Synthesis, Crystal Structure, and Characterization (Vibrational and Solid-State31P MAS NMR Spectroscopy) of the High-Temperature Modification of Calciumcatena-Polyphosphate(V)
Weil, Matthias; Puchberger, Michael; Schmedt auf der Günne, Jörn; Weber, Johannes; Chemistry of Materials 19 (2007) 5067–; doi:10.1021/cm071239i

data_4001394
_publ_section_title
;
 Synthesis, Crystal Structure, and Characterization (Vibrational and
 Solid-State31P MAS NMR Spectroscopy) of the High-Temperature Modification
 of Calciumcatena-Polyphosphate(V)
;
_journal_issue                   21
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5067
_journal_paper_doi               10.1021/cm071239i
_journal_volume                  19
_journal_year                    2007
_chemical_formula_structural     'Ca (P O3)2'
_chemical_formula_sum            'Ca O6 P2'
_chemical_formula_weight         198.02
_chemical_name_systematic
; 
Calcium catena-polyphosphate 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.514(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   13.6835(14)
_cell_length_b                   19.981(2)
_cell_length_c                   6.7535(7)
_cell_measurement_reflns_used    2317
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.505
_cell_measurement_theta_min      3.403
_cell_volume                     1840.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10661
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.004
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.6209
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
HABITUS (Herrendorf, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details 'Flack (1983), 2113 Friedel pairs'
_refine_ls_abs_structure_Flack   0.46(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4929
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.7353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                4065
_reflns_number_total             4929
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cm071239i-file001.cif
_cod_data_source_block           aCaP2O6
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4001394