data_global _publ_requested_journal 'Chem. Mater.' _publ_contact_author ; Dr A. Wright, School of Chemistry, University of Birmingham, Edgbaston, Birmingham, B15 2TT, UK ; _publ_contact_author_email 'a.j.wright@bham.ac.uk' _publ_section_title ; Synthesis and structure of a calcium polyphosphate with a unique criss-cross arrangement of helical phosphate chains ; _publ_section_references ; SHELXTL, program suite for structure solution and refinement, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SMART, program for instrument control and data aquisition, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SAINTPLUS, program suite for data processing, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA ; data_lej078 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ca, 2(O3 P1)' _chemical_formula_sum 'Ca O6 P2' _chemical_formula_weight 198.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.5669(2) _cell_length_b 9.5023(2) _cell_length_c 10.3717(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.474(2) _cell_angle_gamma 90.00 _cell_volume 941.13(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1317 _cell_measurement_theta_min 6.57 _cell_measurement_theta_max 70.31 _exptl_crystal_description 'Block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 17.752 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.1698 _exptl_absorpt_correction_T_max 0.1698 _exptl_absorpt_process_details 'Sadabs in SaintPlus' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 6000 CCD' _diffrn_measurement_method 'CCD slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2836 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 6.57 _diffrn_reflns_theta_max 70.31 _reflns_number_total 1336 _reflns_number_gt 1317 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.6092P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.047(12) _refine_ls_number_reflns 1336 _refine_ls_number_parameters 163 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.3519(4) -0.2838(4) 0.7240(3) 0.0127(7) Uani 1 1 d . . . O2 O 0.5078(4) -0.2810(4) 0.5444(3) 0.0102(7) Uani 1 1 d . . . O3 O 0.4847(3) -0.0571(4) 0.6691(3) 0.0104(7) Uani 1 1 d . . . O4 O 0.6853(3) -0.3793(4) 0.4121(3) 0.0096(7) Uani 1 1 d . . . O5 O 0.5863(3) -0.1376(4) 0.3583(3) 0.0088(7) Uani 1 1 d U . . O6 O 0.7521(4) -0.1779(4) 0.5565(3) 0.0103(7) Uani 1 1 d . . . O7 O 0.5934(4) 0.1850(4) 0.5610(3) 0.0131(7) Uani 1 1 d . . . O8 O 0.7179(4) 0.1899(4) 0.3489(3) 0.0144(8) Uani 1 1 d . . . O9 O 0.7901(3) 0.3574(4) 0.5226(3) 0.0098(7) Uani 1 1 d . . . O10 O 0.5616(3) 0.3926(4) 0.4122(3) 0.0108(7) Uani 1 1 d . . . O11 O 0.7050(4) 0.4605(4) 0.2255(3) 0.0112(7) Uani 1 1 d . . . O12 O 0.4692(3) 0.5803(3) 0.2623(3) 