
data_global

data_new1
#TrackingRef '10397_web_deposit_cif_file_0_TanmoyKumarSaha_1332940051.new.cif'




_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C26 H38 Cl2 N O4 Ta'

_chemical_formula_weight         680.42



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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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                   9.8857(8)

_cell_length_b                   10.6918(8)

_cell_length_c                   13.7932(10)

_cell_angle_alpha                82.367(4)

_cell_angle_beta                 89.663(4)

_cell_angle_gamma                85.383(4)

_cell_volume                     1440.26(19)

_cell_formula_units_Z            2

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    6569

_cell_measurement_theta_min      2.54

_cell_measurement_theta_max      28.57



_exptl_crystal_description       Block

_exptl_crystal_colour            clear

_exptl_crystal_size_max          0.38

_exptl_crystal_size_mid          0.36

_exptl_crystal_size_min          0.35

_exptl_crystal_density_meas      0

_exptl_crystal_density_diffrn    1.569

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             680

_exptl_absorpt_coefficient_mu    4.031

_exptl_absorpt_correction_type   none

_exptl_absorpt_correction_T_min  0.3096

_exptl_absorpt_correction_T_max  0.3328

_exptl_absorpt_process_details   ?



_exptl_special_details           
;

?

;



_diffrn_ambient_temperature      173(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            18573

_diffrn_reflns_av_R_equivalents  0.0422

_diffrn_reflns_av_sigmaI/netI    0.0474

_diffrn_reflns_limit_h_min       -13

_diffrn_reflns_limit_h_max       13

_diffrn_reflns_limit_k_min       -14

_diffrn_reflns_limit_k_max       13

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       16

_diffrn_reflns_theta_min         1.93

_diffrn_reflns_theta_max         28.78

_reflns_number_total             6956

_reflns_number_gt                6307

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'



_refine_special_details          
;

Refinement of F² against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F², conventional R-factors R are based

on F, with F set to zero for negative F². The threshold expression of

F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0832P)²+15.7981P] where P=(Fo²+2Fc²)/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         6956

_refine_ls_number_parameters     348

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.0656

_refine_ls_R_factor_gt           0.0600

_refine_ls_wR_factor_ref         0.1609

_refine_ls_wR_factor_gt          0.1562

_refine_ls_goodness_of_fit_ref   1.048

_refine_ls_restrained_S_all      1.048

_refine_ls_shift/su_max          0.002

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group




















































































C1 C 0.7468(7) 0.4956(7) 0.4895(5) 0.0234(13) Uani 1 1 d . . .
H1 H 0.7577 0.4057 0.4992 0.028 Uiso 1 1 calc R . .
C2 C 0.7375(7) 0.5545(6) 0.3890(5) 0.0218(12) Uani 1 1 d . . .
C3 C 0.7161(7) 0.6866(7) 0.3640(5) 0.0249(13) Uani 1 1 d . . .
C4 C 0.7037(8) 0.7421(7) 0.2646(6) 0.0293(15) Uani 1 1 d . . .
C5 C 0.7150(8) 0.6576(8) 0.1960(5) 0.0295(15) Uani 1 1 d . . .
H5 H 0.7057 0.6920 0.1290 0.035 Uiso 1 1 calc R . .
C6 C 0.7391(7) 0.5252(7) 0.2178(5) 0.0257(14) Uani 1 1 d . A .
C7 C 0.7481(7) 0.4760(7) 0.3162(5) 0.0243(13) Uani 1 1 d . . .
H7 H 0.7617 0.3870 0.3341 0.029 Uiso 1 1 calc R . .
C8 C 0.6739(10) 0.8843(8) 0.2368(6) 0.0372(18) Uani 1 1 d . . .
C9 C 0.5409(11) 0.9311(10) 0.2837(7) 0.049(2) Uani 1 1 d . . .
H9A H 0.4654 0.8894 0.2598 0.074 Uiso 1 1 calc R . .
H9B H 0.5249 1.0230 0.2661 0.074 Uiso 1 1 calc R . .
H9C H 0.5478 0.9107 0.3550 0.074 Uiso 1 1 calc R . .
C10 C 0.7933(12) 0.9512(9) 0.2710(8) 0.049(2) Uani 1 1 d . . .
H10A H 0.8018 0.9333 0.3424 0.074 Uiso 1 1 calc R . .
H10B H 0.7771 1.0427 0.2517 0.074 Uiso 1 1 calc R . .
H10C H 0.8773 0.9202 0.2408 0.074 Uiso 1 1 calc R . .
C11 C 0.6598(13) 0.9203(10) 0.1263(7) 0.053(3) Uani 1 1 d . . .
H11A H 0.7434 0.8918 0.0944 0.080 Uiso 1 1 calc R . .
H11B H 0.6435 1.0124 0.1110 0.080 Uiso 1 1 calc R . .
H11C H 0.5834 0.8797 0.1025 0.080 Uiso 1 1 calc R . .
C12 C 0.7519(9) 0.4398(8) 0.1372(6) 0.0347(17) Uani 1 1 d . . .
C13 C 0.8699(16) 0.4825(15) 0.0701(11) 0.043(4) Uani 0.625(15) 1 d P A 1
H13A H 0.9551 0.4688 0.1073 0.064 Uiso 0.625(15) 1 calc PR A 1
H13B H 0.8529 0.5726 0.0453 0.064 Uiso 0.625(15) 1 calc PR A 1
H13C H 0.8764 0.4331 0.0150 0.064 Uiso 0.625(15) 1 calc PR A 1
C14 C 0.769(2) 0.3057(14) 0.1745(11) 0.050(4) Uani 0.625(15) 1 d P A 1
H14A H 0.7777 0.2561 0.1196 0.075 Uiso 0.625(15) 1 calc PR A 1
H14B H 0.6905 0.2818 0.2141 0.075 Uiso 0.625(15) 1 calc PR A 1
H14C H 0.8516 0.2887 0.2150 0.075 Uiso 0.625(15) 1 calc PR A 1
C15 C 0.6231(18) 0.4703(18) 0.0701(12) 0.051(4) Uani 0.625(15) 1 d P A 1
H15A H 0.6217 0.4077 0.0244 0.076 Uiso 0.625(15) 1 calc PR A 1
H15B H 0.6257 0.5551 0.0334 0.076 Uiso 0.625(15) 1 calc PR A 1
H15C H 0.5414 0.4674 0.1107 0.076 Uiso 0.625(15) 1 calc PR A 1
C15A C 0.887(3) 0.348(3) 0.160(2) 0.054(8) Uani 0.375(15) 1 d P A 2
H15D H 0.8857 0.3071 0.2279 0.081 Uiso 0.375(15) 1 calc PR A 2
H15E H 0.9667 0.3977 0.1505 0.081 Uiso 0.375(15) 1 calc PR A 2
H15F H 0.8927 0.2834 0.1158 0.081 Uiso 0.375(15) 1 calc PR A 2
C14A C 0.757(3) 0.503(2) 0.0378(16) 0.041(6) Uani 0.375(15) 1 d P A 2
H14D H 0.7783 0.4402 -0.0068 0.061 Uiso 0.375(15) 1 calc PR A 2
H14E H 0.8281 0.5628 0.0330 0.061 Uiso 0.375(15) 1 calc PR A 2
H14F H 0.6695 0.5492 0.0200 0.061 Uiso 0.375(15) 1 calc PR A 2
C13A C 0.634(3) 0.347(3) 0.148(2) 0.051(7) Uani 0.375(15) 1 d P A 2
H13D H 0.6471 0.2868 0.1003 0.077 Uiso 0.375(15) 1 calc PR A 2
H13E H 0.5462 0.3964 0.1354 0.077 Uiso 0.375(15) 1 calc PR A 2
H13F H 0.6349 0.3010 0.2141 0.077 Uiso 0.375(15) 1 calc PR A 2
C16 C 0.7555(7) 0.4645(6) 0.6578(5) 0.0216(12) Uani 1 1 d . . .
C17 C 0.6419(8) 0.4296(9) 0.7101(6) 0.0365(18) Uani 1 1 d . . .
H17 H 0.5540 0.4619 0.6869 0.044 Uiso 1 1 calc R . .
C18 C 0.6566(8) 0.3475(8) 0.7963(6) 0.0351(17) Uani 1 1 d . . .
H18 H 0.5783 0.3239 0.8322 0.042 Uiso 1 1 calc R . .
C19 C 0.7826(8) 0.2996(7) 0.8307(5) 0.0304(15) Uani 1 1 d . . .
C20 C 0.8972(8) 0.3354(8) 0.7795(6) 0.0331(16) Uani 1 1 d . . .
H20 H 0.9849 0.3032 0.8032 0.040 Uiso 1 1 calc R . .
C21 C 0.8829(8) 0.4191(8) 0.6930(6) 0.0321(16) Uani 1 1 d . . .
H21 H 0.9613 0.4451 0.6581 0.039 Uiso 1 1 calc R . .
C22 C 0.9109(12) 0.1483(11) 0.9430(8) 0.057(3) Uani 1 1 d . . .
H22A H 0.9441 0.1024 0.8895 0.086 Uiso 1 1 calc R . .
H22B H 0.8984 0.0879 1.0016 0.086 Uiso 1 1 calc R . .
H22C H 0.9771 0.2072 0.9568 0.086 Uiso 1 1 calc R . .
C23 C 0.748(2) 0.6912(12) 0.8085(8) 0.086(5) Uani 1 1 d . . .
H23A H 0.8300 0.6324 0.8231 0.103 Uiso 1 1 calc R . .
H23B H 0.6682 0.6451 0.8310 0.103 Uiso 1 1 calc R . .
C24 C 0.755(2) 0.7983(16) 0.8635(9) 0.101(6) Uani 1 1 d . . .
H24A H 0.8387 0.8397 0.8464 0.152 Uiso 1 1 calc R . .
H24B H 0.7556 0.7679 0.9338 0.152 Uiso 1 1 calc R . .
H24C H 0.6764 0.8590 0.8474 0.152 Uiso 1 1 calc R . .
C25 C 0.7856(14) 1.0528(10) 0.5523(9) 0.060(3) Uani 1 1 d . . .
H25A H 0.7135 1.1211 0.5327 0.072 Uiso 1 1 calc R . .
H25B H 0.8546 1.0556 0.4999 0.072 Uiso 1 1 calc R . .
C26 C 0.8474(16) 1.0759(15) 0.6409(11) 0.084(5) Uani 1 1 d . . .
H26A H 0.7808 1.0692 0.6939 0.126 Uiso 1 1 calc R . .
H26B H 0.8793 1.1612 0.6320 0.126 Uiso 1 1 calc R . .
H26C H 0.9245 1.0134 0.6574 0.126 Uiso 1 1 calc R . .
Cl1 Cl 0.4851(2) 0.7472(2) 0.5859(2) 0.0507(6) Uani 1 1 d . . .
Cl2 Cl 0.9659(3) 0.7318(2) 0.5592(2) 0.0539(7) Uani 1 1 d . . .
N1 N 0.7422(6) 0.5496(6) 0.5673(4) 0.0240(12) Uani 1 1 d . . .
O1 O 0.7091(6) 0.7604(5) 0.4351(4) 0.0301(11) Uani 1 1 d . . .
O2 O 0.7384(7) 0.7252(6) 0.7095(4) 0.0378(13) Uani 1 1 d . . .
O3 O 0.7284(6) 0.9344(5) 0.5611(4) 0.0353(12) Uani 1 1 d . . .
O4 O 0.7858(7) 0.2165(6) 0.9157(4) 0.0414(14) Uani 1 1 d . . .
Ta1 Ta 0.72437(3) 0.76211(3) 0.575010(19) 0.02514(11) Uani 1 1 d . . .






