Structural Assembly from Phosphate to Germanophosphate by Applying Germanate as a Binder
Ya-Xi Huang; Biao Liu; Lei Wen; Xin Zhang; Wei Sun; Jun Lin; Chun-Zuo Huang; Rong-Chuan Zhuang; Jin-Xiao Mi; Jing-Tai Zhao; Inorganic Chemistry 52 (2013) 9169–9171; doi:10.1021/ic401329d

data_4335776
_publ_contact_author_address
;
Department of Materials Science and Engineering
College of Materials,
Xiamen University,
Xiamen 361005, Fujian Province
People's Republic of China
;
_publ_contact_author_email       yaxihuang@xmu.edu.cn
_publ_contact_author_fax         0086-592-2183937
_publ_contact_author_name        'Dr. Ya-Xi Huang'
_publ_contact_author_phone       0086-13950175872
_publ_section_title
;
 Structural Assembly from Phosphate to Germanophosphate by Applying
 Germanate as a Binder
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9169
_journal_page_last               9171
_journal_paper_doi               10.1021/ic401329d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Fe4 Ge2 H7 K3 O28 P6'
_chemical_formula_weight         1126.76
_chemical_name_common
;
K~3~[Fe~4~(HPO~4~)][Ge~2~O(OH)(PO~4~)~2~].2H~2~O
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.672(6)
_cell_length_b                   17.990(6)
_cell_length_c                   6.718(2)
_cell_measurement_reflns_used    6807
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      1.57
_cell_volume                     2256.6(12)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
'DIAMOND (Brandenburg, 2005) and ATOMS (Dowty, 2004)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 2008) and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker Diffraction CCD area-detector'
_diffrn_measurement_method
'1265 images,\f=0, 90, 180 degree, and \D\w=0.3 degree, \c= 54.74 degree'
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6807
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         1.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.247
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SMART (Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.316
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1572
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0232P)^2^+66.0447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                1403
_reflns_number_total             1572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401329d_si_002.cif
_cod_data_source_block           cmcm
_cod_database_code               4335776