# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Mark Murrie' 'Euan Brechin' 'Kyle W Galloway' 'Jesus Gonzalez' 'Alistair R Lennie' 'Stephen Moggach' 'Pascal Parois' 'Simon Parsons' 'R Peacock' 'Fernando Rodriguez' 'Rafael Valiente' 'John E Warren' _publ_contact_author_name 'Mark Murrie' _publ_contact_author_email MARKM@CHEM.GLA.AC.UK _publ_section_title ; Pressure-induced switching in a copper(II) citrate dimer ; _publ_contact_author_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Edinburgh, Edinburgh, EH9 3JJ. ; _publ_contact_author_phone '+44 131 6504806' _publ_contact_author_fax '+44 1865 000000' # Attachment 'pcu201.cif' data_pcu201 _database_code_depnum_ccdc_archive 'CCDC 762644' #TrackingRef 'pcu201.cif' _audit_creation_date 08-04-02 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'pcu201 in Pbca' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.55 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 13.33 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.58 088_ALERT_3_B Poor Data / Parameter Ratio .................... 7.79 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 599 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 1 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 4 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 27 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 46 All of the above are caused by shading of the pressure cell. 732_ALERT_1_B Angle Calc 104(5), Rep 104.6(10) ...... 5.00 su-Ra H81 -O8 -H82 1.555 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(3), Rep 0.819(9) ...... 3.33 su-Ra O8 -H81 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(4), Rep 0.822(10) ...... 4.00 su-Ra O8 -H82 1.555 1.555 These refer to the water solvent molecule. Differences occur as only variances were used to calculate the esd's on the calculated values, while both variances and covariances were used for the reported values. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C7 This refers to the central C-atom in one of the quanadinium cations. Thermal similarity restraints were applied to all C, N, and O atoms. The Principal axes of the thermal ellipsoids for C7 and the surrounding N atoms are all reasonable. Principal axes of the thermal ellipsoids, A**2 C 7. 0.0238 0.0371 0.0469 N 1. 0.0318 0.0494 0.0863 N 2. 0.0275 0.0419 0.0616 N 3. 0.0273 0.0569 0.0839 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 152 No action taken. All 1,2 and 1,3 distances were restrained for the citrate and guanadinium cations. All metal-ligand distances and angles were freely refined. ; _cell_length_a 11.5200(4) _cell_length_b 14.4315(7) _cell_length_c 18.012(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2994.5(5) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0000 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0010 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0030 0.0020 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.2890 0.6120 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C14 H20 Cu2 N6 O14 # Dc = 1.38 Fooo = 1608.00 Mu = 14.84 M = 311.72 # Found Formula = C16 H36 Cu2 N12 O16 # Dc = 1.73 FOOO = 1608.00 Mu = 15.12 M = 389.81 _chemical_formula_sum 'C16 H36 Cu2 N12 O16' _chemical_formula_moiety 'C12 H8 Cu2 O14, 4(C H6 N3), 2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 779.63 _cell_measurement_reflns_used 5214 _cell_measurement_theta_min 2 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.512 # Sheldrick geometric approximatio 0.74 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.47540 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'Refined from ambient pressure coordinates' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 19261 _reflns_number_total 1677 _diffrn_reflns_av_R_equivalents 0.081 # Number of reflections with Friedels Law is 1677 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3074 _diffrn_reflns_theta_min 2.034 _diffrn_reflns_theta_max 17.307 _diffrn_measured_fraction_theta_max 0.545 _diffrn_reflns_theta_full 13.327 _diffrn_measured_fraction_theta_full 0.581 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 1.79 _oxford_diffrn_Wilson_scale 39.85 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.34 _refine_diff_density_max 0.32 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 1667 _refine_ls_number_restraints 152 _refine_ls_number_parameters 214 _oxford_refine_ls_R_factor_ref 0.0576 _refine_ls_wR_factor_ref 0.1091 _refine_ls_goodness_of_fit_ref 0.9194 _refine_ls_shift/su_max 0.000717 # The values computed from all data _oxford_reflns_number_all 1667 _refine_ls_R_factor_all 0.0576 _refine_ls_wR_factor_all 0.1091 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1277 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_gt 0.0944 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 8.03P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.50597(3) 0.52337(3) 0.57658(6) 0.0299 1.0000 Uani . . . . . . . C1 C 0.7107(2) 0.5354(2) 0.4873(3) 0.0299 1.0000 Uani D U . . . . . C2 C 0.7877(3) 0.5326(3) 0.5569(3) 0.0354 1.0000 Uani D U . . . . . C3 C 0.7344(3) 0.5692(3) 0.6286(3) 0.0384 1.0000 Uani D U . . . . . C4 C 0.7733(3) 0.4984(3) 0.4191(3) 0.0308 1.0000 Uani D U . . . . . C5 C 0.7102(3) 0.5192(3) 0.3474(3) 0.0323 1.0000 Uani D U . . . . . C6 C 0.6762(3) 0.6376(2) 0.4755(4) 0.0303 1.0000 Uani D U . . . . . C7 C 0.5525(3) 0.8490(3) 0.6653(3) 0.0359 1.0000 Uani D U . . . . . C8 C 0.4234(3) 0.1793(3) 0.6811(3) 0.0370 1.0000 Uani D U . . . . . N1 N 0.4990(3) 0.8132(3) 0.6062(4) 0.0558 