_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell esds are taken

into account individually in the estimation of esds in distances, angles

and torsion angles; correlations between esds in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag






















































































C1 N1 1.284(9) . ?
C1 C2 1.446(9) . ?
C1 H1 0.9500 . ?
C2 C7 1.390(10) . ?
C2 C3 1.407(10) . ?
C3 O1 1.337(9) . ?
C3 C4 1.421(10) . ?
C4 C5 1.391(11) . ?
C4 C8 1.523(11) . ?
C5 C6 1.409(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.390(10) . ?
C6 C12 1.528(11) . ?
C7 H7 0.9500 . ?
C8 C11 1.526(12) . ?
C8 C10 1.536(14) . ?
C8 C9 1.538(13) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14A 1.45(2) . ?
C12 C14 1.455(17) . ?
C12 C13 1.545(17) . ?
C12 C15 1.565(19) . ?
C12 C13A 1.59(3) . ?
C12 C15A 1.60(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
C16 C21 1.380(10) . ?
C16 C17 1.381(10) . ?
C16 N1 1.443(8) . ?
C17 C18 1.381(11) . ?
C17 H17 0.9500 . ?
C18 C19 1.370(11) . ?
C18 H18 0.9500 . ?
C19 O4 1.372(9) . ?
C19 C20 1.385(11) . ?
C20 C21 1.394(11) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O4 1.410(12) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 O2 1.367(12) . ?
C23 C24 1.462(19) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 O3 1.417(10) . ?
C25 C26 1.428(17) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
Cl1 Ta1 2.386(2) . ?
Cl2 Ta1 2.396(3) . ?
N1 Ta1 2.281(6) . ?
O1 Ta1 1.939(5) . ?
O2 Ta1 1.849(6) . ?
O3 Ta1 1.830(5) . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag



































































































































































