Structure and ^31^P NMR spectroscopy of a new phosphate, Na~8~Ca~1.5~Mg~12.5~(PO~4~)~12~
Jerbi, Hasna; Hidouri, Mourad; Rzeigui, Mohamed; Ben Amara, Mongi; Acta Crystallographica Section C 67 (2011) i17–i20; doi:10.1107/S0108270110054521

data_2018013
_publ_section_title
;
 Structure and ^31^P NMR spectroscopy of a new phosphate,
 Na~8~Ca~1.5~Mg~12.5~(PO~4~)~12~
;
_journal_coeditor_code           KU3038
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i17
_journal_page_last               i20
_journal_paper_doi               10.1107/S0108270110054521
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'Na8 Ca1.5 Mg12.5 (P O4)12'
_chemical_formula_sum            'Ca1.5 Mg12.5 Na8 O48 P12'
_chemical_formula_weight         1687.56
_chemical_melting_point          1072
_chemical_name_common            panitite
_chemical_name_systematic
;
sodium calcium magnesium tetrakis(phosphate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.185(8)
_cell_length_b                   14.860(8)
_cell_length_c                   25.610(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.93
_cell_measurement_theta_min      7.75
_cell_volume                     3876(4)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (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  'Enraf--Nonius TurboCAD-4'
_diffrn_measurement_method       'non-profiled \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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            13798
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.846
_refine_diff_density_min         -1.686
_refine_ls_extinction_coef       0.00040(9)
_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   1.044
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         11269
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0673P)^2^+11.5875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                8933
_reflns_number_total             11269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3038.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'Ca1.50 Mg12.50 Na8 O48 P12'
_cod_database_code               2018013
_cod_database_fobs_code          2018013