# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mark Weller' _publ_contact_author_email MTW@SOTON.AC.UK loop_ _publ_author_name 'Mark Weller' 'Edward Williams' 'Samuel Morris' data_2010erw0100_tri_p1 _database_code_depnum_ccdc_archive 'CCDC 884286' _audit_update_record ; 2012-05-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cs2 Cu3 F4 O12 P4' _chemical_formula_weight 848.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 5.4162(3) _cell_length_b 7.9373(4) _cell_length_c 9.3034(4) _cell_angle_alpha 84.198(3) _cell_angle_beta 73.305(3) _cell_angle_gamma 71.229(3) _cell_volume 362.70(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8202 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 389 _exptl_absorpt_coefficient_mu 9.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8273 _exptl_absorpt_correction_T_max 0.9079 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2957 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.85 _reflns_number_total 2957 _reflns_number_gt 2290 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0000P)^2^+14.4748P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _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 0.35(9) _refine_ls_number_reflns 2957 _refine_ls_number_parameters 141 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.002 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 O2 O 0.075(4) 0.487(3) 0.671(2) 0.024(5) Uiso 1 1 d . . . F3 F 0.894(4) 0.045(3) 0.876(2) 0.022(4) Uiso 1 1 d . . . O4 O 1.122(6) -0.176(4) 0.687(3) 0.034(6) Uiso 1 1 d . . . O6 O 1.038(3) -0.276(2) 0.9415(19) 0.021(4) Uiso 1 1 d . . . O7 O 0.247(3) 0.5335(18) 0.1819(16) 0.015(3) Uiso 1 1 d . . . O9 O 0.358(4) -0.197(2) 0.370(2) 0.034(4) Uiso 1 1 d . . . O10 O 0.346(3) -0.100(2) 0.1030(17) 0.020(4) Uiso 1 1 d . . . F4 F 0.595(4) 0.238(3) 0.193(3) 0.029(5) Uani 1 1 d . . . O14 O 0.447(4) 0.434(2) 0.408(2) 0.029(4) Uiso 1 1 d . . . O17 O 0.785(3) 0.470(2) 0.214(2) 0.034(4) Uiso 1 1 d . . . F2 F 0.109(4) 0.090(3) 0.319(2) 0.026(5) Uiso 1 1 d . . . O19 O -0.023(4) -0.176(3) 0.363(2) 0.045(5) Uiso 1 1 d . . . O20 O -0.406(5) 0.504(3) 0.841(3) 0.029(6) Uiso 1 1 d . . . F1 F -0.170(4) 0.290(3) 0.643(2) 0.021(4) Uiso 1 1 d . . . O22 O 0.657(4) -0.152(3) 0.823(2) 0.016(4) Uiso 1 1 d . . . O21 O -0.309(3) 0.586(2) 0.5429(17) 0.011(3) Uiso 1 1 d . . . P1 P -0.2124(18) 0.4834(12) 0.6802(9) 0.0166(18) Uiso 1 1 d . . . P6 P 0.504(2) 0.4391(14) 0.2450(10) 0.023(2) Uiso 1 1 d . . . P7 P 0.9239(17) -0.1564(11) 0.8338(10) 0.0181(19) Uani 1 1 d . . . P8 P 0.1937(17) -0.1048(12) 0.2729(9) 0.0145(17) Uiso 1 1 d . . . Cu3 Cu 0.4293(11) 0.7109(7) 0.9644(5) 0.0369(13) Uani 1 1 d . . . Cu4 Cu 0.2847(12) -0.3779(8) 0.5510(6) 0.0406(14) Uani 1 1 d . . . Cu5A Cu 0.860(2) -0.3228(14) 0.2376(10) 0.0209(9) Uani 0.411(7) 1 d P . . Cu5B Cu 0.9106(10) -0.3883(7) 0.3298(6) 0.0209(9) Uani 0.589(7) 1 d P . . Cs1 Cs 0.4798(2) 0.06130(16) 0.55481(13) 0.0189(4) Uani 1 1 d . . . Cs2 Cs 0.2287(2) 0.27480(16) 0.96033(13) 0.0208(5) 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 F4 0.039(10) 0.012(7) 0.037(9) -0.006(6) -0.010(7) -0.009(6) P7 0.015(3) 0.007(3) 0.034(4) 0.000(2) -0.007(2) -0.007(2) Cu3 0.056(4) 0.026(3) 0.028(2) -0.019(2) 0.008(2) -0.021(3) Cu4 0.062(4) 0.034(3) 0.028(3) -0.010(2) 0.007(3) -0.032(3) Cu5A 0.024(2) 0.017(3) 0.019(2) -0.0050(18) 0.0042(17) -0.0104(18) Cu5B 0.024(2) 0.017(3) 0.019(2) -0.0050(18) 0.0042(17) -0.0104(18) Cs1 0.0242(10) 0.0165(10) 0.0162(8) -0.0003(8) -0.0034(8) -0.0083(8) Cs2 0.0268(11) 0.0185(10) 0.0169(9) -0.0015(8) -0.0022(8) -0.0096(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 P1 1.55(2) . ? O2 Cu4 1.87(2) 1_565 ? O2 Cs2 3.20(2) . ? O2 Cs1 3.47(2) . ? F3 P7 1.63(2) . ? F3 Cs2 3.232(19) 1_655 ? F3 Cs2 3.37(2) . ? F3 Cs1 3.70(2) 1_655 ? O4 P7 1.46(3) . ? O4 Cu4 1.95(3) 1_655 ? O4 Cs1 3.05(3) 1_655 ? O6 P7 1.439(19) . ? O6 Cu3 2.159(18) 1_645 ? O6 Cs2 3.381(18) 1_645 ? O7 P6 1.597(16) . ? O7 Cu5B 1.897(16) 1_465 ? O7 Cu5A 1.979(19) 1_465 ? O7 Cs2 3.095(14) 1_554 ? O9 P8 1.431(19) . ? O9 Cu4 2.135(19) . ? O9 Cs1 3.138(18) . ? O10 P8 1.561(18) . ? O10 Cu3 1.931(16) 1_544 ? O10 Cs2 3.082(16) 1_554 ? F4 P6 1.60(2) . ? F4 Cs2 3.27(2) 1_554 ? F4 Cs1 3.48(2) . ? F4 Cs2 3.58(2) 1_654 ? O14 P6 1.454(19) . ? O14 Cu4 1.915(19) 1_565 ? O14 Cs1 3.104(18) . ? O17 P6 1.559(19) . ? O17 Cu5A 1.865(19) 1_565 ? O17 Cu5B 2.013(17) 1_565 ? O17 Cs2 2.973(18) 1_654 ? F2 P8 1.53(2) . ? F2 Cs1 3.32(2) . ? F2 Cs2 3.48(2) 1_554 ? F2 Cs1 3.55(2) 1_455 ? O19 P8 1.47(2) . ? O19 Cu5B 1.90(2) 1_455 ? O19 Cu5A 2.07(2) 1_455 ? O19 Cs1 2.94(2) 1_455 ? O20 P1 1.55(3) . ? O20 Cu3 1.91(3) 1_455 ? O20 Cs2 3.02(3) 1_455 ? O20 Cs2 3.76(2) . ? F1 P1 1.54(2) . ? F1 Cs1 3.30(2) . ? F1 Cs1 3.316(19) 1_455 ? F1 Cs2 3.739(19) 1_455 ? O22 P7 1.47(2) . ? O22 Cu3 2.020(19) 1_545 ? O22 Cs1 3.079(18) . ? O22 Cs2 3.55(2) . ? O21 P1 1.570(16) . ? O21 Cu5B 2.026(16) 1_465 ? O21 Cu4 2.107(16) 1_465 ? O21 Cs1 3.576(16) 1_465 ? P1 Cs2 3.924(8) . ? P1 Cs2 4.064(9) 1_455 ? P1 Cs1 4.103(9) . ? P6 Cs2 3.892(9) 1_554 ? P6 Cs2 3.945(10) 1_654 ? P6 Cs1 3.950(9) . ? P7 Cs1 3.938(8) . ? P7 Cs1 4.091(9) 1_655 ? P7 Cs2 4.153(9) . ? P8 Cs1 3.893(9) 1_455 ? P8 Cs1 3.920(8) . ? P8 Cs2 3.981(8) 1_554 ? Cu3 O20 1.91(3) 1_655 ? Cu3 O10 1.931(16) 1_566 ? Cu3 O22 2.02(2) 1_565 ? Cu3 O6 2.159(18) 1_465 ? Cu3 Cs2 3.954(6) . ? Cu3 Cs2 4.251(6) 1_565 ? Cu4 O2 1.87(2) 1_545 ? Cu4 O14 1.915(19) 1_545 ? Cu4 O4 1.95(3) 1_455 ? Cu4 O21 2.107(16) 1_645 ? Cu4 Cs1 3.961(6) . ? Cu4 Cs1 4.230(6) 1_545 ? Cu5A Cu5B 1.017(14) . ? Cu5A O17 1.865(19) 1_545 ? Cu5A O7 1.979(18) 1_645 ? Cu5A O19 2.07(2) 1_655 ? Cu5A Cs2 3.930(10) 1_644 ? Cu5A Cs1 4.066(10) . ? Cu5B O7 1.897(16) 1_645 ? Cu5B O19 1.90(2) 1_655 ? Cu5B O17 2.013(17) 1_545 ? Cu5B O21 2.026(16) 1_645 ? Cu5B Cs1 3.988(5) . ? Cu5B Cs2 4.174(5) 1_644 ? Cs1 O19 2.94(2) 1_655 ? Cs1 O4 3.05(3) 1_455 ? Cs1 F1 3.316(19) 1_655 ? Cs1 F2 3.55(2) 1_655 ? Cs1 O21 3.576(16) 1_645 ? Cs2 O17 2.973(18) 1_456 ? Cs2 O20 3.02(3) 1_655 ? Cs2 O10 3.082(16) 1_556 ? Cs2 O7 3.095(14) 1_556 ? Cs2 F3 3.232(19) 1_455 ? Cs2 F4 3.27(2) 1_556 ? Cs2 O6 3.381(18) 1_465 ? Cs2 F2 3.48(2) 1_556 ? Cs2 F4 3.58(2) 1_456 ? 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 O2 Cu4 131.0(13) . 1_565 ? P1 O2 Cs2 106.4(10) . . ? Cu4 O2 Cs2 121.4(9) 1_565 . ? P1 O2 Cs1 103.1(10) . . ? Cu4 O2 Cs1 100.6(8) 1_565 . ? Cs2 O2 Cs1 73.2(4) . . ? P7 F3 Cs2 141.6(10) . 1_655 ? P7 F3 Cs2 107.0(9) . . ? Cs2 F3 Cs2 110.2(6) 1_655 . ? P7 F3 Cs1 91.7(9) . 1_655 ? Cs2 F3 Cs1 69.6(4) 1_655 1_655 ? Cs2 F3 Cs1 133.4(5) . 1_655 ? P7 O4 Cu4 129.9(17) . 1_655 ? P7 O4 Cs1 126.3(15) . 1_655 ? Cu4 O4 Cs1 102.4(11) 1_655 1_655 ? P7 O6 Cu3 120.4(11) . 1_645 ? P7 O6 Cs2 129.9(9) . 1_645 ? Cu3 O6 Cs2 88.2(6) 1_645 1_645 ? P6 O7 Cu5B 115.3(9) . 1_465 ? P6 O7 Cu5A 144.3(10) . 1_465 ? Cu5B O7 Cu5A 30.3(4) 1_465 1_465 ? P6 O7 Cs2 107.8(7) . 1_554 ? Cu5B O7 Cs2 111.2(6) 1_465 1_554 ? Cu5A O7 Cs2 99.2(6) 1_465 1_554 ? P8 O9 Cu4 130.1(12) . . ? P8 O9 Cs1 112.7(10) . . ? Cu4 O9 Cs1 95.5(6) . . ? P8 O10 Cu3 124.2(10) . 1_544 ? P8 O10 Cs2 114.0(8) . 1_554 ? Cu3 O10 Cs2 114.0(7) 1_544 1_554 ? P6 F4 Cs2 100.7(9) . 1_554 ? P6 F4 Cs1 94.9(10) . . ? Cs2 F4 Cs1 126.5(7) 1_554 . ? P6 F4 Cs2 91.1(9) . 1_654 ? Cs2 F4 Cs2 104.6(6) 1_554 1_654 ? Cs1 F4 Cs2 126.1(6) . 1_654 ? P6 O14 Cu4 130.6(12) . 1_565 ? P6 O14 Cs1 115.3(10) . . ? Cu4 O14 Cs1 112.7(7) 1_565 . ? P6 O17 Cu5A 128.7(12) . 1_565 ? P6 O17 Cu5B 130.0(11) . 1_565 ? Cu5A O17 Cu5B 30.1(5) 1_565 1_565 ? P6 O17 Cs2 117.6(9) . 1_654 ? Cu5A O17 Cs2 106.4(8) 1_565 1_654 ? Cu5B O17 Cs2 112.3(7) 1_565 1_654 ? P8 F2 Cs1 101.3(9) . . ? P8 F2 Cs2 97.5(10) . 1_554 ? Cs1 F2 Cs2 124.7(6) . 1_554 ? P8 F2 Cs1 91.2(10) . 1_455 ? Cs1 F2 Cs1 104.1(6) . 1_455 ? Cs2 F2 Cs1 127.1(6) 1_554 1_455 ? P8 O19 Cu5B 127.5(13) . 1_455 ? P8 O19 Cu5A 112.7(12) . 1_455 ? Cu5B O19 Cu5A 29.2(5) 1_455 1_455 ? P8 O19 Cs1 120.2(11) . 1_455 ? Cu5B O19 Cs1 109.1(8) 1_455 1_455 ? Cu5A O19 Cs1 107.2(8) 1_455 1_455 ? P1 O20 Cu3 128.8(16) . 1_455 ? P1 O20 Cs2 122.3(13) . 1_455 ? Cu3 O20 Cs2 104.4(10) 1_455 1_455 ? P1 O20 Cs2 84.5(10) . . ? Cu3 O20 Cs2 103.1(8) 1_455 . ? Cs2 O20 Cs2 105.7(7) 1_455 . ? P1 F1 Cs1 110.8(9) . . ? P1 F1 Cs1 137.5(10) . 1_455 ? Cs1 F1 Cs1 110.0(6) . 1_455 ? P1 F1 Cs2 90.9(9) . 1_455 ? Cs1 F1 Cs2 134.8(6) . 1_455 ? Cs1 F1 Cs2 68.3(4) 1_455 1_455 ? P7 O22 Cu3 122.9(11) . 1_545 ? P7 O22 Cs1 115.4(10) . . ? Cu3 O22 Cs1 121.6(8) 1_545 . ? P7 O22 Cs2 103.7(10) . . ? Cu3 O22 Cs2 95.5(7) 1_545 . ? Cs1 O22 Cs2 73.3(4) . . ? P1 O21 Cu5B 129.6(10) . 1_465 ? P1 O21 Cu4 115.6(9) . 1_465 ? Cu5B O21 Cu4 110.8(7) 1_465 1_465 ? P1 O21 Cs1 116.7(8) . 1_465 ? Cu5B O21 Cs1 86.1(5) 1_465 1_465 ? Cu4 O21 Cs1 84.1(5) 1_465 1_465 ? F1 P1 O2 103.9(12) . . ? F1 P1 O20 102.4(13) . . ? O2 P1 O20 114.1(12) . . ? F1 P1 O21 101.5(10) . . ? O2 P1 O21 110.5(11) . . ? O20 P1 O21 121.5(12) . . ? F1 P1 Cs2 85.3(7) . . ? O2 P1 Cs2 51.4(8) . . ? O20 P1 Cs2 72.3(9) . . ? O21 P1 Cs2 161.9(7) . . ? F1 P1 Cs2 66.9(8) . 1_455 ? O2 P1 Cs2 136.7(8) . 1_455 ? O20 P1 Cs2 38.9(10) . 1_455 ? O21 P1 Cs2 112.7(7) . 1_455 ? Cs2 P1 Cs2 85.36(16) . 1_455 ? F1 P1 Cs1 48.7(8) . . ? O2 P1 Cs1 55.3(9) . . ? O20 P1 Cs1 122.9(10) . . ? O21 P1 Cs1 113.0(7) . . ? Cs2 P1 Cs1 59.34(12) . . ? Cs2 P1 Cs1 105.4(2) 1_455 . ? O14 P6 O17 95.7(11) . . ? O14 P6 O7 115.2(11) . . ? O17 P6 O7 132.7(10) . . ? O14 P6 F4 106.4(13) . . ? O17 P6 F4 100.6(12) . . ? O7 P6 F4 103.6(10) . . ? O14 P6 Cs2 134.3(8) . 1_554 ? O17 P6 Cs2 126.9(8) . 1_554 ? O7 P6 Cs2 49.2(6) . 1_554 ? F4 P6 Cs2 55.5(8) . 1_554 ? O14 P6 Cs2 125.4(9) . 1_654 ? O17 P6 Cs2 41.9(7) . 1_654 ? O7 P6 Cs2 119.3(7) . 1_654 ? F4 P6 Cs2 65.0(9) . 1_654 ? Cs2 P6 Cs2 87.4(2) 1_554 1_654 ? O14 P6 Cs1 45.3(8) . . ? O17 P6 Cs1 107.0(7) . . ? O7 P6 Cs1 120.3(7) . . ? F4 P6 Cs1 61.3(9) . . ? Cs2 P6 Cs1 100.3(2) 1_554 . ? Cs2 P6 Cs1 105.6(2) 1_654 . ? O6 P7 O4 110.5(13) . . ? O6 P7 O22 118.3(12) . . ? O4 P7 O22 111.9(13) . . ? O6 P7 F3 107.6(10) . . ? O4 P7 F3 100.5(14) . . ? O22 P7 F3 106.4(11) . . ? O6 P7 Cs1 161.6(8) . . ? O4 P7 Cs1 76.3(10) . . ? O22 P7 Cs1 44.9(8) . . ? F3 P7 Cs1 87.2(7) . . ? O6 P7 Cs1 111.1(8) . 1_655 ? O4 P7 Cs1 37.0(11) . 1_655 ? O22 P7 Cs1 129.7(8) . 1_655 ? F3 P7 Cs1 64.8(8) . 1_655 ? Cs1 P7 Cs1 84.81(17) . 1_655 ? O6 P7 Cs2 122.4(8) . . ? O4 P7 Cs2 124.8(11) . . ? O22 P7 Cs2 56.2(8) . . ? F3 P7 Cs2 50.9(7) . . ? Cs1 P7 Cs2 58.81(12) . . ? Cs1 P7 Cs2 104.05(19) 1_655 . ? O9 P8 O19 88.9(12) . . ? O9 P8 F2 103.2(11) . . ? O19 P8 F2 106.1(13) . . ? O9 P8 O10 115.7(12) . . ? O19 P8 O10 136.0(11) . . ? F2 P8 O10 102.9(11) . . ? O9 P8 Cs1 102.1(9) . 1_455 ? O19 P8 Cs1 40.7(8) . 1_455 ? F2 P8 Cs1 65.6(9) . 1_455 ? O10 P8 Cs1 142.1(7) . 1_455 ? O9 P8 Cs1 47.6(8) . . ? O19 P8 Cs1 107.0(9) . . ? F2 P8 Cs1 56.1(8) . . ? O10 P8 Cs1 116.7(7) . . ? Cs1 P8 Cs1 87.77(18) 1_455 . ? O9 P8 Cs2 135.2(9) . 1_554 ? O19 P8 Cs2 134.4(9) . 1_554 ? F2 P8 Cs2 60.0(9) . 1_554 ? O10 P8 Cs2 45.0(6) . 1_554 ? Cs1 P8 Cs2 106.0(2) 1_455 1_554 ? Cs1 P8 Cs2 99.29(19) . 1_554 ? O20 Cu3 O10 165.8(9) 1_655 1_566 ? O20 Cu3 O22 92.4(10) 1_655 1_565 ? O10 Cu3 O22 84.5(7) 1_566 1_565 ? O20 Cu3 O6 90.1(9) 1_655 1_465 ? O10 Cu3 O6 103.4(7) 1_566 1_465 ? O22 Cu3 O6 120.8(8) 1_565 1_465 ? O20 Cu3 Cs2 47.7(8) 1_655 . ? O10 Cu3 Cs2 137.3(5) 1_566 . ? O22 Cu3 Cs2 138.2(6) 1_565 . ? O6 Cu3 Cs2 58.7(5) 1_465 . ? O20 Cu3 Cs2 144.0(8) 1_655 1_565 ? O10 Cu3 Cs2 41.5(5) 1_566 1_565 ? O22 Cu3 Cs2 56.3(6) 1_565 1_565 ? O6 Cu3 Cs2 91.9(5) 1_465 1_565 ? Cs2 Cu3 Cs2 150.61(17) . 1_565 ? O2 Cu4 O14 89.3(9) 1_545 1_545 ? O2 Cu4 O4 93.7(11) 1_545 1_455 ? O14 Cu4 O4 176.5(10) 1_545 1_455 ? O2 Cu4 O21 124.3(8) 1_545 1_645 ? O14 Cu4 O21 82.6(7) 1_545 1_645 ? O4 Cu4 O21 97.1(9) 1_455 1_645 ? O2 Cu4 O9 151.8(9) 1_545 . ? O14 Cu4 O9 87.8(8) 1_545 . ? O4 Cu4 O9 88.7(9) 1_455 . ? O21 Cu4 O9 83.2(7) 1_645 . ? O2 Cu4 Cs1 141.7(7) 1_545 . ? O14 Cu4 Cs1 128.4(6) 1_545 . ? O4 Cu4 Cs1 48.8(8) 1_455 . ? O21 Cu4 Cs1 63.9(4) 1_645 . ? O9 Cu4 Cs1 52.1(5) . . ? O2 Cu4 Cs1 53.6(7) 1_545 1_545 ? O14 Cu4 Cs1 42.6(5) 1_545 1_545 ? O4 Cu4 Cs1 140.9(8) 1_455 1_545 ? O21 Cu4 Cs1 87.5(5) 1_645 1_545 ? O9 Cu4 Cs1 130.4(6) . 1_545 ? Cs1 Cu4 Cs1 151.38(18) . 1_545 ? Cu5B Cu5A O17 83.0(8) . 1_545 ? Cu5B Cu5A O7 70.4(8) . 1_645 ? O17 Cu5A O7 86.7(8) 1_545 1_645 ? Cu5B Cu5A O19 66.0(8) . 1_655 ? O17 Cu5A O19 148.9(9) 1_545 1_655 ? O7 Cu5A O19 85.0(8) 1_645 1_655 ? Cu5B Cu5A Cs2 96.8(6) . 1_644 ? O17 Cu5A Cs2 46.5(6) 1_545 1_644 ? O7 Cu5A Cs2 51.0(4) 1_645 1_644 ? O19 Cu5A Cs2 135.9(7) 1_655 1_644 ? Cu5B Cu5A Cs1 78.4(5) . . ? O17 Cu5A Cs1 130.3(6) 1_545 . ? O7 Cu5A Cs1 127.8(5) 1_645 . ? O19 Cu5A Cs1 43.7(6) 1_655 . ? Cs2 Cu5A Cs1 174.9(3) 1_644 . ? Cu5A Cu5B O7 79.3(7) . 1_645 ? Cu5A Cu5B O19 84.8(8) . 1_655 ? O7 Cu5B O19 92.2(8) 1_645 1_655 ? Cu5A Cu5B O17 66.9(7) . 1_545 ? O7 Cu5B O17 84.8(7) 1_645 1_545 ? O19 Cu5B O17 151.6(7) 1_655 1_545 ? Cu5A Cu5B O21 132.9(8) . 1_645 ? O7 Cu5B O21 147.4(6) 1_645 1_645 ? O19 Cu5B O21 95.8(8) 1_655 1_645 ? O17 Cu5B O21 101.9(7) 1_545 1_645 ? Cu5A Cu5B Cs1 87.1(6) . . ? O7 Cu5B Cs1 135.5(5) 1_645 . ? O19 Cu5B Cs1 44.1(6) 1_655 . ? O17 Cu5B Cs1 127.9(5) 1_545 . ? O21 Cu5B Cs1 63.4(5) 1_645 . ? Cu5A Cu5B Cs2 69.2(6) . 1_644 ? O7 Cu5B Cs2 43.7(4) 1_645 1_644 ? O19 Cu5B Cs2 130.9(6) 1_655 1_644 ? O17 Cu5B Cs2 41.2(5) 1_545 1_644 ? O21 Cu5B Cs2 132.5(5) 1_645 1_644 ? Cs1 Cu5B Cs2 156.24(16) . 1_644 ? O19 Cs1 O4 104.6(7) 1_655 1_455 ? O19 Cs1 O22 86.4(5) 1_655 . ? O4 Cs1 O22 70.5(6) 1_455 . ? O19 Cs1 O14 103.9(5) 1_655 . ? O4 Cs1 O14 140.6(6) 1_455 . ? O22 Cs1 O14 138.0(5) . . ? O19 Cs1 O9 67.8(5) 1_655 . ? O4 Cs1 O9 55.0(6) 1_455 . ? O22 Cs1 O9 107.4(5) . . ? O14 Cs1 O9 114.2(5) . . ? O19 Cs1 F1 153.9(5) 1_655 . ? O4 Cs1 F1 67.9(6) 1_455 . ? O22 Cs1 F1 112.6(5) . . ? O14 Cs1 F1 74.5(5) . . ? O9 Cs1 F1 88.9(5) . . ? O19 Cs1 F1 91.0(5) 1_655 1_655 ? O4 Cs1 F1 143.0(6) 1_455 1_655 ? O22 Cs1 F1 77.4(5) . 1_655 ? O14 Cs1 F1 62.1(5) . 1_655 ? O9 Cs1 F1 157.5(5) . 1_655 ? F1 Cs1 F1 110.0(6) . 1_655 ? O19 Cs1 F2 94.8(6) 1_655 . ? O4 Cs1 F2 74.0(6) 1_455 . ? O22 Cs1 F2 143.6(5) . . ? O14 Cs1 F2 77.0(5) . . ? O9 Cs1 F2 42.1(5) . . ? F1 Cs1 F2 59.3(5) . . ? F1 Cs1 F2 138.9(5) 1_655 . ? O19 Cs1 O2 149.8(5) 1_655 . ? O4 Cs1 O2 105.0(6) 1_455 . ? O22 Cs1 O2 109.1(5) . . ? O14 Cs1 O2 47.4(5) . . ? O9 Cs1 O2 127.2(5) . . ? F1 Cs1 O2 42.0(5) . . ? F1 Cs1 O2 68.5(5) 1_655 . ? F2 Cs1 O2 87.6(5) . . ? O19 Cs1 F4 70.9(5) 1_655 . ? O4 Cs1 F4 126.5(6) 1_455 . ? O22 Cs1 F4 154.0(5) . . ? O14 Cs1 F4 43.1(5) . . ? O9 Cs1 F4 76.2(5) . . ? F1 Cs1 F4 93.0(5) . . ? F1 Cs1 F4 90.1(5) 1_655 . ? F2 Cs1 F4 54.2(4) . . ? O2 Cs1 F4 86.6(5) . . ? O19 Cs1 F2 42.2(5) 1_655 1_655 ? O4 Cs1 F2 146.8(7) 1_455 1_655 ? O22 Cs1 F2 101.0(5) . 1_655 ? O14 Cs1 F2 66.5(5) . 1_655 ? O9 Cs1 F2 100.8(5) . 1_655 ? F1 Cs1 F2 140.4(5) . 1_655 ? F1 Cs1 F2 56.8(5) 1_655 1_655 ? F2 Cs1 F2 104.1(6) . 1_655 ? O2 Cs1 F2 108.0(5) . 1_655 ? F4 Cs1 F2 53.5(4) . 