# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Dr Stephen Moggach RSE Personal Research Fellow The University of Edinburgh Joseph Black Building West Mains Road Edinburgh EH9 3JJ ; _publ_contact_author_email smoggach@staffmail.ed.ac.uk _publ_contact_author_phone '+44(0)131 6504806' #looking for refcif _publ_contact_author_name 'Stephen A. Moggach' loop_ _publ_author_name S.Moggach D.Allan J.Tan A.Graham data_ambient _database_code_depnum_ccdc_archive 'CCDC 846570' #TrackingRef '- ambient.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'ST0085_0m in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.3015(4) _cell_length_b 26.3015(4) _cell_length_c 26.3015(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18194.6(5) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 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' 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 48 # Given Formula = C10.67 H9.33 Cu2 O7.33 # Dc = 1.67 Fooo = 5136.00 Mu = 28.30 M = 95.49 # Found Formula = C6 H2 Cu1 O5 # Dc = 0.95 FOOO = 5136.00 Mu = 14.28 M = 54.41 _chemical_formula_sum 'C6 H2 Cu1 O5' _chemical_formula_moiety 'C6 H2 Cu1 O5' _chemical_compound_source ? _chemical_formula_weight 217.62 _cell_measurement_reflns_used 9841 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.953 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.428 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device 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 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 52632 _reflns_number_total 1196 _diffrn_reflns_av_R_equivalents 0.065 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1196 # Theoretical number of reflections is about 1931 _diffrn_reflns_theta_min 1.548 _diffrn_reflns_theta_max 28.547 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.834 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 2 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 2.26 _oxford_diffrn_Wilson_scale 10007.45 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.77 _refine_diff_density_max 0.69 # 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 1196 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0425 _refine_ls_wR_factor_ref 0.0927 _refine_ls_goodness_of_fit_ref 1.0110 _refine_ls_shift/su_max 0.0018345 _refine_ls_shift/su_mean 0.0001252 # The values computed from all data _oxford_reflns_number_all 1196 _refine_ls_R_factor_all 0.0425 _refine_ls_wR_factor_all 0.0927 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 952 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_gt 0.0835 # 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 constr # 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^) + ( 0.05P)^2^ +29.82P] ,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 Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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 atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.714740(11) 0.214740(11) 0.5000 0.0351 1.0000 Uani S T . . . . O2 O 0.65623(9) 0.15623(9) 0.5000 0.0985 1.0000 Uani S T . . . . O1 O 0.68313(5) 0.25687(5) 0.55241(5) 0.0544 1.0000 Uani . . . . . . C3 C 0.69942(10) 0.36543(7) 0.63457(7) 0.0447 1.0000 Uani S T . . . . C2 C 0.67787(7) 0.32213(7) 0.61313(10) 0.0423 1.0000 Uani S T . . . . C1 C 0.70349(8) 0.29651(8) 0.56901(10) 0.0444 1.0000 Uani S T . . . . H31 H 0.7288 0.3803 0.6197 0.0544 1.0000 Uiso RS . . . . . 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 0.0372(2) 0.0372(2) 0.0309(2) 0.0000 0.0000 -0.01013(18) O2 0.0866(18) 0.0866(18) 0.122(3) 0.0000 0.0000 -0.050(2) O1 0.0560(9) 0.0545(9) 0.0527(8) -0.0134(7) 0.0148(7) -0.0132(7) C3 0.0422(14) 0.0459(9) 0.0459(9) -0.0012(12) 0.0060(8) -0.0060(8) C2 0.0428(9) 0.0428(9) 0.0413(13) -0.0044(8) 0.0044(8) -0.0052(11) C1 0.0488(10) 0.0488(10) 0.0356(13) -0.0026(8) 0.0026(8) -0.0043(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0177114(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 . O1 127_546 1.9543(14) yes Cu1 . O1 103_545 1.9543(14) yes Cu1 . O1 25_556 1.9543(14) yes Cu1 . Cu1 122_665 2.6231(8) yes Cu1 . O2 . 2.176(3) yes Cu1 . O1 . 1.9543(14) yes O1 . C1 . 1.2507(18) yes C3 . C2 34_665 1.3916(18) yes C3 . C2 . 1.3916(18) yes C3 . H31 . 0.950 no C2 . C1 . 1.501(4) yes 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 O1 127_546 Cu1 . O1 103_545 89.71(9) yes O1 127_546 Cu1 . O1 25_556 89.14(9) yes O1 103_545 Cu1 . O1 25_556 168.51(8) yes O1 127_546 Cu1 . Cu1 122_665 84.25(4) yes O1 103_545 Cu1 . Cu1 122_665 84.25(4) yes O1 25_556 Cu1 . Cu1 122_665 84.25(4) yes O1 127_546 Cu1 . O2 . 95.75(4) yes O1 103_545 Cu1 . O2 . 95.75(4) yes O1 25_556 Cu1 . O2 . 95.75(4) yes Cu1 122_665 Cu1 . O2 . 179.995 yes O1 127_546 Cu1 . O1 . 168.51(8) yes O1 103_545 Cu1 . O1 . 89.14(9) yes O1 25_556 Cu1 . O1 . 89.71(9) yes Cu1 122_665 Cu1 . O1 . 84.25(4) yes O2 . Cu1 . O1 . 95.75(4) yes Cu1 . O1 . C1 . 122.46(15) yes C2 34_665 C3 . C2 . 119.8(3) yes C2 34_665 C3 . H31 . 120.1 no C2 . C3 . H31 . 120.1 no C3 57_566 C2 . C3 . 120.2(3) yes C3 57_566 C2 . C1 . 119.84(13) yes C3 . C2 . C1 . 119.84(13) yes C2 . C1 . O1 122_665 116.85(13) yes C2 . C1 . O1 . 116.85(13) yes O1 122_665 C1 . O1 . 126.3(3) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 11:36:36 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 11:36:36 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment '- cubt13.cif' data_cubt13 _database_code_depnum_ccdc_archive 'CCDC 846571' #TrackingRef '- cubt13.