958 0.4951 0.518 Uiso 1 1 calc R . .
H3C H 1.0153 0.1041 0.4761 0.518 Uiso 1 1 calc R . .
C4 C 0.9594(18) 0.115(4) 0.543(2) 0.234(16) Uani 1 1 d U . .
H4A H 0.9586 0.1510 0.5760 0.280 Uiso 1 1 calc R . .
H4B H 0.9662 0.0588 0.5558 0.280 Uiso 1 1 calc R . .
C5 C 0.7372(14) 0.0431(17) 0.4688(10) 0.101(7) Uani 1 1 d U . .
H5A H 0.7704 0.0512 0.4399 0.121 Uiso 1 1 calc R . .
H5B H 0.6874 0.0455 0.4507 0.121 Uiso 1 1 calc R . .
C6 C 0.7507(17) -0.0442(18) 0.4947(12) 0.120(8) Uani 1 1 d U . .
H6A H 0.7988 -0.0468 0.5156 0.144 Uiso 1 1 calc R . .
H6B H 0.7139 -0.0566 0.5202 0.144 Uiso 1 1 calc R . .
C7 C 0.746(2) -0.107(2) 0.4458(15) 0.159(12) Uani 1 1 d U . .
H7A H 0.6981 -0.1033 0.4243 0.191 Uiso 1 1 calc R . .
H7B H 0.7834 -0.0953 0.4207 0.191 Uiso 1 1 calc R . .
C8 C 0.757(3) -0.190(2) 0.472(2) 0.220(19) Uani 1 1 d U . .
H8A H 0.7563 -0.2307 0.4425 0.330 Uiso 1 1 calc R . .
H8B H 0.7184 -0.2012 0.4953 0.330 Uiso 1 1 calc R . .
H8C H 0.8036 -0.1917 0.4941 0.330 Uiso 1 1 calc R . .
C9 C 0.6962(14) 0.1044(13) 0.5594(9) 0.085(6) Uani 1 1 d U . .
H9A H 0.7077 0.0525 0.5783 0.102 Uiso 1 1 calc R . .
H9B H 0.7069 0.1479 0.5869 0.102 Uiso 1 1 calc R . .
C10 C 0.6152(14) 0.1060(14) 0.5410(9) 0.086(6) Uani 1 1 d U . .
H10A H 0.6052 0.0753 0.5062 0.103 Uiso 1 1 calc R . .
H10B H 0.5991 0.1624 0.5342 0.103 Uiso 1 1 calc R . .
C11 C 0.5726(16) 0.0672(14) 0.5879(10) 0.101(7) Uani 1 1 d U . .
H11A H 0.5883 0.0105 0.5936 0.121 Uiso 1 1 calc R . .
H11B H 0.5853 0.0966 0.6230 0.121 Uiso 1 1 calc R . .
C12 C 0.4928(16) 0.0690(16) 0.5749(13) 0.121(9) Uani 1 1 d U . .
H12A H 0.4697 0.0449 0.6055 0.182 Uiso 1 1 calc R . .
H12B H 0.4796 0.0384 0.5409 0.182 Uiso 1 1 calc R . .
H12C H 0.4767 0.1250 0.5697 0.182 Uiso 1 1 calc R . .
C13 C 0.7253(13) 0.1906(14) 0.4772(9) 0.083(6) Uani 1 1 d U . .
H13A H 0.6740 0.1854 0.4631 0.100 Uiso 1 1 calc R . .
H13B H 0.7538 0.1926 0.4448 0.100 Uiso 1 1 calc R . .
C14 C 0.7361(15) 0.2719(15) 0.5101(10) 0.100(7) Uani 1 1 d DU . .
H14A H 0.7881 0.2842 0.5177 0.120 Uiso 1 1 calc R . .
H14B H 0.7148 0.2679 0.5458 0.120 Uiso 1 1 calc R . .
C15 C 0.6963(18) 0.3421(15) 0.4721(11) 0.124(9) Uani 1 1 d DU . .
H15A H 0.6448 0.3284 0.4632 0.148 Uiso 1 1 calc R . .
H15B H 0.7189 0.3473 0.4371 0.148 Uiso 1 1 calc R . .
