#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/10/2011076.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011076 loop_ _publ_author_name 'Elnagar, Hassan Y.' 'Ranken, Paul F.' 'Fronczek, Frank R.' _publ_section_title ; A pentaerythritol-derived spirodiphosphonate ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 905 _journal_page_last 906 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C7 H14 O6 P2' _chemical_formula_sum 'C7 H14 O6 P2' _chemical_formula_weight 256.1 _chemical_melting_point 520.5(15) _chemical_name_systematic ; 2,4,8,10-tetraoxa-3,9-diphosphaspiro[5,5]undecane, 3,9,-dimethyl-3,9-dioxide ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90 _cell_angle_beta 94.517(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.4560(14) _cell_length_b 5.5761(9) _cell_length_c 11.9512(12) _cell_measurement_reflns_used 25 _cell_measurement_temperature 100 _cell_measurement_theta_max 18.2 _cell_measurement_theta_min 11.4 _cell_volume 1093.2(2) _computing_cell_refinement 'CAD4 Express' _computing_data_collection 'CAD4 Express (Enraf-Nonius, 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'CIFGEN in MolEN (Fair, 1990)' _computing_structure_refinement 'LSFM in MolEN (Fair, 1990)' _computing_structure_solution 'SIR (Burla et al., 1989)' _diffrn_ambient_temperature 100 _diffrn_measurement_device 'Enraf Nonius CAD4 (with Oxford Cryostream)' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source sealed_tube _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .025 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 6104 _diffrn_reflns_theta_max 35.0 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% .5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .404 _exptl_absorpt_correction_T_max .849 _exptl_absorpt_correction_T_min .828 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method none _exptl_crystal_description fragment _exptl_crystal_F_000 536 _exptl_crystal_size_max .57 _exptl_crystal_size_mid .55 _exptl_crystal_size_min .42 _refine_diff_density_max .64 _refine_diff_density_min -.57 _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef '8(2) x 10^-7^' _refine_ls_extinction_method 'isotropic (Zachariasen, 1963)' _refine_ls_goodness_of_fit_all 1.983 _refine_ls_goodness_of_fit_ref 1.911 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 98 _refine_ls_number_reflns 2137 _refine_ls_number_restraints 4 _refine_ls_R_factor_all .034 _refine_ls_R_factor_gt .031 _refine_ls_shift/su_max .008 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details '4Fo^2^/[\s^2^(Fo^2^) + 0.0004Fo^4^]' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all .047 _refine_ls_wR_factor_ref .047 _reflns_number_gt 1915 _reflns_number_total 2232 _reflns_threshold_expression I>3\s(I) _[local]_cod_data_source_file bk1533.