1_655 ? O19 Cs1 O21 52.1(5) 1_655 1_645 ? O4 Cs1 O21 53.9(6) 1_455 1_645 ? O22 Cs1 O21 61.3(4) . 1_645 ? O14 Cs1 O21 152.6(4) . 1_645 ? O9 Cs1 O21 49.0(4) . 1_645 ? F1 Cs1 O21 120.5(4) . 1_645 ? F1 Cs1 O21 123.4(4) 1_655 1_645 ? F2 Cs1 O21 91.1(5) . 1_645 ? O2 Cs1 O21 158.1(4) . 1_645 ? F4 Cs1 O21 110.2(4) . 1_645 ? F2 Cs1 O21 93.5(4) 1_655 1_645 ? O17 Cs2 O20 107.0(6) 1_456 1_655 ? O17 Cs2 O10 98.6(5) 1_456 1_556 ? O20 Cs2 O10 130.4(5) 1_655 1_556 ? O17 Cs2 O7 51.5(4) 1_456 1_556 ? O20 Cs2 O7 62.6(6) 1_655 1_556 ? O10 Cs2 O7 107.9(4) 1_556 1_556 ? O17 Cs2 O2 103.3(5) 1_456 . ? O20 Cs2 O2 71.6(6) 1_655 . ? O10 Cs2 O2 141.8(5) 1_556 . ? O7 Cs2 O2 110.3(5) 1_556 . ? O17 Cs2 F3 96.3(5) 1_456 1_455 ? O20 Cs2 F3 145.7(6) 1_655 1_455 ? O10 Cs2 F3 67.9(4) 1_556 1_455 ? O7 Cs2 F3 147.5(5) 1_556 1_455 ? O2 Cs2 F3 78.8(5) . 1_455 ? O17 Cs2 F4 82.8(5) 1_456 1_556 ? O20 Cs2 F4 72.3(6) 1_655 1_556 ? O10 Cs2 F4 69.6(5) 1_556 1_556 ? O7 Cs2 F4 46.4(4) 1_556 1_556 ? O2 Cs2 F4 143.6(5) . 1_556 ? F3 Cs2 F4 136.9(5) 1_455 1_556 ? O17 Cs2 F3 140.3(5) 1_456 . ? O20 Cs2 F3 66.2(6) 1_655 . ? O10 Cs2 F3 67.0(5) 1_556 . ? O7 Cs2 F3 96.1(4) 1_556 . ? O2 Cs2 F3 110.3(5) . . ? F3 Cs2 F3 110.2(6) 1_455 . ? F4 Cs2 F3 57.6(5) 1_556 . ? O17 Cs2 O6 63.0(4) 1_456 1_465 ? O20 Cs2 O6 53.3(6) 1_655 1_465 ? O10 Cs2 O6 158.4(4) 1_556 1_465 ? O7 Cs2 O6 52.4(4) 1_556 1_465 ? O2 Cs2 O6 58.4(5) . 1_465 ? F3 Cs2 O6 122.6(4) 1_455 1_465 ? F4 Cs2 O6 95.5(5) 1_556 1_465 ? F3 Cs2 O6 119.1(5) . 1_465 ? O17 Cs2 F2 58.4(5) 1_456 1_556 ? O20 Cs2 F2 125.4(6) 1_655 1_556 ? O10 Cs2 F2 42.8(5) 1_556 1_556 ? O7 Cs2 F2 71.4(5) 1_556 1_556 ? O2 Cs2 F2 156.5(5) . 1_556 ? F3 Cs2 F2 88.2(5) 1_455 1_556 ? F4 Cs2 F2 54.6(4) 1_556 1_556 ? F3 Cs2 F2 92.5(5) . 1_556 ? O6 Cs2 F2 115.9(5) 1_465 1_556 ? O17 Cs2 O22 144.7(4) 1_456 . ? O20 Cs2 O22 102.2(6) 1_655 . ? O10 Cs2 O22 46.5(4) 1_556 . ? O7 Cs2 O22 133.6(4) 1_556 . ? O2 Cs2 O22 104.4(5) . . ? F3 Cs2 O22 68.4(5) 1_455 . ? F4 Cs2 O22 87.7(5) 1_556 . ? F3 Cs2 O22 41.9(5) . . ? O6 Cs2 O22 152.1(4) 1_465 . ? F2 Cs2 O22 88.6(5) 1_556 . ? O17 Cs2 F4 42.3(5) 1_456 1_456 ? O20 Cs2 F4 148.2(6) 1_655 1_456 ? O10 Cs2 F4 73.1(5) 1_556 1_456 ? O7 Cs2 F4 91.8(4) 1_556 1_456 ? O2 Cs2 F4 103.4(5) . 1_456 ? F3 Cs2 F4 55.7(5) 1_455 1_456 ? F4 Cs2 F4 104.6(6) 1_556 1_456 ? F3 Cs2 F4 139.9(4) . 1_456 ? O6 Cs2 F4 96.7(5) 1_465 1_456 ? F2 Cs2 F4 53.3(4) 1_556 1_456 ? O22 Cs2 F4 109.3(5) . 1_456 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.937 _refine_diff_density_min -2.521 _refine_diff_density_rms 0.445 # Attachment '- CsCu2(PO3F)2F_XI.cif' data_2011erw026_pnma _database_code_depnum_ccdc_archive 'CCDC 884287' #TrackingRef '- CsCu2(PO3F)2F_XI.cif' _audit_update_record ; 2012-05-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cs Cu2 F3 O6 P2' _chemical_formula_weight 474.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.0219(5) _cell_length_b 6.2059(4) _cell_length_c 14.3280(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 802.21(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6763 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 10.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2677 _exptl_absorpt_correction_T_max 0.7841 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6746 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1003 _reflns_number_gt 753 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0000P)^2^+28.4906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1003 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 0.1658(11) 0.0540(14) 0.6153(8) 0.051(3) Uani 1 1 d . . . O2 O 0.3696(11) 0.2500 0.5286(8) 0.023(3) Uani 1 2 d S . . O3B O -0.430(3) -0.039(4) 0.6280(15) 0.023(2) Uiso 0.390(13) 1 d P . . O3A O -0.4885(16) -0.048(2) 0.6346(9) 0.023(2) Uiso 0.610(13) 1 d P . . O4A O 0.031(2) -0.2500 0.7161(14) 0.031(4) Uani 0.610(13) 2 d SP . . F4B F -0.082(3) -0.2500 0.7626(18) 0.031(4) Uani 0.390(13) 2 d SP . . F1 F 0.3023(10) -0.2500 0.5038(7) 0.027(2) Uani 1 2 d S . . F5A F -0.269(2) -0.2500 0.6712(14) 0.062(6) Uani 0.610(13) 2 d SP . . O5B O 0.192(4) -0.2500 0.744(3) 0.062(6) Uani 0.390(13) 2 d SP . . F7 F 0.1136(14) 0.2500 0.4735(9) 0.090(6) Uani 1 2 d S . . P4 P 0.2091(5) 0.2500 0.5618(3) 0.0227(9) Uani 1 2 d S . . P5 P -0.4378(5) -0.2500 0.6818(3) 0.0207(9) Uani 1 2 d S . . Cu2 Cu 0.1856(3) -0.2500 0.61312(15) 0.0319(6) Uani 1 2 d S . . Cu3 Cu 0.5000 0.0000 0.5000 0.0217(4) Uani 1 2 d S . . Cs1 Cs -0.15274(13) 0.2500 0.69101(8) 0.0326(3) Uani 1 2 d S . . 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 0.057(6) 0.013(4) 0.083(7) 0.001(5) 0.050(6) -0.002(4) O2 0.010(5) 0.021(6) 0.038(6) 0.000 0.011(5) 0.000 O4A 0.034(9) 0.024(8) 0.035(9) 0.000 -0.011(7) 0.000 F4B 0.034(9) 0.024(8) 0.035(9) 0.000 -0.011(7) 0.000 F1 0.020(5) 0.019(5) 0.043(6) 0.000 0.008(4) 0.000 F5A 0.032(9) 0.109(17) 0.044(10) 0.000 0.027(8) 0.000 O5B 0.032(9) 0.109(17) 0.044(10) 0.000 0.027(8) 0.000 F7 0.035(7) 0.20(2) 0.040(7) 0.000 0.001(6) 0.000 P4 0.026(2) 0.0134(19) 0.029(2) 0.000 0.0086(18) 0.000 P5 0.027(2) 0.0144(19) 0.021(2) 0.000 0.0008(18) 0.000 Cu2 0.0569(16) 0.0109(9) 0.0280(11) 0.000 0.0144(11) 0.000 Cu3 0.0340(11) 0.0117(8) 0.0194(9) 0.0022(7) 0.0048(8) 0.0052(8) Cs1 0.0263(6) 0.0410(7) 0.0305(6) 0.000 0.0068(5) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P4 1.490(9) . ? O1 Cu2 1.895(9) . ? O1 Cs1 3.304(9) . ? O1 Cs1 3.444(12) 6_657 ? O2 P4 1.524(10) . ? O2 Cu3 1.990(6) 3_656 ? O2 Cu3 1.990(6) . ? O3B O3A 0.54(2) . ? O3B P5 1.52(2) . ? O3B Cu3 1.96(2) 1_455 ? O3B Cs1 3.21(2) . ? O3B Cs1 3.74(2) 6_557 ? O3A P5 1.494(14) . ? O3A Cu3 1.955(13) 1_455 ? O3A Cs1 3.444(14) 6_557 ? O3A Cs1 3.641(15) . ? O4A F4B 1.22(3) . ? O4A P5 1.490(19) 6_657 ? O4A O5B 1.51(4) . ? O4A Cu2 2.03(2) . ? O4A Cs1 3.535(9) 1_545 ? O4A Cs1 3.535(9) . ? F4B P5 1.53(2) 6_657 ? F4B Cs1 3.329(9) 1_545 ? F4B Cs1 3.329(9) . ? F1 Cu2 1.887(9) . ? F1 Cu3 2.365(7) . ? F1 Cu3 2.365(7) 3_646 ? F1 Cs1 3.100(10) 5_556 ? F5A O5B 1.26(4) 6_557 ? F5A P5 1.527(19) . ? F5A Cs1 3.289(7) . ? F5A Cs1 3.289(7) 1_545 ? O5B F5A 1.26(4) 6_657 ? O5B P5 1.58(3) 6_657 ? O5B Cu2 1.88(4) . ? O5B Cs1 3.53(2) 6_657 ? O5B Cs1 3.53(2) 6_647 ? F7 P4 1.531(14) . ? P4 O1 1.490(9) 7_565 ? P4 Cs1 3.753(4) . ? P4 Cs1 3.754(5) 6_657 ? P5 O4A 1.490(19) 6_557 ? P5 O3A 1.494(14) 7 ? P5 O3B 1.52(2) 7 ? P5 F4B 1.53(2) 6_557 ? P5 O5B 1.58(3) 6_557 ? P5 Cs1 4.032(3) . ? P5 Cs1 4.032(3) 1_545 ? P5 Cs1 4.088(3) 6_547 ? P5 Cs1 4.088(3) 6_557 ? Cu2 O1 1.895(9) 7 ? Cu2 Cs1 4.368(2) 5_556 ? Cu3 O3B 1.96(2) 1_655 ? Cu3 O3B 1.96(2) 5_556 ? Cu3 O3A 1.955(13) 1_655 ? Cu3 O3A 1.955(13) 5_556 ? Cu3 O2 1.990(6) 5_656 ? Cu3 F1 2.365(7) 5_656 ? Cs1 F1 3.100(10) 5_556 ? Cs1 O3B 3.21(2) 7_565 ? Cs1 F5A 3.289(7) 1_565 ? Cs1 O1 3.304(9) 7_565 ? Cs1 F4B 3.329(9) 1_565 ? Cs1 O1 3.444(12) 4_456 ? Cs1 O1 3.444(12) 6_557 ? Cs1 O3A 3.444(14) 4_556 ? 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 P4 O1 Cu2 141.2(6) . . ? P4 O1 Cs1 95.5(4) . . ? Cu2 O1 Cs1 117.0(4) . . ? P4 O1 Cs1 90.1(5) . 6_657 ? Cu2 O1 Cs1 108.7(5) . 6_657 ? Cs1 O1 Cs1 91.1(2) . 6_657 ? P4 O2 Cu3 128.8(2) . 3_656 ? P4 O2 Cu3 128.8(2) . . ? Cu3 O2 Cu3 102.5(4) 3_656 . ? O3A O3B P5 77(3) . . ? O3A O3B Cu3 82(3) . 1_455 ? P5 O3B Cu3 124.6(14) . 1_455 ? O3A O3B Cs1 141(4) . . ? P5 O3B Cs1 112.0(11) . . ? Cu3 O3B Cs1 116.5(9) 1_455 . ? O3A O3B Cs1 53(3) . 6_557 ? P5 O3B Cs1 92.1(9) . 6_557 ? Cu3 O3B Cs1 114.7(9) 1_455 6_557 ? Cs1 O3B Cs1 87.4(5) . 6_557 ? O3B O3A P5 82(3) . . ? O3B O3A Cu3 82(3) . 1_455 ? P5 O3A Cu3 126.2(9) . 1_455 ? O3B O3A Cs1 119(3) . 6_557 ? P5 O3A Cs1 104.7(6) . 6_557 ? Cu3 O3A Cs1 127.6(6) 1_455 6_557 ? O3B O3A Cs1 34(3) . . ? P5 O3A Cs1 94.1(6) . . ? Cu3 O3A Cs1 100.7(5) 1_455 . ? Cs1 O3A Cs1 85.6(3) 6_557 . ? F4B O4A P5 67.9(15) . 6_657 ? F4B O4A O5B 131(2) . . ? P5 O4A O5B 63.4(16) 6_657 . ? F4B O4A Cu2 166.6(18) . . ? P5 O4A Cu2 125.6(12) 6_657 . ? O5B O4A Cu2 62.1(16) . . ? F4B O4A Cs1 70.3(6) . 1_545 ? P5 O4A Cs1 100.9(5) 6_657 1_545 ? O5B O4A Cs1 118.6(3) . 1_545 ? Cu2 O4A Cs1 104.4(4) . 1_545 ? F4B O4A Cs1 70.3(6) . . ? P5 O4A Cs1 100.9(5) 6_657 . ? O5B O4A Cs1 118.6(3) . . ? Cu2 O4A Cs1 104.4(4) . . ? Cs1 O4A Cs1 122.7(6) 1_545 . ? O4A F4B P5 64.6(15) . 6_657 ? O4A F4B Cs1 89.5(7) . 1_545 ? P5 F4B Cs1 108.9(5) 6_657 1_545 ? O4A F4B Cs1 89.5(7) . . ? P5 F4B Cs1 108.9(5) 6_657 . ? Cs1 F4B Cs1 137.5(8) 1_545 . ? Cu2 F1 Cu3 116.1(4) . . ? Cu2 F1 Cu3 116.1(4) . 3_646 ? Cu3 F1 Cu3 82.0(3) . 3_646 ? Cu2 F1 Cs1 120.3(4) . 5_556 ? Cu3 F1 Cs1 107.9(3) . 5_556 ? Cu3 F1 Cs1 107.9(3) 3_646 5_556 ? O5B F5A P5 68.2(17) 6_557 . ? O5B F5A Cs1 90.3(7) 6_557 . ? P5 F5A Cs1 108.0(3) . . ? O5B F5A Cs1 90.3(7) 6_557 1_545 ? P5 F5A Cs1 108.0(3) . 1_545 ? Cs1 F5A Cs1 141.3(7) . 1_545 ? F5A O5B O4A 122(3) 6_657 . ? F5A O5B P5 64.0(18) 6_657 6_657 ? O4A O5B P5 57.6(14) . 6_657 ? F5A O5B Cu2 166(3) 6_657 . ? O4A O5B Cu2 72.7(19) . . ? P5 O5B Cu2 130(2) 6_657 . ? F5A O5B Cs1 68.8(9) 6_657 6_657 ? O4A O5B Cs1 116.9(6) . 6_657 ? P5 O5B Cs1 96.8(9) 6_657 6_657 ? Cu2 O5B Cs1 105.9(7) . 6_657 ? F5A O5B Cs1 68.8(9) 6_657 6_647 ? O4A O5B Cs1 116.9(6) . 6_647 ? P5 O5B Cs1 96.8(9) 6_657 6_647 ? Cu2 O5B Cs1 105.9(7) . 6_647 ? Cs1 O5B Cs1 123.2(12) 6_657 6_647 ? O1 P4 O1 109.4(7) 7_565 . ? O1 P4 O2 114.2(5) 7_565 . ? O1 P4 O2 114.2(5) . . ? O1 P4 F7 106.1(6) 7_565 . ? O1 P4 F7 106.1(6) . . ? O2 P4 F7 106.1(7) . . ? O1 P4 Cs1 61.2(4) 7_565 . ? O1 P4 Cs1 61.2(4) . . ? O2 P4 Cs1 168.6(5) . . ? F7 P4 Cs1 85.3(5) . . ? O1 P4 Cs1 66.5(5) 7_565 6_657 ? O1 P4 Cs1 66.5(5) . 6_657 ? O2 P4 Cs1 88.8(5) . 6_657 ? F7 P4 Cs1 165.1(5) . 6_657 ? Cs1 P4 Cs1 79.83(8) . 6_657 ? O4A P5 O3A 112.7(7) 6_557 7 ? O4A P5 O3A 112.7(7) 6_557 . ? O3A P5 O3A 113.8(11) 7 . ? O4A P5 O3B 120.4(8) 6_557 . ? O3A P5 O3B 120.4(8) 7 . ? O3A P5 O3B 20.6(9) . . ? O4A P5 O3B 120.4(9) 6_557 7 ? O3A P5 O3B 20.6(9) 7 7 ? O3A P5 O3B 120.4(8) . 7 ? O3B P5 O3B 118.8(17) . 7 ? O4A P5 F5A 106.7(11) 6_557 . ? O3A P5 F5A 105.0(7) 7 . ? O3A P5 F5A 105.0(7) . . ? O3B P5 F5A 84.4(10) . . ? O3B P5 F5A 84.4(10) 7 . ? O4A P5 F4B 47.6(12) 6_557 6_557 ? O3A P5 F4B 88.5(8) 7 6_557 ? O3A P5 F4B 88.5(8) . 6_557 ? O3B P5 F4B 107.7(10) . 6_557 ? O3B P5 F4B 107.7(10) 7 6_557 ? F5A P5 F4B 154.3(13) . 6_557 ? O4A P5 O5B 58.9(17) 6_557 6_557 ? O3A P5 O5B 122.0(6) 7 6_557 ? O3A P5 O5B 122.0(6) . 6_557 ? O3B P5 O5B 107.8(11) . 6_557 ? O3B P5 O5B 107.8(11) 7 6_557 ? F5A P5 O5B 47.8(16) . 6_557 ? F4B P5 O5B 106.5(19) 6_557 6_557 ? O4A P5 Cs1 95.1(5) 6_557 . ? O3A P5 Cs1 148.7(6) 7 . ? O3A P5 Cs1 64.2(6) . . ? O3B P5 Cs1 47.5(9) . . ? O3B P5 Cs1 130.5(9) 7 . ? F5A P5 Cs1 50.85(11) . . ? F4B P5 Cs1 121.8(5) 6_557 . ? O5B P5 Cs1 60.3(7) 6_557 . ? O4A P5 Cs1 95.1(5) 6_557 1_545 ? O3A P5 Cs1 64.2(6) 7 1_545 ? O3A P5 Cs1 148.7(6) . 1_545 ? O3B P5 Cs1 130.5(9) . 1_545 ? O3B P5 Cs1 47.5(9) 7 1_545 ? F5A P5 Cs1 50.85(11) . 1_545 ? F4B P5 Cs1 121.8(4) 6_557 1_545 ? O5B P5 Cs1 60.3(7) 6_557 1_545 ? Cs1 P5 Cs1 100.62(10) . 1_545 ? O4A P5 Cs1 58.1(4) 6_557 6_547 ? O3A P5 Cs1 54.6(5) 7 6_547 ? O3A P5 Cs1 133.8(6) . 6_547 ? O3B P5 Cs1 154.3(9) . 6_547 ? O3B P5 Cs1 66.1(9) 7 6_547 ? F5A P5 Cs1 121.1(4) . 6_547 ? F4B P5 Cs1 50.42(19) 6_557 6_547 ? O5B P5 Cs1 93.1(10) 6_557 6_547 ? Cs1 P5 Cs1 150.72(11) . 6_547 ? Cs1 P5 Cs1 72.78(2) 1_545 6_547 ? O4A P5 Cs1 58.1(4) 6_557 6_557 ? O3A P5 Cs1 133.8(6) 7 6_557 ? O3A P5 Cs1 54.6(5) . 6_557 ? O3B P5 Cs1 66.1(9) . 6_557 ? O3B P5 Cs1 154.3(9) 7 6_557 ? F5A P5 Cs1 121.1(4) . 6_557 ? F4B P5 Cs1 50.42(19) 6_557 6_557 ? O5B P5 Cs1 93.1(10) 6_557 6_557 ? Cs1 P5 Cs1 72.78(2) . 6_557 ? Cs1 P5 Cs1 150.72(11) 1_545 6_557 ? Cs1 P5 Cs1 98.77(9) 6_547 6_557 ? O5B Cu2 F1 144.3(11) . . ? O5B Cu2 O1 89.2(4) . . ? F1 Cu2 O1 93.8(3) . . ? O5B Cu2 O1 89.2(4) . 7 ? F1 Cu2 O1 93.8(3) . 7 ? O1 Cu2 O1 169.0(6) . 7 ? O5B Cu2 O4A 45.2(12) . . ? F1 Cu2 O4A 170.5(6) . . ? O1 Cu2 O4A 85.6(3) . . ? O1 Cu2 O4A 85.6(3) 7 . ? O5B Cu2 Cs1 177.9(11) . 5_556 ? F1 Cu2 Cs1 37.8(3) . 5_556 ? O1 Cu2 Cs1 90.6(4) . 5_556 ? O1 Cu2 Cs1 90.6(4) 7 5_556 ? O4A Cu2 Cs1 132.7(5) . 5_556 ? O3B Cu3 O3B 180.000(3) 1_655 5_556 ? O3B Cu3 O3A 15.9(7) 1_655 1_655 ? O3B Cu3 O3A 164.1(7) 5_556 1_655 ? O3B Cu3 O3A 164.1(7) 1_655 5_556 ? O3B Cu3 O3A 15.9(7) 5_556 5_556 ? O3A Cu3 O3A 180.000(1) 1_655 5_556 ? O3B Cu3 O2 95.4(8) 1_655 . ? O3B Cu3 O2 84.6(8) 5_556 . ? O3A Cu3 O2 87.0(5) 1_655 . ? O3A Cu3 O2 93.0(5) 5_556 . ? O3B Cu3 O2 84.6(8) 1_655 5_656 ? O3B Cu3 O2 95.4(8) 5_556 5_656 ? O3A Cu3 O2 93.0(5) 1_655 5_656 ? O3A Cu3 O2 87.0(5) 5_556 5_656 ? O2 Cu3 O2 180.000(1) . 5_656 ? O3B Cu3 F1 81.9(7) 1_655 5_656 ? O3B Cu3 F1 98.1(7) 5_556 5_656 ? O3A Cu3 F1 94.8(5) 1_655 5_656 ? O3A Cu3 F1 85.2(5) 5_556 5_656 ? O2 Cu3 F1 86.5(3) . 5_656 ? O2 Cu3 F1 93.5(3) 5_656 5_656 ? O3B Cu3 F1 98.1(7) 1_655 . ? O3B Cu3 F1 81.9(7) 5_556 . ? O3A Cu3 F1 85.2(5) 1_655 . ? O3A Cu3 F1 94.8(5) 5_556 . ? O2 Cu3 F1 93.5(3) . . ? O2 Cu3 F1 86.5(3) 5_656 . ? F1 Cu3 F1 180.0(3) 5_656 . ? F1 Cs1 O3B 53.7(4) 5_556 . ? F1 Cs1 O3B 53.7(4) 5_556 7_565 ? O3B Cs1 O3B 68.0(8) . 7_565 ? F1 Cs1 F5A 77.5(4) 5_556 . ? O3B Cs1 F5A 36.7(5) . . ? O3B Cs1 F5A 104.7(5) 7_565 . ? F1 Cs1 F5A 77.5(4) 5_556 1_565 ? O3B Cs1 F5A 104.7(5) . 1_565 ? O3B Cs1 F5A 36.7(5) 7_565 1_565 ? F5A Cs1 F5A 141.3(7) . 1_565 ? F1 Cs1 O1 94.8(3) 5_556 7_565 ? O3B Cs1 O1 142.4(5) . 7_565 ? O3B Cs1 O1 112.3(5) 7_565 7_565 ? F5A Cs1 O1 126.7(3) . 7_565 ? F5A Cs1 O1 84.4(3) 1_565 7_565 ? F1 Cs1 O1 94.8(3) 5_556 . ? O3B Cs1 O1 112.3(4) . . ? O3B Cs1 O1 142.4(5) 7_565 . ? F5A Cs1 O1 84.4(3) . . ? F5A Cs1 O1 126.7(3) 1_565 . ? O1 Cs1 O1 43.2(3) 7_565 . ? F1 Cs1 F4B 111.1(4) 5_556 1_565 ? O3B Cs1 F4B 139.2(6) . 1_565 ? O3B Cs1 F4B 73.4(6) 7_565 1_565 ? F5A Cs1 F4B 165.2(6) . 1_565 ? F5A Cs1 F4B 37.7(5) 1_565 1_565 ? O1 Cs1 F4B 65.9(5) 7_565 1_565 ? O1 Cs1 F4B 106.2(5) . 1_565 ? F1 Cs1 F4B 111.1(4) 5_556 . ? O3B Cs1 F4B 73.4(6) . . ? O3B Cs1 F4B 139.2(6) 7_565 . ? F5A Cs1 F4B 37.7(5) . . ? F5A Cs1 F4B 165.2(6) 1_565 . ? O1 Cs1 F4B 106.2(5) 7_565 . ? O1 Cs1 F4B 65.9(5) . . ? F4B Cs1 F4B 137.5(8) 1_565 . ? F1 Cs1 O1 121.2(2) 5_556 4_456 ? O3B Cs1 O1 93.1(4) . 4_456 ? O3B Cs1 O1 70.0(4) 7_565 4_456 ? F5A Cs1 O1 104.5(3) . 4_456 ? F5A Cs1 O1 65.4(3) 1_565 4_456 ? O1 Cs1 O1 123.2(3) 7_565 4_456 ? O1 Cs1 O1 143.9(2) . 4_456 ? F4B Cs1 O1 60.9(5) 1_565 4_456 ? F4B Cs1 O1 99.9(5) . 4_456 ? F1 Cs1 O1 121.2(2) 5_556 6_557 ? O3B Cs1 O1 70.0(4) . 6_557 ? O3B Cs1 O1 93.1(4) 7_565 6_557 ? F5A Cs1 O1 65.4(3) . 6_557 ? F5A Cs1 O1 104.5(3) 1_565 6_557 ? O1 Cs1 O1 143.9(2) 7_565 6_557 ? O1 Cs1 O1 123.2(3) . 6_557 ? F4B Cs1 O1 99.9(5) 1_565 6_557 ? F4B Cs1 O1 60.9(5) . 6_557 ? O1 Cs1 O1 41.4(3) 4_456 6_557 ? F1 Cs1 O3A 147.2(2) 5_556 4_556 ? O3B Cs1 O3A 147.2(5) . 4_556 ? O3B Cs1 O3A 103.8(4) 7_565 4_556 ? F5A Cs1 O3A 135.0(4) . 4_556 ? F5A Cs1 O3A 72.1(4) 1_565 4_556 ? O1 Cs1 O3A 70.5(3) 7_565 4_556 ? O1 Cs1 O3A 93.5(3) . 4_556 ? F4B Cs1 O3A 36.3(5) 1_565 4_556 ? F4B Cs1 O3A 101.3(5) . 