N2 N 0.4860(8) -0.0803(10) 0.1931(6) 0.063(4) Uani 1 1 d . . .
C16 C 0.7039(19) 0.4291(16) 0.5075(13) 0.144(12) Uani 1 1 d DU . .
H16A H 0.6818 0.4727 0.4845 0.215 Uiso 1 1 calc R . .
H16B H 0.7550 0.4411 0.5173 0.215 Uiso 1 1 calc R . .
H16C H 0.6795 0.4241 0.5412 0.215 Uiso 1 1 calc R . .
C17 C 0.4205(11) -0.0496(13) 0.2200(10) 0.077(5) Uani 1 1 d U . .
H17A H 0.4069 -0.0907 0.2466 0.092 Uiso 1 1 calc R . .
H17B H 0.3798 -0.0441 0.1909 0.092 Uiso 1 1 calc R . .
C18 C 0.4312(14) 0.0331(16) 0.2510(10) 0.097(6) Uani 1 1 d U . .
H18A H 0.4498 0.0734 0.2259 0.116 Uiso 1 1 calc R . .
H18B H 0.4674 0.0265 0.2832 0.116 Uiso 1 1 calc R . .
C19 C 0.356(2) 0.066(2) 0.2722(15) 0.155(11) Uani 1 1 d U . .
H19A H 0.3352 0.0225 0.2933 0.186 Uiso 1 1 calc R . .
H19B H 0.3679 0.1113 0.2982 0.186 Uiso 1 1 calc R . .
C20 C 0.299(3) 0.095(4) 0.228(2) 0.26(2) Uani 1 1 d U . .
H20A H 0.2589 0.1189 0.2462 0.391 Uiso 1 1 calc R . .
H20B H 0.2812 0.0494 0.2054 0.391 Uiso 1 1 calc R . .
H20C H 0.3195 0.1357 0.2052 0.391 Uiso 1 1 calc R . .
C21 C 0.5503(10) -0.0983(12) 0.2365(8) 0.065(5) Uani 1 1 d U . .
H21A H 0.5611 -0.0490 0.2588 0.078 Uiso 1 1 calc R . .
H21B H 0.5930 -0.1105 0.2168 0.078 Uiso 1 1 calc R . .
C22 C 0.5386(10) -0.1698(13) 0.2770(8) 0.068(5) Uani 1 1 d U . .
H22A H 0.4981 -0.1569 0.2990 0.082 Uiso 1 1 calc R . .
H22B H 0.5260 -0.2193 0.2554 0.082 Uiso 1 1 calc R . .
C23 C 0.6088(12) -0.1851(14) 0.3169(10) 0.082(6) Uani 1 1 d U . .
H23A H 0.6496 -0.1939 0.2943 0.098 Uiso 1 1 calc R . .
H23B H 0.6195 -0.1360 0.3394 0.098 Uiso 1 1 calc R . .
C24 C 0.6040(16) -0.2557(18) 0.3549(13) 0.125(10) Uani 1 1 d U . .
H24A H 0.6499 -0.2621 0.3777 0.187 Uiso 1 1 calc R . .
H24B H 0.5936 -0.3047 0.3330 0.187 Uiso 1 1 calc R . .
H24C H 0.5654 -0.2464 0.3788 0.187 Uiso 1 1 calc R . .
C25 C 0.4622(11) -0.1577(12) 0.1607(10) 0.076(5) Uani 1 1 d U . .
H25A H 0.4442 -0.1969 0.1869 0.091 Uiso 1 1 calc R . .
H25B H 0.4215 -0.1439 0.1332 0.091 Uiso 1 1 calc R . .
C26 C 0.5206(13) -0.1991(12) 0.1306(9) 0.077(5) Uani 1 1 d U . .
H26A H 0.5357 -0.1627 0.1015 0.093 Uiso 1 1 calc R . .
H26B H 0.5632 -0.2099 0.1571 0.093 Uiso 1 1 calc R . .
C27 C 0.4931(16) -0.2782(14) 0.1043(12) 0.110(8) Uani 1 1 d U . .
H27A H 0.4499 -0.2675 0.0784 0.132 Uiso 1 1 calc R . .