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '519-522 K' was changed to '520.5(15)' - the average value was taken and precision was estimated. '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 8 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '519-522 K' was changed to '520.5(15)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1093.2(4) _cod_database_code 2011076 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol P .01555(10) .01359(10) .01307(10) -.00223(8) -.00033(9) .00213(9) P O1 .0204(3) .0184(3) .0162(3) -.0078(3) -.0009(3) -.0011(3) O O2 .0138(3) .0103(3) .0161(3) -.0009(2) .0014(2) -.0017(2) O O3 .0236(3) .0220(4) .0145(3) -.0015(3) .0016(3) .0054(3) O C1 .0191(5) .0082(5) .0113(5) .0000 -.0005(4) .0000 C C2 .0308(5) .0103(4) .0155(4) -.0059(4) .0002(4) -.0004(3) C C3 .0153(4) .0111(3) .0131(4) .0008(3) -.0009(3) -.0016(3) C C4 .0167(4) .0242(5) .0301(5) .0022(4) .0018(4) .0061(5) C loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol P .37384(2) .31415(5) .40865(2) .01415(5) Uani ? ? P O1 .35845(5) .14492(8) .30174(7) .0182(3) Uani ? ? O O2 .45337(4) .45944(13) .38308(6) .0132(3) Uani ? ? O O3 .38079(5) .18275(15) .51608(7) .0196(3) Uani ? ? O C1 .5 .1653(2) .25 .0121(5) Uani ? ? C C2 .42830(7) .0022(2) .27299(9) .0170(4) Uani ? ? C C3 .52303(6) .3186(2) .35399(8) .0130(4) Uani ? ? C C4 .29603(7) .5333(2) .39320(13) .0230(5) Uani ? ? C H2a .4082(9) -.091(3) .2078(14) .035(4) Uiso ? ? H H2b .4416(8) -.115(2) .3365(11) .020(4) Uiso ? ? H H3a .5634(8) .428(3) .3415(11) .019(4) Uiso ? ? H H3b .5409(9) .212(3) .4193(12) .023(4) Uiso ? ? H H4a .2968(9) .603(3) .3176(13) .047(5) Uiso ? ? H H4b .3078(9) .656(3) .4459(13) .032(4) Uiso ? ? H H4c .2459(9) .477(3) .4122(12) .032(4) Uiso ? ? H loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P O1 . . 1.5924(8) yes P O2 . . 1.5892(7) yes P O3 . . 1.4749(8) yes P C4 . . 1.7691(12) yes O1 C2 . . 1.4611(14) yes O2 C3 . . 1.4539(12) yes C1 C2 . . 1.5315(13) yes C1 C3 . . 1.5315(13) yes C2 H2a . . .974(16) ? C2 H2b . . 1.010(13) ? C3 H3a . . .921(13) ? C3 H3b . . 1.005(14) ? C4 H4a . . .987(16) ? C4 H4b . . .941(14) ? C4 H4c . . .927(14) ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C .002 .002 International_Tables_Vol_IV_Table_2.3.1 H .000 .000 International_Tables_Vol_IV_Table_2.3.1 O .008 .006 International_Tables_Vol_IV_Table_2.3.1 P .090 .095 International_Tables_Vol_IV_Table_2.3.1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 2 5 8 -2 0 -2 -2 5 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 P O2 . 103.25(4) yes O1 P O3 . 113.62(5) ? O1 P C4 . 104.92(5) ? O2 P O3 . 114.34(4) ? O2 P C4 . 103.19(5) ? O3 P C4 . 116.09(6) yes P O1 C2 . 115.67(6) yes P O2 C3 . 116.57(6) yes C2 C1 C2 2_655 107.16(9) yes C2 C1 C3 . 109.32(5) yes C2 C1 C3 2_655 109.40(5) ? C3 C1 C3 2_655 112.11(9) yes O1 C2 C1 . 110.50(8) ? O1 C2 H2a . 104.9(9) ? O1 C2 H2b . 107.7(8) ? C1 C2 H2a . 113.0(9) ? C1 C2 H2b . 113.2(7) ? H2a C2 H2b . 107.2(12) ? O2 C3 C1 . 110.26(7) ? O2 C3 H3a . 106.0(8) ? O2 C3 H3b . 108.7(8) ? C1 C3 H3a . 111.8(8) ? C1 C3 H3b . 109.9(8) ? H3a C3 H3b . 110.1(11) ? P C4 H4a . 107.8(10) ? P C4 H4b . 108.9(9) ? P C4 H4c . 113.1(10) ? H4a C4 H4b . 108.1(14) ? H4a C4 H4c . 115.7(12) ? H4b C4 H4c . 102.8(13) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag O2 P O1 C2 51.87(8) yes O3 P O1 C2 -72.53(8) ? C4 P O1 C2 159.64(7) ? O1 P O2 C3 -52.02(7) yes O3 P O2 C3 71.91(8) ? C4 P O2 C3 -161.09(7) ? P O1 C2 C1 -58.93(9) yes P O2 C3 C1 58.50(9) yes C3 C1 C2 O1 58.49(9) yes C2 C1 C3 O2 -57.95(10) yes