#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:55:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179431 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/28/4332888.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332888
loop_
_publ_author_name
'Piedra-Garza, Luis Fernando'
'Köckerling, Martin'
_publ_section_title
;
 Straightforward Synthesis and Structure of a New Starting Material for
 Niobium Cluster Phases:  [Nb6Cli12(CH3OH)a4Cla2]·6CH3OH
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8829
_journal_page_last               8831
_journal_paper_doi               10.1021/ic061020q
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C4 H16 Nb6 Cl14, 6 C H4 O'
_chemical_formula_sum            'C10 H40 Cl14 Nb6 O10'
_chemical_formula_weight         1374.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'ct.exe (M. Köckerling, 1996)'
_cell_angle_alpha                67.530(7)
_cell_angle_beta                 89.104(7)
_cell_angle_gamma                65.392(6)
_cell_formula_units_Z            1
_cell_length_a                   9.9648(8)
_cell_length_b                   10.0443(9)
_cell_length_c                   12.0320(11)
_cell_measurement_reflns_used    19272
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.3
_cell_volume                     996.91(17)
_computing_cell_refinement       'X-AREA (Stoe & Cie GmbH)'
_computing_data_collection       'X-AREA (Stoe & Cie GmbH)'
_computing_data_reduction        'STOE XRED32 1.28b (Stoe & Cie GmbH)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19219
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    2.642
_exptl_absorpt_correction_T_max  0.4309
_exptl_absorpt_correction_T_min  0.3564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 r.h. blessing, acta cryst. (1995), a51, 33-38
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_description       irregular
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.0003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         5358
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0240P)²+6.2247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                4192
_reflns_number_total             5358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061020qsup1.cif
_cod_data_source_block           Nb6Cl14(MeOH)4*6MeOH
_cod_original_cell_volume        996.91(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332888
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb1 Nb 0.61692(6) 0.62522(6) 0.50452(5) 0.02372(13) Uani 1 1 d .
Nb2 Nb 0.57122(6) 0.49190(6) 0.34076(5) 0.02404(13) Uani 1 1 d .
Nb3 Nb 0.68857(6) 0.28394(6) 0.59954(5) 0.02402(13) Uani 1 1 d .
Cl1 Cl 0.9214(2) 0.0163(2) 0.72189(17) 0.0406(4) Uani 1 1 d .
Cl2 Cl 0.7219(2) 0.6404(2) 0.31612(16) 0.0344(4) Uani 1 1 d .
Cl3 Cl 0.5548(2) 0.6565(2) 0.69508(15) 0.0342(3) Uani 1 1 d .
Cl4 Cl 0.3652(2) 0.7417(2) 0.19485(14) 0.0356(4) Uani 1 1 d .
Cl5 Cl 0.42043(19) 0.89903(17) 0.39087(15) 0.0322(3) Uani 1 1 d .
Cl6 Cl 0.85721(18) 0.39854(19) 0.62001(16) 0.0347(4) Uani 1 1 d .
Cl7 Cl 0.80318(19) 0.24082(19) 0.42629(16) 0.0333(3) Uani 1 1 d .
O1 O 0.7433(6) 0.7611(6) 0.5127(5) 0.0411(12) Uani 1 1 d D
H1 H 0.789(10) 0.722(11) 0.585(3) 0.062 Uiso 1 1 d D
C1 C 0.7692(10) 0.8849(10) 0.4190(8) 0.049(2) Uani 1 1 d .
H1A H 0.8557 0.8890 0.4486 0.074 Uiso 1 1 calc R
H1B H 0.6834 0.9868 0.3974 0.074 Uiso 1 1 calc R
H1C H 0.7859 0.8614 0.3483 0.074 Uiso 1 1 calc R
O2 O 0.6500(7) 0.4879(6) 0.1636(5) 0.0410(12) Uani 1 1 d D
H2 H 0.638(11) 0.581(5) 0.116(7) 0.061 Uiso 1 1 d D
C2 C 0.6991(14) 0.3716(13) 0.1169(9) 0.067(3) Uani 1 1 d .
H2A H 0.7620 0.3934 0.0582 0.101 Uiso 1 1 calc R
H2B H 0.6142 0.3738 0.0782 0.101 Uiso 1 1 calc R
H2C H 0.7549 0.2674 0.1821 0.101 Uiso 1 1 calc R
O3 O 0.8594(11) 0.7285(9) 0.7180(8) 0.090(3) Uani 1 1 d D
H3 H 0.903(14) 0.786(14) 0.715(14) 0.135 Uiso 1 1 d D
C3 C 0.9402(13) 0.5873(13) 0.8165(10) 0.068(3) Uani 1 1 d .
H3A H 0.9665 0.6094 0.8818 0.102 Uiso 1 1 calc R
H3B H 1.0298 0.5238 0.7945 0.102 Uiso 1 1 calc R
H3C H 0.8813 0.5294 0.8428 0.102 Uiso 1 1 calc R
O4 O 0.6452(10) 0.7457(11) -0.0014(8) 0.081(2) Uani 1 1 d D
H4 H 0.731(7) 0.743(18) 0.004(14) 0.122 Uiso 1 1 d D
C4 C 0.5266(17) 0.8674(15) -0.0891(10) 0.087(4) Uani 1 1 d .
