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#$Date: 2019-11-23 20:00:29 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/21/7702102.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_7702102
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         'C5 H12 Cl4 Nb S2'
_chemical_formula_sum            'C5 H12 Cl4 Nb S2'
_chemical_formula_weight         370.98
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_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            8
_cell_length_a                   9.964(3)
_cell_length_b                   9.964(3)
_cell_length_c                   25.113(12)
_cell_measurement_reflns_used    2212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.9
_cell_volume                     2493.3(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            3934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         2.199
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.108
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0521
_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)+(0.0618P)²+1.5104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                841
_reflns_number_total             1225
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2493(2)
_cod_database_code               7702102
_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   0.863
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_file
; 
  
    shelx.res created by SHELXL-2014/7 
  
  
TITL shelx in I-42d 
CELL 0.71073   9.9644   9.9644  25.1132  90.000  90.000  90.000 
ZERR    8.00   0.0034   0.0034   0.0118   0.000   0.000   0.000 
LATT -2 
SYMM -X, -Y, Z 
SYMM Y, -X, -Z 
SYMM -Y, X, -Z 
SYMM 0.5-X, Y, 0.75-Z 
SYMM 0.5+X, -Y, 0.75-Z 
SYMM 0.5-Y, -X, 0.75+Z 
SYMM 0.5+Y, X, 0.75+Z 
SFAC C  H  S  Cl Nb 
UNIT 40 96 16 32 8 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
TWIN 
SIZE 0.072 0.048 0.027 
TEMP -173 
WGHT    0.061800    1.510400 
BASF   0.13637 
FVAR       0.17661 
MOLE 1 
NB1   5    0.000000    0.500000    1.000181    10.50000    0.04564    0.04829 = 
         0.01825    0.00000    0.00000   -0.00794 
S1    3    0.088971    0.655354    0.923218    11.00000    0.08530    0.05645 = 
         0.03269    0.00730    0.01363   -0.00281 
CL1   4   -0.069254    0.341975    1.063933    11.00000    0.08138    0.05932 = 
         0.02577    0.00593    0.00255   -0.02331 
CL2   4    0.207361    0.395702    0.988300    11.00000    0.05137    0.08835 = 
         0.05829    0.01153    0.00577    0.00919 
C1    1    0.045525    0.824569    0.937935    11.00000    0.12037    0.03451 = 
         0.04802    0.00287    0.02068   -0.01028 
AFIX 137 
H1A   2    0.095598    0.885016    0.914422    11.00000   -1.50000 
H1B   2    0.068022    0.844416    0.975099    11.00000   -1.50000 
H1C   2   -0.050969    0.837459    0.932389    11.00000   -1.50000 
AFIX   0 
C2    1   -0.027944    0.624644    0.867930    11.00000    0.13014    0.06555 = 
         0.02812    0.01199   -0.00759    0.02139 
AFIX  23 
H2A   2   -0.120122    0.618976    0.882466    11.00000   -1.20000 
H2B   2   -0.024915    0.702493    0.843466    11.00000   -1.20000 
AFIX   0 
C3    1    0.000000    0.500000    0.836647    10.50000    0.09304    0.05565 = 
         0.03328    0.00000    0.00000    0.01524 
AFIX  23 
H3A   2    0.078090    0.517506    0.813286    10.50000   -1.20000 
H3B   2   -0.078091    0.482491    0.813286    10.50000   -1.20000 
AFIX   0 
HKLF 4 
  
REM  shelx in I-42d 
REM R1 =  0.0521 for     841 Fo > 4sig(Fo)  and  0.0821 for all    1225 data 
REM     58 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0617      1.5471 
  