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt13 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.3867(12) _cell_length_b 26.3867(12) _cell_length_c 26.3867(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18371.9(14) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 24 # Given Formula = C18 H15 Cu3 O21 # Dc = 1.64 Fooo = 5136.00 Mu = 21.47 M = 94.74 # Found Formula = C12 H4 Cu2 O10 # Dc = 0.94 FOOO = 5136.00 Mu = 14.14 M = 54.41 _chemical_formula_sum 'C12 H4 Cu2 O10' _chemical_formula_moiety 'C12 H4 Cu2 O10' _chemical_compound_source ? _chemical_formula_weight 435.25 _cell_measurement_reflns_used 4761 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.944 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 0.468 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 20789 _reflns_number_total 532 _diffrn_reflns_av_R_equivalents 0.103 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 532 # Theoretical number of reflections is about 806 _diffrn_reflns_theta_min 0.914 _diffrn_reflns_theta_max 14.089 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 13.244 _diffrn_measured_fraction_theta_full 0.969 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 1 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.42 _refine_diff_density_max 0.52 # 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>2.0\s(I) _refine_ls_number_reflns 415 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0440 _refine_ls_wR_factor_ref 0.0456 _refine_ls_goodness_of_fit_ref 1.0214 _refine_ls_shift/su_max 0.0008683 _refine_ls_shift/su_mean 0.0000505 # The values computed from all data _oxford_reflns_number_all 532 _refine_ls_R_factor_all 0.0564 _refine_ls_wR_factor_all 0.0628 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 415 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_gt 0.0456 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.295 0.188 0.108 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.71494(3) 0.21494(3) 0.5000 0.0378 1.0000 Uani S T . . . . O2 O 0.6562(2) 0.1562(2) 0.5000 0.1123 1.0000 Uani S T . . . . O1 O 0.68366(12) 0.25640(13) 0.55268(12) 0.0509 1.0000 Uani . . . . . . C3 C 0.7004(3) 0.36463(18) 0.63537(18) 0.0506 1.0000 Uani S T . . . . C2 C 0.67835(17) 0.32165(17) 0.6146(2) 0.0366 1.0000 Uani S T . . . . C1 C 0.70421(18) 0.29579(18) 0.5696(2) 0.0447 1.0000 Uani S T . . . . H31 H 0.7297 0.3794 0.6206 0.0608 1.0000 Uiso RS . . . . . 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 0.0394(6) 0.0394(6) 0.0345(8) 0.0000 0.0000 -0.0072(6) O2 0.104(5) 0.104(5) 0.128(9) 0.0000 0.0000 -0.060(6) O1 0.053(2) 0.053(2) 0.046(2) -0.0125(19) 0.0077(16) -0.0125(18) C3 0.063(5) 0.044(3) 0.044(3) 0.000(4) 0.009(2) -0.009(2) C2 0.038(3) 0.038(3) 0.034(4) -0.001(2) 0.001(2) -0.001(3) C1 0.045(3) 0.045(3) 0.043(5) 0.002(2) -0.002(2) -0.003(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.01895(9) 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 . O1 127_546 1.952(3) yes Cu1 . O1 103_545 1.952(3) yes Cu1 . O1 25_556 1.952(3) yes Cu1 . Cu1 122_665 2.616(2) yes Cu1 . O2 . 2.191(8) yes Cu1 . O1 . 1.952(3) yes O1 . C1 . 1.254(4) yes C3 . C2 34_665 1.388(5) yes C3 . C2 . 1.388(5) yes C3 . H31 . 0.950 no C2 . C1 . 1.531(9) yes 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 O1 127_546 Cu1 . O1 103_545 90.8(2) yes O1 127_546 Cu1 . O1 25_556 88.1(2) yes O1 103_545 Cu1 . O1 25_556 168.8(2) yes O1 127_546 Cu1 . Cu1 122_665 84.42(10) yes O1 103_545 Cu1 . Cu1 122_665 84.42(10) yes O1 25_556 Cu1 . Cu1 122_665 84.42(10) yes O1 127_546 Cu1 . O2 . 95.58(10) yes O1 103_545 Cu1 . O2 . 95.58(10) yes O1 25_556 Cu1 . O2 . 95.58(10) yes Cu1 122_665 Cu1 . O2 . 179.995 yes O1 127_546 Cu1 . O1 . 168.8(2) yes O1 103_545 Cu1 . O1 . 88.1(2) yes O1 25_556 Cu1 . O1 . 90.8(2) yes Cu1 122_665 Cu1 . O1 . 84.42(10) yes O2 . Cu1 . O1 . 95.58(10) yes Cu1 . O1 . C1 . 122.3(4) yes C2 34_665 C3 . C2 . 118.0(7) yes C2 34_665 C3 . H31 . 121.0 no C2 . C3 . H31 . 121.0 no C3 57_566 C2 . C3 . 122.0(7) yes C3 57_566 C2 . C1 . 118.9(4) yes C3 . C2 . C1 . 118.9(4) yes C2 . C1 . O1 122_665 116.9(3) yes C2 . C1 . O1 . 116.9(3) yes O1 122_665 C1 . O1 . 126.2(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 11:47:32 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 11:47:32 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment '- cubt15.cif' data_cubt15 _database_code_depnum_ccdc_archive 'CCDC 846572' #TrackingRef '- cubt15.