#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:00:29 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/20/7702099.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_7702099
loop_
_publ_author_name
'Chang, Yao-Pang'
'Levason, William'
'Light, Mark E.'
'Reid, Gillian'
_publ_section_title
;
 Niobium tetrachloride complexes with thio-, seleno- and telluro-ether
 coordination - synthesis and structures.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16262
_journal_page_last               16274
_journal_paper_doi               10.1039/c6dt02979e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C8 H24 Cl8 Nb2 Te4'
_chemical_formula_sum            'C8 H24 Cl8 Nb2 Te4'
_chemical_formula_weight         1100.09
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-18 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.48350(10)
_cell_length_b                   10.48350(10)
_cell_length_c                   12.0612(2)
_cell_measurement_reflns_used    10097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9530
_cell_measurement_theta_min      2.5440
_cell_volume                     1325.57(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.748
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    5.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    2.756
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Flack x determined using 501 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.016(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0120
_refine_ls_R_factor_gt           0.0119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0170P)²+0.4852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0295
_refine_ls_wR_factor_ref         0.0295
_reflns_Friedel_coverage         0.621
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1310
_reflns_number_total             1315
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           2016_1905k4
_cod_database_code               7702099
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.444
_shelx_estimated_absorpt_t_max   0.787
_shelx_res_file
; 
  
    2016_1905k4.res created by SHELXL-2014/7 
  
  
TITL 2016_1905k4 in P4(2)2(1)2 
CELL 0.71073  10.4835  10.4835  12.0612  90.000  90.000  90.000 
ZERR   2.0   0.0001   0.0001   0.0002   0.000   0.000   0.000 
LATT -1 
SYMM -X, -Y, Z 
SYMM 0.5-Y, 0.5+X, 0.5+Z 
SYMM 0.5+Y, 0.5-X, 0.5+Z 
SYMM 0.5-X, 0.5+Y, 0.5-Z 
SYMM 0.5+X, 0.5-Y, 0.5-Z 
SYMM Y, X, -Z 
SYMM -Y, -X, -Z 
SFAC C  H  Cl Nb Te 
UNIT 16 48 16 4 8 
OMIT  0   1   1 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND 
BOND $H 
FMAP 2 
PLAN 3 
SIZE 0.162 0.154 0.042 
TEMP -173 
WGHT    0.017000    0.485200 
FVAR       2.69666 
MOLE 1 
NB1   4    0.404872    0.595128    1.000000    10.50000    0.00750    0.00750 = 
         0.00859   -0.00015   -0.00015    0.00014 
TE1   5    0.439257    0.819173    0.853797    11.00000    0.01194    0.00946 = 
         0.01360    0.00222   -0.00042   -0.00001 
CL1   3    0.204705    0.599286    0.888589    11.00000    0.01019    0.01317 = 
         0.01297   -0.00045   -0.00243    0.00039 
CL2   3    0.500000    0.500000    0.823382    10.50000    0.01199    0.01178 = 
         0.00955    0.00000    0.00000    0.00090 
CL3   3    0.642848    0.642848    1.000000    10.50000    0.00893    0.00893 = 
         0.01397    0.00025   -0.00025   -0.00101 
C1    1    0.390599    0.762462    0.689742    11.00000    0.02533    0.01631 = 
         0.01281    0.00202   -0.00065    0.00218 
AFIX 137 
H1A   2    0.308746    0.717326    0.690742    11.00000   -1.50000 
H1B   2    0.456945    0.705824    0.660538    11.00000   -1.50000 
H1C   2    0.383700    0.838121    0.642400    11.00000   -1.50000 
AFIX   0 
C2    1    0.267547    0.923804    0.877263    11.00000    0.01842    0.01276 = 
         0.02251    0.00412    0.00213    0.00567 
AFIX 137 
H2A   2    0.254922    0.982081    0.814687    11.00000   -1.50000 
H2B   2    0.273171    0.972994    0.946183    11.00000   -1.50000 
H2C   2    0.195430    0.864548    0.881731    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_1905k4 in P4(2)2(1)2 
REM R1 =  0.0119 for    1310 Fo > 4sig(Fo)  and  0.0120 for all    1315 data 
REM     54 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0170      0.4852 
  
