#------------------------------------------------------------------------------
#$Date: 2019-11-23 19:00:29 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 234753 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/21/7702104.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_7702104
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 Se2'
_chemical_formula_sum            'C5 H12 Cl4 Nb Se2'
_chemical_formula_weight         464.78
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :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            8
_cell_length_a                   9.9381(2)
_cell_length_b                   9.9381(2)
_cell_length_c                   26.2651(11)
_cell_measurement_reflns_used    6180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0750
_cell_measurement_theta_min      2.2060
_cell_volume                     2594.09(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0831
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            8738
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    7.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46954
_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            Red
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0433P)²+0.5224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1219
_reflns_number_total             1281
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           2016_1802r3
_cod_original_cell_volume        2594.09(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7702104
_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   0.668
_shelx_estimated_absorpt_t_max   0.810
_shelx_res_file
; 
  
    2016_1802r3.res created by SHELXL-2014/7 
  
  
TITL 2016_1802r3 in I4(1)/a 
CELL 0.71073   9.9381   9.9381  26.2651  90.000  90.000  90.000 
ZERR    8.00   0.0002   0.0002   0.0011   0.000   0.000   0.000 
LATT 2 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM 0.75-Y, 0.25+X, 0.25+Z 
SYMM 0.75+Y, 0.75-X, 0.75+Z 
SFAC C  H  Cl Se Nb 
UNIT 40 96 32 16 8 
OMIT 0   1   1 
OMIT 0 4 6 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.06 0.05 0.03 
TWIN -1 0 0 0 1 0 0 0 -1 
TEMP -173 
WGHT    0.043300    0.522400 
BASF   0.45461 
FVAR       0.14716 
NB1   5    0.500000    0.750000    0.378779    10.50000    0.01354    0.01418 = 
         0.01378    0.00000    0.00000   -0.00092 
SE1   4    0.602924    0.594733    0.300595    11.00000    0.01299    0.01520 = 
         0.01555   -0.00019    0.00034    0.00187 
CL1   3    0.420807    0.906758    0.439259    11.00000    0.02769    0.01977 = 
         0.01903   -0.00319    0.00547    0.00149 
CL2   3    0.297638    0.634811    0.365925    11.00000    0.01408    0.02122 = 
         0.02270    0.00085    0.00083   -0.00319 
C1    1    0.545257    0.412617    0.316715    11.00000    0.02884    0.01252 = 
         0.01915   -0.00200    0.00116   -0.00399 
AFIX 137 
H1A   2    0.447113    0.410557    0.320254    11.00000   -1.50000 
H1B   2    0.586952    0.383883    0.348732    11.00000   -1.50000 
H1C   2    0.572652    0.351655    0.289280    11.00000   -1.50000 
AFIX   0 
C2    1    0.471521    0.623451    0.245887    11.00000    0.01762    0.02017 = 
         0.01804   -0.00238   -0.00648    0.00331 
AFIX  23 
H2A   2    0.472204    0.544414    0.222945    11.00000   -1.20000 
H2B   2    0.380481    0.630475    0.260955    11.00000   -1.20000 
AFIX   0 
C3    1    0.500000    0.750000    0.214704    10.50000    0.02963    0.02829 = 
         0.01375    0.00000    0.00000    0.01310 
AFIX  23 
H3A   2    0.421623    0.767639    0.192417    10.50000   -1.20000 
H3B   2    0.578376    0.732362    0.192417    10.50000   -1.20000 
AFIX   0 
HKLF 4 
  
REM  2016_1802r3 in I4(1)/a 
REM R1 =  0.0281 for    1219 Fo > 4sig(Fo)  and  0.0302 for all    1281 data 
REM     58 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0432      0.5384 
  
