# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Paul-Alain Jaffres' _publ_contact_author_email PJAFFRES@UNIV-BREST.FR _publ_section_title ; Meta-phosphonobenzoic acid and copper(II) as precursors of helical chain and lamellar hybrid materials ; loop_ _publ_author_name 'Paul-Alain Jaffres' 'Vincent Caignaert' 'Jean-Pierre Haelters' 'A Leclaire' 'Jean-Michel Rueff' ; C.Simon ; #======================================================================= # Attachment 'compound2-C7H5CuO5P,H2O.cif' #======================================================================= data_(II) _database_code_depnum_ccdc_archive 'CCDC 692180' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C7 H7 Cu1 O6 P1' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C7 H7 Cu1 O6 P1' _chemical_formula_weight 281.6 _chemical_melting_point ? _chemical_compound_source 'hydrothermal synthesis' #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 4.8414(3) _cell_length_b 32.557(3) _cell_length_c 5.7845(9) _cell_angle_alpha 90 _cell_angle_beta 96.016(7) _cell_angle_gamma 90 _cell_volume 906.74(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 100 _cell_measurement_theta_min 6. _cell_measurement_theta_max 35 _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.0625 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.589 _exptl_crystal_description plate _exptl_crystal_size_max 0.241 _exptl_crystal_size_mid 0.223 _exptl_crystal_size_min 0.026 _exptl_crystal_size_rad ? _exptl_crystal_colour 'light green' _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS; Bruker (2001)' _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.935 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Nonius CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\F/\W scan' _diffrn_reflns_number 12609 _diffrn_reflns_theta_min 5.80 _diffrn_reflns_theta_max 35.99 _diffrn_reflns_theta_full 35.99 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measured_fraction_theta_full 0.95 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 4066 _reflns_number_gt 3097 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_gt 0.0295 _refine_ls_R_factor_all 0.0463 _refine_ls_wR_factor_ref 0.0308 _refine_ls_goodness_of_fit_ref 1.64 _refine_ls_goodness_of_fit_gt 1.81 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4066 _refine_ls_number_parameters 165 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.000049F^2^) _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max 0.0008 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.41 _refine_diff_density_min -0.45 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 0.0013(4) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.320 1.265 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.17857(3) 0.242409(6) 0.06000(3) Uani 0.01132(5) 4 1 d . . . P P 0.72964(7) 0.300957(11) 0.06523(6) Uani 0.00933(8) 4 1 d . . . O1 O 0.41673(18) 0.29125(3) 0.04942(17) Uani 0.0130(3) 4 1 d . . . O2 O 0.88452(19) 0.28947(3) 0.30252(17) Uani 0.0141(3) 4 1 d . . . O3 O 0.87168(18) 0.27788(3) -0.12987(17) Uani 0.0117(3) 4 1 d . . . O4 O 0.4294(4) 0.44776(5) 