Synthesis and Characterization of a Fluorotitanophosphate (NH~4~)~0.16~K~1.84~[Ti~2~F~2~(PO~4~)~2~(PO~3~OH)] with a Unique Lamella Framework
Yang, Sihai; Li, Guobao; Liu, Wei; Wang, Wei; Yan, Zhimin; Huang, Yining; Liao, Fuhui; Lin, Jianhua; Inorganic Chemistry 48 (2009) 5449–5453; doi:10.1021/ic900504m

data_4302398
_publ_section_title
;
 Synthesis and Characterization of a Fluorotitanophosphate
 (NH~4~)~0.16~K~1.84~[Ti~2~F~2~(PO~4~)~2~(PO~3~OH)] with a
 Unique Lamella Framework
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5449
_journal_page_last               5453
_journal_paper_doi               10.1021/ic900504m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'F2 H1.64 K1.84 N0.16 O12 P3 Ti2'
_chemical_formula_weight         494.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.406(3)
_cell_length_b                   8.3230(17)
_cell_length_c                   8.8260(18)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      2
_cell_volume                     1173.5(4)
_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  'SHELXL-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 0.992
_diffrn_measured_fraction_theta_max 0.946
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4710
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         33.50
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    2.515
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.46
_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    2.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962.9
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.117
_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     100
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                1881
_reflns_number_total             2182
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338654
_cod_data_source_file            ic900504m_si_002.cif
_cod_data_source_block
;
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302398