1.0000 Uani D U . . . . . N2 N 0.6664(3) 0.8388(3) 0.6733(4) 0.0437 1.0000 Uani D U . . . . . N3 N 0.4947(3) 0.8959(3) 0.7162(4) 0.0560 1.0000 Uani D U . . . . . N4 N 0.3101(3) 0.1946(2) 0.6889(4) 0.0383 1.0000 Uani D U . . . . . N5 N 0.4796(3) 0.2106(3) 0.6233(4) 0.0458 1.0000 Uani D U . . . . . N6 N 0.4785(3) 0.1312(3) 0.7317(4) 0.0532 1.0000 Uani D U . . . . . O1 O 0.6295(2) 0.5470(2) 0.6445(3) 0.0412 1.0000 Uani D U . . . . . O2 O 0.7931(2) 0.6179(2) 0.6699(3) 0.0428 1.0000 Uani D U . . . . . O3 O 0.6011(2) 0.4984(2) 0.3426(3) 0.0417 1.0000 Uani D U . . . . . O4 O 0.7608(2) 0.5559(3) 0.2957(3) 0.0432 1.0000 Uani D U . . . . . O5 O 0.5837(2) 0.66457(17) 0.5056(3) 0.0328 1.0000 Uani D U . . . . . O6 O 0.7462(2) 0.68791(18) 0.4402(3) 0.0378 1.0000 Uani D U . . . . . O7 O 0.61036(18) 0.48020(15) 0.4996(3) 0.0360 1.0000 Uani D U . . . . . O8 O 0.6818(3) 0.1967(2) 0.0526(4) 0.0515 1.0000 Uani D . . . . . . H81 H 0.656(4) 0.1457(17) 0.041(3) 0.0500 1.0000 Uiso D . . . . . . H82 H 0.707(5) 0.218(3) 0.0136(16) 0.0500 1.0000 Uiso D . . . . . . H41 H 0.8490 0.5260 0.4169 0.0369 1.0000 Uiso . . . . . . . H42 H 0.7809 0.4324 0.4240 0.0369 1.0000 Uiso . . . . . . . H21 H 0.8558 0.5687 0.5467 0.0425 1.0000 Uiso . . . . . . . H22 H 0.8094 0.4692 0.5652 0.0425 1.0000 Uiso . . . . . . . H11 H 0.4253 0.8198 0.6010 0.0670 1.0000 Uiso . . . . . . . H12 H 0.5383 0.7834 0.5733 0.0670 1.0000 Uiso . . . . . . . H23 H 0.7010 0.8619 0.7114 0.0524 1.0000 Uiso . . . . . . . H24 H 0.7057 0.8091 0.6404 0.0524 1.0000 Uiso . . . . . . . H31 H 0.5306 0.9185 0.7539 0.0671 1.0000 Uiso . . . . . . . H32 H 0.4210 0.9038 0.7116 0.0671 1.0000 Uiso . . . . . . . H51 H 0.5526 0.1997 0.6185 0.0550 1.0000 Uiso . . . . . . . H52 H 0.4436 0.2422 0.5900 0.0550 1.0000 Uiso . . . . . . . H61 H 0.4417 0.1105 0.7698 0.0641 1.0000 Uiso . . . . . . . H62 H 0.5515 0.1203 0.7269 0.0641 1.0000 Uiso . . . . . . . H43 H 0.2740 0.1736 0.7272 0.0462 1.0000 Uiso . . . . . . . H44 H 0.2730 0.2254 0.6556 0.0462 1.0000 Uiso . . . . . . . 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 0.0178(2) 0.0373(3) 0.0347(12) -0.0045(3) -0.0001(3) -0.00384(17) C1 0.0152(14) 0.0225(15) 0.052(7) 0.001(2) 0.001(2) -0.0011(12) C2 0.0183(16) 0.0319(19) 0.056(8) 0.000(3) -0.006(2) -0.0021(13) C3 0.0203(17) 0.037(2) 0.058(9) 0.000(3) -0.001(2) 0.0011(15) C4 0.0192(17) 0.0351(19) 0.038(8) 0.000(3) -0.002(2) -0.0020(13) C5 0.0235(18) 0.042(2) 0.031(9) -0.014(3) 0.004(2) -0.0045(16) C6 0.0258(17) 0.0247(17) 0.040(8) -0.004(3) -0.005(2) 0.0010(13) C7 0.032(2) 0.0304(19) 0.045(10) -0.002(3) -0.003(3) 0.0073(16) C8 0.032(2) 0.0267(18) 0.052(10) -0.005(3) -0.001(3) 0.0027(15) N1 0.039(2) 0.049(2) 0.079(10) -0.014(3) -0.006(3) 0.0111(17) N2 0.0346(18) 0.055(2) 0.042(9) 0.000(3) 0.002(2) 0.0137(15) N3 0.0315(18) 0.062(2) 0.075(10) -0.012(4) -0.004(2) 0.0120(16) N4 0.0308(17) 0.0465(19) 0.038(9) 0.003(3) 0.004(2) 0.0078(14) N5 0.041(2) 0.053(2) 0.043(10) 0.015(3) 0.009(3) 0.0059(16) N6 0.0336(19) 0.059(2) 0.067(10) 0.021(3) 0.005(2) 0.0113(16) O1 0.0230(13) 0.070(2) 0.031(7) -0.004(3) -0.0020(16) -0.0105(12) O2 0.0284(14) 0.0582(18) 0.042(7) -0.013(3) -0.0010(17) -0.0129(12) O3 0.0227(14) 0.069(2) 0.033(8) 0.005(3) 0.0047(16) -0.0087(12) O4 0.0306(15) 0.076(2) 0.023(8) 0.005(3) 0.0035(19) -0.0148(14) O5 0.0304(14) 0.0326(13) 0.035(7) -0.003(2) 0.0051(16) 0.0086(10) O6 0.0389(15) 0.0298(13) 0.045(7) 0.003(2) 0.0058(19) -0.0048(11) O7 0.0133(11) 0.0248(12) 0.070(7) -0.003(2) -0.0001(14) -0.0036(8) O8 0.0456(19) 0.0367(17) 0.072(9) 0.002(2) -0.009(2) -0.0135(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5379(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . O3 2_666 1.934(5) yes Cu1 . O7 2_666 1.918(4) yes Cu1 . O1 . 1.907(4) yes Cu1 . O5 . 2.567(3) yes Cu1 . O7 . 1.939(4) yes C1 . C2 . 1.536(6) yes C1 . C4 . 1.522(6) yes C1 . C6 . 1.542(4) yes C1 . O7 . 1.421(3) yes C2 . C3 . 1.525(6) yes C2 . H21 . 0.960 no C2 . H22 . 0.960 no C3 . O1 . 1.283(4) yes C3 . O2 . 1.227(5) yes C4 . C5 . 1.513(6) yes C4 . H41 . 0.960 no C4 . H42 . 0.960 no C5 . O3 . 1.295(4) yes C5 . O4 . 1.219(6) yes C6 . O5 . 1.258(4) yes C6 . O6 . 1.257(5) yes C7 . N1 . 1.334(7) yes C7 . N2 . 1.329(4) yes C7 . N3 . 1.319(6) yes C8 . N4 . 1.331(4) yes C8 . N5 . 1.307(7) yes C8 . N6 . 1.310(6) yes N1 . H11 . 0.860 no N1 . H12 . 0.860 no N2 . H23 . 0.861 no N2 . H24 . 0.860 no N3 . H31 . 0.859 no N3 . H32 . 0.860 no N4 . H43 . 0.860 no N4 . H44 . 0.860 no N5 . H51 . 0.860 no N5 . H52 . 0.860 no N6 . H61 . 0.860 no N6 . H62 . 0.860 no O8 . H81 . 0.819(9) no O8 . H82 . 0.822(10) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 2_666 Cu1 . O7 2_666 95.05(16) yes O3 2_666 Cu1 . O1 . 91.3(2) yes O7 2_666 Cu1 . O1 . 169.97(15) yes O3 2_666 Cu1 . O5 . 136.58(13) yes O7 2_666 Cu1 . O5 . 84.79(13) yes O1 . Cu1 . O5 . 85.26(16) yes O3 2_666 Cu1 . O7 . 151.91(13) yes O7 2_666 Cu1 . O7 . 85.02(10) yes O1 . Cu1 . O7 . 93.08(16) yes O5 . Cu1 . O7 . 71.48(11) yes C2 . C1 . C4 . 112.0(3) yes C2 . C1 . C6 . 106.7(3) yes C4 . C1 . C6 . 110.3(4) yes C2 . C1 . O7 . 109.2(4) yes C4 . C1 . O7 . 108.3(3) yes C6 . C1 . O7 . 110.4(2) yes C1 . C2 . C3 . 116.7(3) yes C1 . C2 . H21 . 107.6 no C3 . C2 . H21 . 107.6 no C1 . C2 . H22 . 107.6 no C3 . C2 . H22 . 107.6 no H21 . C2 . H22 . 109.5 no C2 . C3 . O1 . 118.8(4) yes C2 . C3 . O2 . 119.3(3) yes O1 . C3 . O2 . 121.9(4) yes C1 . C4 . C5 . 113.0(3) yes C1 . C4 . H41 . 108.6 no C5 . C4 . H41 . 108.6 no C1 . C4 . H42 . 108.6 no C5 . C4 . H42 . 108.6 no H41 . C4 . H42 . 109.5 no C4 . C5 . O3 . 