0.4203(3) Uani 0.0494(6) 4 1 d . . . O5 O 0.7081(4) 0.49457(5) 0.2832(3) Uani 0.0585(7) 4 1 d . . . O6 O -0.1058(2) 0.19765(4) 0.0668(2) Uani 0.0163(3) 4 1 d . . . C1 C 0.7679(3) 0.35549(4) 0.0141(2) Uani 0.0136(4) 4 1 d . . . C2 C 0.6641(3) 0.38486(5) 0.1627(3) Uani 0.0193(4) 4 1 d . . . C3 C 0.7118(4) 0.42677(5) 0.1275(3) Uani 0.0237(5) 4 1 d . . . C4 C 0.8634(4) 0.43979(6) -0.0546(4) Uani 0.0324(6) 4 1 d . . . C5 C 0.9594(5) 0.41089(6) -0.2047(4) Uani 0.0356(6) 4 1 d . . . C6 C 0.9116(4) 0.36908(5) -0.1713(3) Uani 0.0244(5) 4 1 d . . . C7 C 0.6111(4) 0.45867(6) 0.2867(3) Uani 0.0306(5) 4 1 d . . . H2 H 0.573(4) 0.3762(7) 0.293(4) Uiso 0.030(6) 4 1 d . . . H4 H 0.899(5) 0.4674(9) -0.074(4) Uiso 0.051(7) 4 1 d . . . H5 H 1.046(4) 0.4195(8) -0.336(4) Uiso 0.033(6) 4 1 d . . . H6 H 0.971(4) 0.3498(7) -0.281(3) Uiso 0.024(5) 4 1 d . . . H41 H 0.384(8) 0.4679(14) 0.506(7) Uiso 0.117(15) 4 1 d . . . H61 H -0.238(4) 0.1990(7) -0.021(4) Uiso 0.032(6) 4 1 d . . . H62 H -0.171(5) 0.1978(8) 0.176(5) Uiso 0.045(7) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Cu Cu 0.00957(8) 0.01286(8) 0.01140(8) -0.00100(6) 0.00045(5) 0.00098(6) P P 0.00846(14) 0.01006(15) 0.00954(15) -0.00023(12) 0.00124(11) 0.00024(12) O1 O 0.0080(4) 0.0150(5) 0.0159(5) -0.0010(4) 0.0012(3) 0.0000(4) O2 O 0.0104(4) 0.0201(5) 0.0113(4) -0.0014(4) -0.0012(3) 0.0027(4) O3 O 0.0091(4) 0.0145(5) 0.0116(4) 0.0011(4) 0.0014(3) -0.0025(4) O4 O 0.0677(11) 0.0271(8) 0.0616(11) -0.0101(8) 0.0452(9) -0.0156(7) O5 O 0.0893(13) 0.0189(7) 0.0769(13) -0.0167(8) 0.0548(11) -0.0201(8) O6 O 0.0148(5) 0.0204(6) 0.0133(5) -0.0038(4) -0.0008(4) 0.0014(4) C1 C 0.0142(6) 0.0102(6) 0.0169(6) -0.0010(5) 0.0032(5) 0.0004(5) C2 C 0.0242(7) 0.0150(7) 0.0201(7) -0.0022(6) 0.0091(6) -0.0024(5) C3 C 0.0319(8) 0.0143(7) 0.0268(8) -0.0011(6) 0.0122(7) -0.0041(6) C4 C 0.0486(11) 0.0133(7) 0.0390(10) -0.0061(8) 0.0220(9) -0.0009(7) C5 C 0.0552(12) 0.0196(8) 0.0374(11) -0.0052(8) 0.0305(10) 0.0026(7) C6 C 0.0342(9) 0.0154(7) 0.0268(8) -0.0004(6) 0.0177(7) -0.0002(6) C7 C 0.0408(10) 0.0181(8) 0.0356(10) -0.0025(7) 0.0173(8) -0.0069(7) #======================================================================= # 10. MOLECULAR GEOMETRY 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 Cu O1 . . 1.9688(10) yes Cu O2 . 4_454 2.1450(11) yes Cu O3 . 1_455 2.0989(10) yes Cu O3 . 4_455 2.0437(11) yes Cu O6 . . 2.0079(12) yes P O1 . . 1.5410(10) yes P O2 . . 1.5395(11) yes P O3 . . 1.5730(12) yes P C1 . . 1.8125(13) yes O4 O5 . . 2.235(3) yes O4 C7 . . 1.281(3) yes O4 H41 . . 0.87(4) yes O5 C7 . . 1.261(3) yes O5 H41 . 3_666 1.81(4) yes O6 H61 . . 0.78(2) yes O6 H62 . . 0.74(3) yes C1 C2 . . 1.413(2) yes C1 C6 . . 1.409(2) yes C2 C3 . . 1.402(2) yes C2 H2 . . 0.95(2) yes C3 C4 . . 1.411(3) yes C3 C7 . . 1.503(3) yes C4 C5 . . 1.393(3) yes C4 H4 . . 0.92(3) yes C5 C6 . . 1.398(3) yes C5 H5 . . 0.95(2) yes C6 H6 . . 0.96(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu O2 . . 4_454 93.03(4) yes O1 Cu O3 . . 1_455 85.64(4) yes O1 Cu O3 . . 4_455 94.18(4) yes O1 Cu O6 . . . 172.61(4) yes O2 Cu O3 4_454 . 1_455 104.94(4) yes O2 Cu O3 4_454 . 