N1 C1 C2 128.0(7) . . ?
N1 C1 H1 116.0 . . ?
C2 C1 H1 116.0 . . ?
C7 C2 C3 120.2(6) . . ?
C7 C2 C1 117.7(6) . . ?
C3 C2 C1 122.1(6) . . ?
O1 C3 C2 119.1(6) . . ?
O1 C3 C4 119.8(7) . . ?
C2 C3 C4 121.0(7) . . ?
C5 C4 C3 115.5(7) . . ?
C5 C4 C8 122.9(7) . . ?
C3 C4 C8 121.5(7) . . ?
C4 C5 C6 125.2(7) . . ?
C4 C5 H5 117.4 . . ?
C6 C5 H5 117.4 . . ?
C7 C6 C5 116.7(7) . . ?
C7 C6 C12 121.7(7) . . ?
C5 C6 C12 121.6(7) . . ?
C6 C7 C2 121.3(7) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C4 C8 C11 111.7(7) . . ?
C4 C8 C10 108.4(7) . . ?
C11 C8 C10 107.7(8) . . ?
C4 C8 C9 110.9(7) . . ?
C11 C8 C9 107.7(8) . . ?
C10 C8 C9 110.4(8) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14A C12 C14 130.1(13) . . ?
C14A C12 C6 116.3(11) . . ?
C14 C12 C6 113.3(8) . . ?
C14A C12 C13 46.8(12) . . ?
C14 C12 C13 112.2(11) . . ?
C6 C12 C13 107.7(8) . . ?
C14A C12 C15 57.5(13) . . ?
C14 C12 C15 111.1(12) . . ?
C6 C12 C15 108.0(9) . . ?
C13 C12 C15 104.1(10) . . ?
C14A C12 C13A 110.3(15) . . ?
C14 C12 C13A 55.2(14) . . ?
C6 C12 C13A 109.5(12) . . ?
C13 C12 C13A 142.6(13) . . ?
C15 C12 C13A 60.2(13) . . ?
C14A C12 C15A 109.1(17) . . ?
C14 C12 C15A 49.7(15) . . ?
C6 C12 C15A 106.7(11) . . ?
C13 C12 C15A 68.3(14) . . ?
C15 C12 C15A 145.1(13) . . ?
C13A C12 C15A 104.2(19) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
C12 C15A H15D 109.5 . . ?
C12 C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
C12 C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C12 C14A H14D 109.5 . . ?
C12 C14A H14E 109.5 . . ?
H14D C14A H14E 109.5 . . ?
C12 C14A H14F 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C12 C13A H13D 109.5 . . ?
C12 C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
C12 C13A H13F 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C21 C16 C17 119.7(7) . . ?
C21 C16 N1 119.7(6) . . ?
C17 C16 N1 120.6(6) . . ?
C16 C17 C18 119.7(7) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 121.0(7) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 O4 116.4(7) . . ?
C18 C19 C20 119.7(7) . . ?
O4 C19 C20 123.9(7) . . ?
C19 C20 C21 119.5(7) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C16 C21 C20 120.3(7) . . ?
C16 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 C24 113.8(11) . . ?
O2 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
O2 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 C26 113.0(10) . . ?
O3 C25 H25A 109.0 . . ?
C26 C25 H25A 109.0 . . ?
O3 C25 H25B 109.0 . . ?
C26 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C1 N1 C16 115.0(6) . . ?
C1 N1 Ta1 126.7(5) . . ?
C16 N1 Ta1 118.3(4) . . ?
C3 O1 Ta1 144.5(5) . . ?
C23 O2 Ta1 176.9(7) . . ?
C25 O3 Ta1 157.8(7) . . ?
C19 O4 C22 117.3(7) . . ?
O3 Ta1 O2 100.1(3) . . ?
O3 Ta1 O1 92.6(2) . . ?
O2 Ta1 O1 167.2(2) . . ?
O3 Ta1 N1 169.7(2) . . ?
O2 Ta1 N1 88.1(2) . . ?
O1 Ta1 N1 79.2(2) . . ?
O3 Ta1 Cl1 99.6(2) . . ?
O2 Ta1 Cl1 89.8(2) . . ?
O1 Ta1 Cl1 88.22(19) . . ?
N1 Ta1 Cl1 86.63(16) . . ?
O3 Ta1 Cl2 92.0(2) . . ?
O2 Ta1 Cl2 90.9(2) . . ?
O1 Ta1 Cl2 88.50(19) . . ?
N1 Ta1 Cl2 81.52(16) . . ?
Cl1 Ta1 Cl2 168.10(9) . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag



















































































N1 C1 C2 C7 178.7(7) . . . . ?
N1 C1 C2 C3 -2.4(11) . . . . ?
C7 C2 C3 O1 -178.6(6) . . . . ?
C1 C2 C3 O1 2.5(10) . . . . ?
C7 C2 C3 C4 0.6(11) . . . . ?
C1 C2 C3 C4 -178.3(7) . . . . ?
O1 C3 C4 C5 178.8(7) . . . . ?
C2 C3 C4 C5 -0.4(11) . . . . ?
O1 C3 C4 C8 -3.8(11) . . . . ?
C2 C3 C4 C8 177.1(7) . . . . ?
C3 C4 C5 C6 -1.0(12) . . . . ?
C8 C4 C5 C6 -178.4(8) . . . . ?
C4 C5 C6 C7 2.0(11) . . . . ?
C4 C5 C6 C12 -179.2(7) . . . . ?
C5 C6 C7 C2 -1.8(10) . . . . ?
C12 C6 C7 C2 179.5(7) . . . . ?
C3 C2 C7 C6 0.5(11) . . . . ?
C1 C2 C7 C6 179.5(6) . . . . ?
C5 C4 C8 C11 -0.5(12) . . . . ?
C3 C4 C8 C11 -177.7(8) . . . . ?
C5 C4 C8 C10 -119.0(9) . . . . ?
C3 C4 C8 C10 63.7(10) . . . . ?
C5 C4 C8 C9 119.6(9) . . . . ?
C3 C4 C8 C9 -57.6(11) . . . . ?
C7 C6 C12 C14A -172.7(14) . . . . ?
C5 C6 C12 C14A 8.6(16) . . . . ?
C7 C6 C12 C14 1.9(14) . . . . ?
C5 C6 C12 C14 -176.9(11) . . . . ?
C7 C6 C12 C13 -122.8(9) . . . . ?
C5 C6 C12 C13 58.5(11) . . . . ?
C7 C6 C12 C15 125.4(10) . . . . ?
C5 C6 C12 C15 -53.4(11) . . . . ?
C7 C6 C12 C13A 61.4(15) . . . . ?
C5 C6 C12 C13A -117.3(14) . . . . ?
C7 C6 C12 C15A -50.8(16) . . . . ?
C5 C6 C12 C15A 130.5(15) . . . . ?
C21 C16 C17 C18 -1.3(13) . . . . ?
N1 C16 C17 C18 179.7(8) . . . . ?
C16 C17 C18 C19 -0.2(14) . . . . ?
C17 C18 C19 O4 -178.5(8) . . . . ?
C17 C18 C19 C20 1.2(14) . . . . ?
C18 C19 C20 C21 -0.6(13) . . . . ?
O4 C19 C20 C21 179.1(8) . . . . ?
C17 C16 C21 C20 1.9(12) . . . . ?
N1 C16 C21 C20 -179.1(7) . . . . ?
C19 C20 C21 C16 -1.0(13) . . . . ?
C2 C1 N1 C16 -179.5(6) . . . . ?
C2 C1 N1 Ta1 -2.3(11) . . . . ?
C21 C16 N1 C1 83.8(8) . . . . ?
C17 C16 N1 C1 -97.2(9) . . . . ?
C21 C16 N1 Ta1 -93.7(7) . . . . ?
C17 C16 N1 Ta1 85.3(8) . . . . ?
C2 C3 O1 Ta1 3.7(13) . . . . ?
C4 C3 O1 Ta1 -175.5(6) . . . . ?
C24 C23 O2 Ta1 -176(17) . . . . ?
C26 C25 O3 Ta1 -70(2) . . . . ?
C18 C19 O4 C22 168.6(9) . . . . ?
C20 C19 O4 C22 -11.1(13) . . . . ?
C25 O3 Ta1 O2 84.0(18) . . . . ?
C25 O3 Ta1 O1 -95.9(18) . . . . ?
C25 O3 Ta1 N1 -58(2) . . . . ?
C25 O3 Ta1 Cl1 175.5(17) . . . . ?
C25 O3 Ta1 Cl2 -7.3(18) . . . . ?
C23 O2 Ta1 O3 177(100) . . . . ?
C23 O2 Ta1 O1 -4(19) . . . . ?
C23 O2 Ta1 N1 -10(18) . . . . ?
C23 O2 Ta1 Cl1 77(18) . . . . ?
C23 O2 Ta1 Cl2 -91(18) . . . . ?
C3 O1 Ta1 O3 167.5(9) . . . . ?
C3 O1 Ta1 O2 -11.8(17) . . . . ?
C3 O1 Ta1 N1 -6.1(9) . . . . ?
C3 O1 Ta1 Cl1 -93.0(9) . . . . ?
C3 O1 Ta1 Cl2 75.5(9) . . . . ?
C1 N1 Ta1 O3 -33.7(16) . . . . ?
C16 N1 Ta1 O3 143.5(12) . . . . ?
C1 N1 Ta1 O2 -176.6(6) . . . . ?
C16 N1 Ta1 O2 0.6(5) . . . . ?
C1 N1 Ta1 O1 4.7(6) . . . . ?
C16 N1 Ta1 O1 -178.2(5) . . . . ?
C1 N1 Ta1 Cl1 93.5(6) . . . . ?
C16 N1 Ta1 Cl1 -89.3(5) . . . . ?
C1 N1 Ta1 Cl2 -85.4(6) . . . . ?
C16 N1 Ta1 Cl2 91.8(5) . . . . ?



