Calcium hexakis(dihydrogenphosphito)stannate(IV), Ca[Sn(H~2~PO~2~)~6~], with some remarks on the so-called Ge~2~(H~2~PO~2~)~6~ structure type
Gieschen, Tobias; Reuter, Hans; Acta Crystallographica Section E 69 (2013) i44–; doi:10.1107/S1600536813018205

data_2238327
_publ_section_title
;
 Calcium hexakis(dihydrogenphosphito)stannate(IV), Ca[Sn(H~2~PO~2~)~6~],
 with some remarks on the so-called Ge~2~(H~2~PO~2~)~6~ structure type
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i44
_journal_paper_doi               10.1107/S1600536813018205
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Ca [Sn (H2 P O2)6]'
_chemical_formula_moiety         'Ca H12 O12 P6 Sn'
_chemical_formula_sum            'Ca H12 O12 P6 Sn'
_chemical_formula_weight         548.69
_chemical_name_systematic
;
Calcium hexakis(dihydrogenphosphito)stannate(IV), Ca[Sn(H~2~PO~2~)~6~], with
some remarks on the so-called Ge~2~(H~2~PO~2~)~6~ structure type
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.8619(4)
_cell_length_b                   11.8619(4)
_cell_length_c                   9.8668(4)
_cell_measurement_reflns_used    6570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.86
_cell_volume                     1202.31(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and Mercury
(Macrae <i>et al.</i>, 2008)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18525
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_correction_T_min  0.4593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+3.9531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                731
_reflns_number_total             777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cq2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2238327
_cod_database_fobs_code          2238327