#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:02:21 +0100 (vie 25 de mar de 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024386.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_7024386
loop_
_publ_author_name
'Jura, Marek'
'Levason, William'
'Ratnani, Raju'
'Reid, Gillian'
'Webster, Michael'
_publ_section_title
;
 Six- and eight-coordinate thio- and seleno-ether complexes of NbF5 and
 some comparisons with NbCl5 and NbBr5 adducts.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              883
_journal_page_last               891
_journal_paper_doi               10.1039/b916336k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C4 H10 Cl10 Nb2 Se2'
_chemical_formula_structural     '(C4 H10 Se2) (Cl5 Nb)2'
_chemical_formula_sum            'C4 H10 Cl10 Nb2 Se2'
_chemical_formula_weight         756.36
_chemical_name_common
(2,5-diselenahexane-Se,Se')bis(pentachloroniobium(V))
_chemical_name_systematic
;
(2,5-diselenahexane-Se,Se')bis(pentachloroniobium(V))
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-09-30
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.812(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9033(15)
_cell_length_b                   13.020(4)
_cell_length_c                   11.111(3)
_cell_measurement_reflns_used    33108
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     986.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17501
_diffrn_reflns_theta_full        27.70
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         4.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.184
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0599
_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)+(0.0000P)²+14.0255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                1599
_reflns_number_total             2267
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b916336k.txt
_cod_data_source_block           08mj29
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7024386
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb1 Nb 0.06348(11) 0.75799(6) 0.39968(7) 0.0223(2) Uani 1 1 d .
Se1 Se 0.41445(12) 0.64986(6) 0.39162(8) 0.0220(2) Uani 1 1 d .
Cl1 Cl -0.2108(3) 0.85611(18) 0.3969(2) 0.0315(5) Uani 1 1 d .
Cl2 Cl 0.2859(3) 0.88184(17) 0.4825(2) 0.0317(5) Uani 1 1 d .
Cl3 Cl 0.0756(3) 0.68695(18) 0.5921(2) 0.0313(5) Uani 1 1 d .
Cl4 Cl -0.0878(3) 0.60806(17) 0.3183(2) 0.0312(5) Uani 1 1 d .
Cl5 Cl 0.1243(3) 0.80167(18) 0.2052(2) 0.0297(5) Uani 1 1 d .
C1 C 0.3757(14) 0.5799(8) 0.2347(8) 0.031(2) Uani 1 1 d .
H1A H 0.4822 0.5306 0.2319 0.047 Uiso 1 1 calc R
H1B H 0.3754 0.6305 0.1693 0.047 Uiso 1 1 calc R
H1C H 0.2500 0.5435 0.2239 0.047 Uiso 1 1 calc R
C2 C 0.4015(12) 0.5279(6) 0.4925(8) 0.026(2) Uani 1 1 d .
H2A H 0.3706 0.5481 0.5733 0.031 Uiso 1 1 calc R
H2B H 0.2965 0.4816 0.4535 0.031 Uiso 1 1 calc R
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 0.0234(4) 0.0199(4) 0.0242(4) 0.0011(3) 0.0052(3) 0.0022(3)
Se1 0.0225(4) 0.0180(4) 0.0263(5) 0.0015(4) 0.0061(3) 0.0012(4)
Cl1 0.0305(12) 0.0306(12) 0.0337(13) 0.0000(10) 0.0058(10) 0.0109(10)
Cl2 0.0342(12) 0.0249(11) 0.0346(13) -0.0046(10) 0.0010(10) 0.0007(9)
Cl3 0.0345(12) 0.0347(12) 0.0264(12) 0.0076(10) 0.0101(9) 0.0093(10)
Cl4 0.0272(11) 0.0281(12) 0.0386(14) -0.0035(10) 0.0060(10) -0.0038(9)
Cl5 0.0340(12) 0.0283(12) 0.0276(12) 0.0071(10) 0.0078(9) 0.0038(9)
C1 0.039(5) 0.037(5) 0.017(5) 0.005(4) 0.006(4) 0.005(4)
C2 0.027(5) 0.021(4) 0.031(5) 0.000(4) 0.008(4) -0.003(4)
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
Cl1 Nb1 Cl2 96.54(9) .
Cl1 Nb1 Cl3 98.54(9) .
Cl2 Nb1 Cl3 89.05(9) .
Cl1 Nb1 Cl4 98.18(9) .
Cl2 Nb1 Cl4 165.28(9) .
Cl3 Nb1 Cl4 88.53(9) .
Cl1 Nb1 Cl5 96.76(9) .
Cl2 Nb1 Cl5 89.76(9) .
Cl3 Nb1 Cl5 164.69(9) .
Cl4 Nb1 Cl5 88.76(9) .
Cl1 Nb1 Se1 175.20(7) .
Cl2 Nb1 Se1 80.76(7) .
Cl3 Nb1 Se1 85.42(6) .
Cl4 Nb1 Se1 84.58(6) .
Cl5 Nb1 Se1 79.32(6) .
C2 Se1 C1 97.0(4) .
C2 Se1 Nb1 105.9(2) .
C1 Se1 Nb1 105.1(3) .
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 .
C2 C2 Se1 109.3(7) 3_666
C2 C2 H2A 109.8 3_666
Se1 C2 H2A 109.8 .
C2 C2 H2B 109.8 3_666
Se1 C2 H2B 109.8 .
H2A C2 H2B 108.3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl1 2.280(2) .
Nb1 Cl2 2.318(2) .
Nb1 Cl3 2.319(2) .
Nb1 Cl4 2.330(2) .
Nb1 Cl5 2.334(2) .
Nb1 Se1 2.8155(12) .
Se1 C2 1.954(9) .
Se1 C1 1.949(9) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C2 1.527(17) 3_666
C2 H2A 0.9900 .
C2 H2B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
Cl2 Nb1 Se1 C2 119.5(3) .
Cl3 Nb1 Se1 C2 29.7(3) .
Cl4 Nb1 Se1 C2 -59.2(3) .
Cl5 Nb1 Se1 C2 -149.0(3) .
Cl2 Nb1 Se1 C1 -138.5(3) .
Cl3 Nb1 Se1 C1 131.7(3) .
Cl4 Nb1 Se1 C1 42.7(3) .
Cl5 Nb1 Se1 C1 -47.0(3) .
C1 Se1 C2 C2 79.8(9) 3_666
Nb1 Se1 C2 C2 -172.2(8) 3_666
