Syntheses, crystal structures and optical properties of two one-dimensional germanophosphates: HRb~3~Ge~2~(HPO~4~)~6~ and CsGe(HPO~4~)~2~(OH)
Song, Jun-Ling; Lu, Wen-Xiu; Guo, Tian-Shuo; Zhou, Yu-Hua; Acta Crystallographica Section C 74 (2018) 1146–1152; doi:10.1107/S2053229618012792

data_2021237
_publ_section_title
;
 Syntheses, crystal structures and optical properties of two
 one-dimensional germanophosphates: HRb~3~Ge~2~(HPO~4~)~6~ and
 CsGe(HPO~4~)~2~(OH)
;
_journal_coeditor_code           LY3074
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1146
_journal_page_last               1152
_journal_paper_doi               10.1107/S2053229618012792
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'H Rb3 Ge2 (H P O4)6'
_chemical_formula_moiety         'Ge2 H7 O24 P6 Rb3'
_chemical_formula_sum            'Ge2 H7 O24 P6 Rb3'
_chemical_formula_weight         978.47
_chemical_name_systematic
;
Hydrogen hexakis(\m-hydrogen phosphato)digermaniumtrirubidium
;
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.5940(9)
_cell_length_b                   14.5940(9)
_cell_length_c                   8.5522(6)
_cell_measurement_reflns_used    3159
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.88
_cell_volume                     1577.46(18)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4050
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    10.328
_exptl_absorpt_correction_T_max  0.356
_exptl_absorpt_correction_T_min  0.209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1389
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -1.415
_refine_ls_extinction_coef       0.0039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         624
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0392P)^2^+22.1168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                573
_reflns_number_total             624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ly3074sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2021237--2021238.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'H7 Ge2 O24 P6 Rb3'
_cod_database_code               2021237
_cod_database_fobs_code          2021237