0.0108(7) Uani 1 1 d . . . P1 P 0.40858(12) -0.18776(12) 0.62936(12) 0.0067(3) Uani 1 1 d . . . P2 P 0.63730(11) -0.23260(12) 0.46590(10) 0.0066(3) Uani 1 1 d . . . P3 P 0.66240(12) 0.26645(12) 0.46003(11) 0.0066(3) Uani 1 1 d . . . P4 P 0.60208(12) 0.51408(12) 0.31333(11) 0.0065(3) Uani 1 1 d . . . Ca1 Ca 0.72551(10) 0.00805(9) 0.71673(9) 0.0084(2) Uani 1 1 d . . . Ca2 Ca 0.39805(9) 0.17958(10) 0.69975(9) 0.0089(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0146(17) 0.0163(18) 0.0070(15) 0.0041(14) -0.0003(14) -0.0008(15) O2 0.0094(17) 0.0129(17) 0.0086(14) -0.0005(13) 0.0030(13) -0.0027(14) O3 0.0082(15) 0.0128(17) 0.0096(15) 0.0001(13) -0.0035(13) 0.0015(15) O4 0.0073(15) 0.0093(16) 0.0120(16) -0.0020(14) -0.0014(13) -0.0005(13) O5 0.0093(10) 0.0092(10) 0.0076(10) 0.0019(8) -0.0011(8) 0.0001(8) O6 0.0107(16) 0.0127(18) 0.0067(15) 0.0004(13) -0.0054(13) 0.0002(13) O7 0.0087(16) 0.0182(17) 0.0121(16) 0.0046(14) -0.0022(14) 0.0000(14) O8 0.0147(18) 0.0148(18) 0.0133(17) -0.0033(15) -0.0014(15) 0.0035(14) O9 0.0084(16) 0.0106(18) 0.0097(15) 0.0020(13) -0.0056(14) 0.0001(13) O10 0.0082(16) 0.0149(16) 0.0088(15) 0.0020(13) -0.0031(13) 0.0006(13) O11 0.0125(17) 0.0103(15) 0.0109(15) 0.0002(15) 0.0020(14) 0.0026(14) O12 0.0077(15) 0.0104(17) 0.0139(16) 0.0009(14) -0.0020(14) 0.0015(14) P1 0.0055(5) 0.0080(6) 0.0062(5) 0.0004(4) -0.0020(4) -0.0003(5) P2 0.0063(6) 0.0084(6) 0.0050(5) 0.0003(5) -0.0010(5) 0.0009(4) P3 0.0047(5) 0.0073(5) 0.0074(5) 0.0003(5) -0.0015(5) -0.0005(4) P4 0.0055(6) 0.0080(6) 0.0058(5) 0.0005(4) -0.0010(4) 0.0003(5) Ca1 0.0072(5) 0.0083(4) 0.0096(4) -0.0002(4) -0.0008(3) 0.0000(3) Ca2 0.0075(5) 0.0096(5) 0.0093(4) 0.0011(4) -0.0020(4) 0.0000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 P1 1.467(4) . ? O1 Ca1 2.317(4) 3_445 ? O2 P2 1.591(4) . ? O2 P1 1.601(4) . ? O3 P1 1.486(4) . ? O3 Ca1 2.407(3) . ? O3 Ca2 2.424(4) . ? O4 P2 1.580(3) . ? O4 P4 1.616(3) 1_545 ? O5 P2 1.494(3) . ? O5 Ca1 2.384(3) 2_554 ? O5 Ca2 2.397(3) 2_554 ? O6 P2 1.495(3) . ? O6 Ca2 2.396(3) 3_545 ? O6 Ca1 2.449(3) . ? O7 P3 1.488(4) . ? O7 Ca2 2.428(4) . ? O7 Ca1 2.605(4) . ? O8 P3 1.488(4) . ? O8 Ca1 2.331(4) 2_554 ? O8 Ca2 2.688(4) 4_554 ? O9 P1 1.595(3) 3 ? O9 P3 1.601(3) . ? O10 P3 1.598(4) . ? O10 P4 1.607(4) . ? O11 P4 1.472(4) . ? O11 Ca2 2.305(4) 4_554 ? O12 P4 1.487(3) . ? O12 Ca2 2.457(3) 2_564 ? O12 Ca1 2.496(3) 4_454 ? P1 O9 1.595(3) 3_445 ? P4 O4 1.616(3) 1_565 ? Ca1 O1 2.317(4) 3 ? Ca1 O8 2.331(4) 2 ? Ca1 O5 2.384(3) 2 ? Ca1 O12 2.496(3) 4 ? Ca2 O11 2.305(4) 4_455 ? Ca2 O6 2.396(3) 3_455 ? Ca2 O5 2.397(3) 2 ? Ca2 O12 2.457(3) 2_565 ? Ca2 O8 2.688(4) 4_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 O1 Ca1 136.2(2) . 