REM Highest difference peak  0.836,  deepest hole -0.723,  1-sigma level  0.154 
Q1    1   0.5497  0.6736  0.3388  11.00000  0.05    0.84 
Q2    1   0.5823  0.8153  0.3795  11.00000  0.05    0.62 
Q3    1   0.6894  0.6654  0.3023  11.00000  0.05    0.62 
Q4    1   0.4928  0.6089  0.3138  11.00000  0.05    0.58 
Q5    1   0.4128  0.8205  0.3786  11.00000  0.05    0.54 
;
_shelx_res_checksum              36484
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.5000 0.7500 0.37878(2) 0.01383(16) Uani 1 2 d S T P
Se1 Se 0.60292(5) 0.59473(4) 0.30059(2) 0.01458(14) Uani 1 1 d . . .
Cl1 Cl 0.42081(12) 0.90676(12) 0.43926(5) 0.0222(3) Uani 1 1 d . . .
Cl2 Cl 0.29764(12) 0.63481(13) 0.36593(5) 0.0193(3) Uani 1 1 d . . .
C1 C 0.5453(5) 0.4126(4) 0.3167(2) 0.0202(11) Uani 1 1 d . . .
H1A H 0.4471 0.4106 0.3203 0.030 Uiso 1 1 calc R U .
H1B H 0.5870 0.3839 0.3487 0.030 Uiso 1 1 calc R U .
H1C H 0.5727 0.3517 0.2893 0.030 Uiso 1 1 calc R U .
C2 C 0.4715(5) 0.6235(4) 0.2459(2) 0.0186(10) Uani 1 1 d . . .
H2A H 0.4722 0.5444 0.2229 0.022 Uiso 1 1 calc R U .
H2B H 0.3805 0.6305 0.2610 0.022 Uiso 1 1 calc R U .
C3 C 0.5000 0.7500 0.2147(3) 0.0239(17) Uani 1 2 d S T P
H3A H 0.4216 0.7676 0.1924 0.029 Uiso 0.5 1 calc R U P
H3B H 0.5784 0.7324 0.1924 0.029 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 0.0135(3) 0.0142(3) 0.0138(3) 0.000 0.000 -0.0009(2)
Se1 0.0130(2) 0.0152(2) 0.0156(3) -0.00019(18) 0.00034(18) 0.00187(19)
Cl1 0.0277(6) 0.0198(5) 0.0190(7) -0.0032(5) 0.0055(5) 0.0015(4)
Cl2 0.0141(5) 0.0212(6) 0.0227(7) 0.0009(5) 0.0008(4) -0.0032(4)
C1 0.029(3) 0.013(2) 0.019(3) -0.002(2) 0.001(2) -0.004(2)
C2 0.018(2) 0.020(2) 0.018(2) -0.002(2) -0.0065(19) 0.0033(19)
C3 0.030(4) 0.028(4) 0.014(4) 0.000 0.000 0.013(3)
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'
Se Se -0.0929 2.2259 '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 163.40(7) . 6_564
Cl2 Nb1 Cl1 97.67(4) . .
Cl2 Nb1 Cl1 93.49(4) 6_564 .
Cl2 Nb1 Cl1 93.49(4) . 6_564
Cl2 Nb1 Cl1 97.67(4) 6_564 6_564
Cl1 Nb1 Cl1 95.39(7) . 6_564
Cl2 Nb1 Se1 81.25(3) . 6_564
Cl2 Nb1 Se1 86.43(4) 6_564 6_564
Cl1 Nb1 Se1 90.47(3) . 6_564
Cl1 Nb1 Se1 172.62(3) 6_564 6_564
Cl2 Nb1 Se1 86.43(4) . .
Cl2 Nb1 Se1 81.25(3) 6_564 .
Cl1 Nb1 Se1 172.62(3) . .
Cl1 Nb1 Se1 90.47(3) 6_564 .
Se1 Nb1 Se1 84.07(3) 6_564 .
C1 Se1 C2 95.7(2) . .
C1 Se1 Nb1 104.40(15) . .
C2 Se1 Nb1 102.50(15) . .
Se1 C1 H1A 109.5 . .
Se1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Se1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 Se1 112.9(3) . .
C3 C2 H2A 109.0 . .
Se1 C2 H2A 109.0 . .
C3 C2 H2B 109.0 . .
Se1 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C2 C3 C2 115.1(6) . 6_564
C2 C3 H3A 108.5 . .
C2 C3 H3A 108.5 6_564 .
C2 C3 H3B 108.5 . .
C2 C3 H3B 108.5 6_564 .
H3A C3 H3B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl2 2.3386(12) .
Nb1 Cl2 2.3386(12) 6_564
Nb1 Cl1 2.3600(13) .
Nb1 Cl1 2.3601(13) 6_564
Nb1 Se1 2.7647(7) 6_564
Nb1 Se1 2.7648(7) .
Se1 C1 1.945(4) .
Se1 C2 1.963(5) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.527(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C2 1.527(6) 6_564
C3 H3A 0.9900 .
C3 H3B 0.9900 .
