Composition Space of the (CuO,1/2Nb~2~O~5~)/(HF)~x~.pyridine/H~2~O System. Structure and Synthesis of [pyH^+^]~2-~[CuNb~2~(py)~4~O~2~F~10~]^2+^ and CuNb(py)~4~OF~5~
Paramasivan Halasyamani; Michael J. Willis; Charlotte L. Stern; Paul M. Lundquist; George K. Wong; Kenneth R. Poeppelmeier; Inorganic Chemistry 35 (1996) 1367–1371; doi:10.1021/ic951189w

data_4323785
_publ_contact_author
;
    Poeppelmeier, Kenneth
    Department of Chemistry
    Northwestern University
    Evanston, Illinois 60208-3113
    USA
;
_publ_contact_author_email       ' krp@nwu.edu'
_publ_contact_author_fax         ' (708) 491-7713'
_publ_contact_author_phone       '(708) 491-3505'
_publ_section_title
;
 Composition Space of the (CuO,1/2Nb~2~O~5~)/(HF)~x~.pyridine/H~2~O
 System. Structure and Synthesis of
 [pyH^+^]~2-~[CuNb~2~(py)~4~O~2~F~10~]^2+^ and CuNb(py)~4~OF~5~
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1367
_journal_page_last               1371
_journal_paper_doi               10.1021/ic951189w
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source        'hydro(solvato)thermal synthesis'
_chemical_formula_moiety         'C20 H20 Cu F5 N4 Nb O'
_chemical_formula_sum            'C20 H20 Cu F5 N4 Nb O'
_chemical_formula_weight         583.85
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Mon Jun 12 09:50:38 1995'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 97.77(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.561(3)
_cell_length_b                   13.546(6)
_cell_length_c                   16.103(4)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    173.2
_cell_measurement_theta_max      16.7
_cell_measurement_theta_min      15.1
_cell_volume                     2282.5(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      173.2
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_orient_matrix_UB_11      -0.00996
_diffrn_orient_matrix_UB_12      -0.00200
_diffrn_orient_matrix_UB_13      0.06086
_diffrn_orient_matrix_UB_21      0.08669
_diffrn_orient_matrix_UB_22      -0.03044
_diffrn_orient_matrix_UB_23      0.01289
_diffrn_orient_matrix_UB_31      0.03896
_diffrn_orient_matrix_UB_32      0.06722
_diffrn_orient_matrix_UB_33      0.00765
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  18.10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5748
_diffrn_reflns_theta_max         27.46
_diffrn_standards_decay_%        -2.10
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      1.69(1)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164.00
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.78
_refine_ls_extinction_coef       1.63663
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   0.757
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2148
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0264
_refine_ls_shift/esd_max         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0377
_reflns_number_observed          2148
_reflns_number_total             2724
_reflns_observed_criterion       3.00
_cod_data_source_file            ic951189w_1.cif
_cod_data_source_block           CuNbmono
_cod_original_cell_volume        2282(1)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C20 H20 Cu F5 N4 Nb O '
_cod_database_code               4323785