118.5(4) yes C4 . C5 . O4 . 120.6(3) yes O3 . C5 . O4 . 120.9(5) yes C1 . C6 . O5 . 117.0(3) yes C1 . C6 . O6 . 117.2(3) yes O5 . C6 . O6 . 125.6(3) yes N1 . C7 . N2 . 119.9(4) yes N1 . C7 . N3 . 121.3(4) yes N2 . C7 . N3 . 118.7(4) yes N4 . C8 . N5 . 120.8(4) yes N4 . C8 . N6 . 119.3(4) yes N5 . C8 . N6 . 119.8(4) yes C7 . N1 . H11 . 120.0 no C7 . N1 . H12 . 120.0 no H11 . N1 . H12 . 120.0 no C7 . N2 . H23 . 120.0 no C7 . N2 . H24 . 120.1 no H23 . N2 . H24 . 119.9 no C7 . N3 . H31 . 120.0 no C7 . N3 . H32 . 119.9 no H31 . N3 . H32 . 120.1 no C8 . N4 . H43 . 120.0 no C8 . N4 . H44 . 120.0 no H43 . N4 . H44 . 120.0 no C8 . N5 . H51 . 120.0 no C8 . N5 . H52 . 120.0 no H51 . N5 . H52 . 120.0 no C8 . N6 . H61 . 120.0 no C8 . N6 . H62 . 120.0 no H61 . N6 . H62 . 120.0 no C3 . O1 . Cu1 . 127.2(4) yes C5 . O3 . Cu1 2_666 127.4(4) yes Cu1 . O5 . C6 . 105.4(2) yes C1 . O7 . Cu1 . 115.8(3) yes C1 . O7 . Cu1 2_666 118.2(3) yes Cu1 . O7 . Cu1 2_666 94.98(10) yes H81 . O8 . H82 . 104.6(10) no # Attachment 'pcu202.cif' data_pcu202 _database_code_depnum_ccdc_archive 'CCDC 762645' #TrackingRef 'pcu202.cif' _audit_creation_date 08-04-02 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'pcu202 in Pbca' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.56 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 12.98 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.60 088_ALERT_3_B Poor Data / Parameter Ratio .................... 7.50 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 534 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 4 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 22 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 44 All of the above are caused by shading of the pressure cell. 732_ALERT_1_B Angle Calc 105(5), Rep 104.3(10) ...... 5.00 su-Ra H81 -O8 -H82 1.555 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(3), Rep 0.816(9) ...... 3.33 su-Ra O8 -H81 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(3), Rep 0.820(10) ...... 3.00 su-Ra O8 -H82 1.555 1.555 These refer to the water solvent molecule. Differences occur as only variances were used to calculate the esd's on the calculated values, while both variances and covariances were used for the reported values. 152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? This could be caused by rounding errors. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 152 No action taken. All 1,2 and 1,3 distances were restrained for the citrate and guanadinium cations. All metal-ligand distances and angles were freely refined. ; _cell_length_a 11.2728(8) _cell_length_b 13.8681(11) _cell_length_c 18.219(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2848.2(6) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0000 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0010 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0030 0.0020 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.2890 0.6120 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C14 H20 Cu2 N6 O14 # Dc = 1.45 Fooo = 1608.00 Mu = 15.60 M = 311.72 # Found Formula = C16 H36 Cu2 N12 O16 # Dc = 1.82 FOOO = 1608.00 Mu = 15.90 M = 389.81 _chemical_formula_sum 'C16 H36 Cu2 N12 O16' _chemical_formula_moiety 'C12 H8 Cu2 O14, 4(C H6 N3), 2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 779.63 _cell_measurement_reflns_used 4715 _cell_measurement_theta_min 2 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.590 # Sheldrick geometric approximatio 0.73 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.85 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.47540 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'Refined from ambient pressure coordinates' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 18483 _reflns_number_total 1623 _diffrn_reflns_av_R_equivalents 0.067 # Number of reflections with Friedels Law is 1623 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2924 _diffrn_reflns_theta_min 2.102 _diffrn_reflns_theta_max 17.307 _diffrn_measured_fraction_theta_max 0.555 _diffrn_reflns_theta_full 12.980 _diffrn_measured_fraction_theta_full 0.596 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.27 _refine_diff_density_max 0.28 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 1606 _refine_ls_number_restraints 152 _refine_ls_number_parameters 214 _oxford_refine_ls_R_factor_ref 0.0496 _refine_ls_wR_factor_ref 0.0887 _refine_ls_goodness_of_fit_ref 0.8574 _refine_ls_shift/su_max 0.000405 # The values computed from all data _oxford_reflns_number_all 1606 _refine_ls_R_factor_all 0.0496 _refine_ls_wR_factor_all 0.0887 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1204 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_gt 0.0777 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 5.59P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.50754(3) 0.52623(3) 0.57508(4) 0.0268 1.0000 Uani . . . . . . . C1 C 0.7155(2) 0.53182(19) 0.4868(3) 0.0270 1.0000 Uani D U . . . . . C2 C 0.7962(2) 0.5281(2) 0.5547(3) 0.0248 1.0000 Uani D U . . . . . C3 C 0.7433(2) 0.5650(2) 0.6260(3) 0.0261 1.0000 Uani D U . . . . . C4 C 0.7781(2) 0.4922(2) 0.4190(3) 0.0240 1.0000 Uani D U . . . . . C5 C 0.7125(2) 0.5150(2) 0.3492(3) 0.0265 1.0000 Uani D U . . . . . C6 C 0.6809(2) 0.6376(2) 0.4759(3) 0.0234 1.0000 Uani D U . . . . . C7 C 0.5579(3) 0.8484(2) 0.6665(3) 0.0308 1.0000 Uani D U . . . . . C8 C 0.4130(3) 0.1803(2) 0.6864(3) 0.0309 1.0000 Uani D U . . . . . N1 N 0.5036(2) 0.8139(2) 0.6075(3) 0.0446 1.0000 Uani D U . . . . . N2 N 0.6741(2) 0.8373(2) 0.6740(3) 0.0363 