4_556 ? O1 Cs1 O3A 55.3(3) 4_456 4_556 ? O1 Cs1 O3A 79.0(3) 6_557 4_556 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.586 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.334 # Attachment '- Cu3(PO3F)3_X.cif' data_2010erw0090_p-1 _database_code_depnum_ccdc_archive 'CCDC 884288' #TrackingRef '- Cu3(PO3F)3_X.cif' _audit_update_record ; 2012-05-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F3 O9 P3' _chemical_formula_weight 484.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1709(3) _cell_length_b 9.2647(4) _cell_length_c 9.6755(4) _cell_angle_alpha 64.084(3) _cell_angle_beta 73.977(2) _cell_angle_gamma 73.464(3) _cell_volume 469.52(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9094 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 7.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7106 _exptl_absorpt_correction_T_max 0.7580 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9415 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.87 _reflns_number_total 2166 _reflns_number_gt 1598 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0764P)^2^+32.4217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2166 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.2431 _refine_ls_wR_factor_gt 0.2145 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.005 _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 Cu1 Cu 0.2153(3) 0.4058(2) 0.22444(19) 0.0130(4) Uani 1 1 d . . . Cu2 Cu 0.4209(3) 0.3495(2) 0.5035(2) 0.0214(5) Uani 1 1 d . . . Cu3 Cu 0.0027(3) 0.1047(2) 0.3068(2) 0.0219(5) Uani 1 1 d . . . P4 P -0.0815(6) 0.2837(4) 0.5631(4) 0.0108(7) Uani 1 1 d . . . P6 P 0.5517(7) 0.0308(6) 0.2660(7) 0.0397(13) Uani 1 1 d . . . O1 O 0.4985(16) 0.4271(11) 0.2585(11) 0.0120(19) Uiso 1 1 d . . . P5 P 0.7240(5) 0.4649(4) 0.1484(4) 0.0116(7) Uani 1 1 d . . . O2 O 0.0722(17) -0.1214(12) 0.4355(12) 0.019(2) Uani 1 1 d . . . O3 O -0.0705(15) 0.3487(12) 0.2288(11) 0.015(2) Uani 1 1 d . . . O4 O 0.6946(16) 0.4029(11) 0.5186(12) 0.015(2) Uani 1 1 d . . . F3 F -0.0690(15) 0.2691(12) 0.7276(10) 0.026(2) Uani 1 1 d . . . O5 O 0.1302(16) 0.3567(11) 0.4545(11) 0.0133(19) Uiso 1 1 d . . . O6 O 0.3145(18) 0.1344(12) 0.2655(12) 0.020(2) Uani 1 1 d . . . O7 O 0.2571(17) 0.5377(13) 0.0062(11) 0.020(2) Uani 1 1 d . . . F2 F 0.7403(18) 0.6370(13) 0.1284(14) 0.038(3) Uani 1 1 d . . . O8 O 0.574(2) -0.1457(15) 0.3184(17) 0.037(3) Uani 1 1 d . . . O9 O 0.710(4) 0.090(3) 0.297(2) 0.080(6) Uiso 1 1 d . . . F1 F 1.347(4) 0.919(2) -0.077(2) 0.131(10) 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 Cu1 0.0064(8) 0.0185(9) 0.0146(8) -0.0044(7) -0.0038(6) -0.0048(6) Cu2 0.0147(9) 0.0210(10) 0.0264(10) 0.0039(7) -0.0161(8) -0.0099(7) Cu3 0.0139(9) 0.0180(9) 0.0322(11) -0.0053(8) -0.0093(8) -0.0029(7) P4 0.0069(15) 0.0107(16) 0.0163(17) -0.0055(13) -0.0044(13) -0.0012(12) P6 0.0106(19) 0.020(2) 0.076(4) -0.003(2) -0.016(2) -0.0017(16) P5 0.0030(15) 0.0166(17) 0.0141(17) -0.0039(13) -0.0046(12) -0.0008(12) O2 0.017(5) 0.013(5) 0.028(6) -0.009(4) -0.002(4) -0.005(4) O3 0.002(4) 0.025(5) 0.017(5) -0.008(4) 0.001(4) -0.004(4) O4 0.012(5) 0.010(5) 0.030(5) -0.009(4) -0.007(4) -0.003(4) F3 0.018(4) 0.036(5) 0.021(5) -0.008(4) -0.004(4) -0.008(4) O6 0.017(5) 0.018(5) 0.020(5) -0.001(4) -0.010(4) 0.000(4) O7 0.016(5) 0.030(6) 0.010(5) 0.002(4) -0.010(4) -0.005(4) F2 0.027(5) 0.033(6) 0.056(7) -0.021(5) -0.003(5) -0.006(4) O8 0.020(6) 0.025(6) 0.056(9) -0.001(6) -0.013(6) -0.008(5) F1 0.115(16) 0.055(10) 0.097(14) 0.028(10) 0.023(12) 0.035(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu1 O7 1.908(10) . ? Cu1 O1 1.942(9) . ? Cu1 O3 1.965(9) . ? Cu1 O5 2.010(9) . ? Cu1 O6 2.289(11) . ? Cu2 O8 1.920(12) 2_656 ? Cu2 O4 1.948(9) . ? Cu2 O5 1.955(10) . ? Cu2 O1 2.109(9) . ? Cu2 O4 2.131(9) 2_666 ? Cu3 O9 1.88(2) 1_455 ? Cu3 O2 1.904(10) . ? Cu3 O6 1.929(11) . ? Cu3 O3 2.000(10) . ? P4 O2 1.482(10) 2_556 ? P4 O4 1.536(10) 1_455 ? P4 O5 1.547(10) . ? P4 F3 1.558(9) . ? P6 O9 1.40(2) . ? P6 O8 1.461(13) . ? P6 O6 1.504(11) . ? P6 F1 1.65(2) 2_765 ? O1 P5 1.525(10) . ? P5 O7 1.479(10) 2_665 ? P5 F2 1.549(11) . ? P5 O3 1.552(10) 1_655 ? O2 P4 1.482(10) 2_556 ? O3 P5 1.552(10) 1_455 ? O4 P4 1.536(10) 1_655 ? O4 Cu2 2.131(9) 2_666 ? O7 P5 1.479(10) 2_665 ? O8 Cu2 1.920(12) 2_656 ? O9 Cu3 1.88(2) 1_655 ? F1 P6 1.65(2) 2_765 ? 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 O7 Cu1 O1 95.9(4) . . ? O7 Cu1 O3 94.6(4) . . ? O1 Cu1 O3 169.0(4) . . ? O7 Cu1 O5 157.1(4) . . ? O1 Cu1 O5 80.8(4) . . ? O3 Cu1 O5 90.6(4) . . ? O7 Cu1 O6 110.4(4) . . ? O1 Cu1 O6 97.6(4) . . ? O3 Cu1 O6 75.7(4) . . ? O5 Cu1 O6 92.5(4) . . ? O8 Cu2 O4 97.3(5) 2_656 . ? O8 Cu2 O5 96.9(5) 2_656 . ? O4 Cu2 O5 165.0(4) . . ? O8 Cu2 O1 137.2(5) 2_656 . ? O4 Cu2 O1 94.5(4) . . ? O5 Cu2 O1 78.1(4) . . ? O8 Cu2 O4 132.3(5) 2_656 2_666 ? O4 Cu2 O4 77.8(4) . 2_666 ? O5 Cu2 O4 89.1(4) . 2_666 ? O1 Cu2 O4 90.3(4) . 2_666 ? O9 Cu3 O2 92.7(7) 1_455 . ? O9 Cu3 O6 166.8(7) 1_455 . ? O2 Cu3 O6 93.6(4) . . ? O9 Cu3 O3 93.4(7) 1_455 . ? O2 Cu3 O3 163.3(4) . . ? O6 Cu3 O3 83.7(4) . . ? O2 P4 O4 112.1(6) 2_556 1_455 ? O2 P4 O5 111.0(6) 2_556 . ? O4 P4 O5 111.0(6) 1_455 . ? O2 P4 F3 110.9(6) 2_556 . ? O4 P4 F3 106.7(5) 1_455 . ? O5 P4 F3 104.8(5) . . ? O9 P6 O8 118.9(11) . . ? O9 P6 O6 114.1(10) . . ? O8 P6 O6 118.4(7) . . ? O9 P6 F1 96.8(14) . 2_765 ? O8 P6 F1 100.7(10) . 2_765 ? O6 P6 F1 101.9(8) . 2_765 ? P5 O1 Cu1 131.8(6) . . ? P5 O1 Cu2 129.0(5) . . ? Cu1 O1 Cu2 98.7(4) . . ? O7 P5 O1 114.1(6) 2_665 . ? O7 P5 F2 109.7(6) 2_665 . ? O1 P5 F2 106.5(6) . . ? O7 P5 O3 111.4(6) 2_665 1_655 ? O1 P5 O3 109.9(5) . 1_655 ? F2 P5 O3 104.7(6) . 1_655 ? P4 O2 Cu3 140.1(7) 2_556 . ? P5 O3 Cu1 127.3(6) 1_455 . ? P5 O3 Cu3 127.2(6) 1_455 . ? Cu1 O3 Cu3 103.5(4) . . ? P4 O4 Cu2 126.8(6) 1_655 . ? P4 O4 Cu2 130.2(5) 1_655 2_666 ? Cu2 O4 Cu2 102.2(4) . 2_666 ? P4 O5 Cu2 129.9(6) . . ? P4 O5 Cu1 125.0(6) . . ? Cu2 O5 Cu1 101.7(4) . . ? P6 O6 Cu3 137.7(7) . . ? P6 O6 Cu1 127.3(6) . . ? Cu3 O6 Cu1 94.8(4) . . ? P5 O7 Cu1 142.8(7) 2_665 . ? P6 O8 Cu2 145.0(10) . 2_656 ? P6 O9 Cu3 155.9(15) . 1_655 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 3.537 _refine_diff_density_min -1.677 _refine_diff_density_rms 0.411 # Attachment '- K2Cu3(PO3F)4_II.cif' data_K2Cu3(PO3F)4_II _database_code_depnum_ccdc_archive 'CCDC 884289' #TrackingRef '- K2Cu3(PO3F)4_II.cif' _audit_update_record ; 2012-05-09 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F4 K2 O12 P4' _chemical_formula_weight 660.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2834(4) _cell_length_b 5.1073(2) _cell_length_c 11.4099(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.211(3) _cell_angle_gamma 90.00 _cell_volume 634.49(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4795 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 317 _exptl_absorpt_coefficient_mu 6.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5731 _exptl_absorpt_correction_T_max 0.7447 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6861 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.66 _reflns_number_total 1448 _reflns_number_gt 1057 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0082P)^2^+19.1185P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1448 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 F1 F 0.2761(4) 0.4436(10) 0.1743(4) 0.0148(10) Uani 1 1 d . . . O2 O 0.0691(4) 0.4491(12) 0.2037(4) 0.0111(11) Uani 1 1 d . . . F3 F 0.4952(4) 0.3598(9) -0.1007(4) 0.0109(9) Uani 1 1 d . . . O4 O 0.2812(5) 0.4464(12) -0.1278(5) 0.0127(12) Uani 1 1 d . . . O5 O 0.3719(5) 0.4045(10) -0.3111(5) 0.0100(11) Uani 1 1 d . . . O6 O 0.4219(4) 0.7969(11) -0.1717(5) 0.0099(11) Uani 1 1 d . . . O7 O 0.1062(5) 0.3155(11) 0.0034(5) 0.0115(11) Uani 1 1 d . . . O8 O 0.1409(5) 0.7848(11) 0.0697(5) 0.0103(11) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.0000 0.0091(3) Uani 1 2 d S . . Cu2 Cu 0.60817(8) -0.0131(2) 0.32533(8) 0.0103(2) Uani 1 1 d . . . K3 K 0.33875(14) 0.0255(4) 0.02821(14) 0.0119(4) Uani 1 1 d . . . P4 P 0.13827(16) 0.5032(4) 0.11089(16) 0.0073(4) Uani 1 1 d . . . P5 P 0.38430(16) 0.5157(4) -0.18524(16) 0.0082(4) 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 F1 0.010(2) 0.017(3) 0.017(2) 0.0023(19) 0.0030(17) -0.0010(18) O2 0.008(2) 0.020(3) 0.007(2) -0.001(2) 0.0034(18) 0.000(2) F3 0.008(2) 0.012(2) 0.010(2) -0.0026(17) -0.0009(16) 0.0034(17) O4 0.010(2) 0.016(3) 0.011(2) 0.002(2) 0.003(2) 0.001(2) O5 0.011(3) 0.006(3) 0.013(3) -0.002(2) 0.003(2) 0.001(2) O6 0.009(2) 0.008(3) 0.014(3) -0.005(2) 0.004(2) -0.001(2) O7 0.009(2) 0.012(3) 0.013(3) -0.003(2) 0.002(2) 0.001(2) O8 0.012(2) 0.004(3) 0.015(3) -0.003(2) 0.004(2) -0.003(2) Cu1 0.0070(6) 0.0067(7) 0.0129(6) 0.0012(5) 0.0015(4) 0.0005(5) Cu2 0.0072(4) 0.0120(5) 0.0122(4) 0.0012(4) 0.0033(3) -0.0002(4) K3 0.0110(7) 0.0112(9) 0.0143(7) 0.0030(7) 0.0048(6) 0.0021(7) P4 0.0065(8) 0.0074(10) 0.0081(8) 0.0003(8) 0.0019(6) 0.0002(8) P5 0.0074(8) 0.0082(10) 0.0087(8) 0.0024(8) 0.0016(6) 0.0009(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P4 1.564(4) . ? F1 K3 2.908(5) . ? O2 P4 1.497(5) . ? O2 Cu2 1.949(5) 2 ? O2 K3 2.987(5) 2 ? F3 P5 1.580(4) . ? F3 K3 2.693(5) 3_655 ? F3 K3 3.092(5) . ? O4 P5 1.520(5) . ? O4 Cu2 1.915(5) 4_565 ? O4 K3 2.758(6) . ? O4 K3 3.425(6) 1_565 ? O5 P5 1.516(5) . ? O5 Cu2 2.023(5) 3_655 ? O5 K3 3.013(5) 2_554 ? O6 P5 1.494(6) . ? O6 Cu2 2.023(5) 3_665 ? O6 K3 2.912(5) 3_665 ? O6 K3 2.928(5) 1_565 ? O7 P4 1.523(6) . ? O7 Cu1 2.002(6) . ? O7 Cu2 2.274(5) 4_565 ? O7 K3 2.961(5) . ? O8 P4 1.516(6) . ? O8 Cu1 1.925(5) 1_565 ? O8 K3 2.697(5) 1_565 ? Cu1 O8 1.925(5) 3_565 ? Cu1 O8 1.925(5) 1_545 ? Cu1 O7 2.002(6) 3 ? Cu1 K3 3.7529(15) . ? Cu1 K3 3.7529(15) 3 ? Cu2 O4 1.915(5) 4_666 ? Cu2 O2 1.949(5) 2_545 ? Cu2 O5 2.023(5) 3_655 ? Cu2 O6 2.023(5) 3_665 ? Cu2 O7 2.274(5) 4_666 ? Cu2 K3 3.8948(19) 4_666 ? Cu2 K3 3.9198(18) . ? Cu2 K3 3.977(2) 4_656 ? K3 F3 2.693(5) 3_655 ? K3 O8 2.697(5) 1_545 ? K3 O6 2.912(5) 3_665 ? K3 O6 2.928(5) 1_545 ? K3 O2 2.987(5) 2_545 ? K3 O5 3.013(5) 2_544 ? K3 O4 3.425(6) 1_545 ? K3 P4 3.617(3) . ? P4 K3 3.774(3) 1_565 ? P5 K3 3.692(3) 1_565 ? 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 P4 F1 K3 103.9(2) . . ? P4 O2 Cu2 124.3(3) . 2 ? P4 O2 K3 126.4(3) . 2 ? Cu2 O2 K3 103.12(19) 2 2 ? P5 F3 K3 158.7(3) . 3_655 ? P5 F3 K3 96.26(19) . . ? K3 F3 K3 83.60(13) 3_655 . ? P5 O4 Cu2 132.7(3) . 4_565 ? P5 O4 K3 112.5(3) . . ? Cu2 O4 K3 111.7(2) 4_565 . ? P5 O4 K3 87.8(2) . 1_565 ? Cu2 O4 K3 91.8(2) 4_565 1_565 ? K3 O4 K3 110.94(17) . 1_565 ? P5 O5 Cu2 117.5(3) . 3_655 ? P5 O5 K3 124.0(3) . 2_554 ? Cu2 O5 K3 102.5(2) 3_655 2_554 ? P5 O6 Cu2 117.2(3) . 3_665 ? P5 O6 K3 123.6(3) . 3_665 ? Cu2 O6 K3 103.7(2) 3_665 3_665 ? P5 O6 K3 108.9(3) . 1_565 ? Cu2 O6 K3 116.2(2) 3_665 1_565 ? K3 O6 K3 82.94(14) 3_665 1_565 ? P4 O7 Cu1 122.5(3) . . ? P4 O7 Cu2 112.6(3) . 4_565 ? Cu1 O7 Cu2 119.1(2) . 4_565 ? P4 O7 K3 102.8(2) . . ? Cu1 O7 K3 96.3(2) . . ? Cu2 O7 K3 95.24(18) 4_565 . ? P4 O8 Cu1 126.1(3) . 1_565 ? P4 O8 K3 124.9(3) . 1_565 ? Cu1 O8 K3 107.4(2) 1_565 1_565 ? O8 Cu1 O8 180.0(3) 3_565 1_545 ? O8 Cu1 O7 88.5(2) 3_565 . ? O8 Cu1 O7 91.5(2) 1_545 . ? O8 Cu1 O7 91.5(2) 3_565 3 ? O8 Cu1 O7 88.5(2) 1_545 3 ? O7 Cu1 O7 180.0 . 3 ? O8 Cu1 K3 136.71(16) 3_565 . ? O8 Cu1 K3 43.29(16) 1_545 . ? O7 Cu1 K3 51.64(15) . . ? O7 Cu1 K3 128.36(15) 3 . ? O8 Cu1 K3 43.29(16) 3_565 3 ? O8 Cu1 K3 136.71(16) 1_545 3 ? O7 Cu1 K3 128.36(15) . 3 ? O7 Cu1 K3 51.64(15) 3 3 ? K3 Cu1 K3 180.00(7) . 3 ? O4 Cu2 O2 172.2(2) 4_666 2_545 ? O4 Cu2 O5 94.1(2) 4_666 3_655 ? O2 Cu2 O5 91.1(2) 2_545 3_655 ? O4 Cu2 O6 94.1(2) 4_666 3_665 ? O2 Cu2 O6 88.6(2) 2_545 3_665 ? O5 Cu2 O6 117.8(2) 3_655 3_665 ? O4 Cu2 O7 85.4(2) 4_666 4_666 ? O2 Cu2 O7 86.9(2) 2_545 4_666 ? O5 Cu2 O7 122.5(2) 3_655 4_666 ? O6 Cu2 O7 119.5(2) 3_665 4_666 ? O4 Cu2 K3 41.15(17) 4_666 4_666 ? O2 Cu2 K3 131.29(17) 2_545 4_666 ? O5 Cu2 K3 127.48(15) 3_655 4_666 ? O6 Cu2 K3 95.73(15) 3_665 4_666 ? O7 Cu2 K3 49.21(13) 4_666 4_666 ? O4 Cu2 K3 137.34(16) 4_666 . ? O2 Cu2 K3 47.92(15) 2_545 . ? O5 Cu2 K3 93.30(15) 3_655 . ? O6 Cu2 K3 46.19(14) 3_665 . ? O7 Cu2 K3 124.29(14) 4_666 . ? K3 Cu2 K3 136.67(3) 4_666 . ? O4 Cu2 K3 59.39(18) 4_666 4_656 ? O2 Cu2 K3 121.26(17) 2_545 4_656 ? O5 Cu2 K3 47.70(15) 3_655 4_656 ? O6 Cu2 K3 143.01(15) 3_665 4_656 ? O7 Cu2 K3 85.99(14) 4_666 4_656 ? K3 Cu2 K3 80.90(3) 4_666 4_656 ? K3 Cu2 K3 140.98(3) . 4_656 ? F3 K3 O8 98.87(16) 3_655 1_545 ? F3 K3 O4 142.65(15) 3_655 . ? O8 K3 O4 113.77(16) 1_545 . ? F3 K3 F1 127.91(14) 3_655 . ? O8 K3 F1 84.09(15) 1_545 . ? O4 K3 F1 75.28(15) . . ? F3 K3 O6 65.61(15) 3_655 3_665 ? O8 K3 O6 137.02(16) 1_545 3_665 ? O4 K3 O6 98.43(16) . 3_665 ? F1 K3 O6 77.16(14) . 3_665 ? F3 K3 O6 66.97(14) 3_655 1_545 ? O8 K3 O6 113.85(16) 1_545 1_545 ? O4 K3 O6 82.96(16) . 1_545 ? F1 K3 O6 156.25(16) . 1_545 ? O6 K3 O6 97.06(14) 3_665 1_545 ? F3 K3 O7 157.27(16) 3_655 . ? O8 K3 O7 59.42(16) 1_545 . ? O4 K3 O7 59.71(15) . . ? F1 K3 O7 49.07(13) . . ? O6 K3 O7 124.45(16) 3_665 . ? O6 K3 O7 125.60(15) 1_545 . ? F3 K3 O2 64.06(14) 3_655 2_545 ? O8 K3 O2 80.93(15) 1_545 2_545 ? O4 K3 O2 136.26(17) . 2_545 ? F1 K3 O2 65.20(14) . 2_545 ? O6 K3 O2 56.10(15) 3_665 2_545 ? O6 K3 O2 130.49(15) 1_545 2_545 ? O7 K3 O2 103.00(15) . 2_545 ? F3 K3 O5 115.97(15) 3_655 2_544 ? O8 K3 O5 62.64(15) 1_545 2_544 ? O4 K3 O5 68.15(15) . 2_544 ? F1 K3 O5 111.35(14) . 2_544 ? O6 K3 O5 160.29(15) 3_665 2_544 ? O6 K3 O5 67.81(14) 1_545 2_544 ? O7 K3 O5 62.36(15) . 2_544 ? O2 K3 O5 143.42(15) 2_545 2_544 ? F3 K3 F3 96.40(13) 3_655 . ? O8 K3 F3 159.65(15) 1_545 . ? O4 K3 F3 47.90(13) . . ? F1 K3 F3 97.03(13) . . ? O6 K3 F3 62.25(13) 3_665 . ? O6 K3 F3 60.64(14) 1_545 . ? O7 K3 F3 106.30(15) . . ? O2 K3 F3 118.07(13) 2_545 . ? O5 K3 F3 98.49(13) 2_544 . ? F3 K3 O4 63.29(13) 3_655 1_545 ? O8 K3 O4 69.20(15) 1_545 1_545 ? O4 K3 O4 110.94(17) . 1_545 ? F1 K3 O4 152.94(13) . 1_545 ? O6 K3 O4 125.65(14) 3_665 1_545 ? O6 K3 O4 46.09(14) 1_545 1_545 ? O7 K3 O4 109.87(14) . 1_545 ? O2 K3 O4 112.77(15) 2_545 1_545 ? O5 K3 O4 52.74(14) 2_544 1_545 ? F3 K3 O4 106.48(13) . 1_545 ? F3 K3 P4 147.68(11) 3_655 . ? O8 K3 P4 70.03(12) 1_545 . ? O4 K3 P4 65.47(12) . . ? F1 K3 P4 24.82(9) . . ? O6 K3 P4 101.21(12) 3_665 . ? O6 K3 P4 145.34(12) 1_545 . ? O7 K3 P4 24.26(11) . . ? O2 K3 P4 83.95(11) 2_545 . ? O5 K3 P4 86.59(11) 2_544 . ? F3 K3 P4 103.06(10) . . ? O4 K3 P4 132.21(10) 1_545 . ? O2 P4 O8 116.8(3) . . ? O2 P4 O7 113.3(3) . . ? O8 P4 O7 111.6(3) . . ? O2 P4 F1 106.1(3) . . ? O8 P4 F1 103.3(3) . . ? O7 P4 F1 104.3(3) . . ? O2 P4 K3 122.5(2) . . ? O8 P4 K3 119.7(2) . . ? O7 P4 K3 53.0(2) . . ? F1 P4 K3 51.31(18) . . ? O2 P4 K3 140.0(2) . 1_565 ? O8 P4 K3 35.9(2) . 1_565 ? O7 P4 K3 106.0(2) . 1_565 ? F1 P4 K3 70.41(19) . 1_565 ? K3 P4 K3 87.40(5) . 1_565 ? O6 P5 O5 114.3(3) . . ? O6 P5 O4 114.1(3) . . ? O5 P5 O4 115.5(3) . . ? O6 P5 F3 105.3(3) . . ? O5 P5 F3 104.5(3) . . ? O4 P5 F3 101.1(3) . . ? O6 P5 K3 133.0(2) . . ? O5 P5 K3 112.6(2) . . ? O4 P5 K3 44.7(2) . . ? F3 P5 K3 58.04(17) . . ? O6 P5 K3 48.6(2) . 