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_4323786
_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         'C30 H32 Cu F10 N6 Nb2 O2'
_chemical_formula_sum            'C30 H32 Cu F10 N6 Nb2 O2'
_chemical_formula_weight         947.96
_space_group_IT_number           98
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      98
_symmetry_space_group_name_Hall  'I 4bw 2bw'
_symmetry_space_group_name_H-M   'I 41 2 2'
_audit_creation_date             'Fri Apr 21 17:16:01 1995'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.408(3)
_cell_length_b                   11.408(3)
_cell_length_c                   30.36(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      12.2
_cell_volume                     3951(2)
_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    SHELXS-86
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega/theta scans'
_diffrn_orient_matrix_UB_11      0.04810
_diffrn_orient_matrix_UB_12      0.04498
_diffrn_orient_matrix_UB_13      -0.02176
_diffrn_orient_matrix_UB_21      -0.07305
_diffrn_orient_matrix_UB_22      0.03513
_diffrn_orient_matrix_UB_23      -0.01251
_diffrn_orient_matrix_UB_31      0.00617
_diffrn_orient_matrix_UB_32      0.06652
_diffrn_orient_matrix_UB_33      0.02133
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.95
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1962
_diffrn_reflns_theta_max         24.94
_diffrn_standards_decay_%        -1.39
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa_analytical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      1.59(1)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1884.00
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.85
_refine_ls_extinction_coef       0.31440
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.424
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         872
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         0.0160
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0440
_reflns_number_observed          872
_reflns_number_total             1094
_reflns_observed_criterion       3.00
_cod_data_source_file            ic951189w_2.cif
_cod_data_source_block           CuNbtet
_cod_database_code               4323786