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt15 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.3368(12) _cell_length_b 26.3368(12) _cell_length_c 26.3368(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18267.9(14) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 24 # Given Formula = C18 H15 Cu3 O21 # Dc = 1.65 Fooo = 5136.00 Mu = 21.60 M = 94.74 # Found Formula = C12 H4 Cu2 O10 # Dc = 0.95 FOOO = 5136.00 Mu = 14.22 M = 54.41 _chemical_formula_sum 'C12 H4 Cu2 O10' _chemical_formula_moiety 'C12 H4 Cu2 O10' _chemical_compound_source ? _chemical_formula_weight 435.25 _cell_measurement_reflns_used 4487 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.949 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 0.471 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 20785 _reflns_number_total 526 _diffrn_reflns_av_R_equivalents 0.104 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 526 # Theoretical number of reflections is about 794 _diffrn_reflns_theta_min 0.915 _diffrn_reflns_theta_max 14.085 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 13.240 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 1 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.38 _refine_diff_density_max 0.44 # 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>2.0\s(I) _refine_ls_number_reflns 408 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0380 _refine_ls_wR_factor_ref 0.0411 _refine_ls_goodness_of_fit_ref 0.9896 _refine_ls_shift/su_max 0.0004354 _refine_ls_shift/su_mean 0.0000261 # The values computed from all data _oxford_reflns_number_all 526 _refine_ls_R_factor_all 0.0502 _refine_ls_wR_factor_all 0.0572 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 408 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_gt 0.0411 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.296 0.205 0.113 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.5000 0.21500(3) 0.28500(3) 0.0358 1.0000 Uani S T . . . . O1 O 0.44712(11) 0.25660(12) 0.31632(11) 0.0508 1.0000 Uani . . . . . . O2 O 0.5000 0.15711(19) 0.34289(19) 0.1003 1.0000 Uani S T . . . . C3 C 0.36449(16) 0.3001(2) 0.36449(16) 0.0444 1.0000 Uani S T . . . . C4 C 0.3863(2) 0.32165(15) 0.32165(15) 0.0383 1.0000 Uani S T . . . . C5 C 0.4302(2) 0.29629(16) 0.29629(16) 0.0405 1.0000 Uani S T . . . . H31 H 0.3789 0.2704 0.3789 0.0462 1.0000 Uiso RS . . . . . 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 0.0325(7) 0.0374(5) 0.0374(5) 0.0074(5) 0.0000 0.0000 O1 0.049(2) 0.055(2) 0.048(2) 0.0126(16) 0.0113(14) 0.0133(17) O2 0.112(7) 0.094(4) 0.094(4) 0.053(5) 0.0000 0.0000 C3 0.043(2) 0.048(4) 0.043(2) 0.004(2) 0.000(3) 0.004(2) C4 0.036(4) 0.040(2) 0.040(2) 0.007(3) 0.0026(19) 0.0026(19) C5 0.039(4) 0.042(2) 0.042(2) 0.004(3) -0.001(2) -0.001(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.01979(9) 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 . O1 90_655 1.955(3) yes Cu1 . O1 116_655 1.955(3) yes Cu1 . O1 163_555 1.955(3) yes Cu1 . Cu1 162_655 2.607(2) yes Cu1 . O1 . 1.955(3) yes Cu1 . O2 . 2.156(7) yes O1 . C5 . 1.253(4) yes C3 . C4 9_555 1.387(4) yes C3 . C4 . 1.387(4) yes C3 . H31 . 0.948 no C4 . C5 . 1.494(8) yes 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 O1 90_655 Cu1 . O1 116_655 88.02(19) yes O1 90_655 Cu1 . O1 163_555 168.76(17) yes O1 116_655 Cu1 . O1 163_555 90.88(19) yes O1 90_655 Cu1 . Cu1 162_655 84.38(9) yes O1 116_655 Cu1 . Cu1 162_655 84.38(9) yes O1 163_555 Cu1 . Cu1 162_655 84.38(9) yes O1 90_655 Cu1 . O1 . 90.88(19) yes O1 116_655 Cu1 . O1 . 168.76(17) yes O1 163_555 Cu1 . O1 . 88.02(19) yes Cu1 162_655 Cu1 . O1 . 84.38(9) yes O1 90_655 Cu1 . O2 . 95.62(9) yes O1 116_655 Cu1 . O2 . 95.62(9) yes O1 163_555 Cu1 . O2 . 95.62(9) yes Cu1 162_655 Cu1 . O2 . 179.995 yes O1 . Cu1 . O2 . 95.62(9) yes Cu1 . O1 . C5 . 122.9(3) yes C4 9_555 C3 . C4 . 120.4(6) yes C4 9_555 C3 . H31 . 119.8 no C4 . C3 . H31 . 119.8 no C3 . C4 . C3 17_555 119.6(6) yes C3 . C4 . C5 . 120.1(3) yes C3 17_555 C4 . C5 . 120.1(3) yes C4 . C5 . O1 113_555 117.4(3) yes C4 . C5 . O1 . 117.4(3) yes O1 113_555 C5 . O1 . 125.2(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 12:40:26 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 12:40:26 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment '- cubt16.cif' data_cubt16 _database_code_depnum_ccdc_archive 'CCDC 846573' #TrackingRef '- cubt16.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt16 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.3081(12) _cell_length_b 26.3081(12) _cell_length_c 26.3081(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18208.3(14) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 24 # Given Formula = C18 H15 Cu3 O21 # Dc = 1.66 Fooo = 5136.00 Mu = 21.67 M = 94.74 # Found Formula = C12 H4 Cu2 O10 # Dc = 0.95 FOOO = 5136.00 Mu = 14.27 M = 54.41 _chemical_formula_sum 'C12 H4 Cu2 O10' _chemical_formula_moiety 'C12 H4 Cu2 O10' _chemical_compound_source ? _chemical_formula_weight 435.25 _cell_measurement_reflns_used 4436 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.953 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.427 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 20834 _reflns_number_total 528 _diffrn_reflns_av_R_equivalents 0.106 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 528 # Theoretical number of reflections is about 794 _diffrn_reflns_theta_min 0.916 _diffrn_reflns_theta_max 14.060 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 13.357 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 1 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.73 _refine_diff_density_max 0.58 # 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>2.0\s(I) _refine_ls_number_reflns 413 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0456 _refine_ls_wR_factor_ref 0.0511 _refine_ls_goodness_of_fit_ref 1.0076 _refine_ls_shift/su_max 0.0003793 _refine_ls_shift/su_mean 0.0000239 # The values computed from all data _oxford_reflns_number_all 528 _refine_ls_R_factor_all 0.0612 _refine_ls_wR_factor_all 0.0685 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 413 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_gt 0.0511 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.416 0.341 0.193 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.5000 0.21496(3) 0.28504(3) 0.0360 1.0000 Uani S T . . . . O1 O 0.44716(14) 0.25638(14) 0.31634(13) 0.0519 1.0000 Uani . . . . . . O2 O 0.5000 0.1574(2) 0.3426(2) 0.0995 1.0000 Uani S T . . . . C3 C 0.36441(19) 0.3000(3) 0.36441(19) 0.0467 1.0000 Uani S T . . . . C4 C 0.3860(3) 0.32176(18) 0.32176(18) 0.0396 1.0000 Uani S T . . . . C5 C 0.4301(2) 0.29602(19) 0.29602(19) 0.0404 1.0000 Uani S T . . . . H31 H 0.3786 0.2700 0.3786 0.0462 1.0000 Uiso RS . . . . . 