3_445 ? P2 O2 P1 128.9(2) . . ? P1 O3 Ca1 136.0(2) . . ? P1 O3 Ca2 130.24(19) . . ? Ca1 O3 Ca2 93.75(12) . . ? P2 O4 P4 129.4(2) . 1_545 ? P2 O5 Ca1 127.08(19) . 2_554 ? P2 O5 Ca2 127.6(2) . 2_554 ? Ca1 O5 Ca2 95.04(12) 2_554 2_554 ? P2 O6 Ca2 124.9(2) . 3_545 ? P2 O6 Ca1 125.1(2) . . ? Ca2 O6 Ca1 93.89(12) 3_545 . ? P3 O7 Ca2 144.9(2) . . ? P3 O7 Ca1 123.57(19) . . ? Ca2 O7 Ca1 88.88(11) . . ? P3 O8 Ca1 151.1(2) . 2_554 ? P3 O8 Ca2 119.45(19) . 4_554 ? Ca1 O8 Ca2 89.42(12) 2_554 4_554 ? P1 O9 P3 129.0(2) 3 . ? P3 O10 P4 124.9(2) . . ? P4 O11 Ca2 147.4(2) . 4_554 ? P4 O12 Ca2 134.74(19) . 2_564 ? P4 O12 Ca1 133.94(19) . 4_454 ? Ca2 O12 Ca1 91.25(11) 2_564 4_454 ? O1 P1 O3 121.96(19) . . ? O1 P1 O9 110.8(2) . 3_445 ? O3 P1 O9 106.48(18) . 3_445 ? O1 P1 O2 106.25(19) . . ? O3 P1 O2 108.54(19) . . ? O9 P1 O2 100.76(18) 3_445 . ? O5 P2 O6 117.0(2) . . ? O5 P2 O4 110.97(19) . . ? O6 P2 O4 108.09(19) . . ? O5 P2 O2 109.12(19) . . ? O6 P2 O2 110.13(19) . . ? O4 P2 O2 100.23(19) . . ? O7 P3 O8 119.0(2) . . ? O7 P3 O10 108.89(19) . . ? O8 P3 O10 111.3(2) . . ? O7 P3 O9 110.8(2) . . ? O8 P3 O9 106.18(19) . . ? O10 P3 O9 98.77(17) . . ? O11 P4 O12 121.1(2) . . ? O11 P4 O10 110.0(2) . . ? O12 P4 O10 107.28(18) . . ? O11 P4 O4 106.66(19) . 1_565 ? O12 P4 O4 109.76(19) . 1_565 ? O10 P4 O4 100.06(18) . 1_565 ? O1 Ca1 O8 134.80(13) 3 2 ? O1 Ca1 O5 81.31(12) 3 2 ? O8 Ca1 O5 90.92(12) 2 2 ? O1 Ca1 O3 135.80(13) 3 . ? O8 Ca1 O3 81.35(12) 2 . ? O5 Ca1 O3 72.30(12) 2 . ? O1 Ca1 O6 124.22(13) 3 . ? O8 Ca1 O6 79.92(12) 2 . ? O5 Ca1 O6 151.09(13) 2 . ? O3 Ca1 O6 79.21(12) . . ? O1 Ca1 O12 78.55(12) 3 4 ? O8 Ca1 O12 71.30(12) 2 4 ? O5 Ca1 O12 127.39(11) 2 4 ? O3 Ca1 O12 145.45(11) . 4 ? O6 Ca1 O12 75.62(11) . 4 ? O1 Ca1 O7 72.63(12) 3 . ? O8 Ca1 O7 148.67(13) 2 . ? O5 Ca1 O7 77.32(11) 2 . ? O3 Ca1 O7 67.45(11) . . ? O6 Ca1 O7 96.40(12) . . ? O12 Ca1 O7 138.33(12) 4 . ? O11 Ca2 O6 87.56(13) 4_455 3_455 ? O11 Ca2 O5 113.47(13) 4_455 2 ? O6 Ca2 O5 154.78(12) 3_455 2 ? O11 Ca2 O3 76.26(12) 4_455 . ? O6 Ca2 O3 129.35(12) 3_455 . ? O5 Ca2 O3 71.77(11) 2 . ? O11 Ca2 O7 137.06(13) 4_455 . ? O6 Ca2 O7 93.50(12) 3_455 . ? O5 Ca2 O7 80.61(12) 2 . ? O3 Ca2 O7 70.13(11) . . ? O11 Ca2 O12 135.77(12) 4_455 2_565 ? O6 Ca2 O12 77.31(11) 3_455 2_565 ? O5 Ca2 O12 77.80(12) 2 2_565 ? O3 Ca2 O12 143.57(12) . 2_565 ? O7 Ca2 O12 85.76(12) . 2_565 ? O11 Ca2 O8 69.72(12) 4_455 4_455 ? O6 Ca2 O8 74.10(11) 3_455 4_455 ? O5 Ca2 O8 99.40(11) 2 4_455 ? O3 Ca2 O8 137.72(11) . 4_455 ? O7 Ca2 O8 151.04(13) . 4_455 ? O12 Ca2 O8 66.20(11) 2_565 4_455 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 70.31 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.468 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.120