_diffrn_measured_fraction_theta_max 0.926

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.975

_refine_diff_density_max         9.940

_refine_diff_density_min         -1.929

_refine_diff_density_rms         0.240

data_global


# Attachment '10398_web_deposit_cif_file_1_TanmoyKumarSaha_1332940051.new.cif'


data_new2
#TrackingRef '10398_web_deposit_cif_file_1_TanmoyKumarSaha_1332940051.new.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H41 Cl3 N Nb O3'
_chemical_formula_weight         578.83

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'
Cl Cl 0.1484 0.1585 '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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   11.0133(8)
_cell_length_b                   11.7231(8)
_cell_length_c                   11.7778(8)
_cell_angle_alpha                90.509(3)
_cell_angle_beta                 111.696(2)
_cell_angle_gamma                93.203(3)
_cell_volume                     1409.98(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8210
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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            16597
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         28.10
_reflns_number_total             6186
_reflns_number_gt                4777
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0403P)²+1.4975P] where P=(Fo²+2Fc²)/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         6186
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5250(3) 0.2317(2) 0.5699(2) 0.0230(6) Uani 1 1 d . . .
C2 C 0.5997(3) 0.2206(2) 0.6950(2) 0.0254(6) Uani 1 1 d . . .
H2 H 0.6783 0.1818 0.7187 0.031 Uiso 1 1 calc R . .
C3 C 0.5607(3) 0.2652(3) 0.7832(2) 0.0282(6) Uani 1 1 d . . .
C4 C 0.4496(3) 0.3282(3) 0.7431(2) 0.0296(6) Uani 1 1 d . . .
H4 H 0.4237 0.3616 0.8038 0.036 Uiso 1 1 calc R . .
C5 C 0.3739(3) 0.3461(2) 0.6222(2) 0.0247(6) Uani 1 1 d . . .
C6 C 0.4091(3) 0.2897(2) 0.5330(2) 0.0223(6) Uani 1 1 d . . .
C7 C 0.5767(2) 0.1934(2) 0.4807(2) 0.0220(6) Uani 1 1 d . . .
H7 H 0.5446 0.2247 0.4017 0.026 Uiso 1 1 calc R . .
C8 C 0.7437(3) 0.0914(2) 0.4289(2) 0.0242(6) Uani 1 1 d . . .
C9 C 0.8847(3) 0.1233(3) 0.5121(3) 0.0360(7) Uani 1 1 d . . .
H9A H 0.8941 0.2047 0.5355 0.054 Uiso 1 1 calc R . .
H9B H 0.9431 0.1080 0.4688 0.054 Uiso 1 1 calc R . .
H9C H 0.9078 0.0777 0.5856 0.054 Uiso 1 1 calc R . .
C10 C 0.7233(3) -0.0363(3) 0.4005(3) 0.0346(7) Uani 1 1 d . . .
H10A H 0.7471 -0.0774 0.4771 0.052 Uiso 1 1 calc R . .
H10B H 0.7785 -0.0582 0.3561 0.052 Uiso 1 1 calc R . .
H10C H 0.6312 -0.0557 0.3501 0.052 Uiso 1 1 calc R . .
C11 C 0.7044(3) 0.1594(3) 0.3136(3) 0.0385(8) Uani 1 1 d . . .
H11A H 0.6123 0.1397 0.2633 0.058 Uiso 1 1 calc R . .
H11B H 0.7593 0.1414 0.2674 0.058 Uiso 1 1 calc R . .
H11C H 0.7163 0.2413 0.3354 0.058 Uiso 1 1 calc R . .
C12 C 0.6320(3) 0.2449(3) 0.9203(3) 0.0398(8) Uani 1 1 d . . .
C13 C 0.7658(4) 0.2000(3) 0.9470(3) 0.0483(9) Uani 1 1 d . . .
H13A H 0.7563 0.1275 0.9014 0.072 Uiso 1 1 calc R . .
H13B H 0.8077 0.1876 1.0348 0.072 Uiso 1 1 calc R . .
H13C H 0.8200 0.2558 0.9220 0.072 Uiso 1 1 calc R . .
C14 C 0.6492(4) 0.3556(4) 0.9957(3) 0.0689(14) Uani 1 1 d . . .
H14A H 0.7017 0.3427 1.0816 0.103 Uiso 1 1 calc R . .
H14B H 0.5631 0.3799 0.9888 0.103 Uiso 1 1 calc R . .
H14C H 0.6939 0.4153 0.9649 0.103 Uiso 1 1 calc R . .
C15 C 0.5478(5) 0.1547(5) 0.9562(4) 0.0878(17) Uani 1 1 d . . .
H15A H 0.5350 0.0853 0.9051 0.132 Uiso 1 1 calc R . .
H15B H 0.4626 0.1844 0.9441 0.132 Uiso 1 1 calc R . .
H15C H 0.5920 0.1368 1.0423 0.132 Uiso 1 1 calc R . .
C16 C 0.2600(3) 0.4248(3) 0.5887(3) 0.0313(7) Uani 1 1 d . . .
C17 C 0.2544(3) 0.4864(3) 0.7017(3) 0.0396(8) Uani 1 1 d . . .
H17A H 0.2382 0.4301 0.7563 0.059 Uiso 1 1 calc R . .
H17B H 0.1836 0.5388 0.6764 0.059 Uiso 1 1 calc R . .
H17C H 0.3380 0.5298 0.7448 0.059 Uiso 1 1 calc R . .
C18 C 0.1293(3) 0.3564(3) 0.5272(3) 0.0433(8) Uani 1 1 d . . .
H18A H 0.1270 0.3202 0.4510 0.065 Uiso 1 1 calc R . .
H18B H 0.0577 0.4078 0.5089 0.065 Uiso 1 1 calc R . .
H18C H 0.1193 0.2974 0.5820 0.065 Uiso 1 1 calc R . .
C19 C 0.2814(3) 0.5173(3) 0.5048(3) 0.0404(8) Uani 1 1 d . . .
H19A H 0.3671 0.5581 0.5458 0.061 Uiso 1 1 calc R . .
H19B H 0.2125 0.5713 0.4868 0.061 Uiso 1 1 calc R . .
H19C H 0.2784 0.4812 0.4283 0.061 Uiso 1 1 calc R . .
C20 C 0.0193(5) 0.4239(4) 0.1605(4) 0.0750(14) Uani 1 1 d . . .
H20A H -0.0456 0.3863 0.1902 0.090 Uiso 1 1 calc R . .
H20B H -0.0095 0.4056 0.0718 0.090 Uiso 1 1 calc R . .
C21 C 0.0216(5) 0.5477(4) 0.1791(4) 0.0773(14) Uani 1 1 d . . .
H21A H 0.0314 0.5652 0.2637 0.116 Uiso 1 1 calc R . .
H21B H -0.0604 0.5763 0.1231 0.116 Uiso 1 1 calc R . .
H21C H 0.0955 0.5846 0.1629 0.116 Uiso 1 1 calc R . .
C22 C 0.1619(8) 0.1240(5) -0.0130(4) 0.133(3) Uani 1 1 d . . .
H22A H 0.2526 0.1014 0.0066 0.159 Uiso 1 1 calc R . .
H22B H 0.1093 0.0544 -0.0076 0.159 Uiso 1 1 calc R . .
C23 C 0.1172(7) 0.1539(6) -0.1279(4) 0.123(3) Uani 1 1 d . . .
H23A H 0.0268 0.1756 -0.1509 0.184 Uiso 1 1 calc R . .
H23B H 0.1197 0.0894 -0.1803 0.184 Uiso 1 1 calc R . .
H23C H 0.1718 0.2189 -0.1379 0.184 Uiso 1 1 calc R . .
Cl1 Cl 0.34304(7) 0.06526(6) 0.28336(6) 0.03197(17) Uani 1 1 d . . .
Cl2 Cl 0.05742(7) 0.14531(7) 0.28037(7) 0.03763(19) Uani 1 1 d . . .
Cl3 Cl 0.41703(8) 0.33984(8) 0.20195(7) 0.0417(2) Uani 1 1 d . . .
H1N H 0.680(3) 0.086(3) 0.565(3) 0.027(8) Uiso 1 1 d . . .
N1 N 0.6638(2) 0.1193(2) 0.5025(2) 0.0230(5) Uani 1 1 d . . .
Nb1 Nb 0.23421(2) 0.25126(2) 0.24173(2) 0.02631(9) Uani 1 1 d . . .
O1 O 0.33174(18) 0.28913(16) 0.41452(16) 0.0253(4) Uani 1 1 d . . .
O2 O 0.1382(2) 0.38072(19) 0.2193(2) 0.0391(5) Uani 1 1 d . . .
O3 O 0.1648(2) 0.20109(19) 0.08061(17) 0.0378(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.405(4) . ?
C1 C2 1.408(3) . ?
C1 C7 1.446(4) . ?
C2 C3 1.372(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(4) . ?
C3 C12 1.540(4) . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.417(4) . ?
C5 C16 1.534(4) . ?
C6 O1 1.339(3) . ?
C7 N1 1.287(3) . ?
C7 H7 0.9500 . ?
C8 N1 1.491(3) . ?
C8 C11 1.514(4) . ?
C8 C10 1.516(4) . ?
C8 C9 1.522(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.515(5) . ?
C12 C14 1.529(5) . ?
C12 C15 1.531(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.526(4) . ?
C16 C17 1.531(4) . ?
C16 C19 1.540(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 O2 1.365(5) . ?
C20 C21 1.464(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.316(6) . ?
C22 O3 1.409(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
Cl1 Nb1 2.5115(8) . ?
Cl2 Nb1 2.4364(8) . ?
Cl3 Nb1 2.4134(8) . ?
N1 H1N 0.80(3) . ?
Nb1 O3 1.841(2) . ?
Nb1 O2 1.863(2) . ?
Nb1 O1 1.9512(18) . ?