1.0000 Uani D U . . . . . N3 N 0.4988(2) 0.8951(2) 0.7183(3) 0.0409 1.0000 Uani D U . . . . . N4 N 0.2970(2) 0.1955(2) 0.6938(3) 0.0358 1.0000 Uani D U . . . . . N5 N 0.4690(2) 0.2113(2) 0.6271(3) 0.0408 1.0000 Uani D U . . . . . N6 N 0.4709(2) 0.1332(2) 0.7377(3) 0.0413 1.0000 Uani D U . . . . . O1 O 0.63609(18) 0.5424(2) 0.6419(3) 0.0369 1.0000 Uani D U . . . . . O2 O 0.80513(19) 0.61274(18) 0.6685(3) 0.0350 1.0000 Uani D U . . . . . O3 O 0.60059(18) 0.49457(19) 0.3454(3) 0.0373 1.0000 Uani D U . . . . . O4 O 0.7630(2) 0.5541(2) 0.2967(3) 0.0447 1.0000 Uani D U . . . . . O5 O 0.58786(18) 0.66579(14) 0.5071(3) 0.0361 1.0000 Uani D U . . . . . O6 O 0.75057(19) 0.68932(16) 0.4394(3) 0.0311 1.0000 Uani D U . . . . . O7 O 0.61236(16) 0.47530(13) 0.4999(2) 0.0294 1.0000 Uani D U . . . . . O8 O 0.6740(2) 0.20299(19) 0.0560(3) 0.0389 1.0000 Uani D . . . . . . H81 H 0.644(3) 0.1510(16) 0.046(3) 0.0500 1.0000 Uiso D . . . . . . H82 H 0.699(4) 0.224(3) 0.0167(13) 0.0500 1.0000 Uiso D . . . . . . H41 H 0.8560 0.5200 0.4162 0.0289 1.0000 Uiso . . . . . . . H42 H 0.7847 0.4235 0.4237 0.0289 1.0000 Uiso . . . . . . . H21 H 0.8655 0.5660 0.5442 0.0298 1.0000 Uiso . . . . . . . H22 H 0.8189 0.4621 0.5621 0.0298 1.0000 Uiso . . . . . . . H11 H 0.4282 0.8210 0.6025 0.0537 1.0000 Uiso . . . . . . . H12 H 0.5438 0.7845 0.5742 0.0537 1.0000 Uiso . . . . . . . H23 H 0.7095 0.8595 0.7122 0.0436 1.0000 Uiso . . . . . . . H24 H 0.7140 0.8078 0.6406 0.0436 1.0000 Uiso . . . . . . . H31 H 0.5357 0.9168 0.7562 0.0491 1.0000 Uiso . . . . . . . H32 H 0.4236 0.9036 0.7141 0.0491 1.0000 Uiso . . . . . . . H51 H 0.5437 0.2007 0.6220 0.0490 1.0000 Uiso . . . . . . . H52 H 0.4306 0.2421 0.5937 0.0490 1.0000 Uiso . . . . . . . H61 H 0.4341 0.1132 0.7761 0.0496 1.0000 Uiso . . . . . . . H62 H 0.5456 0.1224 0.7328 0.0496 1.0000 Uiso . . . . . . . H43 H 0.2606 0.1753 0.7323 0.0431 1.0000 Uiso . . . . . . . H44 H 0.2585 0.2255 0.6600 0.0431 1.0000 Uiso . . . . . . . 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 0.0167(2) 0.0373(3) 0.0265(10) -0.0044(3) -0.0002(2) -0.00287(14) C1 0.0141(13) 0.0242(13) 0.043(6) 0.001(2) -0.0019(17) -0.0005(10) C2 0.0184(14) 0.0294(15) 0.027(7) 0.000(2) -0.0015(17) -0.0016(11) C3 0.0225(15) 0.0329(16) 0.023(7) 0.005(2) -0.0066(18) 0.0016(12) C4 0.0185(14) 0.0303(15) 0.023(7) -0.003(2) 0.0027(17) -0.0004(11) C5 0.0213(15) 0.0345(17) 0.024(8) -0.005(2) 0.001(2) -0.0004(12) C6 0.0235(15) 0.0270(15) 0.020(7) -0.006(2) -0.0075(17) -0.0001(11) C7 0.0297(16) 0.0260(15) 0.037(8) -0.001(2) 0.001(2) 0.0047(13) C8 0.0292(16) 0.0242(15) 0.039(8) -0.001(2) 0.005(2) 0.0005(12) N1 0.0331(16) 0.0454(17) 0.055(8) -0.017(3) -0.001(2) 0.0068(13) N2 0.0323(15) 0.0441(17) 0.032(7) 0.001(2) -0.0027(18) 0.0078(12) N3 0.0300(15) 0.0538(18) 0.039(8) -0.019(3) -0.0032(18) 0.0091(13) N4 0.0287(14) 0.0384(15) 0.040(7) 0.004(2) -0.0009(17) 0.0072(11) N5 0.0331(15) 0.0531(19) 0.036(8) 0.019(3) -0.0013(19) 0.0060(13) N6 0.0288(15) 0.0520(18) 0.043(8) 0.013(3) 0.0026(18) 0.0094(12) O1 0.0200(11) 0.0719(18) 0.019(6) -0.006(2) 0.0010(13) -0.0076(10) O2 0.0307(12) 0.0507(14) 0.023(6) -0.008(2) -0.0002(14) -0.0108(10) O3 0.0208(11) 0.0622(15) 0.029(6) 0.002(2) 0.0042(13) -0.0068(10) O4 0.0301(13) 0.0625(16) 0.041(6) 0.006(2) 0.0033(16) -0.0089(11) O5 0.0240(11) 0.0281(11) 0.056(6) -0.0081(17) 0.0053(14) 0.0051(8) O6 0.0349(12) 0.0300(11) 0.028(6) 0.0016(17) 0.0022(14) -0.0040(9) O7 0.0139(9) 0.0235(10) 0.051(5) -0.0049(16) -0.0008(12) -0.0034(7) O8 0.0384(14) 0.0321(13) 0.046(6) -0.0010(19) -0.0061(17) -0.0088(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5071(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . O7 2_666 1.922(3) yes Cu1 . O3 2_666 1.915(4) yes Cu1 . O1 . 1.905(3) yes Cu1 . O5 . 2.469(3) yes Cu1 . O7 . 1.941(3) yes C1 . C2 . 1.537(5) yes C1 . C4 . 1.525(5) yes C1 . C6 . 1.531(4) yes C1 . O7 . 1.422(3) yes C2 . C3 . 1.519(6) yes C2 . H21 . 0.960 no C2 . H22 . 0.960 no C3 . O1 . 1.282(4) yes C3 . O2 . 1.233(5) yes C4 . C5 . 1.505(6) yes C4 . H41 . 0.960 no C4 . H42 . 0.960 no C5 . O3 . 1.295(3) yes C5 . O4 . 1.238(5) yes C6 . O5 . 1.255(4) yes C6 . O6 . 1.255(4) yes C7 . N1 . 1.327(6) yes C7 . N2 . 1.325(4) yes C7 . N3 . 1.324(5) yes C8 . N4 . 1.331(4) yes C8 . N5 . 1.322(6) yes C8 . N6 . 1.314(5) yes N1 . H11 . 0.860 no N1 . H12 . 0.860 no N2 . H23 . 0.860 no N2 . H24 . 0.860 no N3 . H31 . 0.860 no N3 . H32 . 0.860 no N4 . H43 . 0.860 no N4 . H44 . 0.860 no N5 . H51 . 0.860 no N5 . H52 . 0.860 no N6 . H61 . 0.860 no N6 . H62 . 0.860 no O8 . H81 . 0.816(9) no O8 . H82 . 0.820(10) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O7 2_666 Cu1 . O3 2_666 95.08(14) yes O7 2_666 Cu1 . O1 . 171.91(13) yes O3 2_666 Cu1 . O1 . 91.08(17) yes O7 2_666 Cu1 . O5 . 84.84(11) yes O3 2_666 Cu1 . O5 . 136.93(11) yes O1 . Cu1 . O5 . 87.08(13) yes O7 2_666 Cu1 . O7 . 85.56(8) yes O3 2_666 Cu1 . O7 . 150.00(11) yes O1 . Cu1 . O7 . 91.74(13) yes O5 . Cu1 . O7 . 73.05(10) yes C2 . C1 . C4 . 111.4(3) yes C2 . C1 . C6 . 106.7(3) yes C4 . C1 . C6 . 111.0(3) yes C2 . C1 . O7 . 109.3(3) yes C4 . C1 . O7 . 108.4(3) yes C6 . C1 . O7 . 110.0(2) yes C1 . C2 . C3 . 116.4(3) yes C1 . C2 . H21 . 107.7 no C3 . C2 . H21 . 107.7 no C1 . C2 . H22 . 107.7 no C3 . C2 . H22 . 107.7 no H21 . C2 . H22 . 109.5 no C2 . C3 . O1 . 118.7(3) yes C2 . C3 . O2 . 119.7(3) yes O1 . C3 . O2 . 121.5(4) yes C1 . C4 . C5 . 112.4(3) yes C1 . C4 . H41 . 108.7 no C5 . C4 . H41 . 108.7 no C1 . C4 . H42 . 108.7 no C5 . C4 . H42 . 108.7 no H41 . C4 . H42 . 109.5 no C4 . C5 . O3 . 