H4A H 0.4357 0.8836 -0.0560 0.130 Uiso 1 1 calc R
H4B H 0.5219 0.8399 -0.1567 0.130 Uiso 1 1 calc R
H4C H 0.5386 0.9643 -0.1166 0.130 Uiso 1 1 calc R
O5 O 0.8679(12) 0.8338(12) -0.0138(7) 0.096(3) Uani 1 1 d D
H5 H 0.871(19) 0.887(17) -0.087(5) 0.145 Uiso 1 1 d D
C5 C 0.9121(17) 0.8695(18) 0.0771(11) 0.095(4) Uani 1 1 d .
H5AA H 0.8636 0.9837 0.0530 0.142 Uiso 1 1 calc R
H5BA H 1.0188 0.8319 0.0882 0.142 Uiso 1 1 calc R
H5CA H 0.8842 0.8174 0.1523 0.142 Uiso 1 1 calc R
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'
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 Cl5 81.13(15) . .
O1 Nb1 Cl6 80.73(15) . .
Cl5 Nb1 Cl6 161.86(6) . .
O1 Nb1 Cl2 82.09(15) . .
Cl5 Nb1 Cl2 88.78(6) . .
Cl6 Nb1 Cl2 88.48(6) . .
O1 Nb1 Cl3 80.18(15) . .
Cl5 Nb1 Cl3 88.44(6) . .
Cl6 Nb1 Cl3 88.73(6) . .
Cl2 Nb1 Cl3 162.27(6) . .
O1 Nb1 Nb2 134.00(15) . 2_666
Cl5 Nb1 Nb2 96.01(4) . 2_666
Cl6 Nb1 Nb2 96.75(5) . 2_666
Cl2 Nb1 Nb2 143.91(5) . 2_666
Cl3 Nb1 Nb2 53.82(4) . 2_666
O1 Nb1 Nb2 136.05(15) . .
Cl5 Nb1 Nb2 96.69(5) . .
Cl6 Nb1 Nb2 96.16(5) . .
Cl2 Nb1 Nb2 53.96(4) . .
Cl3 Nb1 Nb2 143.77(5) . .
Nb2 Nb1 Nb2 89.95(2) 2_666 .
O1 Nb1 Nb3 134.31(14) . .
Cl5 Nb1 Nb3 144.55(5) . .
Cl6 Nb1 Nb3 53.59(4) . .
Cl2 Nb1 Nb3 96.26(4) . .
Cl3 Nb1 Nb3 96.14(4) . .
Nb2 Nb1 Nb3 60.477(19) 2_666 .
Nb2 Nb1 Nb3 60.14(2) . .
O1 Nb1 Nb3 134.70(14) . 2_666
Cl5 Nb1 Nb3 53.57(4) . 2_666
Cl6 Nb1 Nb3 144.57(5) . 2_666
Cl2 Nb1 Nb3 96.20(5) . 2_666
Cl3 Nb1 Nb3 96.21(5) . 2_666
Nb2 Nb1 Nb3 60.10(2) 2_666 2_666
Nb2 Nb1 Nb3 60.36(2) . 2_666
Nb3 Nb1 Nb3 90.97(2) . 2_666
O2 Nb2 Cl7 81.38(15) . .
O2 Nb2 Cl4 80.57(15) . .
Cl7 Nb2 Cl4 161.95(6) . .
O2 Nb2 Cl3 81.93(15) . 2_666
Cl7 Nb2 Cl3 89.15(6) . 2_666
Cl4 Nb2 Cl3 88.16(6) . 2_666
O2 Nb2 Cl2 80.23(15) . .
Cl7 Nb2 Cl2 88.59(6) . .
Cl4 Nb2 Cl2 88.52(6) . .
Cl3 Nb2 Cl2 162.16(6) 2_666 .
O2 Nb2 Nb1 135.95(15) . 2_666
Cl7 Nb2 Nb1 96.74(5) . 2_666
Cl4 Nb2 Nb1 96.09(5) . 2_666
Cl3 Nb2 Nb1 54.02(4) 2_666 2_666
Cl2 Nb2 Nb1 143.82(5) . 2_666
O2 Nb2 Nb1 134.00(15) . .
Cl7 Nb2 Nb1 96.29(5) . .
Cl4 Nb2 Nb1 96.33(5) . .
Cl3 Nb2 Nb1 144.06(5) 2_666 .
Cl2 Nb2 Nb1 53.77(4) . .
Nb1 Nb2 Nb1 90.05(2) 2_666 .
O2 Nb2 Nb3 134.98(14) . .
Cl7 Nb2 Nb3 53.60(4) . .
Cl4 Nb2 Nb3 144.45(5) . .
Cl3 Nb2 Nb3 96.63(5) 2_666 .
Cl2 Nb2 Nb3 96.24(5) . .
Nb1 Nb2 Nb3 60.48(2) 2_666 .
