Single-Crystal Growth and Characterization of Disilver(I) Monofluorophosphate(V), Ag2PO3F: Crystal Structure, Thermal Behavior, Vibrational Spectroscopy, and Solid-State 19F, 31P, and 109Ag MAS NMR Spectroscopy
Matthias Weil; Michael Puchberger; Ekkehard Füglein; Enrique J. Baran; Julia Vannahme; Hans J. Jakobsen; Jørgen Skibsted; Inorganic Chemistry 46 (2007) 801–808; doi:10.1021/ic061765w

data_4307223
_publ_contact_author_address
;  
Institut f\"ur Chemische Technologien und Analytik
Technische Universit\"at Wien
Getreidemarkt 9/164
A-1060 Vienna
Austria       
;
_publ_contact_author_email       mweil@mail.zserv.tuwien.ac.at
_publ_contact_author_fax         '+43 1 58801 17199'
_publ_contact_author_name
;       
Matthias Weil       
;
_publ_contact_author_phone       '+43 1 58801 17122'
_publ_section_title
;
Single-Crystal Growth and Characterization of Disilver(I)
Monofluorophosphate(V), Ag2PO3F: Crystal Structure, Thermal Behavior,
Vibrational Spectroscopy, and Solid-State 19F, 31P, and 109Ag MAS NMR
Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              801
_journal_page_last               808
_journal_paper_doi               10.1021/ic061765w
_journal_volume                  46
_journal_year                    2007
_chemical_formula_structural     'Ag2 (P O3 F)'
_chemical_formula_sum            'Ag2 F O3 P'
_chemical_formula_weight         313.71
_chemical_name_systematic
; 
Disilver(I) monofluorophosphate(V) 
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.178(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.2456(8)
_cell_length_b                   5.5854(5)
_cell_length_c                   14.7840(13)
_cell_measurement_reflns_used    2522
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.402
_cell_measurement_theta_min      2.756
_cell_volume                     763.45(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-AXS Apex CCD diffractometer'
_diffrn_measurement_method       \w
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4176
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.562
_exptl_absorpt_correction_T_max  0.9017
_exptl_absorpt_correction_T_min  0.1438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.00095(11)
_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   1.133
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+2.1565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                1093
_reflns_number_total             1165
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic061765wsi20060918_075820.cif
_cod_data_source_block           Ag2PO3F
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4307223