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 0.0328(8) 0.0377(6) 0.0377(6) 0.0080(5) 0.0000 0.0000 O1 0.051(2) 0.053(2) 0.052(2) 0.0140(19) 0.0114(17) 0.012(2) O2 0.118(8) 0.090(5) 0.090(5) 0.057(6) 0.0000 0.0000 C3 0.044(3) 0.052(5) 0.044(3) 0.004(2) 0.000(4) 0.004(2) C4 0.037(4) 0.041(3) 0.041(3) 0.005(3) 0.007(2) 0.007(2) C5 0.040(4) 0.041(3) 0.041(3) 0.000(4) -0.001(2) -0.001(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.01997(11) 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 . O1 90_655 1.949(3) yes Cu1 . O1 116_655 1.949(3) yes Cu1 . O1 163_555 1.949(3) yes Cu1 . C5 4_655 2.831(6) yes Cu1 . C5 91_555 2.831(6) yes Cu1 . C5 162_655 2.831(6) yes Cu1 . Cu1 162_655 2.607(2) yes Cu1 . O1 . 1.949(3) yes Cu1 . O2 . 2.143(8) yes Cu1 . C5 . 2.831(6) yes O1 . C5 . 1.255(5) yes C3 . C4 9_555 1.382(5) yes C3 . C4 . 1.382(5) yes C3 . H31 . 0.950 no C4 . C5 . 1.504(10) yes 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 O1 90_655 Cu1 . O1 116_655 87.9(2) yes O1 90_655 Cu1 . O1 163_555 168.9(2) yes O1 116_655 Cu1 . O1 163_555 91.0(2) yes O1 90_655 Cu1 . C5 4_655 84.96(17) yes O1 116_655 Cu1 . C5 4_655 21.92(12) yes O1 163_555 Cu1 . C5 4_655 89.95(17) yes O1 90_655 Cu1 . C5 91_555 147.02(12) yes O1 116_655 Cu1 . C5 91_555 89.95(17) yes O1 163_555 Cu1 . C5 91_555 21.92(12) yes C5 4_655 Cu1 . C5 91_555 81.0(2) yes O1 90_655 Cu1 . C5 162_655 21.92(12) yes O1 116_655 Cu1 . C5 162_655 84.96(17) yes O1 163_555 Cu1 . C5 162_655 147.02(12) yes C5 4_655 Cu1 . C5 162_655 74.4(3) yes C5 91_555 Cu1 . C5 162_655 125.16(13) yes O1 90_655 Cu1 . Cu1 162_655 84.46(10) yes O1 116_655 Cu1 . Cu1 162_655 84.46(10) yes O1 163_555 Cu1 . Cu1 162_655 84.46(10) yes C5 4_655 Cu1 . Cu1 162_655 62.58(7) yes C5 91_555 Cu1 . Cu1 162_655 62.58(7) yes O1 90_655 Cu1 . O1 . 91.0(2) yes O1 116_655 Cu1 . O1 . 168.9(2) yes O1 163_555 Cu1 . O1 . 87.9(2) yes C5 4_655 Cu1 . O1 . 147.02(12) yes C5 91_555 Cu1 . O1 . 84.96(17) yes O1 90_655 Cu1 . O2 . 95.54(10) yes O1 116_655 Cu1 . O2 . 95.54(10) yes O1 163_555 Cu1 . O2 . 95.54(10) yes C5 4_655 Cu1 . O2 . 117.42(7) yes C5 91_555 Cu1 . O2 . 117.42(7) yes O1 90_655 Cu1 . C5 . 89.95(17) yes O1 116_655 Cu1 . C5 . 147.02(12) yes O1 163_555 Cu1 . C5 . 84.96(17) yes C5 4_655 Cu1 . C5 . 125.16(13) yes C5 91_555 Cu1 . C5 . 74.4(3) yes C5 162_655 Cu1 . Cu1 162_655 62.58(7) yes C5 162_655 Cu1 . O1 . 89.95(17) yes Cu1 162_655 Cu1 . O1 . 84.46(10) yes C5 162_655 Cu1 . O2 . 117.42(7) yes Cu1 162_655 Cu1 . O2 . 179.995 yes O1 . Cu1 . O2 . 95.54(10) yes C5 162_655 Cu1 . C5 . 81.0(2) yes Cu1 162_655 Cu1 . C5 . 62.58(7) yes O1 . Cu1 . C5 . 21.92(12) yes O2 . Cu1 . C5 . 117.42(7) yes Cu1 . O1 . C5 . 122.7(4) yes C4 9_555 C3 . C4 . 119.8(8) yes C4 9_555 C3 . H31 . 120.1 no C4 . C3 . H31 . 120.1 no C3 . C4 . C3 17_555 120.2(8) yes C3 . C4 . C5 . 119.8(4) yes C3 17_555 C4 . C5 . 119.8(4) yes C4 . C5 . O1 113_555 117.3(3) yes C4 . C5 . O1 . 117.3(3) yes O1 113_555 C5 . O1 . 125.5(6) yes C4 . C5 . Cu1 . 152.38(8) yes O1 113_555 C5 . Cu1 . 90.2(4) yes O1 . C5 . Cu1 . 35.4(3) yes C4 . C5 . Cu1 4_655 152.38(8) yes O1 113_555 C5 . Cu1 4_655 35.4(3) yes O1 . C5 . Cu1 4_655 90.2(4) yes Cu1 . C5 . Cu1 4_655 54.84(13) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 12:44:25 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 12:44:25 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment '- cubt17.cif' data_cubt17 _database_code_depnum_ccdc_archive 'CCDC 846574' #TrackingRef '- cubt17.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt17 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.2896(15) _cell_length_b 26.2896(15) _cell_length_c 26.2896(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18169.9(18) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 48 # Given Formula = C9 H7.50 Cu1.50 O10.50 # Dc = 1.66 Fooo = 5136.00 Mu = 21.71 M = 94.74 # Found Formula = C6 H2 Cu1 O5 # Dc = 0.95 FOOO = 5136.00 Mu = 14.30 M = 54.41 _chemical_formula_sum 'C6 H2 Cu1 O5' _chemical_formula_moiety 'C6 H2 Cu1 O5' _chemical_compound_source ? _chemical_formula_weight 217.62 _cell_measurement_reflns_used 2740 _cell_measurement_theta_min 2 _cell_measurement_theta_max 14 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.955 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.430 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 12998 _reflns_number_total 396 _diffrn_reflns_av_R_equivalents 0.104 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 396 # Theoretical number of reflections is about 752 _diffrn_reflns_theta_min 1.498 _diffrn_reflns_theta_max 13.808 _diffrn_measured_fraction_theta_max 0.770 _diffrn_reflns_theta_full 13.808 _diffrn_measured_fraction_theta_full 