1_565 ? O5 P5 K3 153.5(2) . 1_565 ? O4 P5 K3 68.0(2) . 1_565 ? F3 P5 K3 100.25(17) . 1_565 ? K3 P5 K3 88.57(5) . 1_565 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.950 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.238 # Attachment '- KCu3(PO3F)2(PO2(OH)2)F2_IV.cif' data_2010erw0025_c2_over_c _database_code_depnum_ccdc_archive 'CCDC 884290' #TrackingRef '- KCu3(PO3F)2(PO2(OH)2)F2_IV.cif' _audit_update_record ; 2011-03-18 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F4 K O10 P3 ' _chemical_formula_weight 564.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 18.9720(7) _cell_length_b 7.4973(4) _cell_length_c 7.7663(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.629(2) _cell_angle_gamma 90.00 _cell_volume 1073.56(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7320 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _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 3.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 6.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5474 _exptl_absorpt_correction_T_max 0.5474 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6010 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1232 _reflns_number_gt 1028 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0104P)^2^+45.3089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1232 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 F1 F 0.3822(2) 0.0310(5) 0.8662(5) 0.0139(8) Uani 1 1 d . . . F2 F 0.16570(19) 0.1675(5) 0.5673(5) 0.0107(8) Uani 1 1 d . . . O1 O 0.0596(2) -0.0221(6) 0.7052(6) 0.0104(9) Uani 1 1 d . . . O2 O 0.2630(2) 0.0551(6) 0.9338(6) 0.0078(9) Uani 1 1 d . . . O3 O -0.0321(2) -0.2648(6) 0.5960(6) 0.0104(9) Uani 1 1 d . . . O5 O 0.3677(2) 0.2590(6) 1.0724(6) 0.0082(9) Uani 1 1 d . . . O4 O 0.3066(2) 0.2853(6) 0.7464(6) 0.0090(9) Uani 1 1 d . . . Cu1 Cu 0.15990(4) 0.03076(10) 0.81086(10) 0.0079(2) Uani 1 1 d . . . Cu2 Cu 0.2500 -0.2500 1.0000 0.0079(3) Uani 1 2 d S . . P1 P 0.0000 -0.1303(3) 0.7500 0.0087(5) Uani 1 2 d S . . P2 P 0.32590(8) 0.1663(2) 0.9094(2) 0.0068(3) Uani 1 1 d . . . K1 K 0.5000 0.1499(3) 0.2500 0.0149(4) Uani 1 2 d S . . 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 F1 0.0126(18) 0.0134(19) 0.017(2) -0.0031(16) 0.0055(16) 0.0049(15) F2 0.0107(17) 0.0125(18) 0.0080(17) 0.0020(15) 0.0003(14) -0.0022(15) O1 0.0051(19) 0.014(2) 0.012(2) 0.0029(18) 0.0002(17) -0.0010(18) O2 0.008(2) 0.007(2) 0.009(2) 0.0027(17) 0.0005(17) 0.0012(16) O3 0.015(2) 0.007(2) 0.010(2) -0.0034(17) 0.0039(19) 0.0017(18) O5 0.009(2) 0.010(2) 0.005(2) 0.0019(17) 0.0017(17) 0.0014(17) O4 0.010(2) 0.008(2) 0.008(2) 0.0042(18) 0.0004(18) -0.0004(17) Cu1 0.0067(4) 0.0079(4) 0.0089(4) -0.0012(3) 0.0017(3) -0.0005(3) Cu2 0.0087(5) 0.0083(5) 0.0066(5) 0.0001(4) 0.0014(4) 0.0015(4) P1 0.0093(10) 0.0073(11) 0.0105(11) 0.000 0.0039(9) 0.000 P2 0.0064(7) 0.0073(7) 0.0072(7) 0.0005(6) 0.0027(6) 0.0004(6) K1 0.0098(9) 0.0188(11) 0.0149(10) 0.000 0.0008(8) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P2 1.566(4) . ? F1 K1 2.932(4) 5_656 ? F1 K1 3.396(4) 1_556 ? F2 Cu2 1.899(3) 4_556 ? F2 Cu1 2.177(4) . ? O1 P1 1.497(4) . ? O1 Cu1 1.928(4) . ? O1 K1 3.061(5) 7_556 ? O2 P2 1.504(4) . ? O2 Cu1 1.972(4) . ? O2 Cu2 2.370(4) . ? O3 P1 1.573(5) . ? O3 K1 2.962(4) 3_445 ? O3 K1 3.130(5) 7_546 ? O5 P2 1.496(5) . ? O5 Cu1 1.950(4) 7_557 ? O5 K1 2.691(4) 1_556 ? O4 P2 1.521(4) . ? O4 Cu2 1.979(4) 4_556 ? O4 Cu1 2.030(4) 4_556 ? Cu1 O5 1.950(4) 7_557 ? Cu1 O4 2.030(4) 4_546 ? Cu1 Cu2 2.8857(8) . ? Cu1 K1 3.8054(16) 7_556 ? Cu2 F2 1.899(3) 4_546 ? Cu2 F2 1.899(3) 6_556 ? Cu2 O4 1.979(4) 6_556 ? Cu2 O4 1.979(4) 4_546 ? Cu2 O2 2.370(4) 7_547 ? Cu2 Cu1 2.8857(8) 7_547 ? P1 O1 1.497(4) 2_556 ? P1 O3 1.573(5) 2_556 ? P1 K1 3.602(3) 7_556 ? P2 K1 3.7154(16) 1_556 ? K1 O5 2.691(4) 2_656 ? K1 O5 2.691(4) 1_554 ? K1 F1 2.932(4) 5_656 ? K1 F1 2.932(4) 6 ? K1 O3 2.962(4) 3 ? K1 O3 2.962(4) 4 ? K1 O1 3.061(5) 8 ? K1 O1 3.061(5) 7_556 ? K1 O3 3.130(5) 8_545 ? K1 O3 3.130(5) 7_546 ? K1 F1 3.396(4) 2_656 ? K1 F1 3.396(4) 1_554 ? 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 P2 F1 K1 166.8(2) . 5_656 ? P2 F1 K1 89.01(17) . 1_556 ? K1 F1 K1 90.00(10) 5_656 1_556 ? Cu2 F2 Cu1 127.64(18) 4_556 . ? P1 O1 Cu1 137.4(3) . . ? P1 O1 K1 98.5(2) . 7_556 ? Cu1 O1 K1 96.78(17) . 7_556 ? P2 O2 Cu1 135.8(3) . . ? P2 O2 Cu2 133.5(2) . . ? Cu1 O2 Cu2 82.75(15) . . ? P1 O3 K1 134.6(2) . 3_445 ? P1 O3 K1 107.2(2) . 7_546 ? K1 O3 K1 94.84(12) 3_445 7_546 ? P2 O5 Cu1 128.5(3) . 7_557 ? P2 O5 K1 122.4(2) . 1_556 ? Cu1 O5 K1 109.09(18) 7_557 1_556 ? P2 O4 Cu2 134.0(3) . 4_556 ? P2 O4 Cu1 133.5(3) . 4_556 ? Cu2 O4 Cu1 92.06(17) 4_556 4_556 ? O1 Cu1 O5 91.05(19) . 7_557 ? O1 Cu1 O2 172.72(19) . . ? O5 Cu1 O2 92.52(18) 7_557 . ? O1 Cu1 O4 92.79(19) . 4_546 ? O5 Cu1 O4 165.13(18) 7_557 4_546 ? O2 Cu1 O4 82.19(17) . 4_546 ? O1 Cu1 F2 88.52(16) . . ? O5 Cu1 F2 95.59(16) 7_557 . ? O2 Cu1 F2 97.44(16) . . ? O4 Cu1 F2 98.86(16) 4_546 . ? O1 Cu1 Cu2 118.26(14) . . ? O5 Cu1 Cu2 122.98(13) 7_557 . ? O2 Cu1 Cu2 54.57(12) . . ? O4 Cu1 Cu2 43.27(12) 4_546 . ? F2 Cu1 Cu2 129.84(10) . . ? O1 Cu1 K1 53.02(14) . 7_556 ? O5 Cu1 K1 41.94(13) 7_557 7_556 ? O2 Cu1 K1 132.26(13) . 7_556 ? O4 Cu1 K1 145.53(13) 4_546 7_556 ? F2 Cu1 K1 78.34(10) . 7_556 ? Cu2 Cu1 K1 151.81(3) . 7_556 ? F2 Cu2 F2 180.000(1) 4_546 6_556 ? F2 Cu2 O4 85.52(16) 4_546 6_556 ? F2 Cu2 O4 94.48(16) 6_556 6_556 ? F2 Cu2 O4 94.48(16) 4_546 4_546 ? F2 Cu2 O4 85.52(16) 6_556 4_546 ? O4 Cu2 O4 180.0 6_556 4_546 ? F2 Cu2 O2 96.73(15) 4_546 . ? F2 Cu2 O2 83.27(15) 6_556 . ? O4 Cu2 O2 106.17(16) 6_556 . ? O4 Cu2 O2 73.83(16) 4_546 . ? F2 Cu2 O2 83.27(15) 4_546 7_547 ? F2 Cu2 O2 96.73(15) 6_556 7_547 ? O4 Cu2 O2 73.83(16) 6_556 7_547 ? O4 Cu2 O2 106.17(16) 4_546 7_547 ? O2 Cu2 O2 180.00(5) . 7_547 ? F2 Cu2 Cu1 57.74(11) 4_546 7_547 ? F2 Cu2 Cu1 122.26(11) 6_556 7_547 ? O4 Cu2 Cu1 44.66(12) 6_556 7_547 ? O4 Cu2 Cu1 135.34(12) 4_546 7_547 ? O2 Cu2 Cu1 137.31(10) . 7_547 ? O2 Cu2 Cu1 42.69(10) 7_547 7_547 ? F2 Cu2 Cu1 122.26(11) 4_546 . ? F2 Cu2 Cu1 57.74(11) 6_556 . ? O4 Cu2 Cu1 135.34(12) 6_556 . ? O4 Cu2 Cu1 44.66(12) 4_546 . ? O2 Cu2 Cu1 42.69(10) . . ? O2 Cu2 Cu1 137.31(10) 7_547 . ? Cu1 Cu2 Cu1 180.0 7_547 . ? O1 P1 O1 114.4(4) 2_556 . ? O1 P1 O3 110.2(2) 2_556 . ? O1 P1 O3 110.4(2) . . ? O1 P1 O3 110.4(2) 2_556 2_556 ? O1 P1 O3 110.2(2) . 2_556 ? O3 P1 O3 100.3(4) . 2_556 ? O1 P1 K1 57.19(19) 2_556 7_556 ? O1 P1 K1 57.19(19) . 7_556 ? O3 P1 K1 129.86(18) . 7_556 ? O3 P1 K1 129.86(18) 2_556 7_556 ? O5 P2 O2 115.4(2) . . ? O5 P2 O4 114.0(3) . . ? O2 P2 O4 112.8(2) . . ? O5 P2 F1 103.3(2) . . ? O2 P2 F1 105.6(2) . . ? O4 P2 F1 104.1(2) . . ? O5 P2 K1 37.69(17) . 1_556 ? O2 P2 K1 119.41(18) . 1_556 ? O4 P2 K1 127.64(18) . 1_556 ? F1 P2 K1 66.07(15) . 1_556 ? O5 K1 O5 144.6(2) 2_656 1_554 ? O5 K1 F1 67.15(12) 2_656 5_656 ? O5 K1 F1 132.01(12) 1_554 5_656 ? O5 K1 F1 132.01(12) 2_656 6 ? O5 K1 F1 67.15(12) 1_554 6 ? F1 K1 F1 124.91(17) 5_656 6 ? O5 K1 O3 80.56(12) 2_656 3 ? O5 K1 O3 91.89(13) 1_554 3 ? F1 K1 O3 135.54(12) 5_656 3 ? F1 K1 O3 59.07(12) 6 3 ? O5 K1 O3 91.89(13) 2_656 4 ? O5 K1 O3 80.56(12) 1_554 4 ? F1 K1 O3 59.07(12) 5_656 4 ? F1 K1 O3 135.54(12) 6 4 ? O3 K1 O3 155.07(19) 3 4 ? O5 K1 O1 57.08(13) 2_656 8 ? O5 K1 O1 89.41(13) 1_554 8 ? F1 K1 O1 93.33(11) 5_656 8 ? F1 K1 O1 141.73(12) 6 8 ? O3 K1 O1 93.82(13) 3 8 ? O3 K1 O1 62.60(12) 4 8 ? O5 K1 O1 89.41(13) 2_656 7_556 ? O5 K1 O1 57.08(13) 1_554 7_556 ? F1 K1 O1 141.73(12) 5_656 7_556 ? F1 K1 O1 93.33(11) 6 7_556 ? O3 K1 O1 62.60(12) 3 7_556 ? O3 K1 O1 93.82(13) 4 7_556 ? O1 K1 O1 48.54(16) 8 7_556 ? O5 K1 O3 123.38(13) 2_656 8_545 ? O5 K1 O3 90.59(13) 1_554 8_545 ? F1 K1 O3 63.23(12) 5_656 8_545 ? F1 K1 O3 66.24(12) 6 8_545 ? O3 K1 O3 118.86(13) 3 8_545 ? O3 K1 O3 85.16(12) 4 8_545 ? O1 K1 O3 147.29(11) 8 8_545 ? O1 K1 O3 147.20(11) 7_556 8_545 ? O5 K1 O3 90.59(13) 2_656 7_546 ? O5 K1 O3 123.38(13) 1_554 7_546 ? F1 K1 O3 66.24(12) 5_656 7_546 ? F1 K1 O3 63.23(12) 6 7_546 ? O3 K1 O3 85.16(12) 3 7_546 ? O3 K1 O3 118.86(13) 4 7_546 ? O1 K1 O3 147.20(11) 8 7_546 ? O1 K1 O3 147.29(11) 7_556 7_546 ? O3 K1 O3 45.39(16) 8_545 7_546 ? O5 K1 F1 44.64(11) 2_656 2_656 ? O5 K1 F1 150.59(11) 1_554 2_656 ? F1 K1 F1 75.94(8) 5_656 2_656 ? F1 K1 F1 90.00(10) 6 2_656 ? O3 K1 F1 59.60(11) 3 2_656 ? O3 K1 F1 128.27(11) 4 2_656 ? O1 K1 F1 98.91(11) 8 2_656 ? O1 K1 F1 108.90(11) 7_556 2_656 ? O3 K1 F1 96.99(11) 8_545 2_656 ? O3 K1 F1 52.68(11) 7_546 2_656 ? O5 K1 F1 150.59(11) 2_656 1_554 ? O5 K1 F1 44.64(11) 1_554 1_554 ? F1 K1 F1 90.00(10) 5_656 1_554 ? F1 K1 F1 75.94(8) 6 1_554 ? O3 K1 F1 128.27(11) 3 1_554 ? O3 K1 F1 59.60(11) 4 1_554 ? O1 K1 F1 108.90(11) 8 1_554 ? O1 K1 F1 98.91(11) 7_556 1_554 ? O3 K1 F1 52.68(11) 8_545 1_554 ? O3 K1 F1 96.99(11) 7_546 1_554 ? F1 K1 F1 149.55(15) 2_656 1_554 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.873 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.230 # Attachment '- Na2Cu2(P2O7)F2)_VIII.cif' data_2010erw0120 _database_code_depnum_ccdc_archive 'CCDC 884291' #TrackingRef '- Na2Cu2(P2O7)F2)_VIII.cif' _audit_update_record ; 2011-05-31 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu2 F2 Na2 O7 P2' _chemical_formula_weight 385.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 15.7149(12) _cell_length_b 4.7342(3) _cell_length_c 9.4993(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.705(4) _cell_angle_gamma 90.00 _cell_volume 696.61(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5428 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour Blue _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 3.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 6.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5618 _exptl_absorpt_correction_T_max 0.5618 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3605 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 27.60 _reflns_number_total 801 _reflns_number_gt 726 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0479P)^2^+16.9315P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 801 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 F1 F 0.30426(16) -0.1141(6) 0.8900(3) 0.0129(5) Uani 1 1 d . . . O2 O 0.5000 0.5810(8) 0.7500 0.0070(8) Uani 1 2 d S . . O4 O 0.63039(17) 0.6482(6) 0.9383(3) 0.0079(6) Uani 1 1 d . . . O1 O 0.53219(18) 0.2161(6) 0.9406(3) 0.0083(6) Uani 1 1 d . . . O3 O 0.62973(18) 0.2653(6) 0.7566(3) 0.0085(6) Uani 1 1 d . . . Cu1 Cu 0.41381(3) 0.05358(10) 0.91263(5) 0.00677(19) Uani 1 1 d . . . P2 P 0.57835(7) 0.4245(2) 0.85279(10) 0.0062(2) Uani 1 1 d . . . Na1 Na 0.24539(10) -0.5457(4) 0.86987(17) 0.0112(4) 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 F1 0.0095(11) 0.0132(12) 0.0155(12) 0.0002(10) 0.0007(9) -0.0021(10) O2 0.0086(19) 0.008(2) 0.0046(17) 0.000 0.0011(14) 0.000 O4 0.0074(13) 0.0080(14) 0.0077(13) -0.0001(11) -0.0002(10) 0.0004(11) O1 0.0103(13) 0.0067(14) 0.0082(13) 0.0028(11) 0.0023(10) -0.0010(11) O3 0.0089(13) 0.0089(14) 0.0076(13) -0.0019(11) 0.0012(10) -0.0010(11) Cu1 0.0067(3) 0.0076(3) 0.0056(3) 0.00124(17) 0.00017(18) -0.00070(17) P2 0.0067(5) 0.0075(5) 0.0044(5) 0.0003(4) 0.0007(4) -0.0002(4) Na1 0.0104(8) 0.0115(9) 0.0110(9) 0.0021(6) -0.0004(7) -0.0017(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 Cu1 1.875(2) . ? F1 Na1 2.238(3) . ? F1 Na1 2.481(3) 4_556 ? F1 Na1 2.643(3) 7_547 ? F1 Na1 2.841(3) 1_565 ? O2 P2 1.616(2) 2_656 ? O2 P2 1.616(2) . ? O4 P2 1.492(3) . ? O4 Cu1 2.194(3) 5_667 ? O4 Na1 2.483(3) 5_657 ? O4 Na1 2.487(3) 3_565 ? O1 P2 1.549(3) . ? O1 Cu1 1.974(3) 5_657 ? O1 Cu1 1.989(3) . ? O3 P2 1.518(3) . ? O3 Cu1 1.920(3) 2_656 ? O3 Na1 2.443(3) 3 ? O3 Na1 2.625(3) 2_666 ? Cu1 O3 1.920(3) 2_656 ? Cu1 O1 1.974(3) 5_657 ? Cu1 O4 2.194(3) 5_667 ? Cu1 Cu1 2.9724(9) 5_657 ? Cu1 Na1 3.2259(17) 1_565 ? Cu1 Na1 3.3790(17) 4_556 ? Cu1 Na1 3.5030(17) 7_547 ? P2 Na1 3.425(2) 3 ? Na1 O3 2.443(3) 3_445 ? Na1 F1 2.481(3) 4_546 ? Na1 O4 2.483(3) 5_657 ? Na1 O4 2.487(3) 3_435 ? Na1 O3 2.625(3) 2_646 ? Na1 F1 2.643(3) 7_547 ? Na1 F1 2.841(3) 1_545 ? Na1 Na1 3.123(3) 7_537 ? Na1 Cu1 3.2259(17) 1_545 ? Na1 Na1 3.305(2) 4_546 ? Na1 Na1 3.305(2) 4_556 ? 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 Cu1 F1 Na1 139.00(14) . . ? Cu1 F1 Na1 100.82(11) . 4_556 ? Na1 F1 Na1 88.75(10) . 4_556 ? Cu1 F1 Na1 100.29(11) . 7_547 ? Na1 F1 Na1 99.03(10) . 7_547 ? Na1 F1 Na1 137.08(12) 4_556 7_547 ? Cu1 F1 Na1 83.63(10) . 1_565 ? Na1 F1 Na1 137.20(12) . 1_565 ? Na1 F1 Na1 76.43(9) 4_556 1_565 ? Na1 F1 Na1 69.32(8) 7_547 1_565 ? P2 O2 P2 125.5(3) 2_656 . ? P2 O4 Cu1 127.16(16) . 5_667 ? P2 O4 Na1 123.48(17) . 5_657 ? Cu1 O4 Na1 86.99(10) 5_667 5_657 ? P2 O4 Na1 128.83(16) . 3_565 ? Cu1 O4 Na1 96.72(12) 5_667 3_565 ? Na1 O4 Na1 77.86(10) 5_657 3_565 ? P2 O1 Cu1 127.43(17) . 5_657 ? P2 O1 Cu1 133.39(17) . . ? Cu1 O1 Cu1 97.18(12) 5_657 . ? P2 O3 Cu1 127.79(17) . 2_656 ? P2 O3 Na1 117.76(16) . 3 ? Cu1 O3 Na1 100.82(13) 2_656 3 ? P2 O3 Na1 128.38(17) . 2_666 ? Cu1 O3 Na1 89.04(11) 2_656 2_666 ? Na1 O3 Na1 81.31(9) 3 2_666 ? F1 Cu1 O3 86.22(12) . 2_656 ? F1 Cu1 O1 94.84(11) . 5_657 ? O3 Cu1 O1 168.32(12) 2_656 5_657 ? F1 Cu1 O1 177.53(12) . . ? O3 Cu1 O1 95.91(12) 2_656 . ? O1 Cu1 O1 82.82(12) 5_657 . ? F1 Cu1 O4 87.83(11) . 5_667 ? O3 Cu1 O4 95.60(11) 2_656 5_667 ? O1 Cu1 O4 96.06(11) 5_657 5_667 ? O1 Cu1 O4 93.19(11) . 5_667 ? F1 Cu1 Cu1 136.44(8) . 5_657 ? O3 Cu1 Cu1 135.99(9) 2_656 5_657 ? O1 Cu1 Cu1 41.61(8) 5_657 5_657 ? O1 Cu1 Cu1 41.21(8) . 5_657 ? O4 Cu1 Cu1 96.16(7) 5_667 5_657 ? F1 Cu1 Na1 61.09(9) . 1_565 ? O3 Cu1 Na1 54.45(9) 2_656 1_565 ? O1 Cu1 Na1 135.67(9) 5_657 1_565 ? O1 Cu1 Na1 121.22(9) . 1_565 ? O4 Cu1 Na1 50.24(8) 5_667 1_565 ? Cu1 Cu1 Na1 145.27(4) 5_657 1_565 ? F1 Cu1 Na1 46.16(8) . 4_556 ? O3 Cu1 Na1 45.25(9) 2_656 4_556 ? O1 Cu1 Na1 130.06(9) 5_657 4_556 ? O1 Cu1 Na1 135.26(9) . 4_556 ? O4 Cu1 Na1 109.24(8) 5_667 4_556 ? Cu1 Cu1 Na1 154.53(4) 5_657 4_556 ? Na1 Cu1 Na1 59.99(3) 1_565 4_556 ? F1 Cu1 Na1 47.94(8) . 7_547 ? O3 Cu1 Na1 108.08(9) 2_656 7_547 ? O1 Cu1 Na1 80.86(9) 5_657 7_547 ? O1 Cu1 Na1 132.08(9) . 7_547 ? O4 Cu1 Na1 44.83(8) 5_667 7_547 ? Cu1 Cu1 Na1 110.06(3) 5_657 7_547 ? Na1 Cu1 Na1 55.12(5) 1_565 7_547 ? Na1 Cu1 Na1 87.72(4) 4_556 7_547 ? O4 P2 O3 112.45(16) . . ? O4 P2 O1 114.99(16) . . ? O3 P2 O1 110.66(17) . . ? O4 P2 O2 107.18(18) . . ? O3 P2 O2 106.99(13) . . ? O1 P2 O2 103.83(14) . . ? O4 P2 Na1 95.18(12) . 3 ? O3 P2 Na1 39.15(11) . 3 ? O1 P2 Na1 89.15(12) . 3 ? O2 P2 Na1 145.71(9) . 3 ? F1 Na1 O3 75.73(10) . 3_445 ? F1 Na1 F1 105.08(11) . 4_546 ? O3 Na1 F1 63.56(10) 3_445 4_546 ? F1 Na1 O4 81.57(11) . 5_657 ? O3 Na1 O4 151.08(12) 3_445 5_657 ? F1 Na1 O4 141.34(11) 4_546 5_657 ? F1 Na1 O4 144.88(12) . 3_435 ? O3 Na1 O4 86.95(11) 3_445 3_435 ? F1 Na1 O4 93.65(10) 4_546 3_435 ? O4 Na1 O4 102.14(10) 5_657 3_435 ? F1 Na1 O3 91.15(11) . 2_646 ? O3 Na1 O3 124.19(9) 3_445 2_646 ? F1 Na1 O3 68.55(9) 4_546 2_646 ? O4 Na1 O3 73.34(10) 5_657 2_646 ? O4 Na1 O3 123.60(11) 3_435 2_646 ? F1 Na1 F1 80.97(10) . 