Octahedral Niobium Chloride Clusters as Building Blocks of Templated Prussian Blue Framework Analogues
Bangbo Yan; Huajun Zhou; Abdessadek Lachgar; Inorganic Chemistry 42 (2003) 8818–8822; doi:10.1021/ic034514l

data_4312767
_publ_contact_author_address
;
    Department of Chemistry, 
    Wake Forest University, 
    Winston-Salem, NC 27109
;
_publ_contact_author_email       lachgar@wfu.edu
_publ_contact_author_fax         '(336) 758-4656'
_publ_contact_author_name        'Abdessadek Lachgar'
_publ_contact_author_phone       '(336) 758-4676'
_publ_section_title
;
 Octahedral Niobium Chloride Clusters as Building Blocks of Templated
 Prussian Blue Framework Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8818
_journal_page_last               8822
_journal_paper_doi               10.1021/ic034514l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C20 H48 Cl12 K2 N8 Nb6 O6'
_chemical_formula_weight         1557.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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_method           SHELXTL-PC
_cell_angle_alpha                90.00
_cell_angle_beta                 105.262(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6404(13)
_cell_length_b                   14.385(2)
_cell_length_c                   16.494(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.77
_cell_measurement_theta_min      3.06
_cell_volume                     2664.5(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL-PC'
_computing_molecular_graphics    'Bruker SHELXTL-PC'
_computing_publication_material  'Bruker SHELXTL-PC'
_computing_structure_refinement  'Bruker SHELXTL-PC'
_computing_structure_solution    'Bruker SHELXTL-PC'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8345
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 397
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.7327
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular parallelepiped'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.00012(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL-PC
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0799P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                4485
_reflns_number_total             6682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034514lsi20030514_053953_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312767