0.770 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 2 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.52 _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>2.0\s(I) _refine_ls_number_reflns 302 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0422 _refine_ls_wR_factor_ref 0.0486 _refine_ls_goodness_of_fit_ref 1.0709 _refine_ls_shift/su_max 0.0000809 _refine_ls_shift/su_mean 0.0000109 # The values computed from all data _oxford_reflns_number_all 396 _refine_ls_R_factor_all 0.0577 _refine_ls_wR_factor_all 0.0681 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 302 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_gt 0.0486 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.351 0.255 0.139 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.5000 0.21499(4) 0.28501(4) 0.0354 1.0000 Uani S T . . . . O1 O 0.44703(17) 0.25656(16) 0.31648(15) 0.0515 1.0000 Uani . . . . . . O2 O 0.5000 0.1577(3) 0.3423(3) 0.0960 1.0000 Uani S T . . . . C3 C 0.3644(2) 0.3011(3) 0.3644(2) 0.0449 1.0000 Uani S T . . . . C4 C 0.3869(3) 0.3219(2) 0.3219(2) 0.0331 1.0000 Uani S T . . . . C5 C 0.4302(3) 0.2962(2) 0.2962(2) 0.0398 1.0000 Uani S T . . . . H31 H 0.3786 0.2711 0.3786 0.0462 1.0000 Uiso RS . . . . . 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 0.0308(10) 0.0377(7) 0.0377(7) 0.0057(7) 0.0000 0.0000 O1 0.053(3) 0.049(3) 0.052(3) 0.011(2) 0.010(2) 0.011(2) O2 0.109(9) 0.089(5) 0.089(5) 0.047(7) 0.0000 0.0000 C3 0.052(4) 0.031(6) 0.052(4) 0.003(3) -0.010(5) 0.003(3) C4 0.038(5) 0.031(3) 0.031(3) 0.014(4) 0.006(3) 0.006(3) C5 0.042(6) 0.039(3) 0.039(3) -0.006(5) 0.005(3) 0.005(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.02011(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 . O1 116_655 1.954(4) yes Cu1 . O1 163_555 1.954(4) yes Cu1 . O1 90_655 1.954(4) yes Cu1 . Cu1 162_655 2.603(3) yes Cu1 . O1 . 1.954(4) yes Cu1 . O2 . 2.129(9) yes O1 . C5 . 1.251(5) yes C3 . C4 9_555 1.377(5) yes C3 . C4 . 1.377(5) yes C3 . H31 . 0.949 no C4 . C5 . 1.488(11) yes 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 O1 116_655 Cu1 . O1 163_555 90.9(3) yes O1 116_655 Cu1 . O1 90_655 88.0(3) yes O1 163_555 Cu1 . O1 90_655 169.0(2) yes O1 116_655 Cu1 . Cu1 162_655 84.48(12) yes O1 163_555 Cu1 . Cu1 162_655 84.48(12) yes O1 90_655 Cu1 . Cu1 162_655 84.48(12) yes O1 116_655 Cu1 . O1 . 169.0(2) yes O1 163_555 Cu1 . O1 . 88.0(3) yes O1 90_655 Cu1 . O1 . 90.9(3) yes Cu1 162_655 Cu1 . O1 . 84.48(12) yes O1 116_655 Cu1 . O2 . 95.52(12) yes O1 163_555 Cu1 . O2 . 95.52(12) yes O1 90_655 Cu1 . O2 . 95.52(12) yes Cu1 162_655 Cu1 . O2 . 179.995 yes O1 . Cu1 . O2 . 95.52(12) yes Cu1 . O1 . C5 . 122.5(4) yes C4 9_555 C3 . C4 . 122.4(10) yes C4 9_555 C3 . H31 . 118.8 no C4 . C3 . H31 . 118.8 no C3 17_555 C4 . C3 . 117.5(10) yes C3 17_555 C4 . C5 . 121.1(5) yes C3 . C4 . C5 . 121.1(5) yes C4 . C5 . O1 . 117.1(4) yes C4 . C5 . O1 113_555 117.1(4) yes O1 . C5 . O1 113_555 125.8(8) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 12:50:52 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 12:50:52 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment '- cubt18.cif' data_cubt18 _database_code_depnum_ccdc_archive 'CCDC 846575' #TrackingRef '- cubt18.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt18 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.2564(15) _cell_length_b 26.2564(15) _cell_length_c 26.2564(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 18101.1(18) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 48 # Given Formula = C9 H7.50 Cu1.50 O10.50 # Dc = 1.67 Fooo = 5136.00 Mu = 21.80 M = 94.74 # Found Formula = C6 H2 Cu1 O5 # Dc = 0.96 FOOO = 5136.00 Mu = 14.35 M = 54.41 _chemical_formula_sum 'C6 H2 Cu1 O5' _chemical_formula_moiety 'C6 H2 Cu1 O5' _chemical_compound_source ? _chemical_formula_weight 217.62 _cell_measurement_reflns_used 2893 _cell_measurement_theta_min 2 _cell_measurement_theta_max 14 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.958 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.435 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 13152 _reflns_number_total 398 _diffrn_reflns_av_R_equivalents 0.096 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 398 # Theoretical number of reflections is about 752 _diffrn_reflns_theta_min 1.500 _diffrn_reflns_theta_max 13.826 _diffrn_measured_fraction_theta_max 0.773 _diffrn_reflns_theta_full 13.826 _diffrn_measured_fraction_theta_full 0.773 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 2 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.47 _refine_diff_density_max 0.35 # 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>2.0\s(I) _refine_ls_number_reflns 298 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0367 _refine_ls_wR_factor_ref 0.0417 _refine_ls_goodness_of_fit_ref 1.1033 _refine_ls_shift/su_max 0.0001653 _refine_ls_shift/su_mean 0.0000141 # The values computed from all data _oxford_reflns_number_all 398 _refine_ls_R_factor_all 0.0546 _refine_ls_wR_factor_all 0.0645 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 298 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_gt 0.0417 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.244 0.139 0.625E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.5000 0.21505(4) 0.28495(4) 0.0369 1.0000 Uani S T . . . . O1 O 0.44689(15) 0.25669(15) 0.31644(14) 0.0529 1.0000 Uani . . . . . . O2 O 0.5000 0.1580(3) 0.3420(3) 0.1053 1.0000 Uani S T . . . . C3 C 0.3646(2) 0.3004(3) 0.3646(2) 0.0537 1.0000 Uani S T . . . . C4 C 0.3870(3) 0.32224(19) 0.32224(19) 0.0348 1.0000 Uani S T . . . . C5 C 0.4296(3) 0.2959(2) 0.2959(2) 0.0388 1.0000 Uani S T . . . . H31 H 0.3787 0.2704 0.3787 0.0462 1.0000 Uiso RS . . . . . 