7_547 ? O3 Na1 F1 84.36(10) 3_445 7_547 ? F1 Na1 F1 143.80(12) 4_546 7_547 ? O4 Na1 F1 74.48(9) 5_657 7_547 ? O4 Na1 F1 66.91(9) 3_435 7_547 ? O3 Na1 F1 147.65(10) 2_646 7_547 ? F1 Na1 F1 137.20(12) . 1_545 ? O3 Na1 F1 144.08(11) 3_445 1_545 ? F1 Na1 F1 89.28(10) 4_546 1_545 ? O4 Na1 F1 63.82(9) 5_657 1_545 ? O4 Na1 F1 70.94(9) 3_435 1_545 ? O3 Na1 F1 56.48(9) 2_646 1_545 ? F1 Na1 F1 110.68(8) 7_547 1_545 ? F1 Na1 Na1 122.32(11) . 7_537 ? O3 Na1 Na1 130.82(11) 3_445 7_537 ? F1 Na1 Na1 132.18(11) 4_546 7_537 ? O4 Na1 Na1 51.12(8) 5_657 7_537 ? O4 Na1 Na1 51.02(8) 3_435 7_537 ? O3 Na1 Na1 102.28(10) 2_646 7_537 ? F1 Na1 Na1 58.33(8) 7_547 7_537 ? F1 Na1 Na1 52.35(7) 1_545 7_537 ? F1 Na1 Cu1 101.98(8) . 1_545 ? O3 Na1 Cu1 160.64(9) 3_445 1_545 ? F1 Na1 Cu1 99.34(8) 4_546 1_545 ? O4 Na1 Cu1 42.77(7) 5_657 1_545 ? O4 Na1 Cu1 103.97(9) 3_435 1_545 ? O3 Na1 Cu1 36.52(6) 2_646 1_545 ? F1 Na1 Cu1 114.51(8) 7_547 1_545 ? F1 Na1 Cu1 35.28(5) 1_545 1_545 ? Na1 Na1 Cu1 66.95(6) 7_537 1_545 ? F1 Na1 Na1 130.33(11) . 4_546 ? O3 Na1 Na1 104.12(10) 3_445 4_546 ? F1 Na1 Na1 42.61(8) 4_546 4_546 ? O4 Na1 Na1 104.20(9) 5_657 4_546 ? O4 Na1 Na1 83.17(8) 3_435 4_546 ? O3 Na1 Na1 46.96(8) 2_646 4_546 ? F1 Na1 Na1 148.59(9) 7_547 4_546 ? F1 Na1 Na1 46.87(5) 1_545 4_546 ? Na1 Na1 Na1 95.76(5) 7_537 4_546 ? Cu1 Na1 Na1 62.30(4) 1_545 4_546 ? F1 Na1 Na1 48.64(7) . 4_556 ? O3 Na1 Na1 51.74(8) 3_445 4_556 ? F1 Na1 Na1 56.70(9) 4_546 4_556 ? O4 Na1 Na1 121.68(10) 5_657 4_556 ? O4 Na1 Na1 135.71(11) 3_435 4_556 ? O3 Na1 Na1 78.80(9) 2_646 4_556 ? F1 Na1 Na1 116.32(8) 7_547 4_556 ? F1 Na1 Na1 132.30(9) 1_545 4_556 ? Na1 Na1 Na1 170.94(10) 7_537 4_556 ? Cu1 Na1 Na1 112.19(7) 1_545 4_556 ? Na1 Na1 Na1 91.49(8) 4_546 4_556 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.615 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.163 # Attachment '- Rb2Cu3(PO3F)4_I.cif' data_Rb2Cu3(PO3F)4_I _database_code_depnum_ccdc_archive 'CCDC 884292' #TrackingRef '- Rb2Cu3(PO3F)4_I.cif' _audit_update_record ; 2012-05-09 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F4 O12 P4 Rb2' _chemical_formula_weight 753.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7491(4) _cell_length_b 9.4344(5) _cell_length_c 9.2186(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.186(4) _cell_angle_gamma 90.00 _cell_volume 671.20(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10729 _cell_measurement_theta_min 3.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 353 _exptl_absorpt_coefficient_mu 12.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4162 _exptl_absorpt_correction_T_max 0.8346 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7600 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.57 _reflns_number_total 1535 _reflns_number_gt 1291 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0049P)^2^+13.2791P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1535 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 F1 F 0.4911(5) 0.1640(4) -0.0470(4) 0.0152(8) Uani 1 1 d . . . F2 F 0.6868(5) 0.7020(4) -0.1475(4) 0.0163(8) Uani 1 1 d . . . O3 O 0.9060(6) 0.6582(5) 0.0484(5) 0.0132(9) Uani 1 1 d . . . O4 O 0.6804(6) 0.1678(5) 0.1793(5) 0.0129(9) Uani 1 1 d . . . O5 O 0.9581(6) 0.8376(5) -0.1466(5) 0.0098(9) Uani 1 1 d . . . O6 O 0.7300(6) 0.3343(5) -0.0275(5) 0.0136(10) Uani 1 1 d . . . O7 O 0.7788(6) 0.0715(5) -0.0579(5) 0.0162(10) Uani 1 1 d . . . O8 O 0.9438(6) 0.5797(5) -0.2153(5) 0.0150(10) Uani 1 1 d . . . Rb1 Rb 0.61772(8) 0.53951(7) 0.18568(7) 0.01399(17) Uani 1 1 d . . . Cu2 Cu 1.11182(10) 0.64409(8) 0.18411(8) 0.01030(19) Uani 1 1 d . . . Cu3 Cu 1.0000 0.5000 0.5000 0.0125(2) Uani 1 2 d S . . P4 P 0.8888(2) 0.68881(18) -0.11295(18) 0.0103(3) Uani 1 1 d . . . P5 P 0.6834(2) 0.18608(18) 0.01708(17) 0.0102(3) 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 F1 0.0116(18) 0.015(2) 0.018(2) 0.0007(15) -0.0007(15) 0.0004(15) F2 0.016(2) 0.017(2) 0.0153(19) -0.0020(16) -0.0005(15) -0.0038(16) O3 0.016(2) 0.013(2) 0.011(2) 0.0007(17) 0.0013(18) -0.0016(19) O4 0.012(2) 0.016(2) 0.010(2) -0.0002(17) 0.0002(17) 0.0000(18) O5 0.014(2) 0.008(2) 0.007(2) 0.0005(16) 0.0013(17) -0.0002(17) O6 0.017(2) 0.012(2) 0.013(2) -0.0006(17) 0.0038(18) 0.0018(19) O7 0.013(2) 0.018(3) 0.018(2) -0.0020(19) -0.0013(18) 0.0049(19) O8 0.023(3) 0.010(2) 0.012(2) -0.0039(18) 0.0045(18) 0.0001(19) Rb1 0.0157(3) 0.0137(3) 0.0125(3) -0.0005(2) 0.0008(2) -0.0001(2) Cu2 0.0121(4) 0.0106(4) 0.0082(4) 0.0006(3) 0.0013(3) -0.0001(3) Cu3 0.0119(5) 0.0101(5) 0.0152(5) 0.0037(4) -0.0015(4) -0.0024(4) P4 0.0118(8) 0.0087(8) 0.0105(8) -0.0010(6) 0.0018(6) -0.0006(6) P5 0.0114(8) 0.0098(8) 0.0095(8) 0.0001(6) 0.0007(6) 0.0016(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P5 1.566(4) . ? F1 Rb1 3.158(4) 3_665 ? F1 Rb1 3.341(4) 4_565 ? F2 P4 1.573(4) . ? F2 Rb1 2.907(4) 4_575 ? F2 Rb1 3.276(4) 3_665 ? F2 Rb1 3.517(4) . ? O3 P4 1.510(5) . ? O3 Cu2 1.940(5) . ? O3 Rb1 2.891(4) . ? O4 P5 1.508(5) . ? O4 Cu2 1.965(5) 2_745 ? O4 Rb1 2.979(4) 2_645 ? O4 Rb1 3.542(5) . ? O5 P4 1.544(5) . ? O5 Cu3 2.050(4) 2_755 ? O5 Cu2 2.055(4) 4_575 ? O5 Rb1 3.155(4) 4_575 ? O6 P5 1.511(5) . ? O6 Cu2 1.987(4) 3_765 ? O6 Rb1 2.946(4) . ? O6 Rb1 3.177(5) 3_665 ? O7 P5 1.512(5) . ? O7 Cu3 1.874(5) 2_745 ? O7 Rb1 2.776(5) 4_565 ? O8 P4 1.485(5) . ? O8 Cu2 2.179(5) 3_765 ? O8 Rb1 3.566(5) 3_765 ? Rb1 O7 2.776(5) 4_566 ? Rb1 F2 2.907(4) 4_576 ? Rb1 O4 2.979(4) 2_655 ? Rb1 O5 3.155(4) 4_576 ? Rb1 F1 3.158(4) 3_665 ? Rb1 O6 3.177(5) 3_665 ? Rb1 F2 3.276(4) 3_665 ? Rb1 F1 3.341(4) 4_566 ? Cu2 O4 1.965(5) 2_755 ? Cu2 O6 1.987(4) 3_765 ? Cu2 O5 2.055(4) 4_576 ? Cu2 O8 2.179(5) 3_765 ? Cu2 Rb1 4.0417(10) 1_655 ? Cu3 O7 1.874(5) 2_755 ? Cu3 O7 1.874(5) 4_566 ? Cu3 O5 2.050(4) 2_745 ? Cu3 O5 2.050(4) 4_576 ? Cu3 Rb1 3.9694(7) 3_766 ? P4 Rb1 3.7044(18) 4_575 ? P5 Rb1 3.7205(18) 4_565 ? P5 Rb1 3.8539(18) 3_665 ? P5 Rb1 4.0033(17) 2_645 ? 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 P5 F1 Rb1 104.19(18) . 3_665 ? P5 F1 Rb1 91.25(16) . 4_565 ? Rb1 F1 Rb1 107.23(11) 3_665 4_565 ? P4 F2 Rb1 107.78(19) . 4_575 ? P4 F2 Rb1 131.3(2) . 3_665 ? Rb1 F2 Rb1 115.48(12) 4_575 3_665 ? P4 F2 Rb1 90.94(17) . . ? Rb1 F2 Rb1 142.41(13) 4_575 . ? Rb1 F2 Rb1 68.01(7) 3_665 . ? P4 O3 Cu2 130.0(3) . . ? P4 O3 Rb1 120.2(2) . . ? Cu2 O3 Rb1 108.30(18) . . ? P5 O4 Cu2 124.3(3) . 2_745 ? P5 O4 Rb1 122.9(2) . 2_645 ? Cu2 O4 Rb1 107.91(18) 2_745 2_645 ? P5 O4 Rb1 85.3(2) . . ? Cu2 O4 Rb1 101.98(17) 2_745 . ? Rb1 O4 Rb1 106.42(13) 2_645 . ? P4 O5 Cu3 125.8(2) . 2_755 ? P4 O5 Cu2 117.7(2) . 4_575 ? Cu3 O5 Cu2 111.7(2) 2_755 4_575 ? P4 O5 Rb1 98.2(2) . 4_575 ? Cu3 O5 Rb1 97.10(15) 2_755 4_575 ? Cu2 O5 Rb1 96.50(15) 4_575 4_575 ? P5 O6 Cu2 118.1(3) . 3_765 ? P5 O6 Rb1 109.5(2) . . ? Cu2 O6 Rb1 131.0(2) 3_765 . ? P5 O6 Rb1 104.9(2) . 3_665 ? Cu2 O6 Rb1 100.47(17) 3_765 3_665 ? Rb1 O6 Rb1 76.72(11) . 3_665 ? P5 O7 Cu3 126.8(3) . 2_745 ? P5 O7 Rb1 117.3(2) . 4_565 ? Cu3 O7 Rb1 115.8(2) 2_745 4_565 ? P4 O8 Cu2 121.1(3) . 3_765 ? P4 O8 Rb1 119.8(2) . 3_765 ? Cu2 O8 Rb1 83.27(14) 3_765 3_765 ? O7 Rb1 O3 102.30(13) 4_566 . ? O7 Rb1 F2 79.58(13) 4_566 4_576 ? O3 Rb1 F2 78.11(12) . 4_576 ? O7 Rb1 O6 100.54(14) 4_566 . ? O3 Rb1 O6 71.08(13) . . ? F2 Rb1 O6 148.53(12) 4_576 . ? O7 Rb1 O4 95.94(13) 4_566 2_655 ? O3 Rb1 O4 133.23(13) . 2_655 ? F2 Rb1 O4 63.30(12) 4_576 2_655 ? O6 Rb1 O4 146.41(13) . 2_655 ? O7 Rb1 O5 55.25(12) 4_566 4_576 ? O3 Rb1 O5 55.06(12) . 4_576 ? F2 Rb1 O5 47.67(11) 4_576 4_576 ? O6 Rb1 O5 106.51(12) . 4_576 ? O4 Rb1 O5 106.94(12) 2_655 4_576 ? O7 Rb1 F1 139.61(12) 4_566 3_665 ? O3 Rb1 F1 70.63(11) . 3_665 ? F2 Rb1 F1 60.04(10) 4_576 3_665 ? O6 Rb1 F1 113.34(11) . 3_665 ? O4 Rb1 F1 67.70(11) 2_655 3_665 ? O5 Rb1 F1 93.06(10) 4_576 3_665 ? O7 Rb1 O6 146.03(13) 4_566 3_665 ? O3 Rb1 O6 108.12(12) . 3_665 ? F2 Rb1 O6 92.08(11) 4_576 3_665 ? O6 Rb1 O6 103.28(11) . 3_665 ? O4 Rb1 O6 51.81(12) 2_655 3_665 ? O5 Rb1 O6 136.37(11) 4_576 3_665 ? F1 Rb1 O6 45.42(11) 3_665 3_665 ? O7 Rb1 F2 95.34(12) 4_566 3_665 ? O3 Rb1 F2 143.13(11) . 3_665 ? F2 Rb1 F2 137.44(5) 4_576 3_665 ? O6 Rb1 F2 74.02(11) . 3_665 ? O4 Rb1 F2 75.47(11) 2_655 3_665 ? O5 Rb1 F2 150.50(10) 4_576 3_665 ? F1 Rb1 F2 114.15(10) 3_665 3_665 ? O6 Rb1 F2 68.81(11) 3_665 3_665 ? O7 Rb1 F1 45.14(11) 4_566 4_566 ? O3 Rb1 F1 146.70(11) . 4_566 ? F2 Rb1 F1 98.30(10) 4_576 4_566 ? O6 Rb1 F1 103.81(11) . 4_566 ? O4 Rb1 F1 68.56(11) 2_655 4_566 ? O5 Rb1 F1 97.94(10) 4_576 4_566 ? F1 Rb1 F1 136.23(6) 3_665 4_566 ? O6 Rb1 F1 105.08(10) 3_665 4_566 ? F2 Rb1 F1 54.74(9) 3_665 4_566 ? O7 Rb1 F2 144.65(12) 4_566 . ? O3 Rb1 F2 42.61(11) . . ? F2 Rb1 F2 93.50(5) 4_576 . ? O6 Rb1 F2 68.05(11) . . ? O4 Rb1 F2 111.91(11) 2_655 . ? O5 Rb1 F2 94.65(10) 4_576 . ? F1 Rb1 F2 46.90(9) 3_665 . ? O6 Rb1 F2 68.03(10) 3_665 . ? F2 Rb1 F2 111.99(7) 3_665 . ? F1 Rb1 F2 166.62(9) 4_566 . ? O7 Rb1 O4 65.72(12) 4_566 . ? O3 Rb1 O4 105.29(12) . . ? F2 Rb1 O4 145.15(11) 4_576 . ? O6 Rb1 O4 44.68(11) . . ? O4 Rb1 O4 121.46(10) 2_655 . ? O5 Rb1 O4 105.21(11) 4_576 . ? F1 Rb1 O4 154.46(10) 3_665 . ? O6 Rb1 O4 118.38(11) 3_665 . ? F2 Rb1 O4 53.71(10) 3_665 . ? F1 Rb1 O4 59.53(10) 4_566 . ? F2 Rb1 O4 112.65(10) . . ? O3 Cu2 O4 169.5(2) . 2_755 ? O3 Cu2 O6 92.86(19) . 3_765 ? O4 Cu2 O6 86.00(19) 2_755 3_765 ? O3 Cu2 O5 89.11(18) . 4_576 ? O4 Cu2 O5 90.09(18) 2_755 4_576 ? O6 Cu2 O5 168.94(18) 3_765 4_576 ? O3 Cu2 O8 89.47(19) . 3_765 ? O4 Cu2 O8 100.72(19) 2_755 3_765 ? O6 Cu2 O8 109.73(18) 3_765 3_765 ? O5 Cu2 O8 81.15(17) 4_576 3_765 ? O3 Cu2 Rb1 43.94(13) . . ? O4 Cu2 Rb1 139.76(13) 2_755 . ? O6 Cu2 Rb1 133.58(14) 3_765 . ? O5 Cu2 Rb1 52.42(12) 4_576 . ? O8 Cu2 Rb1 63.56(13) 3_765 . ? O3 Cu2 Rb1 139.43(13) . 1_655 ? O4 Cu2 Rb1 44.53(13) 2_755 1_655 ? O6 Cu2 Rb1 50.62(13) 3_765 1_655 ? O5 Cu2 Rb1 130.30(12) 4_576 1_655 ? O8 Cu2 Rb1 88.07(13) 3_765 1_655 ? Rb1 Cu2 Rb1 151.42(3) . 1_655 ? O7 Cu3 O7 180.00(13) 2_755 4_566 ? O7 Cu3 O5 89.72(19) 2_755 2_745 ? O7 Cu3 O5 90.28(19) 4_566 2_745 ? O7 Cu3 O5 90.28(19) 2_755 4_576 ? O7 Cu3 O5 89.72(19) 4_566 4_576 ? O5 Cu3 O5 180.00(18) 2_745 4_576 ? O7 Cu3 Rb1 39.01(14) 2_755 3_766 ? O7 Cu3 Rb1 140.99(14) 4_566 3_766 ? O5 Cu3 Rb1 52.07(12) 2_745 3_766 ? O5 Cu3 Rb1 127.93(12) 4_576 3_766 ? O7 Cu3 Rb1 140.99(14) 2_755 . ? O7 Cu3 Rb1 39.01(14) 4_566 . ? O5 Cu3 Rb1 127.93(12) 2_745 . ? O5 Cu3 Rb1 52.07(12) 4_576 . ? Rb1 Cu3 Rb1 180.0 3_766 . ? O8 P4 O3 119.3(3) . . ? O8 P4 O5 112.2(3) . . ? O3 P4 O5 111.7(3) . . ? O8 P4 F2 105.3(3) . . ? O3 P4 F2 102.2(2) . . ? O5 P4 F2 104.2(2) . . ? O8 P4 Rb1 110.1(2) . 4_575 ? O3 P4 Rb1 128.44(19) . 4_575 ? O5 P4 Rb1 57.48(17) . 4_575 ? F2 P4 Rb1 48.37(15) . 4_575 ? O8 P4 Rb1 113.9(2) . . ? O3 P4 Rb1 40.15(18) . . ? O5 P4 Rb1 133.92(17) . . ? F2 P4 Rb1 65.12(15) . . ? Rb1 P4 Rb1 106.75(4) 4_575 . ? O4 P5 O6 113.7(3) . . ? O4 P5 O7 115.1(3) . . ? O6 P5 O7 113.5(3) . . ? O4 P5 F1 105.0(2) . . ? O6 P5 F1 105.3(2) . . ? O7 P5 F1 102.7(2) . . ? O4 P5 Rb1 137.4(2) . 4_565 ? O6 P5 Rb1 108.92(19) . 4_565 ? O7 P5 Rb1 41.55(18) . 4_565 ? F1 P5 Rb1 63.86(15) . 4_565 ? O4 P5 Rb1 71.00(19) . . ? O6 P5 Rb1 48.05(17) . . ? O7 P5 Rb1 156.9(2) . . ? F1 P5 Rb1 96.60(16) . . ? Rb1 P5 Rb1 147.06(5) 4_565 . ? O4 P5 Rb1 119.67(19) . 3_665 ? O6 P5 Rb1 52.79(18) . 3_665 ? O7 P5 Rb1 123.93(19) . 3_665 ? F1 P5 Rb1 52.61(15) . 3_665 ? Rb1 P5 Rb1 87.38(3) 4_565 3_665 ? Rb1 P5 Rb1 60.16(3) . 3_665 ? O4 P5 Rb1 38.66(18) . 2_645 ? O6 P5 Rb1 132.44(18) . 2_645 ? O7 P5 Rb1 113.9(2) . 2_645 ? F1 P5 Rb1 67.59(15) . 2_645 ? Rb1 P5 Rb1 108.64(4) 4_565 2_645 ? Rb1 P5 Rb1 85.05(3) . 2_645 ? Rb1 P5 Rb1 101.49(4) 3_665 2_645 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.917 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.220 # Attachment '- RbCu3(PO3F)2(PO2(OH)2)F2_IV.cif' data_2010erw0027_c2_over_c _database_code_depnum_ccdc_archive 'CCDC 884293' #TrackingRef '- RbCu3(PO3F)2(PO2(OH)2)F2_IV.cif' _audit_update_record ; 2011-01-07 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F6 O8 P3 Rb' _chemical_formula_weight 611.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 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' '-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 19.0898(5) _cell_length_b 7.5722(3) _cell_length_c 7.8191(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.683(2) _cell_angle_gamma 90.00 _cell_volume 1098.19(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11733 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 10.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4136 _exptl_absorpt_correction_T_max 0.4136 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5615 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.56 _reflns_number_total 1262 _reflns_number_gt 1164 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0585P)^2^+48.8150P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1262 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 0.608 _refine_ls_restrained_S_all 0.608 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 F1 F 0.11708(12) 0.0355(3) 0.1300(3) 0.0136(5) Uani 1 1 d . . . F2 F 0.16688(12) 0.3363(3) -0.4333(3) 0.0111(5) Uani 1 1 d . . . O5 O 0.26308(14) 0.4449(4) -0.0701(4) 0.0095(5) Uani 1 1 d . . . O1 O -0.05957(14) 0.5197(4) -0.2067(4) 0.0102(5) Uani 1 1 d . . . O2 O -0.03204(16) -0.2422(4) -0.4035(4) 0.0119(6) Uani 1 1 d . . . O3 O 0.19327(14) 0.7141(4) -0.2454(3) 0.0088(5) Uani 1 1 d . . . O4 O 0.13522(15) 0.2637(4) -0.0707(4) 0.0099(5) Uani 1 1 d . . . Rb1 Rb 0.0000 0.14000(7) -0.2500 0.01062(14) Uani 1 2 d S . . Cu1 Cu 0.16055(2) 0.47017(6) -0.18975(6) 0.00775(14) Uani 1 1 d . . . Cu2 Cu 0.2500 0.2500 -0.5000 0.00792(16) Uani 1 2 d S . . P1 P 0.17494(5) 0.16847(13) 0.09149(12) 0.0066(2) Uani 1 1 d . . . P2 P 0.0000 -0.37483(18) -0.2500 0.0085(3) Uani 1 2 d S . . 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 F1 0.0086(11) 0.0141(12) 0.0181(12) 0.0018(9) 0.0035(9) -0.0039(9) F2 0.0098(11) 0.0131(11) 0.0105(11) -0.0014(9) 0.0027(9) 0.0017(9) O5 0.0053(12) 0.0103(13) 0.0122(13) -0.0009(10) 0.0008(10) 0.0011(10) O1 0.0059(12) 0.0149(14) 0.0101(13) -0.0002(11) 0.0021(10) -0.0008(10) O2 0.0175(14) 0.0083(13) 0.0095(13) 0.0038(10) 0.0021(11) 0.0005(11) O3 0.0078(12) 0.0085(12) 0.0081(12) 0.0007(10) -0.0020(10) -0.0024(10) O4 0.0084(12) 0.0114(13) 0.0084(13) 0.0009(10) -0.0008(10) -0.0010(10) Rb1 0.0071(2) 0.0123(3) 0.0117(3) 0.000 0.00062(18) 0.000 Cu1 0.0045(2) 0.0092(2) 0.0091(2) 0.00128(16) 0.00074(17) 0.00027(16) Cu2 0.0063(3) 0.0098(3) 0.0074(3) -0.0001(2) 0.0010(2) 0.0020(2) P1 0.0048(4) 0.0080(4) 0.0068(4) 0.0005(3) 0.0012(3) -0.0003(3) P2 0.0078(6) 0.0079(6) 0.0103(6) 0.000 0.0030(5) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P1 1.576(2) . ? F1 Rb1 2.938(2) 5 ? F1 Rb1 3.363(2) . ? F2 Cu2 1.900(2) . ? F2 Cu1 2.186(2) . ? O5 P1 1.503(3) 7 ? O5 Cu1 1.969(3) . ? O5 Cu2 2.401(3) 4_554 ? O1 P2 1.493(3) 1_565 ? O1 Cu1 1.942(3) 2_554 ? O1 Rb1 3.139(3) . ? O2 P2 1.573(3) . ? O2 Rb1 3.016(3) 5_554 ? O2 Rb1 3.138(3) . ? O3 P1 1.526(3) 6_565 ? O3 Cu2 1.986(3) 4_554 ? O3 Cu1 2.030(3) . ? O4 P1 1.499(3) . ? O4 Cu1 1.939(3) . ? O4 Rb1 2.792(3) . ? Rb1 O4 2.792(3) 2_554 ? Rb1 F1 2.938(2) 6 ? Rb1 F1 2.938(2) 5 ? Rb1 O2 3.016(3) 5_554 ? Rb1 O2 3.016(3) 6_556 ? Rb1 O2 3.138(3) 2_554 ? Rb1 O1 3.139(3) 2_554 ? Rb1 F1 3.363(2) 2_554 ? Cu1 O1 1.942(3) 2_554 ? Cu1 Cu2 2.8998(5) 4_554 ? Cu2 F2 1.900(2) 7_554 ? Cu2 O3 1.986(3) 4_544 ? Cu2 O3 1.986(3) 6_565 ? Cu2 O5 2.401(3) 6_565 ? Cu2 O5 2.401(3) 4_544 ? Cu2 Cu1 2.8998(5) 4_544 ? Cu2 Cu1 2.8998(5) 6_565 ? P1 O5 1.503(3) 7 ? P1 O3 1.526(3) 6_566 ? P2 O1 1.493(3) 2_544 ? P2 O1 1.493(3) 1_545 ? P2 O2 1.573(3) 2_554 ? P2 Rb1 3.6738(15) 1_545 ? 