REM Highest difference peak  0.298,  deepest hole -0.236,  1-sigma level  0.075 
Q1    1   0.5201  0.6108  0.9956  11.00000  0.05    0.30 
Q2    1   0.4437  0.7133  0.8485  11.00000  0.05    0.28 
Q3    1   0.5000  0.5000  1.0000  10.25000  0.05    0.28 
;
_shelx_res_checksum              86614
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-y, -x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Nb1 Nb 0.40487(3) 0.59513(3) 1.0000 0.00786(9) Uani 1 2 d S T P
Te1 Te 0.43926(2) 0.81917(2) 0.85380(2) 0.01167(7) Uani 1 1 d . . .
Cl1 Cl 0.20471(7) 0.59929(8) 0.88859(6) 0.01211(16) Uani 1 1 d . . .
Cl2 Cl 0.5000 0.5000 0.82338(8) 0.0111(2) Uani 1 2 d S T P
Cl3 Cl 0.64285(7) 0.64285(7) 1.0000 0.0106(2) Uani 1 2 d S T P
C1 C 0.3906(4) 0.7625(3) 0.6897(3) 0.0182(7) Uani 1 1 d . . .
H1A H 0.3087 0.7173 0.6907 0.027 Uiso 1 1 calc R U .
H1B H 0.4569 0.7058 0.6605 0.027 Uiso 1 1 calc R U .
H1C H 0.3837 0.8381 0.6424 0.027 Uiso 1 1 calc R U .
C2 C 0.2675(3) 0.9238(3) 0.8773(3) 0.0179(7) Uani 1 1 d . . .
H2A H 0.2549 0.9821 0.8147 0.027 Uiso 1 1 calc R U .
H2B H 0.2732 0.9730 0.9462 0.027 Uiso 1 1 calc R U .
H2C H 0.1954 0.8645 0.8817 0.027 Uiso 1 1 calc R U .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.00750(13) 0.00750(13) 0.00859(18) -0.00015(11) -0.00015(11) 0.00014(15)
Te1 0.01194(11) 0.00946(11) 0.01360(11) 0.00222(8) -0.00042(8) -0.00001(8)
Cl1 0.0102(4) 0.0132(4) 0.0130(4) -0.0005(3) -0.0024(3) 0.0004(3)
Cl2 0.0120(6) 0.0118(6) 0.0096(5) 0.000 0.000 0.0009(4)
Cl3 0.0089(3) 0.0089(3) 0.0140(5) 0.0003(3) -0.0003(3) -0.0010(4)
C1 0.025(2) 0.0163(18) 0.0128(15) 0.0020(13) -0.0007(14) 0.0022(16)
C2 0.0184(18) 0.0128(17) 0.0225(18) 0.0041(14) 0.0021(15) 0.0057(15)
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'
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'
Te Te -0.5308 1.6751 '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
Cl1 Nb1 Cl1 105.14(4) . 8_667
Cl1 Nb1 Cl3 81.47(2) . 2_665
Cl1 Nb1 Cl3 145.299(19) 8_667 2_665
Cl1 Nb1 Cl3 145.299(19) . .
Cl1 Nb1 Cl3 81.47(2) 8_667 .
Cl3 Nb1 Cl3 112.68(3) 2_665 .
Cl1 Nb1 Cl2 83.45(2) . .
Cl1 Nb1 Cl2 141.729(19) 8_667 .
Cl3 Nb1 Cl2 72.182(11) 2_665 .
Cl3 Nb1 Cl2 72.182(11) . .
Cl1 Nb1 Cl2 141.729(19) . 7_557
Cl1 Nb1 Cl2 83.45(2) 8_667 7_557
Cl3 Nb1 Cl2 72.182(11) 2_665 7_557
Cl3 Nb1 Cl2 72.183(11) . 7_557
Cl2 Nb1 Cl2 112.99(3) . 7_557
Cl1 Nb1 Nb1 127.43(2) . 2_665
Cl1 Nb1 Nb1 127.43(2) 8_667 2_665
Cl3 Nb1 Nb1 56.338(15) 2_665 2_665
Cl3 Nb1 Nb1 56.339(15) . 2_665
Cl2 Nb1 Nb1 56.493(14) . 2_665
Cl2 Nb1 Nb1 56.493(14) 7_557 2_665
Cl1 Nb1 Te1 76.55(2) . .
Cl1 Nb1 Te1 69.825(19) 8_667 .
Cl3 Nb1 Te1 143.341(5) 2_665 .
Cl3 Nb1 Te1 74.008(11) . .
Cl2 Nb1 Te1 76.432(10) . .
Cl2 Nb1 Te1 139.392(5) 7_557 .
Nb1 Nb1 Te1 118.367(8) 2_665 .
Cl1 Nb1 Te1 69.824(19) . 8_667
Cl1 Nb1 Te1 76.55(2) 8_667 8_667
Cl3 Nb1 Te1 74.009(11) 2_665 8_667
Cl3 Nb1 Te1 143.342(5) . 8_667
Cl2 Nb1 Te1 139.392(5) . 8_667
Cl2 Nb1 Te1 76.432(10) 7_557 8_667
Nb1 Nb1 Te1 118.368(8) 2_665 8_667
Te1 Nb1 Te1 123.264(16) . 8_667
C2 Te1 C1 93.72(14) . .
C2 Te1 Nb1 103.12(10) . .
C1 Te1 Nb1 107.65(10) . .
Nb1 Cl2 Nb1 67.02(3) . 2_665
Nb1 Cl3 Nb1 67.32(3) . 2_665
Te1 C1 H1A 109.5 . .
Te1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Te1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Te1 C2 H2A 109.5 . .
Te1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Te1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl1 2.4922(8) .
Nb1 Cl1 2.4922(8) 8_667
Nb1 Cl3 2.5445(9) 2_665
Nb1 Cl3 2.5445(9) .
Nb1 Cl2 2.5548(9) .
Nb1 Cl2 2.5548(9) 7_557
Nb1 Nb1 2.8208(8) 2_665
Nb1 Te1 2.9591(3) .
Nb1 Te1 2.9591(3) 8_667
Te1 C2 2.127(3) .
Te1 C1 2.128(3) .
Cl2 Nb1 2.5548(9) 2_665
Cl3 Nb1 2.5445(9) 2_665
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