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 0.0342(10) 0.0383(6) 0.0383(6) 0.0063(6) 0.0000 0.0000 O1 0.054(3) 0.050(3) 0.054(3) 0.009(2) 0.010(2) 0.015(2) O2 0.116(9) 0.100(5) 0.100(5) 0.043(7) 0.0000 0.0000 C3 0.062(4) 0.037(6) 0.062(4) 0.004(3) -0.006(5) 0.004(3) C4 0.038(5) 0.033(3) 0.033(3) 0.013(4) 0.003(3) 0.003(3) C5 0.038(5) 0.039(3) 0.039(3) -0.004(4) 0.003(3) 0.003(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.02035(10) 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 . O1 116_655 1.955(4) yes Cu1 . O1 163_555 1.955(4) yes Cu1 . O1 90_655 1.955(4) yes Cu1 . C5 162_655 2.828(6) yes Cu1 . C5 91_555 2.828(6) yes Cu1 . C5 4_655 2.828(6) yes Cu1 . Cu1 162_655 2.596(3) yes Cu1 . O1 . 1.955(4) yes Cu1 . O2 . 2.117(10) yes Cu1 . C5 . 2.828(6) yes O1 . C5 . 1.247(5) yes C3 . C4 9_555 1.382(5) yes C3 . C4 . 1.382(5) yes C3 . H31 . 0.948 no C4 . C5 . 1.487(10) yes 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 O1 116_655 Cu1 . O1 163_555 91.0(2) yes O1 116_655 Cu1 . O1 90_655 87.9(2) yes O1 163_555 Cu1 . O1 90_655 168.9(2) yes O1 116_655 Cu1 . C5 162_655 84.72(18) yes O1 163_555 Cu1 . C5 162_655 147.12(13) yes O1 90_655 Cu1 . C5 162_655 21.83(14) yes O1 116_655 Cu1 . C5 91_555 90.20(18) yes O1 163_555 Cu1 . C5 91_555 21.83(14) yes O1 90_655 Cu1 . C5 91_555 147.12(13) yes C5 162_655 Cu1 . C5 91_555 125.37(14) yes O1 116_655 Cu1 . C5 4_655 21.83(14) yes O1 163_555 Cu1 . C5 4_655 90.20(18) yes O1 90_655 Cu1 . C5 4_655 84.72(18) yes C5 162_655 Cu1 . C5 4_655 74.1(3) yes C5 91_555 Cu1 . C5 4_655 81.6(3) yes O1 116_655 Cu1 . Cu1 162_655 84.46(11) yes O1 163_555 Cu1 . Cu1 162_655 84.46(11) yes O1 90_655 Cu1 . Cu1 162_655 84.46(11) yes C5 162_655 Cu1 . Cu1 162_655 62.69(7) yes C5 91_555 Cu1 . Cu1 162_655 62.69(7) yes O1 116_655 Cu1 . O1 . 168.9(2) yes O1 163_555 Cu1 . O1 . 87.9(2) yes O1 90_655 Cu1 . O1 . 91.0(2) yes C5 162_655 Cu1 . O1 . 90.20(18) yes C5 91_555 Cu1 . O1 . 84.72(18) yes O1 116_655 Cu1 . O2 . 95.54(11) yes O1 163_555 Cu1 . O2 . 95.54(11) yes O1 90_655 Cu1 . O2 . 95.54(11) yes C5 162_655 Cu1 . O2 . 117.31(7) yes C5 91_555 Cu1 . O2 . 117.31(7) yes O1 116_655 Cu1 . C5 . 147.12(13) yes O1 163_555 Cu1 . C5 . 84.72(18) yes O1 90_655 Cu1 . C5 . 90.20(18) yes C5 162_655 Cu1 . C5 . 81.6(3) yes C5 91_555 Cu1 . C5 . 74.1(3) yes C5 4_655 Cu1 . Cu1 162_655 62.69(7) yes C5 4_655 Cu1 . O1 . 147.12(13) yes Cu1 162_655 Cu1 . O1 . 84.46(11) yes C5 4_655 Cu1 . O2 . 117.31(7) yes Cu1 162_655 Cu1 . O2 . 179.995 yes O1 . Cu1 . O2 . 95.54(11) yes C5 4_655 Cu1 . C5 . 125.37(14) yes Cu1 162_655 Cu1 . C5 . 62.69(7) yes O1 . Cu1 . C5 . 21.83(14) yes O2 . Cu1 . C5 . 117.31(7) yes Cu1 . O1 . C5 . 122.5(4) yes C4 9_555 C3 . C4 . 120.9(9) yes C4 9_555 C3 . H31 . 119.5 no C4 . C3 . H31 . 119.5 no C3 . C4 . C3 17_555 119.0(9) yes C3 . C4 . C5 . 120.1(5) yes C3 17_555 C4 . C5 . 120.1(5) yes C4 . C5 . O1 113_555 117.1(4) yes C4 . C5 . O1 . 117.1(4) yes O1 113_555 C5 . O1 . 125.6(7) yes C4 . C5 . Cu1 . 152.65(8) yes O1 113_555 C5 . Cu1 . 90.2(4) yes O1 . C5 . Cu1 . 35.7(3) yes C4 . C5 . Cu1 4_655 152.65(8) yes O1 113_555 C5 . Cu1 4_655 35.7(3) yes O1 . C5 . Cu1 4_655 90.2(4) yes Cu1 . C5 . Cu1 4_655 54.63(14) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 12:54:31 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 12:54:31 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment '- cubt20.cif' data_cubt20 _database_code_depnum_ccdc_archive 'CCDC 846576' #TrackingRef '- cubt20.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt20 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 25.9467(17) _cell_length_b 25.9467(17) _cell_length_c 25.9467(17) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 17468.1(20) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 48 # Given Formula = C9 H7.50 Cu1.50 O10.50 # Dc = 1.73 Fooo = 5136.00 Mu = 22.59 M = 94.74 # Found Formula = C6 H2 Cu1 O5 # Dc = 0.99 FOOO = 5136.00 Mu = 14.87 M = 54.41 _chemical_formula_sum 'C6 H2 Cu1 O5' _chemical_formula_moiety 'C6 H2 Cu1 O5' _chemical_compound_source ? _chemical_formula_weight 217.62 _cell_measurement_reflns_used 2474 _cell_measurement_theta_min 2 _cell_measurement_theta_max 13 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.993 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.487 # 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 0.64 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 12870 _reflns_number_total 313 _diffrn_reflns_av_R_equivalents 0.117 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 313 # Theoretical number of reflections is about 440 _diffrn_reflns_theta_min 0.929 _diffrn_reflns_theta_max 11.674 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 9.106 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 1 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.51 _refine_diff_density_max 0.39 # 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>2.0\s(I) _refine_ls_number_reflns 230 