#------------------------------------------------------------------------------
#$Date: 2019-11-23 19:00:29 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 234753 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/20/7702098.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_7702098
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         'C4 H12 Cl8 Nb2 Se2'
_chemical_formula_sum            'C4 H12 Cl8 Nb2 Se2'
_chemical_formula_weight         687.48
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_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            4
_cell_length_a                   10.4725(8)
_cell_length_b                   7.2592(5)
_cell_length_c                   22.5009(12)
_cell_measurement_reflns_used    2802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1190
_cell_measurement_theta_min      1.8230
_cell_volume                     1710.6(2)
_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 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  0.0657
_diffrn_reflns_av_unetI/netI     0.0362
_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       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5388
_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         25.988
_diffrn_reflns_theta_min         1.810
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    6.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70713
_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            Yellow
_exptl_crystal_density_diffrn    2.669
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0291
_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)+(0.0308P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                763
_reflns_number_total             888
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           2016_1604r1
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               7702098
_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   0.727
_shelx_estimated_absorpt_t_max   0.876
_shelx_res_file
; 
  
    2016_1604r1.res created by SHELXL-2014/7 
  
  
TITL 2016_1604r1 in Cmce 
CELL 0.71073  10.472544   7.259181  22.500915  90.0000  90.0000  90.0000 
ZERR    4.   0.000821   0.000540   0.001153   0.0000   0.0000   0.0000 
LATT 7 
SYMM -x,-y+1/2, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x,-y,-z 
SFAC C  H  Cl Se Nb 
UNIT 16 48 32 8 8 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
TEMP -173 
SIZE 0.05 0.03 0.02 
WGHT    0.030800 
FVAR       1.17365 
MOLE 1 
NB1   5    0.500000    0.035764    0.433160    10.50000    0.01462    0.01079 = 
         0.00661   -0.00034    0.00000    0.00000 
SE1   4    0.500000    0.352781    0.366104    10.50000    0.02183    0.01301 = 
         0.00896    0.00158    0.00000    0.00000 
CL1   3    0.282842    0.078187    0.429273    11.00000    0.01565    0.01638 = 
         0.01286    0.00016   -0.00065    0.00005 
CL2   3    0.500000   -0.131778    0.341963    10.50000    0.02299    0.01756 = 
         0.00815   -0.00339    0.00000    0.00000 
CL3   3    0.500000   -0.256806    0.483291    10.50000    0.01897    0.01062 = 
         0.00860   -0.00074    0.00000    0.00000 
C1    1    0.363015    0.318963    0.309633    11.00000    0.02172    0.02447 = 
         0.01336    0.00521   -0.00509    0.00104 
AFIX 137 
H1A   2    0.372400    0.407682    0.277097    11.00000   -1.50000 
H1B   2    0.280863    0.338590    0.329504    11.00000   -1.50000 
H1C   2    0.366299    0.193464    0.293655    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_1604r1 in Cmce 
REM R1 =  0.0291 for     763 Fo > 4sig(Fo)  and  0.0391 for all     888 data 
REM     44 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0311      0.0000 
  
REM Highest difference peak  0.649,  deepest hole -0.692,  1-sigma level  0.158 
Q1    1   0.5000 -0.2295  0.2716  10.50000  0.05    0.65 
Q2    1   0.3949  0.0534  0.4589  11.00000  0.05    0.64 
Q3    1   0.5000 -0.1200  0.4332  10.50000  0.05    0.58 
Q4    1   0.5000  0.4989  0.3701  10.50000  0.05    0.58 
Q5    1   0.4041  0.0565  0.4041  11.00000  0.05    0.58 
;
_shelx_res_checksum              28006
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, 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 0.5000 0.03576(7) 0.43316(2) 0.01067(17) Uani 1 2 d S T P
Se1 Se 0.5000 0.35278(8) 0.36610(2) 0.01460(18) Uani 1 2 d S T P
Cl1 Cl 0.28284(11) 0.07819(15) 0.42927(4) 0.0150(3) Uani 1 1 d . . .
Cl2 Cl 0.5000 -0.1318(2) 0.34196(5) 0.0162(3) Uani 1 2 d S T P
Cl3 Cl 0.5000 -0.25681(18) 0.48329(5) 0.0127(3) Uani 1 2 d S T P
C1 C 0.3630(5) 0.3190(6) 0.30963(17) 0.0199(10) Uani 1 1 d . . .
H1A H 0.3724 0.4077 0.2771 0.030 Uiso 1 1 calc R U .
H1B H 0.2809 0.3386 0.3295 0.030 Uiso 1 1 calc R U .
H1C H 0.3663 0.1935 0.2937 0.030 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 0.0146(3) 0.0108(3) 0.0066(3) -0.00034(19) 0.000 0.000
Se1 0.0218(4) 0.0130(3) 0.0090(3) 0.0016(2) 0.000 0.000
Cl1 0.0157(6) 0.0164(5) 0.0129(5) 0.0002(4) -0.0006(4) 0.0000(5)
Cl2 0.0230(9) 0.0176(8) 0.0082(6) -0.0034(5) 0.000 0.000
Cl3 0.0190(8) 0.0106(7) 0.0086(6) -0.0007(5) 0.000 0.000
C1 0.022(3) 0.024(2) 0.013(2) 0.0052(17) -0.0051(18) 0.001(2)
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
Cl1 Nb1 Cl1 163.98(6) 12_655 .
Cl1 Nb1 Cl2 92.04(3) 12_655 .
Cl1 Nb1 Cl2 92.04(3) . .
Cl1 Nb1 Cl3 97.83(3) 12_655 .
Cl1 Nb1 Cl3 97.83(3) . .
Cl2 Nb1 Cl3 87.32(5) . .
Cl1 Nb1 Cl3 86.67(3) 12_655 9_656
Cl1 Nb1 Cl3 86.67(3) . 9_656
Cl2 Nb1 Cl3 170.17(5) . 9_656
Cl3 Nb1 Cl3 102.51(4) . 9_656
Cl1 Nb1 Se1 82.36(3) 12_655 .
Cl1 Nb1 Se1 82.36(3) . .
Cl2 Nb1 Se1 87.40(4) . .
Cl3 Nb1 Se1 174.72(4) . .
Cl3 Nb1 Se1 82.77(4) 9_656 .
Cl1 Nb1 Nb1 93.46(2) 12_655 9_656
Cl1 Nb1 Nb1 93.46(2) . 9_656
Cl2 Nb1 Nb1 139.55(5) . 9_656
Cl3 Nb1 Nb1 52.23(3) . 9_656
Cl3 Nb1 Nb1 50.28(3) 9_656 9_656
Se1 Nb1 Nb1 133.05(3) . 9_656
C1 Se1 C1 95.9(3) 12_655 .
C1 Se1 Nb1 104.73(13) 12_655 .
C1 Se1 Nb1 104.73(13) . .
Nb1 Cl3 Nb1 77.49(4) . 9_656
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl1 2.2966(12) 12_655
Nb1 Cl1 2.2966(12) .
Nb1 Cl2 2.3854(13) .
Nb1 Cl3 2.4048(14) .
Nb1 Cl3 2.4715(13) 9_656
Nb1 Se1 2.7518(8) .
Nb1 Nb1 3.0524(9) 9_656
Se1 C1 1.932(4) 12_655
Se1 C1 1.932(4) .
Cl3 Nb1 2.4716(13) 9_656
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
