Straightforward Synthesis and Structure of a New Starting Material for Niobium Cluster Phases: [Nb6Cli12(CH3OH)a4Cla2]·6CH3OH
Piedra-Garza, Luis Fernando; Köckerling, Martin; Inorganic Chemistry 45 (2006) 8829–8831; doi:10.1021/ic061020q

data_4332888
_publ_section_title
;
 Straightforward Synthesis and Structure of a New Starting Material for
 Niobium Cluster Phases:&#x00A0; [Nb6Cli12(CH3OH)a4Cla2]&#x00B7;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. K\"ockerling, 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       '\w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0240P)^2^+6.2247P] where P=(Fo^2^+2Fc^2^)/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