Nb1 Nb2 Nb3 60.29(2) . .
O2 Nb2 Nb3 133.99(14) . 2_666
Cl7 Nb2 Nb3 144.62(5) . 2_666
Cl4 Nb2 Nb3 53.43(4) . 2_666
Cl3 Nb2 Nb3 96.05(5) 2_666 2_666
Cl2 Nb2 Nb3 96.02(4) . 2_666
Nb1 Nb2 Nb3 60.17(2) 2_666 2_666
Nb1 Nb2 Nb3 60.29(2) . 2_666
Nb3 Nb2 Nb3 91.02(2) . 2_666
Cl7 Nb3 Cl6 88.64(6) . .
Cl7 Nb3 Cl4 164.34(6) . 2_666
Cl6 Nb3 Cl4 89.02(6) . 2_666
Cl7 Nb3 Cl5 88.87(6) . 2_666
Cl6 Nb3 Cl5 164.65(6) . 2_666
Cl4 Nb3 Cl5 89.30(6) 2_666 2_666
Cl7 Nb3 Cl1 81.87(6) . .
Cl6 Nb3 Cl1 82.40(6) . .
Cl4 Nb3 Cl1 82.47(6) 2_666 .
Cl5 Nb3 Cl1 82.24(6) 2_666 .
Cl7 Nb3 Nb2 53.33(4) . .
Cl6 Nb3 Nb2 95.48(5) . .
Cl4 Nb3 Nb2 142.34(5) 2_666 .
Cl5 Nb3 Nb2 95.16(5) 2_666 .
Cl1 Nb3 Nb2 135.20(5) . .
Cl7 Nb3 Nb1 95.56(4) . .
Cl6 Nb3 Nb1 53.23(4) . .
Cl4 Nb3 Nb1 95.43(5) 2_666 .
Cl5 Nb3 Nb1 142.12(5) 2_666 .
Cl1 Nb3 Nb1 135.63(5) . .
Nb2 Nb3 Nb1 59.57(2) . .
Cl7 Nb3 Nb1 95.75(5) . 2_666
Cl6 Nb3 Nb1 142.25(4) . 2_666
Cl4 Nb3 Nb1 95.57(5) 2_666 2_666
Cl5 Nb3 Nb1 53.10(4) 2_666 2_666
Cl1 Nb3 Nb1 135.34(5) . 2_666
Nb2 Nb3 Nb1 59.42(2) . 2_666
Nb1 Nb3 Nb1 89.03(2) . 2_666
Cl7 Nb3 Nb2 142.31(5) . 2_666
Cl6 Nb3 Nb2 95.64(5) . 2_666
Cl4 Nb3 Nb2 53.36(4) 2_666 2_666
Cl5 Nb3 Nb2 95.58(4) 2_666 2_666
Cl1 Nb3 Nb2 135.82(5) . 2_666
Nb2 Nb3 Nb2 88.98(2) . 2_666
Nb1 Nb3 Nb2 59.353(19) . 2_666
Nb1 Nb3 Nb2 59.35(2) 2_666 2_666
Nb1 Cl2 Nb2 72.27(5) . .
Nb2 Cl3 Nb1 72.17(5) 2_666 .
Nb2 Cl4 Nb3 73.21(5) . 2_666
Nb1 Cl5 Nb3 73.33(4) . 2_666
Nb1 Cl6 Nb3 73.18(5) . .
Nb2 Cl7 Nb3 73.07(5) . .
C1 O1 Nb1 131.9(5) . .
C2 O2 Nb2 133.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O1 2.235(5) .
Nb1 Cl5 2.4478(16) .
Nb1 Cl6 2.4482(18) .
Nb1 Cl2 2.4597(17) .
Nb1 Cl3 2.4662(17) .
Nb1 Nb2 2.9013(8) 2_666
Nb1 Nb2 2.9044(8) .
Nb1 Nb3 2.9256(8) .
Nb1 Nb3 2.9325(9) 2_666
Nb2 O2 2.269(5) .
Nb2 Cl7 2.4490(17) .
Nb2 Cl4 2.4594(18) .
Nb2 Cl3 2.4600(18) 2_666
Nb2 Cl2 2.4656(17) .
Nb2 Nb1 2.9013(8) 2_666
Nb2 Nb3 2.9212(9) .
Nb2 Nb3 2.9345(8) 2_666
Nb3 Cl7 2.4578(17) .
Nb3 Cl6 2.4598(18) .
Nb3 Cl4 2.4617(17) 2_666
Nb3 Cl5 2.4631(17) 2_666
Nb3 Cl1 2.5814(18) .
Nb3 Nb1 2.9325(9) 2_666
Nb3 Nb2 2.9345(8) 2_666
Cl3 Nb2 2.4600(18) 2_666
Cl4 Nb3 2.4617(17) 2_666
Cl5 Nb3 2.4631(17) 2_666
O1 C1 1.439(9) .
O2 C2 1.392(10) .
O3 C3 1.363(12) .
O4 C4 1.362(15) .
O5 C5 1.401(15) .
