Preparation and Characterization of Dimercury(I) Monofluorophosphate(V), Hg2PO3F: Crystal Structure, Thermal Behavior, Vibrational Spectra, and Solid-State 31P and 19F NMR Spectra
Matthias Weil; Michael Puchberger; Enrique J. Baran; Inorganic Chemistry 43 (2004) 8330–8335; doi:10.1021/ic048741e

data_4312208
_publ_contact_author_address
;  
Institute for Chemical Technologies and Analytics
Division of Structural Chemistry
Vienna University of Technology
Getreidemarkt 9/164-SC
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
;
 Preparation and Characterization of Dimercury(I) Monofluorophosphate(V),
 Hg2PO3F: Crystal Structure, Thermal Behavior, Vibrational Spectra, and
 Solid-State 31P and 19F NMR Spectra
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8330
_journal_page_last               8335
_journal_paper_doi               10.1021/ic048741e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_structural     'Hg2 (P O3 F)'
_chemical_formula_sum            'F Hg2 O3 P'
_chemical_formula_weight         499.15
_chemical_name_systematic
; 
Mercury(I) monofluorophosphate 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.406(2)
_cell_length_b                   12.145(3)
_cell_length_c                   8.567(2)
_cell_measurement_reflns_used    2574
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.376
_cell_measurement_theta_min      2.779
_cell_volume                     978.7(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Atoms for Windows V5.1 (Dowty, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SMART diffractometer with APEX CCD camera'
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5400
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.74
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    62.910
_exptl_absorpt_correction_T_max  0.2711
_exptl_absorpt_correction_T_min  0.0620
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Habitus (Herrendorf, 1993-1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    6.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.255
_refine_diff_density_min         -2.995
_refine_diff_density_rms         0.384
_refine_ls_extinction_coef       0.00019(5)
_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   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0384P)^2^+37.9325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                678
_reflns_number_total             795
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048741esi20040826_072333.cif
_cod_data_source_block           Hg2PO3F
_cod_database_code               4312208