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
C6 C1 C2 120.4(2) . . ?
C6 C1 C7 120.4(2) . . ?
C2 C1 C7 118.9(2) . . ?
C3 C2 C1 121.0(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 116.9(2) . . ?
C2 C3 C12 122.5(3) . . ?
C4 C3 C12 120.6(3) . . ?
C5 C4 C3 125.3(3) . . ?
C5 C4 H4 117.3 . . ?
C3 C4 H4 117.3 . . ?
C4 C5 C6 116.5(2) . . ?
C4 C5 C16 120.8(2) . . ?
C6 C5 C16 122.7(2) . . ?
O1 C6 C1 119.8(2) . . ?
O1 C6 C5 120.7(2) . . ?
C1 C6 C5 119.5(2) . . ?
N1 C7 C1 123.6(2) . . ?
N1 C7 H7 118.2 . . ?
C1 C7 H7 118.2 . . ?
N1 C8 C11 110.6(2) . . ?
N1 C8 C10 107.4(2) . . ?
C11 C8 C10 111.8(2) . . ?
N1 C8 C9 105.0(2) . . ?
C11 C8 C9 111.1(3) . . ?
C10 C8 C9 110.6(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 108.4(3) . . ?
C13 C12 C15 108.5(3) . . ?
C14 C12 C15 110.4(4) . . ?
C13 C12 C3 111.9(3) . . ?
C14 C12 C3 110.7(3) . . ?
C15 C12 C3 106.9(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 C17 107.3(3) . . ?
C18 C16 C5 110.7(2) . . ?
C17 C16 C5 111.8(2) . . ?
C18 C16 C19 111.4(3) . . ?
C17 C16 C19 107.2(3) . . ?
C5 C16 C19 108.4(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O2 C20 C21 112.8(4) . . ?
O2 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
O2 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 O3 120.5(5) . . ?
C23 C22 H22A 107.2 . . ?
O3 C22 H22A 107.2 . . ?
C23 C22 H22B 107.2 . . ?
O3 C22 H22B 107.2 . . ?
H22A C22 H22B 106.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 N1 C8 128.1(2) . . ?
C7 N1 H1N 116(2) . . ?
C8 N1 H1N 116(2) . . ?
O3 Nb1 O2 95.78(9) . . ?
O3 Nb1 O1 170.56(8) . . ?
O2 Nb1 O1 93.00(8) . . ?
O3 Nb1 Cl3 88.14(7) . . ?
O2 Nb1 Cl3 96.58(7) . . ?
O1 Nb1 Cl3 87.41(6) . . ?
O3 Nb1 Cl2 90.22(7) . . ?
O2 Nb1 Cl2 88.45(7) . . ?
O1 Nb1 Cl2 93.49(6) . . ?
Cl3 Nb1 Cl2 174.84(3) . . ?
O3 Nb1 Cl1 85.94(7) . . ?
O2 Nb1 Cl1 172.54(7) . . ?
O1 Nb1 Cl1 85.80(6) . . ?
Cl3 Nb1 Cl1 90.72(3) . . ?
Cl2 Nb1 Cl1 84.29(3) . . ?
C6 O1 Nb1 166.02(17) . . ?
C20 O2 Nb1 145.3(3) . . ?
C22 O3 Nb1 150.3(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.5(4) . . . . ?
C7 C1 C2 C3 173.9(3) . . . . ?
C1 C2 C3 C4 -4.4(4) . . . . ?
C1 C2 C3 C12 173.9(3) . . . . ?
C2 C3 C4 C5 2.2(5) . . . . ?
C12 C3 C4 C5 -176.1(3) . . . . ?
C3 C4 C5 C6 3.9(4) . . . . ?
C3 C4 C5 C16 -175.1(3) . . . . ?
C2 C1 C6 O1 -172.9(2) . . . . ?
C7 C1 C6 O1 13.8(4) . . . . ?
C2 C1 C6 C5 5.8(4) . . . . ?
C7 C1 C6 C5 -167.5(3) . . . . ?
C4 C5 C6 O1 170.9(2) . . . . ?
C16 C5 C6 O1 -10.1(4) . . . . ?
C4 C5 C6 C1 -7.7(4) . . . . ?
C16 C5 C6 C1 171.3(3) . . . . ?
C6 C1 C7 N1 -164.0(3) . . . . ?
C2 C1 C7 N1 22.5(4) . . . . ?
C2 C3 C12 C13 15.4(4) . . . . ?
C4 C3 C12 C13 -166.5(3) . . . . ?
C2 C3 C12 C14 136.4(3) . . . . ?
C4 C3 C12 C14 -45.4(4) . . . . ?
C2 C3 C12 C15 -103.3(4) . . . . ?
C4 C3 C12 C15 74.9(4) . . . . ?
C4 C5 C16 C18 -113.3(3) . . . . ?
C6 C5 C16 C18 67.7(4) . . . . ?
C4 C5 C16 C17 6.3(4) . . . . ?
C6 C5 C16 C17 -172.7(3) . . . . ?
C4 C5 C16 C19 124.3(3) . . . . ?
C6 C5 C16 C19 -54.7(4) . . . . ?
C1 C7 N1 C8 -166.1(3) . . . . ?
C11 C8 N1 C7 -3.2(4) . . . . ?
C10 C8 N1 C7 -125.4(3) . . . . ?
C9 C8 N1 C7 116.7(3) . . . . ?
C1 C6 O1 Nb1 33.1(9) . . . . ?
C5 C6 O1 Nb1 -145.5(6) . . . . ?
O3 Nb1 O1 C6 -30.1(11) . . . . ?
O2 Nb1 O1 C6 171.5(7) . . . . ?
Cl3 Nb1 O1 C6 -92.0(7) . . . . ?
Cl2 Nb1 O1 C6 82.9(7) . . . . ?
Cl1 Nb1 O1 C6 -1.1(7) . . . . ?
C21 C20 O2 Nb1 -172.7(3) . . . . ?
O3 Nb1 O2 C20 39.7(5) . . . . ?
O1 Nb1 O2 C20 -143.8(5) . . . . ?
Cl3 Nb1 O2 C20 128.5(5) . . . . ?
Cl2 Nb1 O2 C20 -50.3(5) . . . . ?
Cl1 Nb1 O2 C20 -63.3(8) . . . . ?
C23 C22 O3 Nb1 -155.2(5) . . . . ?
O2 Nb1 O3 C22 174.7(8) . . . . ?
O1 Nb1 O3 C22 16.4(11) . . . . ?
Cl3 Nb1 O3 C22 78.3(8) . . . . ?
Cl2 Nb1 O3 C22 -96.8(8) . . . . ?
Cl1 Nb1 O3 C22 -12.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.900
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.078