4_455 104.47(4) yes O2 Cu O6 4_454 . . 91.83(4) yes O3 Cu O3 1_455 . 4_455 150.55(4) yes O3 Cu O6 1_455 . . 87.73(4) yes O3 Cu O3 4_455 . 1_455 150.55(4) yes O3 Cu O6 4_455 . . 89.99(4) yes O1 P O2 . . . 112.77(6) yes O1 P O3 . . . 111.13(6) yes O1 P C1 . . . 107.93(6) yes O2 P O3 . . . 108.36(6) yes O2 P C1 . . . 109.57(6) yes O3 P C1 . . . 106.92(6) yes Cu O3 Cu 1_655 . 4_554 121.01(5) yes Cu O3 Cu 4_554 . 1_655 121.01(5) yes C7 O5 H41 . . 3_666 119.6(12) yes H41 O5 H41 . . 3_666 69.2(15) yes H41 O5 H41 3_666 . . 69.2(15) yes H61 O6 H62 . . . 99(3) yes C2 C1 C6 . . . 119.07(13) yes C1 C2 C3 . . . 119.71(15) yes C1 C2 H2 . . . 120.2(14) yes C3 C2 H2 . . . 119.9(14) yes C2 C3 C4 . . . 120.48(16) yes C2 C3 C7 . . . 120.97(16) yes C4 C3 C7 . . . 118.52(16) yes C3 C4 C5 . . . 119.75(18) yes C3 C4 H4 . . . 120.1(16) yes C5 C4 H4 . . . 120.2(16) yes C4 C5 C6 . . . 120.1(2) yes C4 C5 H5 . . . 120.3(16) yes C6 C5 H5 . . . 119.5(16) yes C1 C6 C5 . . . 120.87(17) yes C1 C6 H6 . . . 120.3(13) yes C5 C6 H6 . . . 118.8(13) yes O4 C7 O5 . . . 123.20(19) yes O4 C7 C3 . . . 117.75(17) yes O5 C7 C3 . . . 119.05(18) yes #======================================================================= # Attachment 'compound 1- 5-11-08.cif' #======================================================================= data_(I) _database_code_depnum_ccdc_archive 'CCDC 692181' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28 H16 Cu6 O20 P4, 7(H2 O1)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C28 H30 Cu6 O27 P4' _chemical_formula_weight 1303.7 _chemical_melting_point ? _chemical_compound_source 'hydrothermal synthesis' _chemical_absolute_configuration ad #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 65 2 2' _symmetry_space_group_name_Hall 'P 65 2 ( 0 0 1 )' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x-y,x,5/6+z 3 -y,-x,1/6-z 4 -y,x-y,2/3+z 5 x-y,-y,-z 6 -x,-y,1/2+z 7 x,x-y,5/6-z 8 -x+y,-x,1/3+z 9 y,x,2/3-z 10 y,-x+y,1/6+z 11 -x+y,y,1/2-z 12 -x,-x+y,1/3-z _cell_length_a 14.656(3) _cell_length_b 14.656(3) _cell_length_c 16.905(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3144.8(10) _cell_formula_units_Z 3 _cell_measurement_reflns_used 100 _cell_measurement_theta_min 6. _cell_measurement_theta_max 30. _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.0645 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1926 _exptl_absorpt_coefficient_mu 3.238 _exptl_crystal_description needle _exptl_crystal_size_max 0.378 _exptl_crystal_size_mid 0.064 _exptl_crystal_size_min 0.056 _exptl_crystal_size_rad ? _exptl_crystal_colour green _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.843 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Nonius CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\F/\W scan' _diffrn_reflns_number 18435 _diffrn_reflns_theta_min 5.92 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0917 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 3051 _reflns_number_gt 1881 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_gt 0.0493 _refine_ls_R_factor_all 0.0972 _refine_ls_wR_factor_ref 0.0528 _refine_ls_goodness_of_fit_ref 1.56 _refine_ls_goodness_of_fit_gt 1.89 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 3051 _refine_ls_number_parameters 171 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max 0.0017 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 1.01 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details friedel-pairs _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.320 1.265 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cu1 Cu 0.11674(6) 0.43944(6) 0.19164(4) Uani 0.0316(4) 12 1 d . . . . Cu2 Cu 0 0.16385(7) 0.166667 Uani 0.0304(4) 6 1 d . . . . P P 0.23500(10) 0.31562(11) 0.16090(8) Uani 0.0220(6) 12 1 d . . . . O1 O 0.2553(3) 0.3018(3) 0.2492(2) Uani 0.0250(17) 12 1 d . . . . O2 O 0.2264(3) 0.4146(3) 0.1477(3) Uani 0.041(2) 12 1 d . . . . O3 O 0.1381(3) 0.2170(3) 0.1302(2) Uani 0.0410(19) 12 1 d . . . . O4 O 0.5011(3) 0.5478(3) -0.0775(2) Uani 0.0267(17) 12 1 d . . . . O5 O 0.6009(3) 0.4729(3) -0.1032(2) Uani 0.0318(19) 12 1 d . . . . O6 O 0.2903(4) 0.5805(8) 0.25 Uani 0.087(5) 6 1 d . . . 2 O7 O 0.3693(3) 0.6307(3) 0.083333 Uani 0.072(4) 6 1 d . . . 2 O8 O 0.1390(12) 0.1240(11) -0.0151(8) Uani 0.130(10) 12 0.5 d . . . 2 O9 O -0.0338(6) 0.0338(6) 0.083333 Uani 0.241(11) 6 1 d . . . 2 C1 C 0.3428(4) 0.3222(4) 0.1021(3) Uani 0.019(2) 12 1 d . . . . C2 C 0.3925(4) 0.3971(3) 0.0418(3) Uani 0.022(2) 12 1 d . . . . C3 C 0.4700(4) 0.3951(4) -0.0042(3) Uani 0.018(2) 12 1 d . . . . C4 C 0.4978(5) 0.3169(4) 0.0094(3) Uani 0.030(3) 12 1 d . . . . C5 C 0.4506(5) 0.2454(5) 0.0694(4) Uani 0.035(3) 12 1 d . . . . C6 C 0.3729(5) 0.2472(5) 0.1165(4) Uani 0.033(3) 12 1 d . . . . C7 C 0.5276(4) 0.4776(4) -0.0672(3) Uani 0.021(2) 12 1 d . . . . H2 H 0.3778(3) 0.4423 0.0351(5) Uiso 0.05(2) 12 1 d . . . . H4 H 0.542(4) 0.316(4) -0.012(3) Uiso 0.018(14) 12 1 d . . . . H5 H 0.477(5) 0.213(4) 0.090(4) Uiso 0.037(18) 12 1 d . . . . H6 H 0.352(5) 0.211(5) 0.156(4) Uiso 0.05(2) 12 1 d . . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Cu1 Cu 0.0429(5) 0.0425(4) 0.0267(4) 0.0343(4) 0.0155(3) 0.0167(3) Cu2 Cu 0.0177(5) 0.0319(4) 0.0368(6) 0.0088(2) 0.0003(4) 0.0002(2) P P 0.0198(7) 0.0303(8) 0.0178(7) 0.0140(6) 0.0002(6) -0.0047(6) O1 O 0.027(2) 0.029(2) 0.021(2) 0.0158(18) 0.0058(16) -0.0030(15) O2 O 0.037(2) 0.044(3) 0.053(3) 0.029(2) 0.020(2) 0.019(2) O3 O 0.014(2) 0.052(3) 0.043(3) 0.0054(19) 0.0023(17) -0.020(2) O4 O 0.026(2) 0.020(2) 0.032(2) 0.0094(18) -0.0007(16) 0.0023(16) O5 O 0.030(2) 0.036(2) 0.030(2) 0.0168(20) 0.0103(17) 0.0142(17) O6 O 0.083(5) 0.102(7) 0.083(6) 0.051(4) -0.006(4) 0 O7 O 0.050(3) 0.050(3) 0.123(7) 0.029(4) 0.029(4) 0.029(4) O8 O 0.109(11) 0.146(14) 0.116(11) 0.050(10) -0.034(9) -0.112(10) O9 O 0.103(8) 0.103(8) 0.51(3) 0.041(9) -0.018(12) -0.018(12) C1 C 0.017(3) 0.028(3) 0.015(3) 0.014(2) 0.0015(19) -0.001(2) C2 C 0.018(3) 0.024(3) 0.027(3) 0.012(2) -0.002(2) -0.003(2) C3 C 0.018(2) 0.021(2) 0.015(3) 0.010(2) -0.001(2) 0.000(2) C4 C 0.029(3) 0.033(3) 0.037(4) 0.022(3) 0.021(3) 0.002(3) C5 C 0.051(4) 0.041(4) 0.033(4) 0.038(4) 0.012(3) 0.012(3) C6 C 0.031(3) 0.041(4) 0.022(3) 0.015(3) 0.011(2) 0.012(3) C7 C 0.019(3) 0.023(3) 0.012(2) 0.005(2) -0.003(2) -0.002(2) #======================================================================= # 10. MOLECULAR GEOMETRY 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 Cu1 O1 . 