Syntheses and Structural Characterization of a Series of One-Dimensional Fluorotitanophosphates (NH4)xK4 - x[Ti2PO4F9] (x= 0, 0.70, 1.00, 1.25)
Yang, Sihai; Li, Guobao; Li, Lei; Tian, Shujian; Liao, Fuhui; Xiong, Ming; Lin, Jianhua; Inorganic Chemistry 46 (2007) 11431–11436; doi:10.1021/ic701715k

data_4333495
_publ_section_title
;
 Syntheses and Structural Characterization of a Series of One-Dimensional
 Fluorotitanophosphates (NH4)xK4&#x00A0;-&#x00A0;x[Ti2PO4F9] (x= 0, 0.70,
 1.00, 1.25)
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11431
_journal_page_last               11436
_journal_paper_doi               10.1021/ic701715k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'F9 H2.8 K3.3 N0.7 O4 P Ti2'
_chemical_formula_weight         503.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.8854(12)
_cell_length_b                   11.014(2)
_cell_length_c                   10.227(2)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2
_cell_volume                     637.3(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1375
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.07
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'teXsan (MSC, 1992-1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484.8
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0353P)^2^+10.0744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                1163
_reflns_number_total             1252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701715ksup2.cif
_cod_data_source_block           3k
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'F9 H2.80 K3.30 N0.70 O4 P Ti2'
_cod_database_code               4333495