Structure of calcium tetrasodium bis-cyclotriphosphate CaNa4(P3O9)2 by X-ray diffraction and solid-state NMR
Abrahams, Isaac; Hawkes, Geoffery E.; Ahmed, A.; Franks, Katrin; Knowles, Jonathan C.; Bodart, Philippe R.; Nunes, Teresa; Journal of the Chemical Society, Dalton Transactions  (2002) 1800–; doi:10.1039/b109036b

data_7011200
_publ_section_title
;
 Structure of calcium tetrasodium bis-cyclotriphosphate CaNa4(P3O9)2 by
 X-ray diffraction and solid-state NMR
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1800
_journal_paper_doi               10.1039/b109036b
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Ca1 Na4 O18 P6'
_chemical_formula_structural     'NA4 O18 P6 CA1'
_chemical_formula_sum            'Ca Na4 O18 P6'
_chemical_formula_weight         605.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2001-09-07T18:34:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.60(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.069(2)
_cell_length_b                   8.054(2)
_cell_length_c                   14.164(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.2505
_cell_measurement_theta_min      8.6845
_cell_measurement_wavelength     0.71073
_cell_volume                     1486.1(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.74475E-1
_diffrn_orient_matrix_UB_12      -0.13406E-1
_diffrn_orient_matrix_UB_13      -0.20953E-1
_diffrn_orient_matrix_UB_21      -0.18394E-1
_diffrn_orient_matrix_UB_22      0.34152E-1
_diffrn_orient_matrix_UB_23      0.64373E-1
_diffrn_orient_matrix_UB_31      -0.2868E-2
_diffrn_orient_matrix_UB_32      0.118618
_diffrn_orient_matrix_UB_33      -0.20826E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1466
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_correction_T_min  0.2149
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+7.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.134
_reflns_number_gt                1018
_reflns_number_total             1300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109036b.txt
_cod_data_source_block           aakzn
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7011200
_exptl_absorpt_factor_mur        0.155
_diffrn_standards_decay_corr_max 1.182
_diffrn_standards_decay_corr_min 0.957