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 F1 Rb1 166.11(14) . 5 ? P1 F1 Rb1 91.72(10) . . ? Rb1 F1 Rb1 89.53(6) 5 . ? Cu2 F2 Cu1 128.36(11) . . ? P1 O5 Cu1 136.31(18) 7 . ? P1 O5 Cu2 134.60(16) 7 4_554 ? Cu1 O5 Cu2 82.50(10) . 4_554 ? P2 O1 Cu1 137.99(18) 1_565 2_554 ? P2 O1 Rb1 98.68(13) 1_565 . ? Cu1 O1 Rb1 97.32(11) 2_554 . ? P2 O2 Rb1 136.39(15) . 5_554 ? P2 O2 Rb1 106.95(13) . . ? Rb1 O2 Rb1 92.53(7) 5_554 . ? P1 O3 Cu2 133.82(17) 6_565 4_554 ? P1 O3 Cu1 133.48(16) 6_565 . ? Cu2 O3 Cu1 92.44(11) 4_554 . ? P1 O4 Cu1 131.33(17) . . ? P1 O4 Rb1 119.08(15) . . ? Cu1 O4 Rb1 109.59(11) . . ? O4 Rb1 O4 140.80(12) . 2_554 ? O4 Rb1 F1 68.24(7) . 6 ? O4 Rb1 F1 132.39(7) 2_554 6 ? O4 Rb1 F1 132.39(7) . 5 ? O4 Rb1 F1 68.24(7) 2_554 5 ? F1 Rb1 F1 126.22(10) 6 5 ? O4 Rb1 O2 90.30(8) . 5_554 ? O4 Rb1 O2 79.78(8) 2_554 5_554 ? F1 Rb1 O2 59.87(7) 6 5_554 ? F1 Rb1 O2 137.23(7) 5 5_554 ? O4 Rb1 O2 79.78(8) . 6_556 ? O4 Rb1 O2 90.30(8) 2_554 6_556 ? F1 Rb1 O2 137.23(7) 6 6_556 ? F1 Rb1 O2 59.87(7) 5 6_556 ? O2 Rb1 O2 150.26(11) 5_554 6_556 ? O4 Rb1 O2 125.10(8) . . ? O4 Rb1 O2 92.52(8) 2_554 . ? F1 Rb1 O2 63.57(7) 6 . ? F1 Rb1 O2 67.09(7) 5 . ? O2 Rb1 O2 87.47(7) 5_554 . ? O2 Rb1 O2 121.18(8) 6_556 . ? O4 Rb1 O2 92.52(8) . 2_554 ? O4 Rb1 O2 125.10(8) 2_554 2_554 ? F1 Rb1 O2 67.09(7) 6 2_554 ? F1 Rb1 O2 63.57(7) 5 2_554 ? O2 Rb1 O2 121.18(8) 5_554 2_554 ? O2 Rb1 O2 87.47(7) 6_556 2_554 ? O2 Rb1 O2 45.42(10) . 2_554 ? O4 Rb1 O1 55.35(8) . 2_554 ? O4 Rb1 O1 87.37(8) 2_554 2_554 ? F1 Rb1 O1 93.29(7) 6 2_554 ? F1 Rb1 O1 140.43(7) 5 2_554 ? O2 Rb1 O1 60.83(7) 5_554 2_554 ? O2 Rb1 O1 91.00(8) 6_556 2_554 ? O2 Rb1 O1 147.82(7) . 2_554 ? O2 Rb1 O1 147.48(7) 2_554 2_554 ? O4 Rb1 O1 87.37(8) . . ? O4 Rb1 O1 55.35(8) 2_554 . ? F1 Rb1 O1 140.43(7) 6 . ? F1 Rb1 O1 93.29(7) 5 . ? O2 Rb1 O1 91.00(8) 5_554 . ? O2 Rb1 O1 60.83(7) 6_556 . ? O2 Rb1 O1 147.48(7) . . ? O2 Rb1 O1 147.82(7) 2_554 . ? O1 Rb1 O1 47.36(10) 2_554 . ? O4 Rb1 F1 45.00(7) . . ? O4 Rb1 F1 149.89(7) 2_554 . ? F1 Rb1 F1 77.23(5) 6 . ? F1 Rb1 F1 90.47(6) 5 . ? O2 Rb1 F1 128.35(7) 5_554 . ? O2 Rb1 F1 60.02(7) 6_556 . ? O2 Rb1 F1 98.60(7) . . ? O2 Rb1 F1 54.28(6) 2_554 . ? O1 Rb1 F1 97.40(6) 2_554 . ? O1 Rb1 F1 107.60(7) . . ? O4 Rb1 F1 149.89(7) . 2_554 ? O4 Rb1 F1 45.00(7) 2_554 2_554 ? F1 Rb1 F1 90.47(6) 6 2_554 ? F1 Rb1 F1 77.23(5) 5 2_554 ? O2 Rb1 F1 60.02(7) 5_554 2_554 ? O2 Rb1 F1 128.35(7) 6_556 2_554 ? O2 Rb1 F1 54.28(6) . 2_554 ? O2 Rb1 F1 98.60(7) 2_554 2_554 ? O1 Rb1 F1 107.60(7) 2_554 2_554 ? O1 Rb1 F1 97.40(6) . 2_554 ? F1 Rb1 F1 152.77(8) . 2_554 ? O4 Cu1 O1 91.15(12) . 2_554 ? O4 Cu1 O5 91.50(12) . . ? O1 Cu1 O5 173.59(12) 2_554 . ? O4 Cu1 O3 164.00(11) . . ? O1 Cu1 O3 93.47(11) 2_554 . ? O5 Cu1 O3 82.45(11) . . ? O4 Cu1 F2 96.66(10) . . ? O1 Cu1 F2 88.87(10) 2_554 . ? O5 Cu1 F2 96.62(10) . . ? O3 Cu1 F2 98.73(10) . . ? O4 Cu1 Cu2 121.81(8) . 4_554 ? O1 Cu1 Cu2 118.58(9) 2_554 4_554 ? O5 Cu1 Cu2 55.19(8) . 4_554 ? O3 Cu1 Cu2 43.19(7) . 4_554 ? F2 Cu1 Cu2 129.60(6) . 4_554 ? O4 Cu1 Rb1 42.46(8) . . ? O1 Cu1 Rb1 53.04(9) 2_554 . ? O5 Cu1 Rb1 131.31(8) . . ? O3 Cu1 Rb1 146.22(8) . . ? F2 Cu1 Rb1 78.53(6) . . ? Cu2 Cu1 Rb1 151.871(15) 4_554 . ? F2 Cu2 F2 180.0 7_554 . ? F2 Cu2 O3 85.31(10) 7_554 4_544 ? F2 Cu2 O3 94.69(10) . 4_544 ? F2 Cu2 O3 94.69(10) 7_554 6_565 ? F2 Cu2 O3 85.31(10) . 6_565 ? O3 Cu2 O3 180.0 4_544 6_565 ? F2 Cu2 O5 97.45(10) 7_554 6_565 ? F2 Cu2 O5 82.55(10) . 6_565 ? O3 Cu2 O5 106.85(10) 4_544 6_565 ? O3 Cu2 O5 73.15(10) 6_565 6_565 ? F2 Cu2 O5 82.55(10) 7_554 4_544 ? F2 Cu2 O5 97.45(10) . 4_544 ? O3 Cu2 O5 73.15(10) 4_544 4_544 ? O3 Cu2 O5 106.85(10) 6_565 4_544 ? O5 Cu2 O5 180.0 6_565 4_544 ? F2 Cu2 Cu1 57.31(7) 7_554 4_544 ? F2 Cu2 Cu1 122.69(7) . 4_544 ? O3 Cu2 Cu1 44.37(8) 4_544 4_544 ? O3 Cu2 Cu1 135.63(8) 6_565 4_544 ? O5 Cu2 Cu1 137.68(6) 6_565 4_544 ? O5 Cu2 Cu1 42.32(6) 4_544 4_544 ? F2 Cu2 Cu1 122.69(7) 7_554 6_565 ? F2 Cu2 Cu1 57.31(7) . 6_565 ? O3 Cu2 Cu1 135.63(8) 4_544 6_565 ? O3 Cu2 Cu1 44.37(8) 6_565 6_565 ? O5 Cu2 Cu1 42.32(6) 6_565 6_565 ? O5 Cu2 Cu1 137.68(6) 4_544 6_565 ? Cu1 Cu2 Cu1 180.0 4_544 6_565 ? O4 P1 O5 115.76(16) . 7 ? O4 P1 O3 113.37(16) . 6_566 ? O5 P1 O3 113.26(16) 7 6_566 ? O4 P1 F1 103.41(15) . . ? O5 P1 F1 105.20(15) 7 . ? O3 P1 F1 104.20(15) 6_566 . ? O4 P1 Rb1 40.51(11) . . ? O5 P1 Rb1 118.63(11) 7 . ? O3 P1 Rb1 128.11(11) 6_566 . ? F1 P1 Rb1 63.49(9) . . ? O1 P2 O1 115.3(2) 2_544 1_545 ? O1 P2 O2 109.56(15) 2_544 2_554 ? O1 P2 O2 110.38(15) 1_545 2_554 ? O1 P2 O2 110.38(15) 2_544 . ? O1 P2 O2 109.56(15) 1_545 . ? O2 P2 O2 100.7(2) 2_554 . ? O1 P2 Rb1 57.64(12) 2_544 1_545 ? O1 P2 Rb1 57.64(12) 1_545 1_545 ? O2 P2 Rb1 129.66(11) 2_554 1_545 ? O2 P2 Rb1 129.66(11) . 1_545 ? O1 P2 Rb1 122.36(12) 2_544 . ? O1 P2 Rb1 122.36(12) 1_545 . ? O2 P2 Rb1 50.34(11) 2_554 . ? O2 P2 Rb1 50.34(11) . . ? Rb1 P2 Rb1 180.0 1_545 . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.585 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.152 data_test1 _database_code_depnum_ccdc_archive 'CCDC 884294' # start Validation Reply Form # end Validation Reply Form #Added by publCIF (Thu 24. May 13:48:51 2012) _audit_update_record ; 2012-05-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 Cu3 F4 N2 O12 P4' _chemical_formula_weight 672.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7913(2) _cell_length_b 9.6085(3) _cell_length_c 16.3303(5) _cell_angle_alpha 90.428(2) _cell_angle_beta 94.283(2) _cell_angle_gamma 99.977(2) _cell_volume 892.28(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11458 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 4.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6898 _exptl_absorpt_correction_T_max 0.8246 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15742 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4108 _reflns_number_gt 2960 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0000P)^2^+19.9405P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4108 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 F1 F 0.5802(9) 0.6673(5) 0.2684(3) 0.0162(11) Uani 1 1 d . . . F2 F 0.6579(9) 0.6996(5) 0.5689(3) 0.0163(11) Uani 1 1 d . . . F3 F 1.1319(9) 0.7224(5) 0.1095(3) 0.0149(10) Uani 1 1 d . . . O4 O 0.7648(10) 0.8736(6) 0.4663(3) 0.0095(11) Uani 1 1 d . . . O5 O 1.1660(10) 0.9753(6) 0.1473(3) 0.0131(12) Uani 1 1 d . . . F6 F 0.8421(9) 1.3701(5) 0.2268(3) 0.0187(11) Uani 1 1 d . . . O7 O 0.8872(10) 0.8632(6) 0.0298(3) 0.0101(11) Uani 1 1 d . . . O8 O 0.6142(10) 0.8390(6) 0.1601(3) 0.0133(12) Uani 1 1 d . . . O9 O 0.6074(10) 1.1325(6) 0.4622(3) 0.0108(12) Uani 1 1 d . . . O10 O 1.0927(11) 1.1934(6) 0.2413(3) 0.0149(13) Uani 1 1 d . . . O11 O 1.2045(11) 1.0538(6) 0.3849(3) 0.0138(13) Uani 1 1 d . . . O12 O 0.6757(10) 1.1019(6) -0.0173(4) 0.0139(12) Uani 1 1 d . . . O13 O 0.8270(10) 0.8955(6) 0.3005(3) 0.0130(12) Uani 1 1 d . . . O14 O 0.3877(10) 0.8669(6) 0.2863(3) 0.0123(12) Uani 1 1 d . . . O15 O 0.7040(12) 1.1610(7) 0.3059(4) 0.0220(15) Uani 1 1 d . . . O16 O 0.7095(11) 1.1508(6) 0.1518(4) 0.0172(13) Uani 1 1 d . . . N2 N 0.6616(12) 0.7086(7) 0.8972(4) 0.0127(14) Uiso 1 1 d . . . H2A H 0.7634 0.7442 0.8614 0.019 Uiso 1 1 calc R . . H2B H 0.7161 0.7403 0.9476 0.019 Uiso 1 1 calc R . . H2C H 0.5239 0.7353 0.8845 0.019 Uiso 1 1 calc R . . N1 N 0.1128(12) 0.7256(7) 0.4048(4) 0.0102(13) Uiso 1 1 d . . . H1A H 0.1940 0.7679 0.3650 0.015 Uiso 1 1 calc R . . H1B H 0.1933 0.7476 0.4531 0.015 Uiso 1 1 calc R . . H1C H -0.0252 0.7545 0.4046 0.015 Uiso 1 1 calc R . . C1 C 0.0734(16) 0.5698(9) 0.3910(5) 0.0158(18) Uiso 1 1 d . . . H6A H 0.2241 0.5389 0.3905 0.019 Uiso 1 1 calc R . . H6B H -0.0111 0.5464 0.3378 0.019 Uiso 1 1 calc R . . C2 C -0.0664(15) 0.4917(9) 0.4574(5) 0.0146(17) Uiso 1 1 d . . . H7A H -0.1049 0.3921 0.4424 0.017 Uiso 1 1 calc R . . H7B H -0.2128 0.5271 0.4598 0.017 Uiso 1 1 calc R . . C4 C 0.6300(16) 0.5493(9) 0.8943(5) 0.0173(18) Uiso 1 1 d . . . H4A H 0.7805 0.5204 0.9076 0.021 Uiso 1 1 calc R . . H4B H 0.5738 0.5150 0.8391 0.021 Uiso 1 1 calc R . . C3 C 0.4550(16) 0.4838(10) 0.9548(5) 0.0188(19) Uiso 1 1 d . . . H3A H 0.4217 0.3822 0.9457 0.023 Uiso 1 1 calc R . . H3B H 0.3089 0.5192 0.9439 0.023 Uiso 1 1 calc R . . Cu1 Cu 0.74986(18) 1.02212(11) 0.38684(6) 0.0109(2) Uani 1 1 d . . . Cu2 Cu 0.67995(18) 0.98236(11) 0.07917(6) 0.0110(2) Uani 1 1 d . . . Cu3 Cu 1.20818(18) 1.01799(11) 0.26454(6) 0.0105(2) Uani 1 1 d . . . P4 P 0.6027(4) 0.8280(2) 0.25091(12) 0.0093(4) Uani 1 1 d . . . P5 P 0.6526(4) 0.8573(2) 0.54702(12) 0.0103(4) Uani 1 1 d . . . P6 P 0.8371(4) 1.2064(2) 0.23220(13) 0.0111(4) Uani 1 1 d . . . P7 P 1.1261(4) 0.8735(2) 0.07595(12) 0.0093(4) 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 F1 0.019(3) 0.009(2) 0.021(3) 0.0038(19) 0.004(2) 0.002(2) F2 0.023(3) 0.009(2) 0.018(3) 0.0036(19) 0.001(2) 0.005(2) F3 0.019(3) 0.010(2) 0.016(2) 0.0023(19) 0.001(2) 0.004(2) O4 0.011(3) 0.011(3) 0.007(3) 0.000(2) 0.000(2) 0.004(2) O5 0.014(3) 0.017(3) 0.009(3) -0.001(2) -0.002(2) 0.004(2) F6 0.028(3) 0.008(2) 0.018(3) -0.0011(19) -0.005(2) 0.000(2) O7 0.009(3) 0.017(3) 0.004(3) -0.001(2) -0.002(2) 0.003(2) O8 0.011(3) 0.019(3) 0.009(3) 0.000(2) -0.001(2) 0.002(2) O9 0.010(3) 0.014(3) 0.006(3) 0.001(2) -0.001(2) -0.002(2) O10 0.021(3) 0.012(3) 0.011(3) 0.000(2) -0.004(2) 0.002(2) O11 0.022(3) 0.012(3) 0.005(3) 0.002(2) -0.004(2) -0.003(2) O12 0.006(3) 0.022(3) 0.014(3) 0.007(2) 0.001(2) 0.004(2) O13 0.013(3) 0.019(3) 0.006(3) 0.000(2) 0.000(2) 0.002(2) O14 0.011(3) 0.015(3) 0.012(3) 0.006(2) 0.004(2) 0.003(2) O15 0.026(4) 0.031(4) 0.016(3) 0.012(3) 0.013(3) 0.018(3) O16 0.018(3) 0.019(3) 0.014(3) -0.003(2) -0.001(2) 0.003(3) Cu1 0.0120(5) 0.0136(5) 0.0073(5) 0.0013(4) 0.0008(4) 0.0026(4) Cu2 0.0107(5) 0.0144(5) 0.0076(5) 0.0011(4) -0.0003(4) 0.0014(4) Cu3 0.0117(5) 0.0123(5) 0.0074(5) 0.0004(4) -0.0009(4) 0.0030(4) P4 0.0082(9) 0.0122(10) 0.0066(9) 0.0011(7) -0.0010(7) 0.0000(8) P5 0.0123(10) 0.0122(10) 0.0062(9) 0.0023(8) 0.0002(8) 0.0015(8) P6 0.0125(10) 0.0111(10) 0.0094(10) 0.0014(8) -0.0004(8) 0.0014(8) P7 0.0096(10) 0.0108(10) 0.0073(9) 0.0008(7) 0.0014(7) 0.0009(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P4 1.557(5) . ? F2 P5 1.564(5) . ? F3 P7 1.560(5) . ? O4 P5 1.510(6) . ? O4 Cu1 1.944(5) . ? O5 P7 1.495(6) . ? O5 Cu3 1.943(6) . ? F6 P6 1.571(5) . ? O7 P7 1.513(6) . ? O7 Cu2 2.002(6) . ? O8 P4 1.494(6) . ? O8 Cu2 1.926(6) . ? O9 P5 1.522(6) 2_676 ? O9 Cu1 1.938(6) . ? O10 P6 1.503(7) . ? O10 Cu3 1.948(6) . ? O11 P5 1.501(6) 2_776 ? O11 Cu3 1.995(6) . ? O12 P7 1.537(6) 2_775 ? O12 Cu2 1.958(6) . ? O12 Cu2 2.240(6) 2_675 ? O13 P4 1.519(6) . ? O13 Cu1 1.981(6) . ? O13 Cu3 2.431(6) . ? O14 P4 1.514(6) . ? O14 Cu3 1.947(6) 1_455 ? O15 P6 1.505(6) . ? O15 Cu1 1.922(6) . ? O16 P6 1.505(6) . ? O16 Cu2 1.975(6) . ? N2 C4 1.510(11) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N1 C1 1.487(11) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 C2 1.525(12) . ? C1 H6A 0.9700 . ? C1 H6B 0.9700 . ? C2 C2 1.532(16) 2_566 ? C2 H7A 0.9700 . ? C2 H7B 0.9700 . ? C4 C3 1.528(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 C3 1.540(17) 2_667 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? Cu1 P4 2.870(2) . ? Cu2 O12 2.240(6) 2_675 ? Cu3 O14 1.947(6) 1_655 ? P5 O11 1.501(6) 2_776 ? P5 O9 1.522(6) 2_676 ? P7 O12 1.537(6) 2_775 ? 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 P5 O4 Cu1 127.6(4) . . ? P7 O5 Cu3 151.8(4) . . ? P7 O7 Cu2 113.7(3) . . ? P4 O8 Cu2 139.1(4) . . ? P5 O9 Cu1 122.4(3) 2_676 . ? P6 O10 Cu3 124.5(4) . . ? P5 O11 Cu3 139.6(4) 2_776 . ? P7 O12 Cu2 123.7(3) 2_775 . ? P7 O12 Cu2 114.1(3) 2_775 2_675 ? Cu2 O12 Cu2 101.5(2) . 2_675 ? P4 O13 Cu1 109.5(3) . . ? P4 O13 Cu3 133.9(3) . . ? Cu1 O13 Cu3 102.2(2) . . ? P4 O14 Cu3 133.3(3) . 1_455 ? P6 O15 Cu1 130.5(4) . . ? P6 O16 Cu2 138.4(4) . . ? C4 N2 H2A 109.5 . . ? C4 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C4 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 C2 111.7(7) . . ? N1 C1 H6A 109.3 . . ? C2 C1 H6A 109.3 . . ? N1 C1 H6B 109.3 . . ? C2 C1 H6B 109.3 . . ? H6A C1 H6B 107.9 . . ? C1 C2 C2 113.1(9) . 2_566 ? C1 C2 H7A 109.0 . . ? C2 C2 H7A 109.0 2_566 . ? C1 C2 H7B 109.0 . . ? C2 C2 H7B 109.0 2_566 . ? H7A C2 H7B 107.8 . . ? N2 C4 C3 111.2(7) . . ? N2 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C3 C3 113.1(9) . 2_667 ? C4 C3 H3A 109.0 . . ? C3 C3 H3A 109.0 2_667 . ? C4 C3 H3B 109.0 . . ? C3 C3 H3B 109.0 2_667 . ? H3A C3 H3B 107.8 . . ? O15 Cu1 O9 87.1(3) . . ? O15 Cu1 O4 174.5(3) . . ? O9 Cu1 O4 92.0(2) . . ? O15 Cu1 O13 90.3(3) . . ? O9 Cu1 O13 168.0(2) . . ? O4 Cu1 O13 89.5(2) . . ? O15 Cu1 P4 83.2(2) . . ? O9 Cu1 P4 138.13(17) . . ? O4 Cu1 P4 93.95(17) . . ? O13 Cu1 P4 29.92(17) . . ? O8 Cu2 O12 165.7(2) . . ? O8 Cu2 O16 98.6(3) . . ? O12 Cu2 O16 90.1(3) . . ? O8 Cu2 O7 88.1(2) . . ? O12 Cu2 O7 92.7(2) . . ? O16 Cu2 O7 139.0(2) . . ? O8 Cu2 O12 87.4(2) . 2_675 ? O12 Cu2 O12 78.5(2) . 2_675 ? O16 Cu2 O12 117.5(3) . 2_675 ? O7 Cu2 O12 103.1(2) . 2_675 ? O5 Cu3 O14 92.9(2) . 1_655 ? O5 Cu3 O10 87.9(2) . . ? O14 Cu3 O10 168.1(3) 1_655 . ? O5 Cu3 O11 172.3(3) . . ? O14 Cu3 O11 90.3(2) 1_655 . ? O10 Cu3 O11 90.5(2) . . ? O5 Cu3 O13 97.7(2) . . ? O14 Cu3 O13 98.5(2) 1_655 . ? O10 Cu3 O13 93.2(2) . . ? O11 Cu3 O13 74.9(2) . . ? O8 P4 O14 116.8(3) . . ? O8 P4 O13 114.3(3) . . ? O14 P4 O13 111.3(3) . . ? O8 P4 F1 105.2(3) . . ? O14 P4 F1 103.1(3) . . ? O13 P4 F1 104.4(3) . . ? O8 P4 Cu1 133.9(2) . . ? O14 P4 Cu1 70.9(2) . . ? O13 P4 Cu1 40.6(2) . . ? F1 P4 Cu1 117.4(2) . . ? O11 P5 O4 112.8(3) 2_776 . ? O11 P5 O9 115.6(4) 2_776 2_676 ? O4 P5 O9 112.3(3) . 2_676 ? O11 P5 F2 106.7(3) 2_776 . ? O4 P5 F2 103.4(3) . . ? O9 P5 F2 104.8(3) 2_676 . ? O10 P6 O16 114.8(4) . . ? O10 P6 O15 114.4(4) . . ? O16 P6 O15 113.8(4) . . ? O10 P6 F6 103.8(3) . . ? O16 P6 F6 102.9(3) . . ? O15 P6 F6 105.4(4) . . ? O5 P7 O7 113.9(3) . . ? O5 P7 O12 113.1(3) . 2_775 ? O7 P7 O12 111.4(3) . 2_775 ? O5 P7 F3 108.1(3) . . ? O7 P7 F3 105.0(3) . . ? O12 P7 F3 104.5(3) 2_775 . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.274 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.284 data_2012erw039_p1 _database_code_depnum_ccdc_archive 'CCDC 884295' # start Validation Reply Form _vrf_PUBL004_GLOBAL ; PROBLEM: The contact author's name and address are missing, RESPONSE: ... ; _vrf_PUBL005_GLOBAL ; PROBLEM: _publ_contact_author_email, _publ_contact_author_fax and RESPONSE: ... ; _vrf_PUBL006_GLOBAL ; PROBLEM: _publ_requested_journal is missing RESPONSE: ... ; _vrf_PUBL008_GLOBAL ; PROBLEM: _publ_section_title is missing. Title of paper. RESPONSE: ... ; _vrf_PUBL009_GLOBAL ; PROBLEM: _publ_author_name is missing. List of author(s) name(s). RESPONSE: ... ; _vrf_PUBL010_GLOBAL ; PROBLEM: _publ_author_address is missing. Author(s) address(es). RESPONSE: ... ; _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: ... ; _vrf_PLAT113_2012erw039_p1 ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P-1 RESPONSE: Crystals grow as twinned needles, and as such it proved impossible to collect data on a single crystal, resulting in a number of difficulties, including solving the data in the correct space group. ; _vrf_PLAT201_2012erw039_p1 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 30 RESPONSE: Crystals grow as twinned needles, and as such it proved impossible to collect data on a single crystal, resulting in a number of difficulties, including obtaining reasonale temperature factors. ; _vrf_PLAT221_2012erw039_p1 ; PROBLEM: Large Solvent/Anion C Ueq(max)/Ueq(min) ... 10.0 Ratio RESPONSE: Crystals grow as twinned needles, and as such it proved impossible to collect data on a single crystal, resulting in a number of difficulties, including obtaining reasonale temperature factors. ; _vrf_PLAT223_2012erw039_p1 ; PROBLEM: Large Solvent/Anion H Ueq(max)/Ueq(min) ... 10.0 Ratio RESPONSE: Crystals grow as twinned needles, and as such it proved impossible to collect data on a single crystal, resulting in a number of difficulties, including obtaining reasonale temperature factors. ; _vrf_PLAT430_2012erw039_p1 ; PROBLEM: Short Inter D...A Contact O23 .. O26 .. 2.53 Ang. RESPONSE: Components of neighbouring phosphate tetrahedra - possibly some interactions, such as H-bonding, between close atoms. ; _vrf_PLAT431_2012erw039_p1 ; PROBLEM: Short Inter HL..A Contact F10 .. O26 . 2.43 Ang. RESPONSE: Components of neighbouring phosphate tetrahedra - possibly some interactions, such as H-bonding, between close atoms. ; # end Validation Reply Form #Added by publCIF (Thu 24. May 14:03:25 2012) _audit_update_record ; 2012-05-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cu2 F5 N2 O8 P3' _chemical_formula_weight 531.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.352(3) _cell_length_b 10.146(5) _cell_length_c 11.602(5) _cell_angle_alpha 71.90(2) _cell_angle_beta 78.96(3) _cell_angle_gamma 77.06(2) _cell_volume 686.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1526 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 31.1 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 3.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_source_power 2.5 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_specimen_support Mitegen _diffrn_detector CCD _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7547 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.1898 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 31.32 _reflns_number_total 5608 _reflns_number_gt 3381 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1053P)^2^+14.6882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _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 0.34(6) _refine_ls_number_reflns 5608 _refine_ls_number_parameters 224 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1463 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.2581 _refine_ls_wR_factor_gt 0.1976 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.006 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 F3 F 0.273(3) 0.9318(14) 0.0944(13) 0.011(3) Uiso 1 1 d . . . F4 F 0.945(3) 0.2750(16) 0.4304(14) 0.019(4) Uiso 1 1 d . . . F12 F -0.160(3) 0.7456(15) 0.1452(13) 0.011(3) Uiso 1 1 d . . . F1 F 0.352(3) 0.4587(15) 0.3740(13) 0.011(3) Uiso 1 1 d . . . O5 O 0.269(3) 0.3955(15) 0.7218(13) 0.004(3) Uiso 1 1 d . . . F2 F 0.191(2) 0.9001(14) 0.4355(12) 0.012(3) Uiso 1 1 d . . . O7 O -0.055(3) 0.8298(18) -0.2155(16) 0.015(4) Uiso 1 1 d . . . F5 F 0.022(2) 0.2956(14) 0.0923(12) 0.011(3) Uiso 1 1 d . . . O9 O 0.844(4) 0.536(2) 0.3642(18) 0.014(4) Uiso 1 1 d . . . F11 F 0.357(4) 0.144(2) 0.7084(18) 0.040(5) Uani 1 1 d . . . O11 O 0.075(4) 0.744(2) 0.3405(18) 0.020(4) Uiso 1 1 d . . . O12 O 0.136(3) 0.4572(16) 0.1677(14) 0.003(3) Uiso 1 1 d . . . O13 O 0.023(3) 0.3959(17) 0.5585(15) 0.012(4) Uiso 1 1 d . . . O14 O 0.739(3) 0.4536(17) 0.1772(15) 0.008(3) Uiso 1 1 d . . . O15 O 0.201(3) 0.7958(15) -0.0403(14) 0.006(3) Uiso 1 1 d . . . O16 O 0.243(3) 0.6581(16) 0.5475(14) 0.008(3) Uiso 1 1 d . . . O17 O 0.636(3) 0.3739(17) 0.5493(15) 0.014(4) Uiso 1 1 d . . . O18 O 0.478(3) 0.746(2) 0.3461(17) 0.016(4) Uiso 1 1 d . . . O19 O 0.582(3) 0.8160(15) -0.0354(14) 0.006(3) Uiso 1 1 d . . . O20 O -0.038(3) 0.5592(16) -0.0217(14) 0.008(3) Uiso 1 1 d . . . O23 O 0.471(3) 0.1994(19) 0.8802(17) 0.012(4) Uiso 1 1 d . . . F10 F 0.077(4) 0.198(2) 0.8668(17) 0.056(6) Uani 1 1 d . . . F7 F -0.269(3) 1.017(2) -0.3624(17) 0.026(4) Uiso 1 1 d . . . F8 F 0.119(2) 1.0139(13) -0.3688(12) 0.005(2) Uiso 1 1 d . . . N1 N 0.486(4) 0.249(2) 0.241(2) 0.012(5) Uiso 1 1 d . . . H1A H 0.5968 0.2971 0.2249 0.015 Uiso 1 1 calc R . . H1B H 0.3607 0.3112 0.2414 0.015 Uiso 1 1 calc R . . N2 N 0.726(5) -0.036(3) 0.268(2) 0.018(5) Uiso 1 1 d . . . H2A H 0.6252 -0.0920 0.2961 0.022 Uiso 1 1 calc R . . H2B H 0.8572 -0.0910 0.2598 0.022 Uiso 1 1 calc R . . N3 N 0.376(3) 0.6546(17) 0.7613(15) 0.006(3) Uiso 1 1 d . . . H3A H 0.2502 0.7025 0.7904 0.007 Uiso 1 1 calc R . . H3B H 0.3471 0.6186 0.7053 0.007 Uiso 1 1 calc R . . C15 C 0.536(4) 0.749(3) 0.705(2) 0.017(5) Uiso 1 1 d . . . H15A H 0.4684 0.8313 0.6472 0.020 Uiso 1 1 calc R . . H15B H 0.5724 0.7799 0.7689 0.020 Uiso 1 1 calc R . . C10 C 0.723(3) 0.0420(19) 0.3589(17) 0.003(3) Uiso 1 1 d . . . H10A H 0.8408 0.0960 0.3335 0.003 Uiso 1 1 calc R . . H10B H 0.7438 -0.0241 0.4385 0.003 Uiso 1 1 calc R . . C11 C 0.680(4) 0.063(3) 0.143(2) 0.021(6) Uiso 1 1 d . . . H11A H 0.8113 0.1004 0.1028 0.025 Uiso 1 1 calc R . . H11B H 0.6520 0.0073 0.0948 0.025 Uiso 1 1 calc R . . C12 C 0.503(7) 0.178(4) 0.142(3) 0.050(10) Uiso 1 1 d . . . H12A H 0.3684 0.1440 0.1506 0.060 Uiso 1 1 calc R . . H12B H 0.5180 0.2475 0.0634 0.060 Uiso 1 1 calc R . . C13 C 0.494(4) 0.145(2) 0.3668(19) 0.007(4) Uiso 1 1 d . . . H13A H 0.3749 0.0928 0.3872 0.009 Uiso 1 1 calc R . . H13B H 0.4829 0.1934 0.4285 0.009 Uiso 1 1 calc R . . O25 O 0.369(3) 0.6778(17) 0.1505(15) 0.005(3) Uiso 1 1 d . . . O26 O -0.157(3) 1.0700(16) -0.1836(14) 0.005(3) Uiso 1 1 d . . . C16 C 0.470(5) 0.541(3) 0.861(2) 0.021(6) Uiso 1 1 d . . . H16A H 0.3687 0.4757 0.8990 0.025 Uiso 1 1 calc R . . H16B H 0.4918 0.5804 0.9234 0.025 Uiso 1 1 calc R . . N4 N 0.840(4) 0.574(2) 0.7390(18) 0.017(5) Uiso 1 1 d . . . H4A H 0.8737 0.6109 0.7932 0.021 Uiso 1 1 calc R . . H4B H 0.9663 0.5363 0.7015 0.021 Uiso 1 1 calc R . . C5 C 0.706(4) 0.454(2) 0.8101(19) 0.006(4) Uiso 1 1 d . . . H5A H 0.7786 0.3887 0.8773 0.008 Uiso 1 1 calc R . . H5B H 0.6854 0.4035 0.7561 0.008 Uiso 1 1 calc R . . C4 C 0.725(4) 0.689(2) 0.6465(19) 0.009(4) Uiso 1 1 d . . . H4C H 0.8164 0.7596 0.6055 0.011 Uiso 1 1 calc R . . H4D H 0.6919 0.6522 0.5857 0.011 Uiso 1 1 calc R . . Cu1 Cu 0.3165(4) 0.4255(2) 0.5468(2) 0.0091(6) Uiso 1 1 d . . . Cu2 Cu -0.1092(4) 0.7836(3) -0.0300(2) 0.0095(6) Uani 1 1 d . . . Cu3 Cu 0.6069(8) 0.6031(4) 0.2579(4) 0.0091(3) Uani 1 1 d . . . Cu4 Cu 0.1091(8) 0.6015(4) 0.2540(4) 0.0086(4) Uani 1 1 d . . . P5 P 0.2507(11) 0.7564(6) 0.4127(5) 0.0049(11) Uiso 1 1 d . . . P6 P 0.8496(12) 0.4112(7) 0.4763(6) 0.0080(12) Uiso 1 1 d . . . P7 P -0.0826(12) 0.9796(7) -0.2765(6) 0.0097(13) Uiso 1 1 d . . . P8 P 0.3565(13) 0.8094(7) 0.0344(6) 0.0104(13) Uani 1 1 d . . . P9 P 0.3053(12) 0.2339(7) 0.7903(6) 0.0117(13) Uiso 1 1 d . . . P10 P -0.0378(14) 0.4609(8) 0.0964(7) 0.0165(15) Uiso 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 F11 0.052(11) 0.034(8) 0.034(9) -0.018(7) -0.013(8) 0.014(7) F10 0.060(13) 0.072(13) 0.020(9) 0.000(8) 0.006(8) -0.008(10) Cu2 0.0070(12) 0.0153(11) 0.0052(10) -0.0017(7) -0.0014(8) -0.0013(9) Cu3 0.0080(8) 0.0099(7) 0.0081(7) -0.0017(5) -0.0018(6) 0.0004(6) Cu4 0.0092(8) 0.0098(8) 0.0075(8) -0.0048(6) -0.0010(6) 0.0005(7) P8 0.011(3) 0.007(2) 0.011(2) 0.0002(16) -0.0031(17) 0.0014(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F3 P8 1.552(15) . ? F4 P6 1.587(17) . ? F12 Cu2 1.924(15) . ? F12 Cu3 2.246(16) 1_455 ? F12 Cu4 2.281(16) . ? F1 Cu1 1.904(15) . ? F1 Cu4 2.235(16) . ? F1 Cu3 2.362(15) . ? O5 P9 1.570(16) . ? O5 Cu1 1.931(15) . ? F2 P5 1.514(14) . ? O7 P7 1.449(18) . ? O7 Cu2 2.033(18) . ? F5 P10 1.648(15) . ? O9 P6 1.50(2) . ? O9 Cu3 1.99(2) . ? O9 Cu4 2.02(2) 1_655 ? F11 P9 1.456(19) . ? O11 P5 1.56(2) . ? O11 Cu4 1.96(2) . ? O12 P10 1.491(18) . ? O12 Cu4 1.976(15) . ? O13 P6 1.54(2) 1_455 ? O13 Cu1 1.928(19) . ? O14 P10 1.547(19) 1_655 ? O14 Cu3 1.973(17) . ? O15 P8 1.489(18) . ? O15 Cu2 1.977(17) . ? O16 P5 1.571(17) . ? O16 Cu1 2.304(16) . ? O17 P6 1.516(19) . ? O17 Cu1 1.981(19) . ? O18 P5 1.50(2) . ? O18 Cu3 1.97(2) . ? O19 P8 1.508(18) . ? O19 Cu2 1.926(17) 1_655 ? O20 P10 1.422(17) . ? O20 Cu2 2.194(16) . ? O23 P9 1.53(2) . ? F10 P9 1.60(2) . ? F7 P7 1.60(2) . ? F8 P7 1.533(14) . ? N1 C13 1.51(3) . ? N1 C12 1.51(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C10 1.50(3) . ? N2 C11 1.52(4) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C16 1.47(3) . ? N3 C15 1.47(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C15 C4 1.38(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C10 C13 1.60(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.43(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? O25 P8 1.574(18) . ? O25 Cu4 1.999(18) . ? O25 Cu3 2.010(19) . ? O26 P7 1.566(17) . ? C16 C5 1.67(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? N4 C4 1.48(3) . ? N4 C5 1.57(3) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? Cu2 O19 1.926(17) 1_455 ? Cu3 F12 2.246(16) 1_655 ? Cu4 O9 2.02(2) 1_455 ? P6 O13 1.54(2) 1_655 ? P10 O14 1.547(19) 1_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 Cu2 F12 Cu3 120.5(7) . 1_455 ? Cu2 F12 Cu4 117.9(7) . . ? Cu3 F12 Cu4 89.2(5) 1_455 . ? Cu1 F1 Cu4 123.9(8) . . ? Cu1 F1 Cu3 116.8(7) . . ? Cu4 F1 Cu3 87.3(5) . . ? P9 O5 Cu1 110.7(9) . . ? P7 O7 Cu2 113.6(11) . . ? P6 O9 Cu3 124.9(12) . . ? P6 O9 Cu4 124.8(13) . 1_655 ? Cu3 O9 Cu4 104.8(9) . 1_655 ? P5 O11 Cu4 124.4(13) . . ? P10 O12 Cu4 120.5(10) . . ? P6 O13 Cu1 140.5(11) 1_455 . ? P10 O14 Cu3 119.5(10) 1_655 . ? P8 O15 Cu2 140.9(10) . . ? P5 O16 Cu1 110.0(8) . . ? P6 O17 Cu1 142.0(11) . . ? P5 O18 Cu3 123.2(11) . . ? P8 O19 Cu2 147.8(10) . 1_655 ? P10 O20 Cu2 117.1(9) . . ? C13 N1 C12 112(2) . . ? C13 N1 H1A 109.1 . . ? C12 N1 H1A 109.1 . . ? C13 N1 H1B 109.1 . . ? C12 N1 H1B 109.1 . . ? H1A N1 H1B 107.9 . . ? C10 N2 C11 113(2) . . ? C10 N2 H2A 109.1 . . ? C11 N2 H2A 109.1 . . ? C10 N2 H2B 109.1 . . ? C11 N2 H2B 109.1 . . ? H2A N2 H2B 107.8 . . ? C16 N3 C15 108(2) . . ? C16 N3 H3A 110.2 . . ? C15 N3 H3A 110.2 . . ? C16 N3 H3B 110.2 . . ? C15 N3 H3B 110.2 . . ? H3A N3 H3B 108.5 . . ? C4 C15 N3 115(2) . . ? C4 C15 H15A 108.6 . . ? N3 C15 H15A 108.6 . . ? C4 C15 H15B 108.6 . . ? N3 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? N2 C10 C13 108.3(19) . . ? N2 C10 H10A 110.0 . . ? C13 C10 H10A 110.0 . . ? N2 C10 H10B 110.0 . . ? C13 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C12 C11 N2 116(3) . . ? C12 C11 H11A 108.2 . . ? N2 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? N2 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? C11 C12 N1 115(3) . . ? C11 C12 H12A 108.6 . . ? N1 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? N1 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? N1 C13 C10 105.5(17) . . ? N1 C13 H13A 110.6 . . ? C10 C13 H13A 110.6 . . ? N1 C13 H13B 110.7 . . ? C10 C13 H13B 110.6 . . ? H13A C13 H13B 108.8 . . ? P8 O25 Cu4 124.3(11) . . ? P8 O25 Cu3 127.3(10) . . ? Cu4 O25 Cu3 104.7(8) . . ? N3 C16 C5 110.9(19) . . ? N3 C16 H16A 109.5 . . ? C5 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? C5 C16 H16B 109.5 . . ? H16A C16 H16B 108.0 . . ? C4 N4 C5 113.9(19) . . ? C4 N4 H4A 108.8 . . ? C5 N4 H4A 108.8 . . ? C4 N4 H4B 108.8 . . ? C5 N4 H4B 108.8 . . ? H4A N4 H4B 107.7 . . ? N4 C5 C16 103.6(17) . . ? N4 C5 H5A 111.0 . . ? C16 C5 H5A 111.0 . . ? N4 C5 H5B 111.0 . . ? C16 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C15 C4 N4 108.2(19) . . ? C15 C4 H4C 110.1 . . ? N4 C4 H4C 110.1 . . ? C15 C4 H4D 110.1 . . ? N4 C4 H4D 110.1 . . ? H4C C4 H4D 108.4 . . ? F1 Cu1 O13 90.5(7) . . ? F1 Cu1 O5 177.9(8) . . ? O13 Cu1 O5 87.9(7) . . ? F1 Cu1 O17 91.4(7) . . ? O13 Cu1 O17 157.2(7) . . ? O5 Cu1 O17 90.6(7) . . ? F1 Cu1 O16 97.0(6) . . ? O13 Cu1 O16 99.2(7) . . ? O5 Cu1 O16 82.0(6) . . ? O17 Cu1 O16 103.1(7) . . ? F12 Cu2 O19 90.4(7) . 1_455 ? F12 Cu2 O15 93.5(7) . . ? O19 Cu2 O15 167.3(6) 1_455 . ? F12 Cu2 O7 178.2(7) . . ? O19 Cu2 O7 89.9(7) 1_455 . ? O15 Cu2 O7 85.8(7) . . ? F12 Cu2 O20 93.1(6) . . ? O19 Cu2 O20 98.2(6) 1_455 . ? O15 Cu2 O20 93.7(6) . . ? O7 Cu2 O20 88.6(6) . . ? O18 Cu3 O14 177.3(10) . . ? O18 Cu3 O9 88.8(8) . . ? O14 Cu3 O9 89.3(8) . . ? O18 Cu3 O25 89.8(8) . . ? O14 Cu3 O25 92.2(7) . . ? O9 Cu3 O25 178.1(9) . . ? O18 Cu3 F12 88.4(7) . 1_655 ? O14 Cu3 F12 93.1(6) . 1_655 ? O9 Cu3 F12 81.1(7) . 1_655 ? O25 Cu3 F12 97.6(6) . 1_655 ? O18 Cu3 F1 90.8(7) . . ? O14 Cu3 F1 87.8(6) . . ? O9 Cu3 F1 100.5(7) . . ? O25 Cu3 F1 80.8(6) . . ? F12 Cu3 F1 178.2(8) 1_655 . ? O11 Cu4 O12 178.8(11) . . ? O11 Cu4 O25 88.1(8) . . ? O12 Cu4 O25 93.0(7) . . ? O11 Cu4 O9 87.8(8) . 1_455 ? O12 Cu4 O9 91.1(7) . 1_455 ? O25 Cu4 O9 175.9(9) . 1_455 ? O11 Cu4 F1 90.6(8) . . ? O12 Cu4 F1 90.0(6) . . ? O25 Cu4 F1 84.3(7) . . ? O9 Cu4 F1 96.0(7) 1_455 . ? O11 Cu4 F12 87.4(7) . . ? O12 Cu4 F12 91.9(6) . . ? O25 Cu4 F12 99.8(7) . . ? O9 Cu4 F12 79.7(7) 1_455 . ? F1 Cu4 F12 175.4(7) . . ? O18 P5 F2 106.8(10) . . ? O18 P5 O11 114.5(11) . . ? F2 P5 O11 107.5(10) . . ? O18 P5 O16 111.7(11) . . ? F2 P5 O16 100.7(8) . . ? O11 P5 O16 114.3(10) . . ? O9 P6 O17 118.6(12) . . ? O9 P6 O13 115.8(11) . 1_655 ? O17 P6 O13 112.6(10) . 1_655 ? O9 P6 F4 106.8(10) . . ? O17 P6 F4 100.8(10) . . ? O13 P6 F4 98.7(10) 1_655 . ? O7 P7 F8 110.0(10) . . ? O7 P7 O26 112.1(10) . . ? F8 P7 O26 115.8(8) . . ? O7 P7 F7 108.0(11) . . ? F8 P7 F7 102.6(10) . . ? O26 P7 F7 107.6(10) . . ? O15 P8 O19 112.3(9) . . ? O15 P8 F3 113.3(9) . . ? O19 P8 F3 112.0(9) . . ? O15 P8 O25 108.2(9) . . ? O19 P8 O25 109.0(10) . . ? F3 P8 O25 101.3(9) . . ? F11 P9 O23 113.3(12) . . ? F11 P9 O5 113.5(11) . . ? O23 P9 O5 110.1(10) . . ? F11 P9 F10 103.6(13) . . ? O23 P9 F10 108.3(12) . . ? O5 P9 F10 107.5(11) . . ? O20 P10 O12 116.3(10) . . ? O20 P10 O14 116.5(11) . 