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0647 _refine_ls_wR_factor_ref 0.0699 _refine_ls_goodness_of_fit_ref 0.9994 _refine_ls_shift/su_max 0.0000477 _refine_ls_shift/su_mean 0.0000088 # The values computed from all data _oxford_reflns_number_all 312 _refine_ls_R_factor_all 0.1004 _refine_ls_wR_factor_all 0.1088 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 230 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_gt 0.0699 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.858 0.991 0.486 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.5000 0.21460(7) 0.28540(7) 0.0776 1.0000 Uani S T . . . . O1 O 0.4483(3) 0.2555(3) 0.3166(3) 0.0970 1.0000 Uani . . . . . . O2 O 0.5000 0.1563(4) 0.3437(4) 0.1651 1.0000 Uani S T . . . . C3 C 0.3669(4) 0.3025(6) 0.3669(4) 0.0910 1.0000 Uani S T . . . . C4 C 0.3891(6) 0.3242(5) 0.3242(5) 0.0964 1.0000 Uani S T . . . . C5 C 0.4306(7) 0.2960(5) 0.2960(5) 0.0819 1.0000 Uani S T . . . . H31 H 0.3817 0.2725 0.3817 0.1070 1.0000 Uiso RS . . . . . 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 0.074(2) 0.0792(17) 0.0792(17) 0.0213(14) 0.0000 0.0000 O1 0.096(5) 0.094(6) 0.101(7) 0.021(6) 0.013(4) 0.025(5) O2 0.193(19) 0.151(11) 0.151(11) 0.091(14) 0.0000 0.0000 C3 0.090(9) 0.093(16) 0.090(9) 0.013(8) 0.000(14) 0.013(8) C4 0.093(18) 0.098(10) 0.098(10) 0.019(16) 0.017(12) 0.017(12) C5 0.084(14) 0.081(8) 0.081(8) -0.023(14) 0.005(7) 0.005(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0203(2) 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 . O1 116_655 1.894(8) yes Cu1 . O1 163_555 1.894(8) yes Cu1 . O1 90_655 1.894(8) yes Cu1 . Cu1 162_655 2.598(5) yes Cu1 . O1 . 1.894(8) yes Cu1 . O2 . 2.140(16) yes O1 . C5 . 1.265(10) yes C3 . C4 9_555 1.370(10) yes C3 . C4 . 1.370(10) yes C3 . H31 . 0.950 no C4 . C5 . 1.49(2) yes 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 O1 116_655 Cu1 . O1 163_555 90.3(4) yes O1 116_655 Cu1 . O1 90_655 88.7(4) yes O1 163_555 Cu1 . O1 90_655 169.3(5) yes O1 116_655 Cu1 . Cu1 162_655 84.6(2) yes O1 163_555 Cu1 . Cu1 162_655 84.6(2) yes O1 90_655 Cu1 . Cu1 162_655 84.6(2) yes O1 116_655 Cu1 . O1 . 169.3(5) yes O1 163_555 Cu1 . O1 . 88.7(4) yes O1 90_655 Cu1 . O1 . 90.3(4) yes Cu1 162_655 Cu1 . O1 . 84.6(2) yes O1 116_655 Cu1 . O2 . 95.4(2) yes O1 163_555 Cu1 . O2 . 95.4(2) yes O1 90_655 Cu1 . O2 . 95.4(2) yes Cu1 162_655 Cu1 . O2 . 179.995 yes O1 . Cu1 . O2 . 95.4(2) yes Cu1 . O1 . C5 . 122.8(11) yes C4 9_555 C3 . C4 . 120.7(17) yes C4 9_555 C3 . H31 . 119.6 no C4 . C3 . H31 . 119.6 no C3 17_555 C4 . C3 . 119.2(17) yes C3 17_555 C4 . C5 . 119.9(9) yes C3 . C4 . C5 . 119.9(9) yes C4 . C5 . O1 . 117.4(9) yes C4 . C5 . O1 113_555 117.4(9) yes O1 . C5 . O1 113_555 124.9(18) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 13:02:54 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 13:02:54 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 1 1 1 x . # Attachment '- cubt19.cif' data_cubt19 _database_code_depnum_ccdc_archive 'CCDC 846577' #TrackingRef '- cubt19.cif' _audit_creation_date 11-08-18 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'cubt19 in Fm-3m' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; #end of refcif _cell_length_a 26.1823(18) _cell_length_b 26.1823(18) _cell_length_c 26.1823(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 17948(2) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'F m -3 m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 x+1/2,y+1/2,z -x+1/2,-y+1/2,-z y,z,x -y,-z,-x y,z+1/2,x+1/2 -y,-z+1/2,-x+1/2 y+1/2,z,x+1/2 -y+1/2,-z,-x+1/2 y+1/2,z+1/2,x -y+1/2,-z+1/2,-x z,x,y -z,-x,-y z,x+1/2,y+1/2 -z,-x+1/2,-y+1/2 z+1/2,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 x,y,-z -x,-y,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 x+1/2,y+1/2,-z -x+1/2,-y+1/2,z y,z,-x -y,-z,x y,z+1/2,-x+1/2 -y,-z+1/2,x+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 y+1/2,z+1/2,-x -y+1/2,-z+1/2,x z,x,-y -z,-x,y z,x+1/2,-y+1/2 -z,-x+1/2,y+1/2 z+1/2,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 y,-z,-x -y,z,x y,-z+1/2,-x+1/2 -y,z+1/2,x+1/2 y+1/2,-z,-x+1/2 -y+1/2,z,x+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z,-x,-y -z,x,y z,-x+1/2,-y+1/2 -z,x+1/2,y+1/2 z+1/2,-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,x,-y z,-x,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -z+1/2,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 -x,y,-z x,-y,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 -x+1/2,y+1/2,-z x+1/2,-y+1/2,z -y,z,-x y,-z,x -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 -y+1/2,z,-x+1/2 y+1/2,-z,x+1/2 -y+1/2,z+1/2,-x y+1/2,-z+1/2,x x,-y,-z -x,y,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 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z y,x,z -y,-x,-z y,x+1/2,z+1/2 -y,-x+1/2,-z+1/2 y+1/2,x,z+1/2 -y+1/2,-x,-z+1/2 y+1/2,x+1/2,z -y+1/2,-x+1/2,-z z,y,x -z,-y,-x z,y+1/2,x+1/2 -z,-y+1/2,-x+1/2 z+1/2,y,x+1/2 -z+1/2,-y,-x+1/2 z+1/2,y+1/2,x -z+1/2,-y+1/2,-x x,z,y -x,-z,-y x,z+1/2,y+1/2 -x,-z+1/2,-y+1/2 x+1/2,z,y+1/2 -x+1/2,-z,-y+1/2 x+1/2,z+1/2,y -x+1/2,-z+1/2,-y y,x,-z -y,-x,z y,x+1/2,-z+1/2 -y,-x+1/2,z+1/2 y+1/2,x,-z+1/2 -y+1/2,-x,z+1/2 y+1/2,x+1/2,-z -y+1/2,-x+1/2,z z,y,-x -z,-y,x z,y+1/2,-x+1/2 -z,-y+1/2,x+1/2 z+1/2,y,-x+1/2 -z+1/2,-y,x+1/2 z+1/2,y+1/2,-x -z+1/2,-y+1/2,x x,z,-y -x,-z,y x,z+1/2,-y+1/2 -x,-z+1/2,y+1/2 