data_global

data_new
#TrackingRef 'web_deposit_cif_file_0_MRINMAYMANDAL_1347944148.NEW.CIF'




_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C23 H32 Cl2 N Nb O4'

_chemical_formula_weight         550.31



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'
Nb Nb -2.0727 0.6215 '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   P2(1)/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                   8.1760(3)

_cell_length_b                   23.9385(9)

_cell_length_c                   13.5896(6)

_cell_angle_alpha                90.00

_cell_angle_beta                 94.923(2)

_cell_angle_gamma                90.00

_cell_volume                     2649.96(18)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    8053

_cell_measurement_theta_min      2.27

_cell_measurement_theta_max      26.66



_exptl_crystal_description       Block

_exptl_crystal_colour            red

_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.28

_exptl_crystal_size_min          0.15

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.379

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1136

_exptl_absorpt_coefficient_mu    0.682

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.7962

_exptl_absorpt_correction_T_max  0.9046

_exptl_absorpt_process_details   ' SADABS (Bruker,2004)'



_exptl_special_details           
;

?

;



_diffrn_ambient_temperature      173(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  'Bruker APEXII CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            18999

_diffrn_reflns_av_R_equivalents  0.0217

_diffrn_reflns_av_sigmaI/netI    0.0270

_diffrn_reflns_limit_h_min       -10

_diffrn_reflns_limit_h_max       9

_diffrn_reflns_limit_k_min       -30

_diffrn_reflns_limit_k_max       28

_diffrn_reflns_limit_l_min       -16

_diffrn_reflns_limit_l_max       10

_diffrn_reflns_theta_min         2.27

_diffrn_reflns_theta_max         28.44

_reflns_number_total             5912

_reflns_number_gt                4212

_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'APEXII, Bruker,2004'
_computing_cell_refinement       'APEXII/SAINT, Bruker,2004'
_computing_data_reduction        'SAINT PLUS/XPREP, Bruker,2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'




_refine_special_details          
;

Refinement of F² against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F², conventional R-factors R are based

on F, with F set to zero for negative F². The threshold expression of

F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.1000P)²+0.4512P] where P=(Fo²+2Fc²)/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         5912