1_455 ? O12 P10 O14 111.8(10) . 1_455 ? O20 P10 F5 113.2(9) . . ? O12 P10 F5 98.3(9) . . ? O14 P10 F5 97.7(9) 1_455 . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.287 _refine_diff_density_min -2.133 _refine_diff_density_rms 0.366 data_test2 _database_code_depnum_ccdc_archive 'CCDC 884296' _audit_update_record ; 2012-05-09 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 Cu2 F4 N2 O6 P2' _chemical_formula_weight 477.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9501(4) _cell_length_b 10.8176(3) _cell_length_c 6.1008(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.600(2) _cell_angle_gamma 90.00 _cell_volume 710.33(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5902 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 3.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4931 _exptl_absorpt_correction_T_max 0.8526 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7729 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.60 _reflns_number_total 1620 _reflns_number_gt 1359 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0549P)^2^+9.2083P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1620 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 F1 F 0.2748(3) 0.1821(3) 0.1369(6) 0.0154(7) Uani 1 1 d . . . F2 F 0.3160(3) -0.2565(3) 0.3470(5) 0.0120(7) Uani 1 1 d . . . O3 O 0.3491(4) -0.0286(4) 0.1920(6) 0.0118(8) Uani 1 1 d . . . O4 O 0.4249(4) 0.1099(4) -0.0870(6) 0.0110(8) Uani 1 1 d . . . O5 O 0.4909(4) 0.1510(4) 0.3285(6) 0.0124(8) Uani 1 1 d . . . N4 N 0.2629(5) 0.5350(5) 0.1021(8) 0.0122(10) Uani 1 1 d . . . H4A H 0.3051 0.4787 0.1920 0.018 Uiso 1 1 calc R . . H4B H 0.2605 0.6055 0.1763 0.018 Uiso 1 1 calc R . . H4C H 0.3001 0.5477 -0.0139 0.018 Uiso 1 1 calc R . . C2 C 0.1339(5) 0.4900(6) 0.0214(10) 0.0136(11) Uani 1 1 d . . . H2 H 0.1386 0.4140 -0.0640 0.016 Uiso 1 1 calc R . . C3 C 0.0612(6) 0.5847(7) -0.1327(11) 0.0227(14) Uani 1 1 d . . . H3A H 0.1022 0.5991 -0.2585 0.027 Uiso 1 1 calc R . . H3B H 0.0593 0.6623 -0.0536 0.027 Uiso 1 1 calc R . . C1 C 0.0711(6) 0.4594(7) 0.2170(11) 0.0225(14) Uani 1 1 d . . . H1A H 0.0698 0.5322 0.3093 0.027 Uiso 1 1 calc R . . H1B H 0.1176 0.3953 0.3074 0.027 Uiso 1 1 calc R . . Cu1 Cu 0.43088(6) -0.18688(6) 0.17896(11) 0.0100(2) Uani 1 1 d . . . P2 P 0.39410(14) 0.09946(13) 0.1442(2) 0.0097(3) 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 F1 0.0143(17) 0.0109(17) 0.0223(18) -0.0006(13) 0.0069(14) 0.0035(14) F2 0.0148(17) 0.0100(16) 0.0119(16) 0.0016(12) 0.0042(12) -0.0013(13) O3 0.017(2) 0.0078(19) 0.0125(19) 0.0020(14) 0.0086(16) -0.0004(16) O4 0.013(2) 0.011(2) 0.0111(19) 0.0028(15) 0.0067(15) -0.0001(16) O5 0.018(2) 0.0066(19) 0.0130(19) -0.0003(14) 0.0051(16) -0.0010(16) N4 0.014(2) 0.014(2) 0.009(2) 0.0020(17) 0.0015(18) -0.0002(19) C2 0.008(3) 0.013(3) 0.021(3) -0.003(2) 0.006(2) -0.003(2) C3 0.022(3) 0.028(4) 0.019(3) 0.010(3) 0.008(3) -0.001(3) C1 0.022(3) 0.026(4) 0.019(3) 0.012(3) 0.004(3) -0.002(3) Cu1 0.0141(4) 0.0055(4) 0.0117(4) 0.0006(2) 0.0061(3) 0.0000(3) P2 0.0138(7) 0.0058(7) 0.0108(7) -0.0001(5) 0.0056(5) -0.0001(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P2 1.576(4) . ? F2 Cu1 1.917(3) . ? F2 Cu1 2.263(3) 4_556 ? O3 P2 1.517(4) . ? O3 Cu1 1.940(4) . ? O4 P2 1.514(4) . ? O4 Cu1 1.956(4) 3_655 ? O5 P2 1.503(4) . ? O5 Cu1 1.956(4) 2_655 ? N4 C2 1.490(7) . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? C2 C3 1.514(9) . ? C2 C1 1.519(8) . ? C2 H2 0.9800 . ? C3 C1 1.522(9) 3_565 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C1 C3 1.522(9) 3_565 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? Cu1 O5 1.956(4) 2_645 ? Cu1 O4 1.956(4) 3_655 ? Cu1 F2 2.263(3) 4 ? 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 Cu1 F2 Cu1 105.85(15) . 4_556 ? P2 O3 Cu1 129.0(2) . . ? P2 O4 Cu1 129.0(3) . 3_655 ? P2 O5 Cu1 124.5(2) . 2_655 ? C2 N4 H4A 109.5 . . ? C2 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C2 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? N4 C2 C3 110.0(5) . . ? N4 C2 C1 110.5(5) . . ? C3 C2 C1 111.9(5) . . ? N4 C2 H2 108.1 . . ? C3 C2 H2 108.1 . . ? C1 C2 H2 108.1 . . ? C2 C3 C1 110.9(5) . 3_565 ? C2 C3 H3A 109.5 . . ? C1 C3 H3A 109.5 3_565 . ? C2 C3 H3B 109.5 . . ? C1 C3 H3B 109.5 3_565 . ? H3A C3 H3B 108.1 . . ? C2 C1 C3 110.1(5) . 3_565 ? C2 C1 H1A 109.6 . . ? C3 C1 H1A 109.6 3_565 . ? C2 C1 H1B 109.6 . . ? C3 C1 H1B 109.6 3_565 . ? H1A C1 H1B 108.2 . . ? F2 Cu1 O3 88.35(15) . . ? F2 Cu1 O5 89.63(16) . 2_645 ? O3 Cu1 O5 177.97(16) . 2_645 ? F2 Cu1 O4 164.63(16) . 3_655 ? O3 Cu1 O4 92.26(17) . 3_655 ? O5 Cu1 O4 89.71(17) 2_645 3_655 ? F2 Cu1 F2 93.47(12) . 4 ? O3 Cu1 F2 95.21(15) . 4 ? O5 Cu1 F2 84.84(15) 2_645 4 ? O4 Cu1 F2 101.76(14) 3_655 4 ? O5 P2 O4 114.9(2) . . ? O5 P2 O3 113.8(2) . . ? O4 P2 O3 112.6(2) . . ? O5 P2 F1 106.1(2) . . ? O4 P2 F1 104.9(2) . . ? O3 P2 F1 103.1(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.650 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.217 data_test4 _database_code_depnum_ccdc_archive 'CCDC 884297' _audit_update_record ; 2012-05-09 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F4 H8 N2 O12 P4' _chemical_formula_weight 618.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.8246(7) _cell_length_b 9.4940(8) _cell_length_c 9.1169(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.870(5) _cell_angle_gamma 90.00 _cell_volume 674.82(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 21324 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 301 _exptl_absorpt_coefficient_mu 5.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.8793 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7706 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.64 _reflns_number_total 1549 _reflns_number_gt 1250 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0338P)^2^+18.8865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1549 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.176 _refine_ls_shift/su_mean 0.003 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 F1 F 0.0088(6) 0.1570(5) 0.5464(5) 0.0211(9) Uani 1 1 d . . . F2 F -0.1918(5) -0.2104(5) 0.1474(5) 0.0199(9) Uani 1 1 d . . . O2 O -0.5913(6) 0.1593(5) 0.0480(5) 0.0166(10) Uani 1 1 d . . . O6 O -0.1781(7) 0.1566(5) 0.3161(5) 0.0174(11) Uani 1 1 d . . . O7 O -0.5337(7) 0.1622(5) 0.3546(5) 0.0152(10) Uani 1 1 d . . . N1 N -0.1257(9) -0.0414(7) 0.8218(8) 0.0173(13) Uani 1 1 d . . . O4 O -0.2298(6) 0.3269(5) 0.5217(5) 0.0163(11) Uani 1 1 d . . . O5 O -0.2763(7) 0.0644(6) 0.5585(6) 0.0200(11) Uani 1 1 d . . . O8 O -0.4421(7) -0.0817(5) 0.2184(6) 0.0209(11) Uani 1 1 d . . . H1 H -0.171(11) -0.010(9) 0.739(10) 0.02(2) Uiso 1 1 d . . . H3 H -0.025(12) -0.075(10) 0.806(9) 0.02(2) Uiso 1 1 d . . . H4 H -0.124(9) 0.028(8) 0.879(8) 0.000(16) Uiso 1 1 d . . . H2 H -0.199(14) -0.117(13) 0.854(12) 0.05(3) Uiso 1 1 d . . . Cu1 Cu -0.38473(11) 0.14180(9) 0.18106(9) 0.0148(2) Uani 1 1 d . . . Cu2 Cu -0.5000 0.0000 0.5000 0.0172(3) Uani 1 2 d S . . P3 P -0.1799(2) 0.17800(19) 0.4802(2) 0.0152(4) Uani 1 1 d . . . P4 P -0.3912(2) -0.19163(19) 0.1145(2) 0.0141(4) 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 F1 0.020(2) 0.021(2) 0.022(2) 0.0036(18) -0.0017(17) -0.0008(18) F2 0.020(2) 0.020(2) 0.020(2) 0.0024(18) -0.0003(17) 0.0006(18) O2 0.021(3) 0.015(3) 0.013(2) 0.004(2) 0.0030(19) 0.001(2) O6 0.024(3) 0.014(3) 0.015(2) -0.001(2) 0.003(2) 0.001(2) O7 0.024(3) 0.011(2) 0.010(2) 0.0023(18) 0.0033(19) -0.002(2) N1 0.021(4) 0.009(3) 0.021(3) -0.006(3) -0.002(3) 0.000(3) O4 0.020(3) 0.011(2) 0.019(3) 0.0024(19) 0.005(2) 0.0011(19) O5 0.022(3) 0.020(3) 0.017(2) 0.008(2) -0.002(2) -0.004(2) O8 0.030(3) 0.012(3) 0.021(3) -0.003(2) 0.000(2) -0.003(2) Cu1 0.0186(5) 0.0118(4) 0.0141(4) 0.0002(3) 0.0010(3) 0.0000(3) Cu2 0.0187(6) 0.0112(6) 0.0213(6) 0.0042(5) -0.0014(5) -0.0023(5) P3 0.0177(9) 0.0126(9) 0.0152(9) 0.0011(7) 0.0007(7) 0.0002(7) P4 0.0179(9) 0.0092(8) 0.0148(8) -0.0005(7) -0.0004(7) -0.0007(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 P3 1.560(5) . ? F2 P4 1.573(5) . ? O2 P4 1.508(5) 3_455 ? O2 Cu1 1.944(5) . ? O6 P3 1.511(5) . ? O6 Cu1 1.952(5) . ? O7 P4 1.542(5) 2_455 ? O7 Cu2 2.035(5) . ? O7 Cu1 2.052(5) . ? O4 P3 1.523(5) . ? O4 Cu1 1.992(5) 4_566 ? O5 P3 1.528(5) . ? O5 Cu2 1.888(5) . ? O8 P4 1.486(5) . ? O8 Cu1 2.201(5) . ? Cu1 O4 1.992(5) 4_565 ? Cu2 O5 1.888(5) 3_456 ? Cu2 O7 2.035(5) 3_456 ? P4 O2 1.508(5) 3_455 ? P4 O7 1.542(5) 2_445 ? 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 P4 O2 Cu1 129.2(3) 3_455 . ? P3 O6 Cu1 123.9(3) . . ? P4 O7 Cu2 126.3(3) 2_455 . ? P4 O7 Cu1 118.4(3) 2_455 . ? Cu2 O7 Cu1 112.3(2) . . ? P3 O4 Cu1 120.3(3) . 4_566 ? P3 O5 Cu2 125.4(3) . . ? P4 O8 Cu1 120.6(3) . . ? O2 Cu1 O6 170.9(2) . . ? O2 Cu1 O4 93.3(2) . 4_565 ? O6 Cu1 O4 85.8(2) . 4_565 ? O2 Cu1 O7 88.6(2) . . ? O6 Cu1 O7 90.1(2) . . ? O4 Cu1 O7 165.7(2) 4_565 . ? O2 Cu1 O8 90.5(2) . . ? O6 Cu1 O8 98.1(2) . . ? O4 Cu1 O8 113.7(2) 4_565 . ? O7 Cu1 O8 80.5(2) . . ? O5 Cu2 O5 180.0 . 3_456 ? O5 Cu2 O7 90.3(2) . . ? O5 Cu2 O7 89.7(2) 3_456 . ? O5 Cu2 O7 89.7(2) . 3_456 ? O5 Cu2 O7 90.3(2) 3_456 3_456 ? O7 Cu2 O7 180.000(1) . 3_456 ? O6 P3 O4 113.3(3) . . ? O6 P3 O5 114.5(3) . . ? O4 P3 O5 113.1(3) . . ? O6 P3 F1 106.2(3) . . ? O4 P3 F1 106.1(3) . . ? O5 P3 F1 102.6(3) . . ? O8 P4 O2 118.4(3) . 3_455 ? O8 P4 O7 112.9(3) . 2_445 ? O2 P4 O7 111.0(3) 3_455 2_445 ? O8 P4 F2 105.8(3) . . ? O2 P4 F2 102.5(3) 3_455 . ? O7 P4 F2 104.5(3) 2_445 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.816 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.209 data_test3 _database_code_depnum_ccdc_archive 'CCDC 884298' _audit_update_record ; 2012-05-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 F4 H6 N O10 P3' _chemical_formula_weight 543.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 19.0802(6) _cell_length_b 7.6023(2) _cell_length_c 7.8054(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.789(2) _cell_angle_gamma 90.00 _cell_volume 1099.57(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4966 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 6.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4509 _exptl_absorpt_correction_T_max 0.7430 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6866 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1268 _reflns_number_gt 1158 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0174P)^2^+14.4270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1268 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.004 _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 O6 O 0.46830(16) 0.7441(3) 0.5971(3) 0.0119(6) Uani 1 1 d . . . O4 O 0.69354(15) 0.7861(4) 0.7540(3) 0.0097(5) Uani 1 1 d . . . N1 N 0.5000 1.3596(7) 0.7500 0.0146(10) Uani 1 2 d S . . Cu1 Cu 0.66083(2) 1.02961(6) 0.81028(6) 0.00843(14) Uani 1 1 d . . . Cu2 Cu 0.7500 0.7500 1.0000 0.00808(17) Uani 1 2 d S . . P2 P 0.5000 0.87686(18) 0.7500 0.0086(3) Uani 1 2 d S . . P1 P 0.82526(5) 0.83177(13) 1.40839(12) 0.0074(2) Uani 1 1 d . . . F2 F 0.88278(13) 0.9632(3) 1.3699(3) 0.0146(5) Uani 1 1 d . . . O7 O 0.55979(15) 0.9812(4) 0.7071(4) 0.0124(6) Uani 1 1 d . . . F1 F 0.66725(12) 0.8377(3) 1.0665(3) 0.0117(5) Uani 1 1 d . . . O1 O 0.63492(15) 1.2370(3) 0.9288(3) 0.0096(5) Uani 1 1 d . . . O2 O 0.76334(15) 1.0549(4) 0.9305(3) 0.0103(5) 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 O6 0.0215(15) 0.0071(13) 0.0071(12) -0.0043(10) 0.0035(11) -0.0006(11) O4 0.0114(13) 0.0099(13) 0.0069(12) -0.0011(10) 0.0005(10) 0.0035(11) N1 0.010(2) 0.014(2) 0.018(2) 0.000 0.0010(19) 0.000 Cu1 0.0067(2) 0.0090(3) 0.0095(2) -0.00130(17) 0.00177(18) -0.00009(17) Cu2 0.0081(3) 0.0102(3) 0.0061(3) 0.0002(2) 0.0021(2) 0.0016(2) P2 0.0102(6) 0.0071(6) 0.0091(6) 0.000 0.0035(5) 0.000 P1 0.0069(4) 0.0081(5) 0.0076(4) 0.0001(3) 0.0027(4) -0.0008(3) F2 0.0126(12) 0.0147(12) 0.0176(12) 0.0043(9) 0.0056(10) -0.0026(9) O7 0.0103(14) 0.0152(15) 0.0123(13) 0.0007(11) 0.0037(11) -0.0011(11) F1 0.0106(11) 0.0162(12) 0.0093(10) -0.0021(9) 0.0042(9) 0.0029(9) O1 0.0112(13) 0.0086(13) 0.0085(12) -0.0009(10) 0.0012(10) 0.0004(10) O2 0.0104(13) 0.0112(14) 0.0095(12) 0.0009(10) 0.0027(10) -0.0026(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 P2 1.570(3) . ? O4 P1 1.524(3) 7_667 ? O4 Cu2 1.984(3) . ? O4 Cu1 2.035(3) . ? Cu1 O7 1.939(3) . ? Cu1 O1 1.951(3) . ? Cu1 O2 1.967(3) . ? Cu1 F1 2.183(2) 6_575 ? Cu1 Cu2 2.8992(5) . ? Cu2 F1 1.897(2) . ? Cu2 F1 1.897(2) 7_667 ? Cu2 O4 1.984(3) 7_667 ? Cu2 O2 2.408(3) 7_667 ? Cu2 O2 2.408(3) . ? Cu2 Cu1 2.8992(5) 7_667 ? P2 O7 1.492(3) 2_656 ? P2 O7 1.492(3) . ? P2 O6 1.570(3) 2_656 ? P1 O1 1.500(3) 4_647 ? P1 O2 1.505(3) 6_576 ? P1 O4 1.524(3) 7_667 ? P1 F2 1.565(2) . ? F1 Cu1 2.183(2) 6_576 ? O1 P1 1.500(3) 4_657 ? O2 P1 1.505(3) 6_575 ? 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 O4 Cu2 133.62(17) 7_667 . ? P1 O4 Cu1 133.70(16) 7_667 . ? Cu2 O4 Cu1 92.33(11) . . ? O7 Cu1 O1 90.63(12) . . ? O7 Cu1 O2 173.66(12) . . ? O1 Cu1 O2 91.73(11) . . ? O7 Cu1 O4 93.64(12) . . ? O1 Cu1 O4 164.42(11) . . ? O2 Cu1 O4 82.57(11) . . ? O7 Cu1 F1 89.00(10) . 6_575 ? O1 Cu1 F1 96.49(10) . 6_575 ? O2 Cu1 F1 96.58(10) . 6_575 ? O4 Cu1 F1 98.56(10) . 6_575 ? O7 Cu1 Cu2 118.51(9) . . ? O1 Cu1 Cu2 122.32(8) . . ? O2 Cu1 Cu2 55.41(8) . . ? O4 Cu1 Cu2 43.13(7) . . ? F1 Cu1 Cu2 129.50(6) 6_575 . ? F1 Cu2 F1 180.000(1) . 7_667 ? F1 Cu2 O4 85.46(10) . . ? F1 Cu2 O4 94.54(10) 7_667 . ? F1 Cu2 O4 94.54(10) . 7_667 ? F1 Cu2 O4 85.46(10) 7_667 7_667 ? O4 Cu2 O4 180.000(1) . 7_667 ? F1 Cu2 O2 97.87(10) . 7_667 ? F1 Cu2 O2 82.13(10) 7_667 7_667 ? O4 Cu2 O2 106.79(10) . 7_667 ? O4 Cu2 O2 73.21(10) 7_667 7_667 ? F1 Cu2 O2 82.13(10) . . ? F1 Cu2 O2 97.87(10) 7_667 . ? O4 Cu2 O2 73.21(10) . . ? O4 Cu2 O2 106.79(10) 7_667 . ? O2 Cu2 O2 180.000(1) 7_667 . ? F1 Cu2 Cu1 57.09(7) . . ? F1 Cu2 Cu1 122.91(7) 7_667 . ? O4 Cu2 Cu1 44.54(8) . . ? O4 Cu2 Cu1 135.46(8) 7_667 . ? O2 Cu2 Cu1 137.75(7) 7_667 . ? O2 Cu2 Cu1 42.25(7) . . ? F1 Cu2 Cu1 122.91(7) . 7_667 ? F1 Cu2 Cu1 57.09(7) 7_667 7_667 ? O4 Cu2 Cu1 135.46(8) . 7_667 ? O4 Cu2 Cu1 44.54(8) 7_667 7_667 ? O2 Cu2 Cu1 42.25(7) 7_667 7_667 ? O2 Cu2 Cu1 137.75(7) . 7_667 ? Cu1 Cu2 Cu1 180.0 . 7_667 ? O7 P2 O7 115.7(2) 2_656 . ? O7 P2 O6 109.62(15) 2_656 . ? O7 P2 O6 110.37(15) . . ? O7 P2 O6 110.37(15) 2_656 2_656 ? O7 P2 O6 109.62(15) . 2_656 ? O6 P2 O6 100.0(2) . 2_656 ? O1 P1 O2 115.51(15) 4_647 6_576 ? O1 P1 O4 113.19(16) 4_647 7_667 ? O2 P1 O4 113.35(16) 6_576 7_667 ? O1 P1 F2 103.44(15) 4_647 . ? O2 P1 F2 105.21(15) 6_576 . ? O4 P1 F2 104.60(14) 7_667 . ? P2 O7 Cu1 138.21(18) . . ? Cu2 F1 Cu1 128.64(11) . 6_576 ? P1 O1 Cu1 130.95(17) 4_657 . ? P1 O2 Cu1 136.06(17) 6_575 . ? P1 O2 Cu2 134.81(16) 6_575 . ? Cu1 O2 Cu2 82.34(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.814 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.163