118.5(4) yes C4 . C5 . O4 . 121.2(3) yes O3 . C5 . O4 . 120.2(4) yes C1 . C6 . O5 . 116.9(3) yes C1 . C6 . O6 . 117.2(3) yes O5 . C6 . O6 . 125.8(3) yes N1 . C7 . N2 . 119.8(4) yes N1 . C7 . N3 . 121.5(3) yes N2 . C7 . N3 . 118.7(4) yes N4 . C8 . N5 . 120.0(4) yes N4 . C8 . N6 . 119.6(4) yes N5 . C8 . N6 . 120.4(3) yes C7 . N1 . H11 . 120.0 no C7 . N1 . H12 . 120.0 no H11 . N1 . H12 . 120.0 no C7 . N2 . H23 . 120.0 no C7 . N2 . H24 . 120.0 no H23 . N2 . H24 . 120.0 no C7 . N3 . H31 . 120.0 no C7 . N3 . H32 . 120.0 no H31 . N3 . H32 . 120.0 no C8 . N4 . H43 . 120.0 no C8 . N4 . H44 . 120.0 no H43 . N4 . H44 . 120.0 no C8 . N5 . H51 . 120.0 no C8 . N5 . H52 . 120.0 no H51 . N5 . H52 . 120.0 no C8 . N6 . H61 . 120.0 no C8 . N6 . H62 . 120.0 no H61 . N6 . H62 . 120.0 no C3 . O1 . Cu1 . 127.1(4) yes C5 . O3 . Cu1 2_666 127.8(4) yes Cu1 . O5 . C6 . 106.83(19) yes C1 . O7 . Cu1 . 114.6(2) yes C1 . O7 . Cu1 2_666 117.4(3) yes Cu1 . O7 . Cu1 2_666 94.44(8) yes H81 . O8 . H82 . 104.3(10) no # Attachment 'pcu203.cif' data_pcu203 _database_code_depnum_ccdc_archive 'CCDC 762646' #TrackingRef 'pcu203.cif' _audit_creation_date 08-04-02 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'pcu203 in Pbca' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; 022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.55 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 12.96 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.59 088_ALERT_3_B Poor Data / Parameter Ratio .................... 7.21 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 502 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 4 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 16 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 40 All of the above are caused by shading of the pressure cell. 732_ALERT_1_B Angle Calc 104(5), Rep 104.2(10) ...... 5.00 su-Ra H81 -O8 -H82 1.555 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(3), Rep 0.817(9) ...... 3.33 su-Ra O8 -H81 1.555 1.555 731_ALERT_1_C Bond Calc 0.82(4), Rep 0.819(10) ...... 4.00 su-Ra O8 -H82 1.555 1.555 These refer to the water solvent molecule. Differences occur as only variances were used to calculate the esd's on the calculated values, while both variances and covariances were used for the reported values. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 152 No action taken. All 1,2 and 1,3 distances were restrained for the citrate and guanadinium cations. All metal-ligand distances and angles were freely refined. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 1 No action taken. ; _cell_length_a 11.1332(5) _cell_length_b 13.4098(7) _cell_length_c 18.367(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2742.1(4) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0000 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0010 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0030 0.0020 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.2890 0.6120 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C14 H20 Cu2 N6 O14 # Dc = 1.51 Fooo = 1608.00 Mu = 16.20 M = 311.72 # Found Formula = C16 H36 Cu2 N12 O16 # Dc = 1.89 FOOO = 1608.00 Mu = 16.52 M = 389.81 _chemical_formula_sum 'C16 H36 Cu2 N12 O16' _chemical_formula_moiety 'C12 H8 Cu2 O14, 4(C H6 N3), 2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 779.63 _cell_measurement_reflns_used 4321 _cell_measurement_theta_min 3 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.652 # Sheldrick geometric approximatio 0.72 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.85 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' synchrotron ' _diffrn_radiation_wavelength 0.47540 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'Refined from ambient pressure coordinates' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 17556 _reflns_number_total 1547 _diffrn_reflns_av_R_equivalents 0.071 # Number of reflections with Friedels Law is 1547 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2800 _diffrn_reflns_theta_min 1.755 _diffrn_reflns_theta_max 17.276 _diffrn_measured_fraction_theta_max 0.552 _diffrn_reflns_theta_full 12.957 _diffrn_measured_fraction_theta_full 0.593 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 1.84 _oxford_diffrn_Wilson_scale 37.88 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.39 _refine_diff_density_max 0.38 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 1543 _refine_ls_number_restraints 152 _refine_ls_number_parameters 214 _oxford_refine_ls_R_factor_ref 0.0557 _refine_ls_wR_factor_ref 0.0921 _refine_ls_goodness_of_fit_ref 0.9629 _refine_ls_shift/su_max 0.000372 # The values computed from all data _oxford_reflns_number_all 1543 _refine_ls_R_factor_all 0.0557 _refine_ls_wR_factor_all 0.0921 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1142 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_gt 0.0772 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 4.94P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.50879(3) 0.52893(3) 0.57394(5) 0.0268 1.0000 Uani . . . . . . . C1 C 0.7182(2) 0.5290(2) 0.4856(3) 0.0239 1.0000 Uani D U . . . . . C2 C 0.8018(3) 0.5259(3) 0.5526(3) 0.0230 1.0000 Uani D U . . . . . C3 C 0.7497(3) 0.5608(3) 0.6245(3) 0.0256 1.0000 Uani D U . . . . . C4 C 0.7800(3) 0.4882(2) 0.4184(3) 0.0262 1.0000 Uani D U . . . . . C5 C 0.7125(3) 0.5137(3) 0.3492(3) 0.0290 1.0000 Uani D U . . . . . C6 C 0.6836(3) 0.6391(2) 0.4752(3) 0.0250 1.0000 Uani D U . . . . . C7 C 0.5596(3) 0.8480(3) 0.6672(3) 0.0334 1.0000 Uani D U . . . . . C8 C 0.4065(3) 0.1809(3) 