_refine_ls_number_parameters     287

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0701

_refine_ls_R_factor_gt           0.0439

_refine_ls_wR_factor_ref         0.1587

_refine_ls_wR_factor_gt          0.1367

_refine_ls_goodness_of_fit_ref   1.029

_refine_ls_restrained_S_all      1.029

_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































































C1 C 0.4514(3) 0.10323(12) 0.6965(2) 0.0495(7) Uani 1 1 d . . .
C2 C 0.4689(4) 0.09738(14) 0.7997(2) 0.0537(7) Uani 1 1 d . . .
C3 C 0.3628(4) 0.06016(14) 0.8397(3) 0.0599(8) Uani 1 1 d . . .
H3 H 0.3730 0.0551 0.9093 0.072 Uiso 1 1 calc R . .
C4 C 0.2427(4) 0.02993(14) 0.7847(3) 0.0614(8) Uani 1 1 d . . .
C5 C 0.2293(4) 0.03642(13) 0.6844(3) 0.0592(8) Uani 1 1 d . . .
H5 H 0.1484 0.0159 0.6453 0.071 Uiso 1 1 calc R . .
C6 C 0.3329(4) 0.07279(12) 0.6385(2) 0.0521(7) Uani 1 1 d . . .
C7 C 0.3133(4) 0.07816(13) 0.5316(2) 0.0553(8) Uani 1 1 d . . .
H7 H 0.2278 0.0566 0.4986 0.066 Uiso 1 1 calc R . .
C8 C 0.3499(4) 0.10397(13) 0.3711(2) 0.0556(7) Uani 1 1 d . . .
C9 C 0.3698(5) 0.05414(14) 0.3239(3) 0.0650(9) Uani 1 1 d . . .
H9 H 0.4133 0.0227 0.3600 0.078 Uiso 1 1 calc R . .
C10 C 0.3269(5) 0.04967(15) 0.2244(3) 0.0677(9) Uani 1 1 d . . .
H10 H 0.3427 0.0153 0.1917 0.081 Uiso 1 1 calc R . .
C11 C 0.2611(4) 0.09467(15) 0.1714(2) 0.0602(8) Uani 1 1 d . . .
C12 C 0.2408(5) 0.14403(16) 0.2184(3) 0.0678(9) Uani 1 1 d . . .
H12 H 0.1943 0.1751 0.1826 0.081 Uiso 1 1 calc R . .
C13 C 0.2885(5) 0.14910(15) 0.3193(3) 0.0702(10) Uani 1 1 d . . .
H13 H 0.2781 0.1840 0.3516 0.084 Uiso 1 1 calc R . .
C14 C 0.5968(5) 0.13189(17) 0.8634(3) 0.0702(10) Uani 1 1 d . . .
C15 C 0.7688(5) 0.1213(2) 0.8307(4) 0.0990(15) Uani 1 1 d . . .
H15A H 0.7693 0.1294 0.7600 0.148 Uiso 1 1 calc R . .
H15B H 0.7989 0.0821 0.8428 0.148 Uiso 1 1 calc R . .
H15C H 0.8481 0.1455 0.8682 0.148 Uiso 1 1 calc R . .
C16 C 0.5541(6) 0.19366(18) 0.8520(4) 0.0940(14) Uani 1 1 d . . .
H16A H 0.4444 0.2003 0.8736 0.141 Uiso 1 1 calc R . .
H16B H 0.5558 0.2045 0.7826 0.141 Uiso 1 1 calc R . .
H16C H 0.6348 0.2159 0.8926 0.141 Uiso 1 1 calc R . .
C17 C 0.6009(6) 0.1167(2) 0.9733(3) 0.1043(17) Uani 1 1 d . . .
H17A H 0.6827 0.1399 1.0112 0.156 Uiso 1 1 calc R . .
H17B H 0.6302 0.0772 0.9822 0.156 Uiso 1 1 calc R . .
H17C H 0.4925 0.1233 0.9968 0.156 Uiso 1 1 calc R . .
C18 C 0.1302(6) -0.00933(19) 0.8345(3) 0.0869(12) Uani 1 1 d . . .
H18A H 0.0509 -0.0259 0.7847 0.130 Uiso 1 1 calc R . .
H18B H 0.0715 0.0115 0.8826 0.130 Uiso 1 1 calc R . .
H18C H 0.1955 -0.0390 0.8684 0.130 Uiso 1 1 calc R . .
C19 C 0.1333(6) 0.1286(3) 0.0190(3) 0.1020(17) Uani 1 1 d . . .
H19A H 0.0369 0.1394 0.0528 0.153 Uiso 1 1 calc R . .
H19B H 0.0980 0.1154 -0.0476 0.153 Uiso 1 1 calc R . .
H19C H 0.2059 0.1609 0.0148 0.153 Uiso 1 1 calc R . .
C20 C 0.7109(10) 0.1415(3) 0.3066(5) 0.150(3) Uani 1 1 d . . .
H20A H 0.7513 0.1029 0.3189 0.180 Uiso 1 1 calc R . .
H20B H 0.6094 0.1387 0.2616 0.180 Uiso 1 1 calc R . .
C21 C 0.8177(13) 0.1673(4) 0.2603(7) 0.197(5) Uani 1 1 d . . .
H21A H 0.7898 0.2071 0.2560 0.295 Uiso 1 1 calc R . .
H21B H 0.8190 0.1518 0.1937 0.295 Uiso 1 1 calc R . .
H21C H 0.9264 0.1628 0.2959 0.295 Uiso 1 1 calc R . .
C22 C 0.9764(8) 0.2110(4) 0.5958(6) 0.168(4) Uani 1 1 d . . .
H22A H 1.0256 0.1961 0.5372 0.201 Uiso 1 1 calc R . .
H22B H 0.9826 0.2522 0.5916 0.201 Uiso 1 1 calc R . .
C23 C 1.0709(9) 0.1964(4) 0.6715(9) 0.204(5) Uani 1 1 d . . .
H23A H 1.0222 0.2079 0.7317 0.306 Uiso 1 1 calc R . .
H23B H 1.1782 0.2143 0.6691 0.306 Uiso 1 1 calc R . .
H23C H 1.0845 0.1557 0.6716 0.306 Uiso 1 1 calc R . .
Cl1 Cl 0.76306(14) 0.07064(4) 0.53345(10) 0.0889(3) Uani 1 1 d . . .
Cl2 Cl 0.44692(15) 0.24047(4) 0.51662(9) 0.0878(3) Uani 1 1 d . . .
N1 N 0.3971(3) 0.10839(11) 0.47629(19) 0.0549(6) Uani 1 1 d . . .
Nb1 Nb 0.62563(4) 0.160842(12) 0.52817(2) 0.06008(15) Uani 1 1 d . . .
O5 O 0.5443(3) 0.13976(10) 0.65193(16) 0.0583(5) Uani 1 1 d . . .
O6 O 0.2194(3) 0.08501(12) 0.07315(18) 0.0782(7) Uani 1 1 d . . .
O7 O 0.6669(4) 0.16327(11) 0.3975(2) 0.0827(8) Uani 1 1 d . . .
O8 O 0.8073(3) 0.19670(11) 0.5850(2) 0.0823(8) Uani 1 1 d . . .






_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell esds are taken

into account individually in the estimation of esds in distances, angles

and torsion angles; correlations between esds in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

































































C1 O5 1.337(4) . ?
C1 C6 1.400(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.387(5) . ?
C2 C14 1.540(5) . ?
C3 C4 1.386(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(5) . ?
C4 C18 1.515(5) . ?
C5 C6 1.398(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.454(4) . ?
C7 N1 1.283(4) . ?
C7 H7 0.9500 . ?
C8 C13 1.362(5) . ?
C8 C9 1.371(5) . ?
C8 N1 1.452(4) . ?
C9 C10 1.372(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.360(5) . ?
C11 O6 1.369(4) . ?
C12 C13 1.399(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C16 1.524(6) . ?
C14 C15 1.532(6) . ?
C14 C17 1.535(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 O6 1.427(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.278(8) . ?
C20 O7 1.416(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.281(9) . ?
C22 O8 1.420(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
Cl1 Nb1 2.4324(11) . ?
Cl2 Nb1 2.3987(11) . ?
N1 Nb1 2.310(3) . ?
Nb1 O8 1.828(2) . ?
Nb1 O7 1.836(3) . ?
Nb1 O5 1.928(2) . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag

























































































































