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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/7/70/21/7702105.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_7702105
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         'C12 H18 Cl4 Nb S2'
_chemical_formula_sum            'C12 H18 Cl4 Nb S2'
_chemical_formula_weight         461.09
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                   19.407(9)
_cell_length_b                   12.502(6)
_cell_length_c                   7.084(3)
_cell_measurement_reflns_used    3061
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1718.8(14)
_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 0.996
_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  0.0746
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8916
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.061
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.452
_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            Yellow
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0328
_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)+(0.0318P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1401
_reflns_number_total             1768
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           0602r3
_cod_original_cell_volume        1718.6(13)
_cod_database_code               7702105
_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   0.936
_shelx_estimated_absorpt_t_max   0.958
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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
_atom_site_refinement_flags_occupancy
Nb1 Nb 0.11126(2) 0.2500 0.31388(6) 0.01693(13) Uani 1 2 d S T P
Cl1 Cl 0.22023(6) 0.2500 0.17556(17) 0.0231(3) Uani 1 2 d S T P
Cl2 Cl 0.03064(6) 0.2500 0.55702(17) 0.0217(3) Uani 1 2 d S T P
Cl3 Cl 0.06241(4) 0.11320(7) 0.12325(12) 0.0234(2) Uani 1 1 d . . .
S1 S 0.16510(4) 0.08570(6) 0.49928(12) 0.0184(2) Uani 1 1 d . . .
C1 C 0.11977(18) -0.1055(3) 0.6556(5) 0.0248(8) Uani 1 1 d . . .
H1A H 0.1444 -0.1433 0.5548 0.037 Uiso 1 1 calc R U .
H1B H 0.0803 -0.1485 0.6966 0.037 Uiso 1 1 calc R U .
H1C H 0.1509 -0.0941 0.7626 0.037 Uiso 1 1 calc R U .
C2 C 0.09468(17) 0.0014(3) 0.5827(5) 0.0226(8) Uani 1 1 d . . .
H2A H 0.0698 0.0391 0.6849 0.027 Uiso 1 1 calc R U .
H2B H 0.0618 -0.0107 0.4779 0.027 Uiso 1 1 calc R U .
C3 C 0.20140(18) 0.1286(3) 0.7252(5) 0.0213(7) Uani 1 1 d . . .
H3A H 0.1671 0.1720 0.7948 0.026 Uiso 1 1 calc R U .
H3B H 0.2128 0.0652 0.8029 0.026 Uiso 1 1 calc R U .
C4 C 0.26551(17) 0.1938(3) 0.6913(5) 0.0203(7) Uani 1 1 d . . .
C5 C 0.32738(18) 0.1401(3) 0.6593(5) 0.0224(7) Uani 1 1 d . . .
H5 H 0.3276 0.0641 0.6580 0.027 Uiso 1 1 calc R U .
C6 C 0.38843(18) 0.1946(3) 0.6292(5) 0.0249(8) Uani 1 1 d . . .
H6 H 0.4301 0.1564 0.6087 0.030 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'
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 Cl1 157.11(5) . .
Cl2 Nb1 Cl3 98.77(4) . 7_565
Cl1 Nb1 Cl3 97.07(4) . 7_565
Cl2 Nb1 Cl3 98.77(4) . .
Cl1 Nb1 Cl3 97.07(4) . .
Cl3 Nb1 Cl3 92.05(5) 7_565 .
Cl2 Nb1 S1 84.17(4) . .
Cl1 Nb1 S1 81.41(3) . .
Cl3 Nb1 S1 174.76(3) 7_565 .
Cl3 Nb1 S1 83.18(4) . .
Cl2 Nb1 S1 84.17(4) . 7_565
Cl1 Nb1 S1 81.41(3) . 7_565
Cl3 Nb1 S1 83.18(4) 7_565 7_565
Cl3 Nb1 S1 174.76(3) . 7_565
S1 Nb1 S1 101.50(5) . 7_565
C2 S1 C3 100.05(17) . .
C2 S1 Nb1 108.22(11) . .
C3 S1 Nb1 110.98(11) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C1 C2 S1 112.3(2) . .
C1 C2 H2A 109.1 . .
S1 C2 H2A 109.1 . .
C1 C2 H2B 109.1 . .
S1 C2 H2B 109.1 . .
H2A C2 H2B 107.9 . .
C4 C3 S1 109.7(2) . .
C4 C3 H3A 109.7 . .
S1 C3 H3A 109.7 . .
C4 C3 H3B 109.7 . .
S1 C3 H3B 109.7 . .
H3A C3 H3B 108.2 . .
C5 C4 C4 118.8(2) . 7_565
C5 C4 C3 118.5(3) . .
C4 C4 C3 122.75(18) 7_565 .
C6 C5 C4 121.7(3) . .
C6 C5 H5 119.2 . .
C4 C5 H5 119.2 . .
C6 C6 C5 119.5(2) 7_565 .
C6 C6 H6 120.2 7_565 .
C5 C6 H6 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl2 2.3269(14) .
Nb1 Cl1 2.3308(15) .
Nb1 Cl3 2.3763(11) 7_565
Nb1 Cl3 2.3763(11) .
Nb1 S1 2.6524(11) .
Nb1 S1 2.6524(11) 7_565
S1 C2 1.824(3) .
S1 C3 1.829(3) .
C1 C2 1.514(5) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.507(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.394(5) .
C4 C4 1.406(6) 7_565
C5 C6 1.384(5) .
C5 H5 0.9500 .
C6 C6 1.384(7) 7_565
C6 H6 0.9500 .