H27B H 0.4789 -0.3151 0.1335 0.132 Uiso 1 1 calc R . .
C28 C 0.553(2) -0.3199(16) 0.0721(14) 0.141(11) Uani 1 1 d U . .
H28A H 0.5344 -0.3712 0.0566 0.212 Uiso 1 1 calc R . .
H28B H 0.5958 -0.3299 0.0977 0.212 Uiso 1 1 calc R . .
H28C H 0.5653 -0.2845 0.0422 0.212 Uiso 1 1 calc R . .
C29 C 0.5165(11) -0.0170(13) 0.1547(8) 0.071(6) Uani 1 1 d U . .
H29A H 0.5576 -0.0413 0.1377 0.085 Uiso 1 1 calc R . .
H29B H 0.5353 0.0293 0.1775 0.085 Uiso 1 1 calc R . .
C30 C 0.4612(12) 0.0146(13) 0.1082(9) 0.079(6) Uani 1 1 d U . .
H30A H 0.4210 0.0422 0.1243 0.095 Uiso 1 1 calc R . .
H30B H 0.4412 -0.0308 0.0851 0.095 Uiso 1 1 calc R . .
C31 C 0.5032(13) 0.0776(12) 0.0709(9) 0.080(6) Uani 1 1 d U . .
H31A H 0.5250 0.1211 0.0949 0.096 Uiso 1 1 calc R . .
H31B H 0.5425 0.0490 0.0543 0.096 Uiso 1 1 calc R . .
C32 C 0.4507(18) 0.1152(15) 0.0241(11) 0.122(10) Uani 1 1 d U . .
H32A H 0.4773 0.1524 0.0021 0.183 Uiso 1 1 calc R . .
H32B H 0.4125 0.1447 0.0405 0.183 Uiso 1 1 calc R . .
H32C H 0.4293 0.0722 0.0002 0.183 Uiso 1 1 calc R . .
N3 N 0.9826(9) 0.4422(12) 0.3018(8) 0.120(10) Uani 1 1 d D . .
C33 C 1.0210(15) 0.5074(15) 0.3368(11) 0.134(11) Uani 1 1 d DU . .
H33A H 1.0489 0.5416 0.3131 0.161 Uiso 1 1 calc R . .
H33B H 1.0554 0.4820 0.3652 0.161 Uiso 1 1 calc R . .
C34 C 0.963(2) 0.567(3) 0.3685(19) 0.189(14) Uani 1 1 d U . .
H34A H 0.9699 0.6225 0.3558 0.226 Uiso 1 1 calc R . .
H34B H 0.9790 0.5655 0.4086 0.226 Uiso 1 1 calc R . .
C35 C 0.872(3) 0.548(5) 0.362(3) 0.37(3) Uani 1 1 d DU . .
H35A H 0.8563 0.5739 0.3258 0.441 Uiso 1 1 calc R . .
H35B H 0.8696 0.4897 0.3546 0.441 Uiso 1 1 calc R . .
C36 C 0.798(2) 0.563(4) 0.398(2) 0.34(3) Uani 1 1 d DU . .
H36A H 0.7594 0.5254 0.3845 0.510 Uiso 1 1 calc R . .
H36B H 0.7802 0.6186 0.3924 0.510 Uiso 1 1 calc R . .
H36C H 0.8109 0.5537 0.4374 0.510 Uiso 1 1 calc R . .
C37 C 0.9237(15) 0.4762(18) 0.2630(13) 0.225(19) Uani 1 1 d DU . .
H37A H 0.9007 0.4319 0.2403 0.270 Uiso 1 1 calc R . .
H37B H 0.8866 0.5001 0.2847 0.270 Uiso 1 1 calc R . .
C38 C 0.945(3) 0.528(2) 0.232(3) 0.216(18) Uani 1 1 d U . .
H38A H 0.9881 0.5071 0.2159 0.259 Uiso 1 1 calc R . .
H38B H 0.9607 0.5760 0.2546 0.259 Uiso 1 1 calc R . .
C39 C 0.886(3) 0.560(3) 0.179(3) 0.25(2) Uani 1 1 d U . .
H39A H 0.8812 0.5123 0.1546 0.299 Uiso 1 1 calc R . .