O5 C1 C6 118.6(3) . . ?
O5 C1 C2 120.3(3) . . ?
C6 C1 C2 121.1(3) . . ?
C3 C2 C1 116.2(3) . . ?
C3 C2 C14 122.8(3) . . ?
C1 C2 C14 120.9(3) . . ?
C4 C3 C2 124.2(3) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 H3 117.9 . . ?
C5 C4 C3 118.1(3) . . ?
C5 C4 C18 121.1(3) . . ?
C3 C4 C18 120.8(3) . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.3(3) . . ?
C5 C6 C7 118.8(3) . . ?
C1 C6 C7 121.9(3) . . ?
N1 C7 C6 128.1(3) . . ?
N1 C7 H7 116.0 . . ?
C6 C7 H7 116.0 . . ?
C13 C8 C9 120.1(3) . . ?
C13 C8 N1 120.4(3) . . ?
C9 C8 N1 119.5(3) . . ?
C8 C9 C10 119.9(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 120.6(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C12 C11 O6 125.0(3) . . ?
C12 C11 C10 119.5(3) . . ?
O6 C11 C10 115.5(3) . . ?
C11 C12 C13 120.0(3) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C8 C13 C12 119.9(3) . . ?
C8 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C16 C14 C15 109.8(4) . . ?
C16 C14 C17 108.4(4) . . ?
C15 C14 C17 107.4(4) . . ?
C16 C14 C2 109.0(3) . . ?
C15 C14 C2 110.1(3) . . ?
C17 C14 C2 112.2(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 C18 H18A 109.5 . . ?
C4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O6 C19 H19A 109.5 . . ?
O6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 O7 119.2(6) . . ?
C21 C20 H20A 107.5 . . ?
O7 C20 H20A 107.5 . . ?
C21 C20 H20B 107.5 . . ?
O7 C20 H20B 107.5 . . ?
H20A C20 H20B 107.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 O8 122.1(7) . . ?
C23 C22 H22A 106.8 . . ?
O8 C22 H22A 106.8 . . ?
C23 C22 H22B 106.8 . . ?
O8 C22 H22B 106.8 . . ?
H22A C22 H22B 106.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 N1 C8 115.2(3) . . ?
C7 N1 Nb1 125.9(2) . . ?
C8 N1 Nb1 118.7(2) . . ?
O8 Nb1 O7 100.59(14) . . ?
O8 Nb1 O5 94.74(11) . . ?
O7 Nb1 O5 163.21(11) . . ?
O8 Nb1 N1 172.05(11) . . ?
O7 Nb1 N1 86.17(11) . . ?
O5 Nb1 N1 78.08(9) . . ?
O8 Nb1 Cl2 97.05(10) . . ?
O7 Nb1 Cl2 94.19(10) . . ?
O5 Nb1 Cl2 90.65(8) . . ?
N1 Nb1 Cl2 86.55(7) . . ?
O8 Nb1 Cl1 92.75(10) . . ?
O7 Nb1 Cl1 86.21(10) . . ?
O5 Nb1 Cl1 86.27(8) . . ?
N1 Nb1 Cl1 83.45(7) . . ?
Cl2 Nb1 Cl1 169.95(4) . . ?
C1 O5 Nb1 144.9(2) . . ?
C11 O6 C19 116.7(3) . . ?
C20 O7 Nb1 156.1(4) . . ?
C22 O8 Nb1 154.9(5) . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag







































































O5 C1 C2 C3 177.5(3) . . . . ?
C6 C1 C2 C3 -0.1(4) . . . . ?
O5 C1 C2 C14 -1.1(5) . . . . ?
C6 C1 C2 C14 -178.7(3) . . . . ?
C1 C2 C3 C4 -0.8(5) . . . . ?
C14 C2 C3 C4 177.7(3) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C2 C3 C4 C18 -179.2(3) . . . . ?
C3 C4 C5 C6 -0.4(5) . . . . ?
C18 C4 C5 C6 179.8(4) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C4 C5 C6 C7 -179.9(3) . . . . ?
O5 C1 C6 C5 -176.9(3) . . . . ?
C2 C1 C6 C5 0.7(5) . . . . ?
O5 C1 C6 C7 2.6(5) . . . . ?
C2 C1 C6 C7 -179.8(3) . . . . ?
C5 C6 C7 N1 -178.9(3) . . . . ?
C1 C6 C7 N1 1.6(5) . . . . ?
C13 C8 C9 C10 -0.4(6) . . . . ?
N1 C8 C9 C10 -179.4(3) . . . . ?
C8 C9 C10 C11 -1.1(6) . . . . ?
C9 C10 C11 C12 0.9(6) . . . . ?
C9 C10 C11 O6 -178.6(4) . . . . ?
O6 C11 C12 C13 -179.8(4) . . . . ?
C10 C11 C12 C13 0.8(6) . . . . ?
C9 C8 C13 C12 2.1(6) . . . . ?
N1 C8 C13 C12 -178.9(3) . . . . ?
C11 C12 C13 C8 -2.3(6) . . . . ?
C3 C2 C14 C16 -115.5(4) . . . . ?
C1 C2 C14 C16 63.0(4) . . . . ?
C3 C2 C14 C15 124.0(4) . . . . ?
C1 C2 C14 C15 -57.5(5) . . . . ?
C3 C2 C14 C17 4.5(5) . . . . ?
C1 C2 C14 C17 -177.0(4) . . . . ?
C6 C7 N1 C8 178.8(3) . . . . ?
C6 C7 N1 Nb1 5.0(5) . . . . ?
C13 C8 N1 C7 116.1(4) . . . . ?
C9 C8 N1 C7 -64.9(4) . . . . ?
C13 C8 N1 Nb1 -69.6(4) . . . . ?
C9 C8 N1 Nb1 109.4(3) . . . . ?
C7 N1 Nb1 O8 15.1(10) . . . . ?
C8 N1 Nb1 O8 -158.5(8) . . . . ?
C7 N1 Nb1 O7 163.5(3) . . . . ?
C8 N1 Nb1 O7 -10.1(2) . . . . ?
C7 N1 Nb1 O5 -10.7(3) . . . . ?
C8 N1 Nb1 O5 175.7(2) . . . . ?
C7 N1 Nb1 Cl2 -102.1(3) . . . . ?
C8 N1 Nb1 Cl2 84.3(2) . . . . ?
C7 N1 Nb1 Cl1 76.9(3) . . . . ?
C8 N1 Nb1 Cl1 -96.7(2) . . . . ?
C6 C1 O5 Nb1 -20.7(5) . . . . ?
C2 C1 O5 Nb1 161.7(3) . . . . ?
O8 Nb1 O5 C1 -155.3(4) . . . . ?
O7 Nb1 O5 C1 0.7(6) . . . . ?
N1 Nb1 O5 C1 21.2(4) . . . . ?
Cl2 Nb1 O5 C1 107.6(4) . . . . ?
Cl1 Nb1 O5 C1 -62.9(4) . . . . ?
C12 C11 O6 C19 -6.6(6) . . . . ?
C10 C11 O6 C19 172.8(4) . . . . ?
C21 C20 O7 Nb1 -131.7(9) . . . . ?
O8 Nb1 O7 C20 106.9(9) . . . . ?
O5 Nb1 O7 C20 -48.7(11) . . . . ?
N1 Nb1 O7 C20 -68.9(9) . . . . ?
Cl2 Nb1 O7 C20 -155.1(9) . . . . ?
Cl1 Nb1 O7 C20 14.8(9) . . . . ?
C23 C22 O8 Nb1 -113.2(11) . . . . ?
O7 Nb1 O8 C22 -37.2(9) . . . . ?
O5 Nb1 O8 C22 135.9(9) . . . . ?
N1 Nb1 O8 C22 110.7(11) . . . . ?
Cl2 Nb1 O8 C22 -132.8(9) . . . . ?
Cl1 Nb1 O8 C22 49.5(9) . . . . ?



_diffrn_measured_fraction_theta_max 0.888

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.724

_refine_diff_density_min         -0.573

_refine_diff_density_rms         0.057