0.6903(3) 0.0254 1.0000 Uani D U . . . . . N1 N 0.5042(3) 0.8139(3) 0.6086(4) 0.0420 1.0000 Uani D U . . . . . N2 N 0.6777(2) 0.8368(3) 0.6735(3) 0.0372 1.0000 Uani D U . . . . . N3 N 0.4996(3) 0.8934(3) 0.7194(3) 0.0391 1.0000 Uani D U . . . . . N4 N 0.2887(2) 0.1954(2) 0.6984(3) 0.0375 1.0000 Uani D U . . . . . N5 N 0.4625(3) 0.2141(3) 0.6312(3) 0.0375 1.0000 Uani D U . . . . . N6 N 0.4656(2) 0.1333(2) 0.7412(3) 0.0384 1.0000 Uani D U . . . . . O1 O 0.64006(19) 0.5401(2) 0.6395(3) 0.0412 1.0000 Uani D U . . . . . O2 O 0.8138(2) 0.6064(2) 0.6676(3) 0.0355 1.0000 Uani D U . . . . . O3 O 0.59949(19) 0.4932(2) 0.3468(3) 0.0380 1.0000 Uani D U . . . . . O4 O 0.7633(2) 0.5543(2) 0.2975(3) 0.0396 1.0000 Uani D U . . . . . O5 O 0.58981(19) 0.66794(17) 0.5072(3) 0.0334 1.0000 Uani D U . . . . . O6 O 0.7524(2) 0.69287(18) 0.4388(3) 0.0282 1.0000 Uani D U . . . . . O7 O 0.61369(17) 0.47177(16) 0.4994(2) 0.0250 1.0000 Uani D U . . . . . O8 O 0.6688(2) 0.2081(2) 0.0590(3) 0.0386 1.0000 Uani D . . . . . . H81 H 0.648(4) 0.1536(18) 0.044(3) 0.0500 1.0000 Uiso D . . . . . . H82 H 0.696(4) 0.236(3) 0.0229(17) 0.0500 1.0000 Uiso D . . . . . . H41 H 0.8593 0.5160 0.4155 0.0317 1.0000 Uiso . . . . . . . H42 H 0.7854 0.4170 0.4226 0.0317 1.0000 Uiso . . . . . . . H21 H 0.8702 0.5671 0.5420 0.0276 1.0000 Uiso . . . . . . . H22 H 0.8276 0.4581 0.5589 0.0276 1.0000 Uiso . . . . . . . H11 H 0.4278 0.8208 0.6041 0.0503 1.0000 Uiso . . . . . . . H12 H 0.5447 0.7847 0.5748 0.0503 1.0000 Uiso . . . . . . . H23 H 0.7143 0.8588 0.7114 0.0447 1.0000 Uiso . . . . . . . H24 H 0.7176 0.8076 0.6395 0.0447 1.0000 Uiso . . . . . . . H31 H 0.5369 0.9151 0.7572 0.0468 1.0000 Uiso . . . . . . . H32 H 0.4232 0.9012 0.7157 0.0468 1.0000 Uiso . . . . . . . H51 H 0.5384 0.2044 0.6261 0.0452 1.0000 Uiso . . . . . . . H52 H 0.4229 0.2453 0.5981 0.0452 1.0000 Uiso . . . . . . . H61 H 0.4285 0.1121 0.7793 0.0458 1.0000 Uiso . . . . . . . H62 H 0.5415 0.1232 0.7366 0.0458 1.0000 Uiso . . . . . . . H43 H 0.2526 0.1738 0.7367 0.0450 1.0000 Uiso . . . . . . . H44 H 0.2487 0.2264 0.6653 0.0450 1.0000 Uiso . . . . . . . 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 0.0160(2) 0.0412(3) 0.0232(11) -0.0044(4) -0.0003(2) -0.00212(16) C1 0.0157(14) 0.0238(15) 0.032(7) 0.007(3) -0.0007(19) -0.0012(12) C2 0.0175(15) 0.0307(17) 0.021(8) -0.003(3) -0.0002(19) -0.0009(12) C3 0.0219(16) 0.0339(18) 0.021(8) 0.004(3) -0.002(2) 0.0000(13) C4 0.0178(15) 0.0260(17) 0.035(8) 0.001(3) 0.000(2) 0.0002(12) C5 0.0208(16) 0.0303(18) 0.036(8) -0.007(3) 0.003(2) -0.0006(13) C6 0.0221(16) 0.0271(17) 0.026(8) -0.004(3) -0.0046(19) 0.0027(13) C7 0.0260(18) 0.0253(17) 0.049(9) 0.004(3) -0.002(2) 0.0008(14) C8 0.0294(18) 0.0239(17) 0.023(9) -0.001(3) -0.002(2) 0.0022(13) N1 0.0296(17) 0.0431(19) 0.053(9) -0.014(3) -0.002(2) 0.0061(14) N2 0.0261(15) 0.0447(18) 0.041(8) 0.002(3) -0.0029(19) 0.0076(13) N3 0.0291(16) 0.0462(19) 0.042(9) -0.011(3) -0.003(2) 0.0102(14) N4 0.0251(15) 0.0376(17) 0.050(8) 0.004(3) 0.0003(19) 0.0066(12) N5 0.0323(17) 0.050(2) 0.030(9) 0.017(3) 0.001(2) 0.0023(14) N6 0.0267(16) 0.0461(18) 0.042(8) 0.011(3) 0.005(2) 0.0076(13) O1 0.0180(12) 0.080(2) 0.025(7) -0.011(3) 0.0014(15) -0.0083(11) O2 0.0289(13) 0.0500(16) 0.028(7) -0.008(2) -0.0016(16) -0.0114(11) O3 0.0191(12) 0.0614(17) 0.033(7) -0.001(2) 0.0015(14) -0.0053(11) O4 0.0269(14) 0.0542(17) 0.038(7) 0.007(2) 0.0013(17) -0.0066(11) O5 0.0250(12) 0.0284(12) 0.047(6) -0.0078(19) 0.0035(15) 0.0041(9) O6 0.0333(13) 0.0306(12) 0.021(6) 0.0017(19) 0.0030(15) -0.0012(10) O7 0.0145(10) 0.0268(11) 0.034(6) -0.0024(18) -0.0008(12) -0.0018(8) O8 0.0338(14) 0.0315(15) 0.050(7) -0.001(2) -0.0046(17) -0.0057(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5290(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . O7 2_666 1.917(4) yes Cu1 . O3 2_666 1.913(4) yes Cu1 . O1 . 1.900(4) yes Cu1 . O5 . 2.407(3) yes Cu1 . O7 . 1.956(4) yes C1 . C2 . 1.543(6) yes C1 . C4 . 1.515(6) yes C1 . C6 . 1.538(4) yes C1 . O7 . 1.417(3) yes C2 . C3 . 1.518(6) yes C2 . H21 . 0.960 no C2 . H22 . 0.960 no C3 . O1 . 1.281(4) yes C3 . O2 . 1.229(5) yes C4 . C5 . 1.515(6) yes C4 . H41 . 0.960 no C4 . H42 . 0.960 no C5 . O3 . 1.288(4) yes C5 . O4 . 1.233(6) yes C6 . O5 . 1.258(4) yes C6 . O6 . 1.246(5) yes C7 . N1 . 1.323(6) yes C7 . N2 . 1.329(4) yes C7 . N3 . 1.317(6) yes C8 . N4 . 1.335(4) yes C8 . N5 . 1.329(6) yes C8 . N6 . 1.309(6) yes N1 . H11 . 0.860 no N1 . H12 . 0.860 no N2 . H23 . 0.860 no N2 . H24 . 0.860 no N3 . H31 . 0.860 no N3 . H32 . 0.860 no N4 . H43 . 0.860 no N4 . H44 . 0.860 no N5 . H51 . 0.860 no N5 . H52 . 0.861 no N6 . H61 . 0.860 no N6 . H62 . 0.860 no O8 . H81 . 0.817(9) no O8 . H82 . 0.819(10) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O7 2_666 Cu1 . O3 2_666 94.91(15) yes O7 2_666 Cu1 . O1 . 173.33(16) yes O3 2_666 Cu1 . O1 . 90.85(18) yes O7 2_666 Cu1 . O5 . 84.96(13) yes O3 2_666 Cu1 . O5 . 138.08(12) yes O1 . Cu1 . O5 . 88.50(15) yes O7 2_666 Cu1 . O7 . 86.04(9) yes O3 2_666 Cu1 . O7 . 148.00(12) yes O1 . Cu1 . O7 . 90.88(15) yes O5 . Cu1 . O7 . 73.91(11) yes C2 . C1 . C4 . 111.5(3) yes C2 . C1 . C6 . 106.0(3) yes C4 . C1 . C6 . 111.0(3) yes C2 . C1 . O7 . 109.8(3) yes C4 . C1 . O7 . 108.8(3) yes C6 . C1 . O7 . 109.6(2) yes C1 . C2 . C3 . 117.1(3) yes C1 . C2 . H21 . 107.6 no C3 . C2 . H21 . 107.6 no C1 . C2 . H22 . 107.5 no C3 . C2 . H22 . 107.5 no H21 . C2 . H22 . 109.4 no C2 . C3 . O1 . 119.0(4) yes C2 . C3 . O2 . 119.5(3) yes O1 . C3 . O2 . 121.6(4) yes C1 . C4 . C5 . 112.1(3) yes C1 . C4 . H41 . 