H39B H 0.8396 0.5618 0.1967 0.299 Uiso 1 1 calc R . .
C40 C 0.879(3) 0.629(3) 0.140(3) 0.27(2) Uani 1 1 d U . .
H40A H 0.8333 0.6255 0.1167 0.403 Uiso 1 1 calc R . .
H40B H 0.9191 0.6278 0.1166 0.403 Uiso 1 1 calc R . .
H40C H 0.8806 0.6800 0.1608 0.403 Uiso 1 1 calc R . .
C41 C 0.952(2) 0.380(2) 0.3381(13) 0.41(4) Uani 1 1 d DU . .
H41A H 0.9369 0.3324 0.3155 0.487 Uiso 1 1 calc R . .
H41B H 0.9087 0.4027 0.3530 0.487 Uiso 1 1 calc R . .
C42 C 1.007(4) 0.353(5) 0.388(3) 0.44(4) Uani 1 1 d DU . .
H42A H 1.0341 0.4002 0.4038 0.532 Uiso 1 1 calc R . .
H42B H 1.0419 0.3139 0.3748 0.532 Uiso 1 1 calc R . .
C43 C 0.960(4) 0.311(5) 0.434(3) 0.48(4) Uani 1 1 d DU . .
H43A H 0.9786 0.2548 0.4359 0.573 Uiso 1 1 calc R . .
H43B H 0.9113 0.3075 0.4149 0.573 Uiso 1 1 calc R . .
C44 C 0.945(6) 0.331(6) 0.501(3) 0.57(5) Uani 1 1 d DU . .
H44A H 0.9287 0.2819 0.5185 0.857 Uiso 1 1 calc R . .
H44B H 0.9082 0.3730 0.5018 0.857 Uiso 1 1 calc R . .
H44C H 0.9899 0.3499 0.5217 0.857 Uiso 1 1 calc R . .
C45 C 1.0380(18) 0.402(2) 0.2689(16) 0.213(17) Uani 1 1 d DU . .
H45A H 1.0578 0.4452 0.2469 0.256 Uiso 1 1 calc R . .
H45B H 1.0776 0.3850 0.2966 0.256 Uiso 1 1 calc R . .
C46 C 1.028(2) 0.346(3) 0.238(2) 0.203(15) Uani 1 1 d U . .
H46A H 1.0148 0.3705 0.2013 0.243 Uiso 1 1 calc R . .
H46B H 0.9835 0.3199 0.2486 0.243 Uiso 1 1 calc R . .
C47 C 1.070(2) 0.284(3) 0.227(2) 0.196(16) Uani 1 1 d U . .
H47A H 1.0389 0.2372 0.2178 0.235 Uiso 1 1 calc R . .
H47B H 1.1001 0.2711 0.2620 0.235 Uiso 1 1 calc R . .
C48 C 1.116(3) 0.295(4) 0.185(3) 0.28(3) Uani 1 1 d U . .
H48A H 1.1471 0.2474 0.1834 0.413 Uiso 1 1 calc R . .
H48B H 1.1463 0.3428 0.1930 0.413 Uiso 1 1 calc R . .
H48C H 1.0874 0.3019 0.1496 0.413 Uiso 1 1 calc R . .
C49 C 0.738(3) -0.116(4) 0.132(3) 0.25(3) Uani 1 1 d U . .
H49 H 0.6847 -0.1088 0.1260 0.297 Uiso 1 1 calc R . .
C50 C 0.757(4) -0.134(4) 0.074(3) 0.33(3) Uani 1 1 d U . .
H50A H 0.7521 -0.0853 0.0516 0.488 Uiso 1 1 calc R . .
H50B H 0.7246 -0.1761 0.0574 0.488 Uiso 1 1 calc R . .
H50C H 0.8069 -0.1538 0.0756 0.488 Uiso 1 1 calc R . .
C51 C 0.744(3) -0.203(4) 0.163(3) 0.31(3) Uani 1 1 d U . .
H51A H 0.7371 -0.1964 0.2017 0.465 Uiso 1 1 calc R . .
H51B H 0.7919 -0.2261 0.1592 0.465 Uiso 1 1 calc R . .
