#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:00:29 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/21/7702106.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_7702106
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         'C2 H6 Cl3 Nb O S'
_chemical_formula_sum            'C2 H6 Cl3 Nb O S'
_chemical_formula_weight         277.39
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 97.049(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3522(11)
_cell_length_b                   14.9254(7)
_cell_length_c                   7.9099(5)
_cell_measurement_reflns_used    4683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3690
_cell_measurement_theta_min      2.7040
_cell_volume                     1681.59(19)
_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 0.997
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13175
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.729
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59489
_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            Green
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0409
_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)+(0.0261P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2339
_reflns_number_total             3295
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           2015_0801ypc1
_cod_original_cell_volume        1681.6(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7702106
_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   0.667
_shelx_estimated_absorpt_t_max   0.941
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Nb1 Nb 0.90516(4) 0.25568(3) 0.56478(6) 0.01056(14) Uani 1 1 d . .
Nb2 Nb 0.37140(4) 0.24387(3) 0.35383(6) 0.01186(14) Uani 1 1 d . .
Cl1 Cl 1.02463(11) 0.15180(9) 0.54159(16) 0.0183(3) Uani 1 1 d . .
Cl2 Cl 0.99207(11) 0.38595(8) 0.56539(17) 0.0190(3) Uani 1 1 d . .
Cl3 Cl 0.75707(10) 0.32452(8) 0.49949(17) 0.0174(3) Uani 1 1 d . .
Cl4 Cl 0.21247(10) 0.21076(9) 0.28465(17) 0.0178(3) Uani 1 1 d . .
Cl5 Cl 0.42600(11) 0.09633(9) 0.36047(18) 0.0220(4) Uani 1 1 d . .
Cl6 Cl 0.51557(10) 0.31407(9) 0.33274(17) 0.0205(3) Uani 1 1 d . .
O1 O 0.8993(3) 0.2434(2) 0.7825(4) 0.0136(8) Uani 1 1 d . .
O2 O 0.3695(3) 0.2618(2) 0.5715(4) 0.0144(9) Uani 1 1 d . .
S1 S 0.80478(11) 0.10642(9) 0.48076(17) 0.0165(3) Uani 1 1 d . .
S2 S 0.30315(11) 0.40740(9) 0.26899(17) 0.0166(3) Uani 1 1 d . .
C1 C 0.8416(4) 0.0281(3) 0.6489(7) 0.0229(15) Uani 1 1 d . .
H1A H 0.8314 0.0543 0.7587 0.034 Uiso 1 1 calc R U
H1B H 0.9084 0.0146 0.6491 0.034 Uiso 1 1 calc R U
H1C H 0.8050 -0.0272 0.6303 0.034 Uiso 1 1 calc R U
C2 C 0.6850(4) 0.1219(4) 0.5166(8) 0.0274(16) Uani 1 1 d . .
H2A H 0.6524 0.0641 0.5075 0.041 Uiso 1 1 calc R U
H2B H 0.6541 0.1633 0.4312 0.041 Uiso 1 1 calc R U
H2C H 0.6828 0.1468 0.6307 0.041 Uiso 1 1 calc R U
C3 C 0.3846(4) 0.4883(4) 0.3695(8) 0.0256(15) Uani 1 1 d . .
H3A H 0.3562 0.5481 0.3594 0.038 Uiso 1 1 calc R U
H3B H 0.4419 0.4880 0.3136 0.038 Uiso 1 1 calc R U
H3C H 0.4003 0.4731 0.4901 0.038 Uiso 1 1 calc R U
C4 C 0.2072(4) 0.4260(4) 0.3908(7) 0.0215(15) Uani 1 1 d . .
H4A H 0.2283 0.4155 0.5118 0.032 Uiso 1 1 calc R U
H4B H 0.1558 0.3847 0.3523 0.032 Uiso 1 1 calc R U
H4C H 0.1851 0.4879 0.3748 0.032 Uiso 1 1 calc R U
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'
O O 0.0106 0.0060 '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
O1 Nb1 O1 172.48(15) . 4_565
O1 Nb1 Cl2 100.26(12) . .
O1 Nb1 Cl2 87.18(9) 4_565 .
O1 Nb1 Cl1 97.63(12) . .
O1 Nb1 Cl1 82.13(10) 4_565 .
Cl2 Nb1 Cl1 99.06(5) . .
O1 Nb1 Cl3 96.34(13) . .
O1 Nb1 Cl3 81.68(10) 4_565 .
Cl2 Nb1 Cl3 96.06(5) . .
Cl1 Nb1 Cl3 157.21(5) . .
O1 Nb1 S1 93.86(12) . .
O1 Nb1 S1 78.70(9) 4_565 .
Cl2 Nb1 S1 165.88(5) . .
Cl1 Nb1 S1 78.87(5) . .
Cl3 Nb1 S1 82.30(5) . .
O2 Nb2 O2 173.16(7) . 4_565
O2 Nb2 Cl4 97.51(13) . .
O2 Nb2 Cl4 82.28(10) 4_565 .
O2 Nb2 Cl5 99.70(12) . .
O2 Nb2 Cl5 87.10(9) 4_565 .
Cl4 Nb2 Cl5 96.97(6) . .
O2 Nb2 Cl6 97.02(12) . .
O2 Nb2 Cl6 81.28(10) 4_565 .
Cl4 Nb2 Cl6 157.61(5) . .
Cl5 Nb2 Cl6 97.26(6) . .
O2 Nb2 S2 93.29(12) . .
O2 Nb2 S2 79.94(9) 4_565 .
Cl4 Nb2 S2 79.49(5) . .
Cl5 Nb2 S2 166.90(5) . .
Cl6 Nb2 S2 82.76(5) . .
Nb1 O1 Nb1 171.9(2) . 4_566
Nb2 O2 Nb2 168.86(19) . 4_566
C2 S1 C1 99.6(3) . .
C2 S1 Nb1 110.44(19) . .
C1 S1 Nb1 104.8(2) . .
C4 S2 C3 99.2(3) . .
C4 S2 Nb2 106.65(18) . .
C3 S2 Nb2 107.6(2) . .
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 . .
S1 C2 H2A 109.5 . .
S1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
S1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
S2 C3 H3A 109.5 . .
S2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
S2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
S2 C4 H4A 109.5 . .
S2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
S2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O1 1.744(3) .
Nb1 O1 2.224(3) 4_565
Nb1 Cl2 2.3097(14) .
Nb1 Cl1 2.3355(14) .
Nb1 Cl3 2.3602(15) .
Nb1 S1 2.6917(15) .
Nb2 O2 1.746(3) .
Nb2 O2 2.232(3) 4_565
Nb2 Cl4 2.3324(16) .
Nb2 Cl5 2.3357(14) .
Nb2 Cl6 2.3435(15) .
Nb2 S2 2.6844(14) .
O1 Nb1 2.224(3) 4_566
O2 Nb2 2.232(3) 4_566
S1 C2 1.792(6) .
S1 C1 1.800(5) .
S2 C4 1.797(5) .
S2 C3 1.797(6) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