108.8 no C5 . C4 . H41 . 108.8 no C1 . C4 . H42 . 108.8 no C5 . C4 . H42 . 108.8 no H41 . C4 . H42 . 109.4 no C4 . C5 . O3 . 117.7(4) yes C4 . C5 . O4 . 121.2(3) yes O3 . C5 . O4 . 121.1(4) yes C1 . C6 . O5 . 116.4(3) yes C1 . C6 . O6 . 117.9(3) yes O5 . C6 . O6 . 125.6(3) yes N1 . C7 . N2 . 119.5(4) yes N1 . C7 . N3 . 121.1(3) yes N2 . C7 . N3 . 119.4(4) yes N4 . C8 . N5 . 120.2(4) yes N4 . C8 . N6 . 119.1(4) yes N5 . C8 . N6 . 120.7(3) yes C7 . N1 . H11 . 120.0 no C7 . N1 . H12 . 120.0 no H11 . N1 . H12 . 120.0 no C7 . N2 . H23 . 120.0 no C7 . N2 . H24 . 120.0 no H23 . N2 . H24 . 120.0 no C7 . N3 . H31 . 120.0 no C7 . N3 . H32 . 120.0 no H31 . N3 . H32 . 120.0 no C8 . N4 . H43 . 120.0 no C8 . N4 . H44 . 120.0 no H43 . N4 . H44 . 120.0 no C8 . N5 . H51 . 120.1 no C8 . N5 . H52 . 120.0 no H51 . N5 . H52 . 119.9 no C8 . N6 . H61 . 120.0 no C8 . N6 . H62 . 120.0 no H61 . N6 . H62 . 120.0 no C3 . O1 . Cu1 . 127.9(4) yes C5 . O3 . Cu1 2_666 128.5(4) yes Cu1 . O5 . C6 . 108.1(2) yes C1 . O7 . Cu1 . 113.8(2) yes C1 . O7 . Cu1 2_666 117.5(3) yes Cu1 . O7 . Cu1 2_666 93.96(9) yes H81 . O8 . H82 . 104.2(10) no # Attachment 'sp8021.cif' data_sp8021 _database_code_depnum_ccdc_archive 'CCDC 762647' #TrackingRef 'sp8021.cif' _audit_creation_date 08-04-01 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'sp8021 in Pbca' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.90 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. 912_ALERT_3_C # Missing FCF Reflections Above STh/L= 0.600 15 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 1616 1616 0 23.01 0.550 1.000 2161 2161 0 25.24 0.600 1.000 2790 2790 0 #----------------------------------------------------------- ACTA Min. Res. --- 26.36 0.625 0.995 3168 3153 15 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is true. ; #end of refcif _cell_length_a 11.716(7) _cell_length_b 14.713(9) _cell_length_c 17.934(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3092(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C8 H19 Cu2 N9 O8 # Dc = 1.07 Fooo = 1608.00 Mu = 14.10 M = 248.19 # Found Formula = C16 H36 Cu2 N12 O16 # Dc = 1.67 FOOO = 1608.00 Mu = 14.65 M = 389.81 _chemical_formula_sum 'C16 H36 Cu2 N12 O16' _chemical_formula_moiety 'C12 H8 Cu2 O14, 4(C H6 N3), 2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 779.63 _cell_measurement_reflns_used 8071 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.36 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_max 0.51 _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.465 # Sheldrick geometric approximatio 0.50 0.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 0.59 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 24482 _reflns_number_total 3153 _diffrn_reflns_av_R_equivalents 0.049 # Number of reflections with Friedels Law is 3153 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3159 _diffrn_reflns_theta_min 2.271 _diffrn_reflns_theta_max 26.365 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.365 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.55 _refine_diff_density_max 0.76 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 3153 _refine_ls_number_restraints 0 _refine_ls_number_parameters 208 _oxford_refine_ls_R_factor_ref 0.0525 _refine_ls_wR_factor_ref 0.0720 _refine_ls_goodness_of_fit_ref 1.0554 _refine_ls_shift/su_max 0.000831 # The values computed from all data _oxford_reflns_number_all 3153 _refine_ls_R_factor_all 0.0525 _refine_ls_wR_factor_all 0.0720 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1876 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_gt 0.0632 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.05 1.07 0.138 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cu1 Cu 0.50516(3) 0.52152(3) 0.577339(18) 0.0317 1.0000 Uani . . . . . . . C1 C 0.7061(2) 0.53840(19) 0.48784(14) 0.0265 1.0000 Uani . . . . . . . C2 C 0.7825(2) 0.5351(2) 0.55836(15) 0.0319 1.0000 Uani . . . . . . . C3 C 0.7279(2) 0.5719(2) 0.63003(15) 0.0341 1.0000 Uani . . . . . . . C4 C 0.7705(2) 0.5025(2) 0.41921(16) 0.0341 1.0000 Uani . . . . . . . C5 C 0.7068(3) 0.5229(2) 0.34690(16) 0.0384 1.0000 Uani . . . . . . . C6 C 0.6730(3) 0.6390(2) 0.47641(15) 0.0325 1.0000 Uani . . . . . . . C7 C 0.5479(3) 0.8491(2) 0.66375(18) 0.0408 1.0000 Uani . . . . . . . C8 C 0.4305(3) 0.1789(2) 0.67950(17) 0.0383 1.0000 Uani . . . . . . . N1 N 0.4934(3) 0.8121(2) 0.60632(17) 0.0544 1.0000 Uani . . . . . . . N2 N 0.6590(3) 0.8397(2) 0.67159(16) 0.0489 1.0000 Uani . . . . . . . N3 N 0.4904(3) 0.8958(2) 0.71420(16) 0.0530 1.0000 Uani . . . . . . . N4 N 0.3196(2) 0.1936(2) 0.68613(15) 0.0457 1.0000 Uani . . . . . . . N5 N 0.4874(3) 0.2115(2) 0.62157(16) 0.0548 1.0000 Uani . . . . . . . N6 N 0.4855(3) 0.1310(2) 0.73001(15) 0.0541 1.0000 Uani . . . . . . . O1 O 0.62566(18) 0.54873(17) 0.64599(11) 0.0441 1.0000 Uani . . . . . . . O2 O 0.78519(19) 0.62033(17) 0.67164(12) 0.0476 1.0000 Uani . . . . . . . O3 O 0.60044(18) 0.50133(17) 0.34218(11) 0.0445 1.0000 Uani . . . . . . . O4 O 0.7581(2) 0.5592(2) 0.29483(11) 0.0529 1.0000 Uani . . . . . . . O5 O 0.5802(2) 0.66454(15) 0.50456(14) 0.0468 1.0000 Uani . . . . . . . O6 O 0.7427(2) 0.68828(15) 0.44155(12) 0.0426 1.0000 Uani . . . . . . . O7 O 0.60912(15) 0.48356(13) 0.49959(10) 0.0282 1.0000 Uani . . . . . . . O8 O 0.6875(2) 0.19291(16) 0.05016(13) 0.0530 1.0000 Uani . . . . . . . H81 H 0.6563 0.1469 0.0325 0.0500 1.0000 Uiso . . . . . . . H82 H 0.7234 0.2154 0.0138 0.0500 1.0000 Uiso . . . . . . . H41 H 0.8442 0.5309 0.4172 0.0410 1.0000 Uiso . . . . . . . H42 