H51C H 0.7072 -0.2394 0.1452 0.465 Uiso 1 1 calc R . .
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'
Ti Ti 0.2776 0.4457 '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
_geom_angle_publ_flag
O3 W1 O9 105.0(6) . . ?
O3 W1 O12 102.2(5) . . ?
O3 W1 O16 102.5(6) . . ?
O3 W1 O17 104.4(6) . . ?
O3 W1 O19 177.5(5) . . ?
O9 W1 O12 152.8(5) . . ?
O9 W1 O16 89.0(6) . . ?
O9 W1 O17 89.0(6) . . ?
O9 W1 O19 77.2(4) . . ?
O12 W1 O16 84.4(5) . . ?
O12 W1 O17 85.0(5) . . ?
O12 W1 O19 75.6(4) . . ?
O16 W1 O17 152.6(5) . . ?
O16 W1 O19 76.2(4) . . ?
O17 W1 O19 76.7(4) . . ?
O2 W2 O8 108.3(10) . . ?
O2 W2 O13 99.6(9) . . ?
O2 W2 O15 103.6(6) . . ?
O2 W2 O16 101.6(7) . . ?
O2 W2 O19 175.1(9) . . ?
O8 W2 O13 152.1(6) . . ?
O8 W2 O15 89.1(6) . . ?
O8 W2 O16 89.5(6) . . ?
O8 W2 O19 76.3(6) . . ?
O13 W2 O15 85.0(5) . . ?
O13 W2 O16 84.0(5) . . ?
O13 W2 O19 75.7(4) . . ?
O15 W2 O16 153.8(5) . . ?
O15 W2 O19 77.5(4) . . ?
O16 W2 O19 76.8(4) . . ?
O5 W3 O7 103.7(7) . . ?
O5 W3 O14 103.1(6) . . ?
O5 W3 O15 104.2(6) . . ?
O5 W3 O18 102.6(6) . . ?
O5 W3 O19 179.0(6) . . ?
O7 W3 O14 153.2(5) . . ?
O7 W3 O15 88.9(7) . . ?
O7 W3 O18 87.8(7) . . ?
O7 W3 O19 77.1(4) . . ?
O14 W3 O15 85.4(5) . . ?
O14 W3 O18 85.6(5) . . ?
O14 W3 O19 76.2(4) . . ?
O15 W3 O18 153.1(5) . . ?
O15 W3 O19 76.4(4) . . ?
O18 W3 O19 76.8(4) . . ?
O4 W4 O10 104.9(9) . . ?
O4 W4 O11 102.4(8) . . ?
O4 W4 O17 104.6(6) . . ?
O4 W4 O18 101.5(6) . . ?
O4 W4 O19 178.2(7) . . ?
O10 W4 O11 152.7(6) . . ?
O10 W4 O17 88.2(6) . . ?
O10 W4 O18 88.7(6) . . ?
O10 W4 O19 76.5(5) . . ?
O11 W4 O17 85.2(5) . . ?
O11 W4 O18 85.7(5) . . ?
O11 W4 O19 76.2(4) . . ?
O17 W4 O18 153.6(5) . . ?
O17 W4 O19 76.5(4) . . ?
O18 W4 O19 77.3(4) . . ?
O6 W5 O11 104.5(8) . . ?
O6 W5 O12 102.9(6) . . ?
O6 W5 O13 102.5(8) . . ?
O6 W5 O14 103.8(6) . . ?
O6 W5 O19 178.7(6) . . ?
O11 W5 O12 86.6(5) . . ?
O11 W5 O13 153.0(5) . . ?
O11 W5 O14 86.5(5) . . ?
O11 W5 O19 76.2(4) . . ?
O12 W5 O13 86.7(5) . . ?
O12 W5 O14 153.4(4) . . ?
O12 W5 O19 76.0(4) . . ?
O13 W5 O14 87.9(5) . . ?
O13 W5 O19 76.8(4) . . ?
O14 W5 O19 77.3(4) . . ?
O1 Ti1 O7 102.0(7) . . ?
O1 Ti1 O8 97.9(11) . . ?
O1 Ti1 O9 101.0(7) . . ?
O1 Ti1 O10 105.0(11) . . ?
