# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/250 data_CRYSTALS_cif _audit_creation_date 00-25-05 _audit_creation_method CRYSTALS_ver_12-03-99 # THIS IS THE DEFAULT SETTING FOR THE TITLE, PROVIDED WHEN NO # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file REFCIF.DAT # This is a character file which you may edit to reflect local conditions # # Items which need looking at are represented by a '?' # Items for which there are choices are prefixed with 'choose from' # # 1. SUBMISSION DETAILS _publ_contact_letter ; ? ; _publ_contact_author_name 'Martin Attfield' _publ_contact_author_address ; School of Crystallography Birkbeck College Malet Street, LONDON WC1E 7HX ; _publ_contact_author_phone ' 020 7631 6813 ' _publ_contact_author_fax ' 020 7631 6270 ' _publ_contact_author_email ' m.attfield@cryst.bbk.ac.uk ' _publ_requested_journal 'Journal of Materials Chemistry' _publ_requested_category CO # choose from: FI FM FO CI CM CO AD# _publ_requested_coeditor_name ' ? ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Al2[O3PCH2CH2PO3](H2O)2F2.H2O: A novel aluminium diphosphonate ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name 'Harvey, Howard' 'Teat, Simon' 'Attfield, Martin' #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; ? ; _publ_section_exptl_prep ; ? ; #========================================================================== # 5. DETAILS #========================================================================== _diffrn_radiation_monochromator 'Silicon (111)' _diffrn_measurement_device-type 'Bruker SMART CCD Area Detector' _computing_data_collection SMART _computing_data_reduction SAINT _computing_cell_refinement SMART _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _chemical_name_systematic ; Aluminium fluoro ethylenediphosphonate hydrate ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _cell_length_a 4.978(3) _cell_angle_alpha 90 _cell_length_b 12.00(1) _cell_angle_beta 91.97(3) _cell_length_c 8.189(6) _cell_angle_gamma 90 _cell_volume 488.9(2) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/m 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z' 'x,-y+1/2,z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Al ' 0.0560 0.0520 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C2 H4 Al2 F2 O9 P2 ' _chemical_formula_moiety ' C1 H2 Al1 F1 O4.50 P1 ' _chemical_compound_source ' Aldrich, Lancaster ' _chemical_formula_weight 325.96 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 160 _cell_formula_units_Z 2 _exptl_crystal_description ' flat plates ' _exptl_crystal_colour ' clear ' _exptl_crystal_size_min 0.005 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_max 0.010 _exptl_crystal_density_diffrn 2.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 324.75 _exptl_absorpt_coefficient_mu 0.69 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293 _diffrn_reflns_number 2749 _reflns_number_total 1338 _diffrn_reflns_av_R_equivalents 0.06 # Number of reflections with Friedels Law is 1338 # Number of reflections without Friedels Law is 0 _reflns_number_gt 868 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 54.875 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -6 _reflns_limit_h_max 6 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _refine_diff_density_min -1.15 _refine_diff_density_max 2.18 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 868 _refine_ls_number_parameters 39 _refine_ls_R_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.1070 _refine_ls_goodness_of_fit_ref 1.0801 _refine_ls_shift/su_max 0.021757 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 3.53 -1.36 2.21 ; _diffrn_radiation_type 'Daresbury Synchrotron radiation source ' _diffrn_radiation_wavelength 0.69420 _diffrn_measurement_method 'Omega scans ' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Al1 0.5000 0.5000 0.0000 0.0036(6) 1.0000 Uiso Al2 0.2416(7) 0.2500 0.1449(4) 0.0062(7) 1.0000 Uiso P1 0.0052(4) 0.48526(18) 0.2322(2) 0.0062(5) 1.0000 Uiso O1 0.0358(12) 0.3584(5) 0.2330(7) 0.0087(11) 1.0000 Uiso O2 0.203(1) 0.5433(5) 0.1192(6) 0.0059(11) 1.0000 Uiso O3 -0.2836(11) 0.5191(5) 0.1928(6) 0.008(1) 1.0000 Uiso O4 0.4997(18) 0.2500 0.3271(11) 0.0136(17) 1.0000 Uiso O5 0.0165(17) 0.2500 -0.054(1) 0.0104(16) 1.0000 Uiso O6 0.437(2) 0.2500 -0.3480(14) 0.028(2) 1.0000 Uiso F1 0.4530(9) 0.3531(4) 0.0477(6) 0.0076(9) 1.0000 Uiso C1 0.0787(17) 0.5307(7) 0.436(1) 0.0122(15) 1.0000 Uiso H11 0.0357(17) 0.6117(7) 0.443(1) 0.02(2) 1.0000 Uiso H12 0.2747(17) 0.5187(7) 0.461(1) 0.02(2) 1.0000 Uiso _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Al1 . O2 . 1.873(5) yes Al1 . O2 2_665 1.873(5) yes Al1 . O3 1_655 1.894(5) yes Al1 . O3 2_565 1.894(5) yes Al1 . F1 . 1.823(5) yes Al1 . F1 2_665 1.823(5) yes Al2 . O1 . 1.821(6) yes Al2 . O1 4_555 1.821(6) yes Al2 . O4 . 1.94(1) yes Al2 . O5 . 1.946(9) yes Al2 . F1 . 1.825(5) yes Al2 . F1 4_555 1.825(5) yes P1 . O1 . 1.530(6) yes P1 . O2 . 1.541(5) yes P1 . O3 . 1.518(6) yes P1 . C1 . 1.780(8) yes C1 . C1 2_566 1.522(16) yes C1 . H11 . 0.998 no C1 . H12 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . Al1 . O2 2_665 179.994 yes O2 . Al1 . O3 1_655 88.2(2) yes O2 2_665 Al1 . O3 1_655 91.8(2) yes O2 . Al1 . O3 2_565 91.8(2) yes O2 2_665 Al1 . O3 2_565 88.2(2) yes O3 1_655 Al1 . O3 2_565 179.994 yes O2 . Al1 . F1 . 92.7(2) yes O2 2_665 Al1 . F1 . 87.3(2) yes O3 1_655 Al1 . F1 . 90.7(2) yes O3 2_565 Al1 . F1 . 89.3(2) yes O2 . Al1 . F1 2_665 87.3(2) yes O2 2_665 Al1 . F1 2_665 92.7(2) yes O3 1_655 Al1 . F1 2_665 89.3(2) yes O3 2_565 Al1 . F1 2_665 90.7(2) yes F1 . Al1 . F1 2_665 179.994 yes O1 . Al2 . O1 4_555 91.3(4) yes O1 . Al2 . O4 . 93.6(3) yes O1 4_555 Al2 . O4 . 93.6(3) yes O1 . Al2 . O5 . 90.9(3) yes O1 4_555 Al2 . O5 . 90.9(3) yes O4 . Al2 . O5 . 173.6(4) yes O1 . Al2 . F1 . 91.7(2) yes O1 4_555 Al2 . F1 . 176.7(3) yes O4 . Al2 . F1 . 87.7(3) yes O5 . Al2 . F1 . 87.6(3) yes O1 . Al2 . F1 4_555 176.7(3) yes O1 4_555 Al2 . F1 4_555 91.7(2) yes O4 . Al2 . F1 4_555 87.7(3) yes O5 . Al2 . F1 4_555 87.6(3) yes F1 . Al2 . F1 4_555 85.4(3) yes O1 . P1 . O2 . 112.8(3) yes O1 . P1 . O3 . 111.1(3) yes O2 . P1 . O3 . 111.8(3) yes O1 . P1 . C1 . 106.5(4) yes O2 . P1 . C1 . 108.0(3) yes O3 . P1 . C1 . 106.3(4) yes Al2 . O1 . P1 . 140.1(4) yes Al1 . O2 . P1 . 136.0(4) yes Al1 1_455 O3 . P1 . 130.7(3) yes Al1 . F1 . Al2 . 146.1(3) yes P1 . C1 . C1 2_566 113.8(8) yes P1 . C1 . H11 . 108.3(3) no C1 2_566 C1 . H11 . 108.4(6) no P1 . C1 . H12 . 108.4(3) no C1 2_566 C1 . H12 . 108.1(6) no H11 . C1 . H12 . 109.769 no