x+1/2,z,-y+1/2 -x+1/2,-z,y+1/2 x+1/2,z+1/2,-y -x+1/2,-z+1/2,y -z,y,-x z,-y,x -z,y+1/2,-x+1/2 z,-y+1/2,x+1/2 -z+1/2,y,-x+1/2 z+1/2,-y,x+1/2 -z+1/2,y+1/2,-x z+1/2,-y+1/2,x -x,z,-y x,-z,y -x,z+1/2,-y+1/2 x,-z+1/2,y+1/2 -x+1/2,z,-y+1/2 x+1/2,-z,y+1/2 -x+1/2,z+1/2,-y x+1/2,-z+1/2,y x,-z,-y -x,z,y x,-z+1/2,-y+1/2 -x,z+1/2,y+1/2 x+1/2,-z,-y+1/2 -x+1/2,z,y+1/2 x+1/2,-z+1/2,-y -x+1/2,z+1/2,y y,-x,-z -y,x,z y,-x+1/2,-z+1/2 -y,x+1/2,z+1/2 y+1/2,-x,-z+1/2 -y+1/2,x,z+1/2 y+1/2,-x+1/2,-z -y+1/2,x+1/2,z z,-y,-x -z,y,x z,-y+1/2,-x+1/2 -z,y+1/2,x+1/2 z+1/2,-y,-x+1/2 -z+1/2,y,x+1/2 z+1/2,-y+1/2,-x -z+1/2,y+1/2,x -y,x,-z y,-x,z -y,x+1/2,-z+1/2 y,-x+1/2,z+1/2 -y+1/2,x,-z+1/2 y+1/2,-x,z+1/2 -y+1/2,x+1/2,-z y+1/2,-x+1/2,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0006 0.0007 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' O 0.0036 0.0026 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 0.2947 0.6374 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 48 # Given Formula = C9 H7.50 Cu1.50 O10.50 # Dc = 1.68 Fooo = 5136.00 Mu = 21.98 M = 94.74 # Found Formula = C6 H2 Cu1 O5 # Dc = 0.97 FOOO = 5136.00 Mu = 14.48 M = 54.41 _chemical_formula_sum 'C6 H2 Cu1 O5' _chemical_formula_moiety 'C6 H2 Cu1 O5' _chemical_compound_source ? _chemical_formula_weight 217.62 _cell_measurement_reflns_used 1940 _cell_measurement_theta_min 2 _cell_measurement_theta_max 14 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 0.966 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 1.448 # Sheldrick geometric approximatio 0.75 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type ' ? ' _diffrn_radiation_wavelength 0.48590 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 9779 _reflns_number_total 383 _diffrn_reflns_av_R_equivalents 0.098 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 383 # Theoretical number of reflections is about 747 _diffrn_reflns_theta_min 1.504 _diffrn_reflns_theta_max 13.834 _diffrn_measured_fraction_theta_max 0.749 _diffrn_reflns_theta_full 13.834 _diffrn_measured_fraction_theta_full 0.749 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 2 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.40 _refine_diff_density_max 0.31 # 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>2.0\s(I) _refine_ls_number_reflns 270 _refine_ls_number_restraints 2 _refine_ls_number_parameters 37 _oxford_refine_ls_R_factor_ref 0.0558 _refine_ls_wR_factor_ref 0.0685 _refine_ls_goodness_of_fit_ref 1.1188 _refine_ls_shift/su_max 0.0001392 _refine_ls_shift/su_mean 0.0000164 # The values computed from all data _oxford_reflns_number_all 383 _refine_ls_R_factor_all 0.0976 _refine_ls_wR_factor_all 0.1061 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 270 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_gt 0.0685 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # 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: 0.520 0.444 0.224 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Cu1 Cu 0.5000 0.21496(6) 0.28504(6) 0.0408 1.0000 Uani S T . . . . O1 O 0.4473(3) 0.2567(2) 0.3169(2) 0.0550 1.0000 Uani . . . . . . O2 O 0.5000 0.1581(4) 0.3419(4) 0.1171 1.0000 Uani S T . . . . C3 C 0.3652(4) 0.3020(6) 0.3652(4) 0.0608 1.0000 Uani S T . . . . C4 C 0.3890(4) 0.3229(3) 0.3229(3) 0.0355 1.0000 Uani S T . . . . C5 C 0.4305(5) 0.2962(3) 0.2962(3) 0.0487 1.0000 Uani S T . . . . H31 H 0.3791 0.2715 0.3791 0.0718 1.0000 Uiso RS . . . . . 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 0.0361(15) 0.0432(11) 0.0432(11) 0.0062(10) 0.0000 0.0000 O1 0.059(4) 0.052(4) 0.054(5) 0.006(3) 0.011(3) 0.011(3) O2 0.137(15) 0.107(8) 0.107(8) 0.054(12) 0.0000 0.0000 C3 0.060(6) 0.063(10) 0.060(6) 0.006(5) -0.004(7) 0.006(5) C4 0.046(8) 0.030(5) 0.030(5) 0.008(6) 0.007(4) 0.007(4) C5 0.038(8) 0.054(5) 0.054(5) 0.002(7) 0.005(5) 0.005(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.02110(19) 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 . O1 116_655 1.948(6) yes Cu1 . O1 163_555 1.948(6) yes Cu1 . O1 90_655 1.948(6) yes Cu1 . Cu1 162_655 2.595(4) yes Cu1 . O1 . 1.948(6) yes Cu1 . O2 . 2.105(15) yes O1 . C5 . 1.247(8) yes C3 . C4 9_555 1.385(8) yes C3 . C4 . 1.385(8) yes C3 . H31 . 0.950 no C4 . C5 . 1.468(16) yes 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 O1 116_655 Cu1 . O1 163_555 90.3(4) yes O1 116_655 Cu1 . O1 90_655 88.7(4) yes O1 163_555 Cu1 . O1 90_655 169.2(4) yes O1 116_655 Cu1 . Cu1 162_655 84.59(18) yes O1 163_555 Cu1 . Cu1 162_655 84.59(18) yes O1 90_655 Cu1 . Cu1 162_655 84.59(18) yes O1 116_655 Cu1 . O1 . 169.2(4) yes O1 163_555 Cu1 . O1 . 88.7(4) yes O1 90_655 Cu1 . O1 . 90.3(4) yes Cu1 162_655 Cu1 . O1 . 84.59(18) yes O1 116_655 Cu1 . O2 . 95.41(18) yes O1 163_555 Cu1 . O2 . 95.41(18) yes O1 90_655 Cu1 . O2 . 95.41(18) yes Cu1 162_655 Cu1 . O2 . 179.995 yes O1 . Cu1 . O2 . 95.41(18) yes Cu1 . O1 . C5 . 122.0(7) yes C4 9_555 C3 . C4 . 124.4(14) yes C4 9_555 C3 . H31 . 117.8 no C4 . C3 . H31 . 117.8 no C3 17_555 C4 . C3 . 115.5(14) yes C3 17_555 C4 . C5 . 121.8(7) yes C3 . C4 . C5 . 121.8(7) yes C4 . C5 . O1 113_555 116.7(6) yes C4 . C5 . O1 . 116.7(6) yes O1 113_555 C5 . O1 . 126.6(12) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/08/11 at 12:58:23 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/08/11 at 12:58:23 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ;