Synthesis, Crystal Structure, NMR Studies, and Thermal Stability of Mixed Iron-Indium Phosphates with Quasi-One-Dimensional Frameworks
X. Tang; A. Jones; A. Lachgar; B. J. Gross; J. L. Yarger; Inorganic Chemistry 38 (1999) 6032–6038; doi:10.1021/ic9905906

data_4322547
_publ_contact_author_address
;     Department of Chemistry
      Wake Forest University
      Winston-Salem, N.C. 27109-7505
      U.S.A.
;
_publ_contact_author_email       lachgar@wfu.edu
_publ_contact_author_fax         '336 758 4656'
_publ_contact_author_name
;
     `Abdessadek Lachgar'
;
_publ_contact_author_phone       '336 758 4676'
_publ_section_title
;
 Synthesis, Crystal Structure, NMR Studies, and Thermal Stability of Mixed
 Iron-Indium Phosphates with Quasi-One-Dimensional Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6032
_journal_page_last               6038
_journal_paper_doi               10.1021/ic9905906
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'Ca2 Fe0.5 H4 In0.5 O13 P3'
_chemical_formula_weight         470.44
_chemical_name_systematic
; 
 ? 
;
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.548(2)
_cell_length_b                   15.670(3)
_cell_length_c                   9.241(2)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.99
_cell_measurement_theta_min      3.24
_cell_volume                     1001.4(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4 diffractometer'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8817
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.513
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0298P)^2^+0.6093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                1885
_reflns_number_total             2213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9905906_2.cif
_cod_data_source_block           aj014
_cod_original_cell_volume        1001.5(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'H4 Ca2 Fe0.50 In0.50 O13 P3'
_cod_database_code               4322547