11_555 2.013(4) yes Cu1 O2 . . 1.963(5) yes Cu1 O4 . 8_565 1.971(6) yes Cu1 O5 . 5_565 1.924(4) yes Cu1 O6 . . 2.542(5) yes Cu2 O1 . 2_554 2.280(5) yes Cu2 O1 . 11_555 2.280(4) yes Cu2 O3 . . 1.873(4) yes Cu2 O3 . 12_555 1.873(4) yes Cu2 O9 . . 2.218(7) yes Cu2 O9 . 10_555 2.218(11) yes P O1 . . 1.555(4) yes P O2 . . 1.534(5) yes P O3 . . 1.524(3) yes P C1 . . 1.828(6) yes O1 O3 . . 2.531(5) yes O2 O3 . . 2.530(6) yes O4 O5 . . 2.267(8) yes O4 C7 . . 1.280(9) yes O5 C7 . . 1.266(8) yes C1 C2 . . 1.405(7) yes C1 C6 . . 1.395(11) yes C2 C3 . . 1.389(9) yes C2 H2 . . 0.800(7) yes C3 C4 . . 1.414(10) yes C3 C7 . . 1.513(7) yes C4 C5 . . 1.371(8) yes C4 H4 . . 0.75(6) yes C5 C6 . . 1.401(11) yes C5 H5 . . 0.82(8) yes C6 H6 . . 0.81(7) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O2 11_555 . . 93.3(2) yes O1 Cu1 O4 11_555 . 8_565 92.9(2) yes O1 Cu1 O5 11_555 . 5_565 152.30(17) yes O1 Cu1 O6 11_555 . . 115.1(2) yes O2 Cu1 O4 . . 8_565 161.10(18) yes O2 Cu1 O5 . . 5_565 91.4(2) yes O2 Cu1 O6 . . . 73.6(2) yes O4 Cu1 O5 8_565 . 5_565 91.3(2) yes O4 Cu1 O6 8_565 . . 87.6(2) yes O5 Cu1 O6 5_565 . . 92.4(2) yes O1 Cu2 O1 2_554 . 11_555 84.98(17) yes O1 Cu2 O3 2_554 . . 97.40(19) yes O1 Cu2 O3 2_554 . 12_555 93.1(2) yes O1 Cu2 O9 2_554 . . 96.0(2) yes O1 Cu2 O9 2_554 . 10_555 176.1(2) yes O1 Cu2 O1 11_555 . 2_554 84.98(17) yes O1 Cu2 O3 11_555 . . 93.14(18) yes O1 Cu2 O3 11_555 . 12_555 97.4(2) yes O1 Cu2 O9 11_555 . . 176.1(3) yes O1 Cu2 O9 11_555 . 10_555 96.0(2) yes O3 Cu2 O3 . . 12_555 165.7(3) yes O3 Cu2 O9 . . . 83.0(2) yes O3 Cu2 O9 . . 10_555 86.3(2) yes O3 Cu2 O3 12_555 . . 165.7(3) yes O3 Cu2 O9 12_555 . . 86.3(2) yes O3 Cu2 O9 12_555 . 10_555 83.0(3) yes O9 Cu2 O9 . . 10_555 83.2(3) yes O9 Cu2 O9 10_555 . . 83.2(3) yes O1 P O2 . . . 112.0(3) yes O1 P O3 . . . 110.60(19) yes O1 P C1 . . . 108.2(3) yes O2 P O3 . . . 111.7(3) yes O2 P C1 . . . 110.4(3) yes O3 P C1 . . . 103.7(2) yes Cu1 O1 Cu2 11_555 . 10_555 110.80(15) yes Cu1 O1 P 11_555 . . 112.1(2) yes Cu2 O1 P 10_555 . . 130.42(18) yes Cu1 O2 P . . . 125.6(2) yes Cu2 O3 P . . . 125.7(3) yes Cu1 O4 C7 4_664 . . 133.1(4) yes Cu1 O5 C7 5_665 . . 124.3(4) yes Cu1 O6 Cu1 . . 11_555 90.4(3) yes Cu2 O9 Cu2 . . 2_554 113.1(5) yes Cu2 O9 Cu2 2_554 . . 113.1(5) yes P C1 C2 . . . 122.2(5) yes P C1 C6 . . . 118.0(4) yes C2 C1 C6 . . . 119.8(6) yes C1 C2 C3 . . . 120.0(6) yes C1 C2 H2 . . . 120.0(8) yes C3 C2 H2 . . . 120.0(7) yes C2 C3 C4 . . . 119.7(5) yes C2 C3 C7 . . . 120.8(6) yes C4 C3 C7 . . . 119.4(5) yes C3 C4 C5 . . . 120.0(7) yes C3 C4 H4 . . . 123(4) yes C5 C4 H4 . . . 117(5) yes C4 C5 C6 . . . 120.7(8) yes C4 C5 H5 . . . 123(4) yes C6 C5 H5 . . . 113(5) yes C1 C6 C5 . . . 119.7(6) yes C1 C6 H6 . . . 120(6) yes C5 C6 H6 . . . 120(6) yes O4 C7 O5 . . . 125.8(5) yes O4 C7 C3 . . . 117.8(5) yes O5 C7 C3 . . . 116.4(6) yes O5 C7 C4 . . . 87.2(4) yes