H 0.7796 0.4380 0.4239 0.0410 1.0000 Uiso . . . . . . . H21 H 0.8499 0.5701 0.5485 0.0382 1.0000 Uiso . . . . . . . H22 H 0.8034 0.4728 0.5670 0.0382 1.0000 Uiso . . . . . . . H11 H 0.4208 0.8188 0.6019 0.0652 1.0000 Uiso . . . . . . . H12 H 0.5307 0.7814 0.5736 0.0652 1.0000 Uiso . . . . . . . H23 H 0.6932 0.8640 0.7090 0.0587 1.0000 Uiso . . . . . . . H24 H 0.6974 0.8092 0.6393 0.0587 1.0000 Uiso . . . . . . . H31 H 0.5256 0.9198 0.7514 0.0636 1.0000 Uiso . . . . . . . H32 H 0.4177 0.9022 0.7099 0.0636 1.0000 Uiso . . . . . . . H51 H 0.5594 0.2013 0.6173 0.0657 1.0000 Uiso . . . . . . . H52 H 0.4525 0.2429 0.5882 0.0657 1.0000 Uiso . . . . . . . H61 H 0.4494 0.1095 0.7679 0.0649 1.0000 Uiso . . . . . . . H62 H 0.5575 0.1213 0.7252 0.0649 1.0000 Uiso . . . . . . . H43 H 0.2831 0.1722 0.7239 0.0548 1.0000 Uiso . . . . . . . H44 H 0.2840 0.2244 0.6527 0.0548 1.0000 Uiso . . . . . . . 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 0.02984(18) 0.0442(2) 0.02117(16) -0.00515(15) -0.00035(14) -0.00447(16) C1 0.0260(13) 0.0311(14) 0.0224(12) -0.0011(11) -0.0003(11) -0.0017(11) C2 0.0290(14) 0.0385(16) 0.0281(14) 0.0002(12) -0.0041(12) -0.0013(12) C3 0.0334(16) 0.0441(17) 0.0247(13) 0.0030(13) -0.0054(12) -0.0011(14) C4 0.0293(14) 0.0405(16) 0.0325(14) -0.0042(13) 0.0020(12) -0.0009(13) C5 0.0346(15) 0.0518(19) 0.0287(14) -0.0107(14) 0.0038(13) -0.0019(15) C6 0.0370(15) 0.0344(15) 0.0262(14) -0.0035(12) -0.0061(12) 0.0001(13) C7 0.0442(18) 0.0426(18) 0.0355(16) 0.0075(14) 0.0023(14) 0.0067(15) C8 0.0453(18) 0.0389(17) 0.0306(15) -0.0008(13) 0.0007(14) 0.0032(14) N1 0.0533(18) 0.0585(19) 0.0513(17) -0.0130(15) -0.0053(15) 0.0110(16) N2 0.0453(16) 0.0622(19) 0.0391(15) 0.0010(14) 0.0011(13) 0.0138(14) N3 0.0459(17) 0.068(2) 0.0447(16) -0.0110(15) -0.0029(14) 0.0123(16) N4 0.0459(16) 0.0549(18) 0.0362(14) 0.0040(13) 0.0007(12) 0.0073(14) N5 0.0565(19) 0.0648(19) 0.0430(16) 0.0194(15) 0.0085(15) 0.0078(16) N6 0.0451(17) 0.074(2) 0.0434(16) 0.0210(15) 0.0075(14) 0.0158(16) O1 0.0359(12) 0.0737(16) 0.0227(10) -0.0067(10) -0.0014(9) -0.0101(11) O2 0.0426(13) 0.0671(16) 0.0329(11) -0.0133(11) -0.0020(10) -0.0144(12) O3 0.0349(11) 0.0739(17) 0.0247(10) -0.0037(11) 0.0011(9) -0.0104(11) O4 0.0407(12) 0.0889(19) 0.0292(10) 0.0052(12) 0.0038(11) -0.0147(13) O5 0.0450(13) 0.0381(13) 0.0574(14) -0.0042(11) 0.0038(12) 0.0075(10) O6 0.0535(13) 0.0364(12) 0.0379(11) 0.0050(10) 0.0020(11) -0.0062(11) O7 0.0295(9) 0.0306(10) 0.0244(9) -0.0029(8) -0.0011(8) -0.0023(8) O8 0.0648(16) 0.0464(14) 0.0477(14) 0.0038(11) -0.0088(12) -0.0153(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.082755(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . O3 2_666 1.931(2) yes Cu1 . O7 2_666 1.924(2) yes Cu1 . O1 . 1.916(2) yes Cu1 . O5 . 2.628(3) yes Cu1 . O7 . 1.934(2) yes C1 . C2 . 1.551(4) yes C1 . C4 . 1.537(4) yes C1 . C6 . 1.544(4) yes C1 . O7 . 1.409(3) yes C2 . C3 . 1.534(4) yes C2 . H21 . 0.960 no C2 . H22 . 0.960 no C3 . O1 . 1.278(4) yes C3 . O2 . 1.231(3) yes C4 . C5 . 1.526(4) yes C4 . H41 . 0.960 no C4 . H42 . 0.960 no C5 . O3 . 1.288(4) yes C5 . O4 . 1.233(4) yes C6 . O5 . 1.256(4) yes C6 . O6 . 1.258(4) yes C7 . N1 . 1.328(4) yes C7 . N2 . 1.316(4) yes C7 . N3 . 1.321(4) yes C8 . N4 . 1.322(4) yes C8 . N5 . 1.324(4) yes C8 . N6 . 1.316(4) yes N1 . H11 . 0.860 no N1 . H12 . 0.860 no N2 . H23 . 0.860 no N2 . H24 . 0.860 no N3 . H31 . 0.860 no N3 . H32 . 0.860 no N4 . H43 . 0.860 no N4 . H44 . 0.860 no N5 . H51 . 0.860 no N5 . H52 . 0.860 no N6 . H61 . 0.860 no N6 . H62 . 0.860 no O8 . H81 . 0.832 no O8 . H82 . 0.843 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 2_666 Cu1 . O7 2_666 94.78(10) yes O3 2_666 Cu1 . O1 . 91.62(10) yes O7 2_666 Cu1 . O1 . 169.08(10) yes O3 2_666 Cu1 . O5 . 136.49(9) yes O7 2_666 Cu1 . O5 . 84.71(9) yes O1 . Cu1 . O5 . 84.56(10) yes O3 2_666 Cu1 . O7 . 153.18(10) yes O7 2_666 Cu1 . O7 . 84.84(10) yes O1 . Cu1 . O7 . 93.42(10) yes O5 . Cu1 . O7 . 70.27(9) yes C2 . C1 . C4 . 111.0(2) yes C2 . C1 . C6 . 106.5(2) yes C4 . C1 . C6 . 110.2(2) yes C2 . C1 . O7 . 109.0(2) yes C4 . C1 . O7 . 108.6(2) yes C6 . C1 . O7 . 111.5(2) yes C1 . C2 . C3 . 115.5(2) yes C1 . C2 . H21 . 107.9 no C3 . C2 . H21 . 107.9 no C1 . C2 . H22 . 107.9 no C3 . C2 . H22 . 107.9 no H21 . C2 . H22 . 109.5 no C2 . C3 . O1 . 119.0(3) yes C2 . C3 . O2 . 119.0(3) yes O1 . C3 . O2 . 122.0(3) yes C1 . C4 . C5 . 111.9(2) yes C1 . C4 . H41 . 108.9 no C5 . C4 . H41 . 108.9 no C1 . C4 . H42 . 108.9 no C5 . C4 . H42 . 108.9 no H41 . C4 . H42 . 109.5 no C4 . C5 . O3 . 118.8(3) yes C4 . C5 . O4 . 119.3(3) yes O3 . C5 . O4 . 121.9(3) yes C1 . C6 . O5 . 116.8(3) yes C1 . C6 . O6 . 117.1(3) yes O5 . C6 . O6 . 126.1(3) yes N1 . C7 . N2 . 121.0(3) yes N1 . C7 . N3 . 119.9(3) yes N2 . C7 . N3 . 119.1(3) yes N4 . C8 . N5 . 120.4(3) yes N4 . C8 . N6 . 120.4(3) yes N5 . C8 . N6 . 119.1(3) yes C7 . N1 . H11 . 120.0 no C7 . N1 . H12 . 120.0 no H11 . N1 . H12 . 120.0 no C7 . N2 . H23 . 120.0 no C7 . N2 . H24 . 120.0 no H23 . N2 . H24 . 120.0 no C7 . N3 . H31 . 120.0 no C7 . N3 . H32 . 120.0 no H31 . N3 . H32 . 120.0 no C8 . N4 . H43 . 120.0 no C8 . N4 . H44 . 120.0 no H43 . N4 . H44 . 120.0 no C8 . N5 . H51 . 120.0 no C8 . N5 . H52 . 120.0 no H51 . N5 . H52 . 120.0 no C8 . N6 . H61 . 120.0 no C8 . N6 . H62 . 120.0 no H61 . N6 . H62 . 120.0 no C3 . O1 . Cu1 . 127.06(18) yes C5 . O3 . Cu1 2_666 127.8(2) yes Cu1 . O5 . C6 . 104.5(2) yes C1 . O7 . Cu1 . 116.75(16) yes C1 . O7 . Cu1 2_666 118.42(16) yes Cu1 . O7 . Cu1 2_666 95.16(9) yes H81 . O8 . H82 . 104.1 no