O1 Ti1 O19 174.6(10) . . ?
O7 Ti1 O8 86.3(7) . . ?
O7 Ti1 O9 156.3(5) . . ?
O7 Ti1 O10 90.3(7) . . ?
O7 Ti1 O19 79.0(4) . . ?
O8 Ti1 O9 84.9(6) . . ?
O8 Ti1 O10 157.1(5) . . ?
O8 Ti1 O19 76.9(4) . . ?
O9 Ti1 O10 89.3(6) . . ?
O9 Ti1 O19 77.6(4) . . ?
O10 Ti1 O19 80.2(5) . . ?
Ti1 O1 C49 160(3) . . ?
W3 O7 Ti1 114.9(6) . . ?
W2 O8 Ti1 115.4(7) . . ?
W1 O9 Ti1 114.8(6) . . ?
W4 O10 Ti1 116.0(6) . . ?
W4 O11 W5 117.3(6) . . ?
W1 O12 W5 117.4(5) . . ?
W2 O13 W5 116.5(5) . . ?
W3 O14 W5 116.7(5) . . ?
W2 O15 W3 116.0(5) . . ?
W1 O16 W2 116.2(6) . . ?
W1 O17 W4 116.4(5) . . ?
W3 O18 W4 116.6(6) . . ?
W1 O19 W2 90.6(4) . . ?
W1 O19 W3 179.0(5) . . ?
W1 O19 W4 90.2(3) . . ?
W1 O19 W5 91.0(3) . . ?
W1 O19 Ti1 90.2(4) . . ?
W2 O19 W3 89.9(3) . . ?
W2 O19 W4 178.4(5) . . ?
W2 O19 W5 91.0(3) . . ?
W2 O19 Ti1 91.4(4) . . ?
W3 O19 W4 89.2(3) . . ?
W3 O19 W5 89.8(3) . . ?
W3 O19 Ti1 88.9(3) . . ?
W4 O19 W5 90.4(3) . . ?
W4 O19 Ti1 87.2(3) . . ?
W5 O19 Ti1 177.3(5) . . ?
C1 N1 C5 112.3(19) . . ?
C1 N1 C9 107.2(19) . . ?
C1 N1 C13 114(2) . . ?
C5 N1 C9 110.6(18) . . ?
C5 N1 C13 103.4(17) . . ?
C9 N1 C13 109.5(17) . . ?
N1 C1 C2 114(2) . . ?
C1 C2 C4 101(3) . . ?
C2 C4 C3 102(4) . . ?
N1 C5 C6 115(2) . . ?
C5 C6 C7 108(2) . . ?
C6 C7 C8 107(3) . . ?
N1 C9 C10 116.2(18) . . ?
C9 C10 C11 109(2) . . ?
C10 C11 C12 113(2) . . ?
N1 C13 C14 113.6(17) . . ?
C13 C14 C15 107.2(19) . . ?
C14 C15 C16 108(2) . . ?
C17 N2 C21 111.8(15) . . ?
C17 N2 C25 107.0(14) . . ?
C17 N2 C29 112.8(16) . . ?
C21 N2 C25 110.6(15) . . ?
C21 N2 C29 103.6(12) . . ?
C25 N2 C29 111.1(15) . . ?
N2 C17 C18 115.3(16) . . ?
C17 C18 C19 112(2) . . ?
C18 C19 C20 117(3) . . ?
N2 C21 C22 115.4(14) . . ?
C21 C22 C23 110.5(15) . . ?
C22 C23 C24 114.2(19) . . ?
N2 C25 C26 115.6(15) . . ?
C25 C26 C27 111(2) . . ?
C26 C27 C28 111(2) . . ?
N2 C29 C30 114.3(15) . . ?
C29 C30 C31 107.5(17) . . ?
C30 C31 C32 111.1(19) . . ?
C33 N3 C37 111.5(11) . . ?
C33 N3 C41 110.1(11) . . ?
C33 N3 C45 107.6(11) . . ?
C37 N3 C41 109.4(11) . . ?
C37 N3 C45 109.5(11) . . ?
C41 N3 C45 108.7(11) . . ?
N3 C33 C34 112(2) . . ?
