[pyH]2[Cu(py)4(MX6)2] (MX6= ZrF62-, NbOF52-, MoO2F42-; py = Pyridine): Rarely Observed Ordering of Metal Oxide Fluoride Anions
Kevin R. Heier; Alexander J. Norquist; Christopher G. Wilson; Charlotte L. Stern; Kenneth R. Poeppelmeier; Inorganic Chemistry 37 (1998) 76–80; doi:10.1021/ic970951m

data_4322595
_publ_contact_author
;
Poeppelmeier, Kenneth R.
Department of Chemistry
Northwestern University
Evanston IL 60208-3313
;
_publ_contact_author_email       'krp@nwu.edu '
_publ_contact_author_fax         '847 491-7716 '
_publ_contact_author_phone       '847 491-3505 '
_publ_section_title
;
 [pyH]2[Cu(py)4(MX6)2] (MX6= ZrF62-, NbOF52-, MoO2F42-; py = Pyridine):
 Rarely Observed Ordering of Metal Oxide Fluoride Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              76
_journal_page_last               80
_journal_paper_doi               10.1021/ic970951m
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        'hydro(solvato)thermal synthesis'
_chemical_formula_moiety         'C30 H32 Cu F12 N6 Zr2 '
_chemical_formula_sum            'C30 H32 Cu F12 N6 Zr2'
_chemical_formula_weight         950.59
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      139
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_audit_creation_date             'Tue Jun 24 09:21:27 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.047(1)
_cell_length_b                   11.047(1)
_cell_length_c                   16.763(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    426.4
_cell_measurement_theta_max      13.6
_cell_measurement_theta_min      11.4
_cell_volume                     2045.7(5)
_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      426.4
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega/theta scans'
_diffrn_orient_matrix_UB_11      0.06480
_diffrn_orient_matrix_UB_12      0.02433
_diffrn_orient_matrix_UB_13      -0.03842
_diffrn_orient_matrix_UB_21      -0.04565
_diffrn_orient_matrix_UB_22      -0.03964
_diffrn_orient_matrix_UB_23      -0.04438
_diffrn_orient_matrix_UB_31      -0.04363
_diffrn_orient_matrix_UB_32      0.07771
_diffrn_orient_matrix_UB_33      -0.01061
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  .0201
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            1678
_diffrn_reflns_theta_max         29.96
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa_analytical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      1.55(1)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       cube
_exptl_crystal_F_000             942.00
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.19
_refine_ls_extinction_coef       2.58224
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.204
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         929
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0314
_refine_ls_shift/esd_max         11.1100
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0342
_reflns_number_observed          929
_reflns_number_total             1134
_reflns_observed_criterion       3.00
_cod_data_source_file            ic970951m_1.cif
_cod_data_source_block           Cu(py)4_[ZrF6]2_*_2Hpy
_cod_original_cell_volume        2045.6(4)
_cod_original_sg_symbol_H-M      'I 4/m m m '
_cod_original_formula_sum        'C30 H32 Cu F12 N6 Zr2 '
_cod_database_code               4322595