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_4333497
_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 H5 K2.75 N1.25 O4 P Ti2'
_chemical_formula_weight         491.85
_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                 106.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.8962(12)
_cell_length_b                   11.011(2)
_cell_length_c                   10.252(2)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     639.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6091
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         33.49
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.389
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.102
_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     105
_refine_ls_number_reflns         2468
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0372P)^2^+0.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                2222
_reflns_number_total             2468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701715ksup4.cif
_cod_data_source_block           3k
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4333497