C33 C34 C35 122(4) . . ?
C34 C35 C36 140(5) . . ?
N3 C37 C38 113(3) . . ?
C37 C38 C39 117(5) . . ?
C38 C39 C40 137(5) . . ?
N3 C41 C42 113(3) . . ?
C41 C42 C43 107(5) . . ?
C42 C43 C44 136(6) . . ?
N3 C45 C46 127(4) . . ?
C45 C46 C47 131(5) . . ?
C46 C47 C48 117(6) . . ?
O1 C49 C50 126(6) . . ?
O1 C49 C51 118(6) . . ?
C50 C49 C51 104(4) . . ?
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
W1 O3 1.721(11) . ?
W1 O9 1.874(12) . ?
W1 O12 1.964(10) . ?
W1 O16 1.939(11) . ?
W1 O17 1.939(12) . ?
W1 O19 2.322(9) . ?
W2 O2 1.722(15) . ?
W2 O8 1.897(15) . ?
W2 O13 1.994(14) . ?
W2 O15 1.948(12) . ?
W2 O16 1.933(12) . ?
W2 O19 2.302(10) . ?
W3 O5 1.716(12) . ?
W3 O7 1.882(14) . ?
W3 O14 1.962(11) . ?
W3 O15 1.935(13) . ?
W3 O18 1.929(12) . ?
W3 O19 2.357(9) . ?
W4 O4 1.711(14) . ?
W4 O10 1.893(15) . ?
W4 O11 1.942(13) . ?
W4 O17 1.940(12) . ?
W4 O18 1.938(12) . ?
W4 O19 2.331(10) . ?
W5 O6 1.702(14) . ?
W5 O11 1.935(12) . ?
W5 O12 1.923(11) . ?
W5 O13 1.893(11) . ?
W5 O14 1.928(11) . ?
W5 O19 2.334(9) . ?
Ti1 O1 1.768(15) . ?
Ti1 O7 1.938(14) . ?
Ti1 O8 1.95(2) . ?
Ti1 O9 1.962(13) . ?
Ti1 O10 1.827(18) . ?
Ti1 O19 2.240(10) . ?
O1 C49 1.33(5) . ?
N1 C1 1.50(3) . ?
N1 C5 1.56(3) . ?
N1 C9 1.55(3) . ?
N1 C13 1.52(3) . ?
C1 C2 1.51(4) . ?
C2 C4 1.66(5) . ?
C3 C4 1.45(6) . ?
C5 C6 1.56(4) . ?
C6 C7 1.54(3) . ?
C7 C8 1.50(5) . ?
C9 C10 1.50(3) . ?
C10 C11 1.55(3) . ?
C11 C12 1.46(4) . ?
C13 C14 1.54(3) . ?
C14 C15 1.59(3) . ?
C15 C16 1.64(3) . ?
N2 C17 1.49(3) . ?
N2 C21 1.52(2) . ?
N2 C25 1.52(2) . ?
N2 C29 1.52(2) . ?
C17 C18 1.54(3) . ?
C18 C19 1.60(4) . ?
C19 C20 1.48(5) . ?
C21 C22 1.54(3) . ?
C22 C23 1.54(3) . ?
C23 C24 1.47(3) . ?
C25 C26 1.50(3) . ?
C26 C27 1.50(3) . ?
C27 C28 1.55(4) . ?
C29 C30 1.52(3) . ?
C30 C31 1.60(3) . ?
C31 C32 1.53(3) . ?
N3 C33 1.48(2) . ?
N3 C37 1.46(2) . ?
N3 C41 1.47(2) . ?
N3 C45 1.49(2) . ?
C33 C34 1.66(4) . ?
C34 C35 1.69(6) . ?
C35 C36 1.69(3) . ?
C37 C38 1.21(4) . ?
C38 C39 1.66(7) . ?
C39 C40 1.47(7) . ?
C41 C42 1.54(7) . ?
C42 C43 1.61(4) . ?
C43 C44 1.68(4) . ?
C45 C46 1.18(5) . ?
C46 C47 1.29(5) . ?
C47 C48 1.39(6) . ?
C49 C50 1.49(7) . ?
C49 C51 1.58(8) . ?
