Syntheses and structural characterization of a series of one-dimensional fluorotitanophosphates (NH4)(x)K(4-x)[Ti(2)PO(4)F(9)] (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_4339202
_publ_section_title
;
 Syntheses and structural characterization of a series of one-dimensional
 fluorotitanophosphates (NH4)(x)K(4-x)[Ti(2)PO(4)F(9)] (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 K4 O4 P Ti2'
_chemical_formula_weight         518.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   None
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8402(12)
_cell_length_b                   11.000(2)
_cell_length_c                   19.436(4)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1248.5(4)
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4141
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        -0.35
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.859
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'teXsan (MSC, 1992-1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.0130(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_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     185
_refine_ls_number_reflns         3809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+4.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                3063
_reflns_number_total             3809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701715k-file004.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1248.4(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4339202