REM Highest difference peak  0.867,  deepest hole -0.533,  1-sigma level  0.120 
Q1    1  -0.0175  0.6778  0.9213  11.00000  0.05    0.87 
Q2    1   0.1722  0.4402  0.9615  11.00000  0.05    0.71 
Q3    1  -0.0743  0.4978  0.9981  11.00000  0.05    0.63 
Q4    1  -0.0011  0.5824  1.0007  11.00000  0.05    0.58 
Q5    1   0.0000  0.5000  1.0271  10.50000  0.05    0.53 
;
_shelx_res_checksum              55139
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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 0.0000 0.5000 1.00018(4) 0.0374(4) Uani 1 2 d S T P
S1 S 0.0890(5) 0.6554(4) 0.92322(10) 0.0581(11) Uani 1 1 d . . .
Cl1 Cl -0.0693(4) 0.3420(4) 1.06393(8) 0.0555(10) Uani 1 1 d . . .
Cl2 Cl 0.2074(4) 0.3957(4) 0.98830(12) 0.0660(10) Uani 1 1 d . . .
C1 C 0.0455(18) 0.8246(12) 0.9379(4) 0.068(5) Uani 1 1 d . . .
H1A H 0.0956 0.8850 0.9144 0.101 Uiso 1 1 calc R U .
H1B H 0.0680 0.8444 0.9751 0.101 Uiso 1 1 calc R U .
H1C H -0.0510 0.8375 0.9324 0.101 Uiso 1 1 calc R U .
C2 C -0.0279(19) 0.6246(14) 0.8679(4) 0.075(5) Uani 1 1 d . . .
H2A H -0.1201 0.6190 0.8825 0.090 Uiso 1 1 calc R U .
H2B H -0.0249 0.7025 0.8435 0.090 Uiso 1 1 calc R U .
C3 C 0.0000 0.5000 0.8366(6) 0.061(5) Uani 1 2 d S T P
H3A H 0.0781 0.5175 0.8133 0.073 Uiso 0.5 1 calc R U P
H3B H -0.0781 0.4825 0.8133 0.073 Uiso 0.5 1 calc R U P
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 0.0456(9) 0.0483(9) 0.0183(5) 0.000 0.000 -0.0079(8)
S1 0.085(3) 0.056(2) 0.0327(11) 0.0073(15) 0.0136(16) -0.003(2)
Cl1 0.081(3) 0.059(2) 0.0258(9) 0.0059(14) 0.0025(14) -0.023(2)
Cl2 0.0514(19) 0.088(3) 0.0583(15) 0.0115(18) 0.0058(15) 0.009(2)
C1 0.120(14) 0.035(7) 0.048(5) 0.003(6) 0.021(8) -0.010(9)
C2 0.130(16) 0.066(9) 0.028(4) 0.012(6) -0.008(7) 0.021(12)
C3 0.093(16) 0.056(12) 0.033(7) 0.000 0.000 0.015(16)
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'
S S 0.1246 0.1234 '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'
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
Cl2 Nb1 Cl2 165.30(16) . 2_565
Cl2 Nb1 Cl1 97.22(15) . 2_565
Cl2 Nb1 Cl1 92.80(15) 2_565 2_565
Cl2 Nb1 Cl1 92.79(15) . .
Cl2 Nb1 Cl1 97.22(15) 2_565 .
Cl1 Nb1 Cl1 94.08(15) 2_565 .
Cl2 Nb1 S1 86.69(14) . 2_565
Cl2 Nb1 S1 82.51(14) 2_565 2_565
Cl1 Nb1 S1 173.88(13) 2_565 2_565
Cl1 Nb1 S1 90.42(10) . 2_565
Cl2 Nb1 S1 82.51(14) . .
Cl2 Nb1 S1 86.69(14) 2_565 .
Cl1 Nb1 S1 90.42(10) 2_565 .
Cl1 Nb1 S1 173.88(13) . .
S1 Nb1 S1 85.41(16) 2_565 .
C1 S1 C2 99.2(7) . .
C1 S1 Nb1 108.8(4) . .
C2 S1 Nb1 104.1(5) . .
S1 C1 H1A 109.5 . .
S1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 S1 114.6(10) . .
C3 C2 H2A 108.6 . .
S1 C2 H2A 108.6 . .
C3 C2 H2B 108.6 . .
S1 C2 H2B 108.6 . .
H2A C2 H2B 107.6 . .
C2 C3 C2 116.6(12) . 2_565
C2 C3 H3A 108.1 . .
C2 C3 H3A 108.1 2_565 .
C2 C3 H3B 108.1 . .
C2 C3 H3B 108.1 2_565 .
H3A C3 H3B 107.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl2 2.332(4) .
Nb1 Cl2 2.332(4) 2_565
Nb1 Cl1 2.349(3) 2_565
Nb1 Cl1 2.349(3) .
Nb1 S1 2.630(3) 2_565
Nb1 S1 2.630(3) .
S1 C1 1.780(13) .
S1 C2 1.838(14) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.496(15) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C2 1.496(15) 2_565
C3 H3A 0.9900 .
C3 H3B 0.9900 .
