#------------------------------------------------------------------------------ #$Date: 2016-11-11 03:50:57 +0200 (Fri, 11 Nov 2016) $ #$Revision: 188382 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/19/2241944.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2241944 loop_ _publ_author_name 'Dickie, Diane A.' 'Kemp, Richard A.' _publ_section_title ; Crystal structure of catena-poly[diammonium [di-\m-oxalato-cuprate(II)]] ; _journal_coeditor_code PJ2038 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1780 _journal_page_last 1782 _journal_paper_doi 10.1107/S2056989016017631 _journal_volume 72 _journal_year 2016 _chemical_formula_moiety '2(H4 N1 +), C4 Cu O8 2-' _chemical_formula_sum 'C4 H8 Cu N2 O8' _chemical_formula_weight 275.66 _chemical_name_common '(N H4)2 [Cu (C2 O4)2]' _chemical_name_systematic ; catena-Poly[diammonium [di-\m-oxalato-cuprate(II)]] ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 96.992(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 4.8564(2) _cell_length_b 13.5188(5) _cell_length_c 6.7205(3) _cell_measurement_reflns_used 5449 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 33.1333 _cell_measurement_theta_min 3.0137 _cell_volume 437.94(3) _computing_cell_refinement ; SAINT (Bruker, 2015) ; _computing_data_collection ; BIS (Bruker, 2015) ; _computing_data_reduction ; SAINT (Bruker, 2015) ; _computing_molecular_graphics ; DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 8277 _diffrn_reflns_theta_full 33.15 _diffrn_reflns_theta_max 33.15 _diffrn_reflns_theta_min 3.01 _exptl_absorpt_coefficient_mu 2.526 _exptl_absorpt_correction_T_max 0.54 _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2015) ; _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 278 _exptl_crystal_size_max 0.434 _exptl_crystal_size_mid 0.278 _exptl_crystal_size_min 0.278 _refine_diff_density_max 0.370 _refine_diff_density_min -0.513 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 86 _refine_ls_number_reflns 1672 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0179 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.1971P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0509 _reflns_number_gt 1537 _reflns_number_total 1672 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file pj2038sup1.cif _cod_data_source_block I _cod_database_code 2241944 _shelx_hkl_file ; -1 0 0 159.58 2.60 -1 0 0 155.48 2.80 -1 0 0 163.48 2.80 -1 0 0 155.88 2.70 1 0 0 163.78 2.70 1 0 0 160.38 2.80 2 0 0 1185.38 18.10 2 0 0 1209.28 17.90 -2 0 0 1180.68 17.90 -2 0 0 1216.78 18.20 -2 0 0 1192.38 18.10 -2 0 0 1225.48 17.50 3 0 0 438.76 7.70 -3 0 0 448.86 7.70 -3 0 0 435.36 8.00 3 0 0 467.95 8.10 -3 0 0 468.35 7.10 -4 0 0 542.45 10.00 -4 0 0 543.45 9.40 4 0 0 555.64 9.60 -5 0 0 49.10 2.50 -5 0 0 53.19 2.10 5 0 0 47.90 2.10 -6 0 0 355.36 8.40 6 0 0 370.76 8.00 -6 0 0 363.66 7.50 -7 0 0 110.89 4.50 7 0 0 97.59 4.00 0 -1 0 0.00 0.10 1 -1 0 3.80 0.30 -1 -1 0 3.90 0.30 1 -1 0 4.30 0.30 -1 -1 0 4.90 0.40 -1 -1 0 5.20 0.40 -1 -1 0 4.60 0.40 -1 1 0 3.70 0.30 -1 1 0 4.80 0.40 -1 1 0 4.50 0.40 1 1 0 4.10 0.30 -2 -1 0 34.10 1.20 -2 -1 0 32.50 1.00 -2 -1 0 32.00 1.20 2 -1 0 32.20 1.10 -2 -1 0 35.40 1.30 2 -1 0 31.70 1.20 -2 1 0 32.70 1.20 -2 1 0 32.10 1.00 2 1 0 32.30 1.10 -2 1 0 34.30 0.80 2 1 0 32.80 1.20 -2 1 0 31.60 1.20 -3 -1 0 9.90 1.00 -3 -1 0 10.00 0.80 3 -1 0 9.40 0.80 -3 -1 0 9.40 0.80 -3 -1 0 9.40 0.60 3 -1 0 9.30 0.70 3 1 0 10.10 0.90 -3 1 0 8.50 0.90 -3 1 0 10.00 0.50 -3 1 0 9.90 0.80 3 1 0 10.50 0.80 -3 1 0 9.60 0.80 4 -1 0 36.30 1.60 -4 -1 0 40.00 1.80 -4 1 0 39.70 1.90 -4 1 0 38.40 1.60 4 1 0 36.00 1.60 5 -1 0 82.09 2.90 -5 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480.05 9.20 -4 -2 0 470.75 8.70 -4 2 0 479.35 9.00 -4 2 0 483.85 8.20 -5 -2 0 63.99 2.70 5 -2 0 61.49 2.40 -5 -2 0 62.79 2.50 5 2 0 59.39 2.40 -5 2 0 60.89 2.70 -5 2 0 59.59 2.10 6 -2 0 221.58 5.80 -6 -2 0 226.28 6.20 -6 -2 0 227.68 5.60 6 2 0 221.18 5.80 -6 2 0 227.88 6.30 -7 -2 0 115.29 4.60 -7 -2 0 118.69 4.10 7 -2 0 120.99 4.40 -7 2 0 116.99 4.70 7 2 0 118.19 4.40 0 -3 0 5.10 0.40 -1 -3 0 12.40 0.50 1 -3 0 11.10 0.60 1 -3 0 12.20 0.50 -1 -3 0 11.90 0.60 -1 -3 0 11.00 0.60 -1 -3 0 12.00 0.60 1 3 0 11.30 0.50 -1 3 0 10.90 0.50 -1 3 0 12.20 0.50 1 3 0 12.00 0.60 -1 3 0 11.00 0.60 -2 -3 0 98.79 2.40 -2 -3 0 97.89 2.40 -2 -3 0 98.99 2.30 2 -3 0 100.99 2.20 2 -3 0 100.79 2.40 -2 -3 0 93.19 2.20 -2 3 0 99.89 2.40 -2 3 0 94.39 2.30 2 3 0 99.09 2.40 -2 3 0 94.59 2.30 2 3 0 98.29 2.20 -2 3 0 98.49 1.90 3 -3 0 91.79 2.60 -3 -3 0 95.69 2.60 -3 -3 0 89.19 2.30 -3 -3 0 93.89 2.70 3 -3 0 96.49 2.40 -3 -3 0 91.39 2.70 3 3 0 91.69 2.40 -3 3 0 93.19 2.60 -3 3 0 94.09 2.60 -3 3 0 89.79 2.10 -4 -3 0 112.19 3.20 -4 -3 0 109.09 3.20 -4 -3 0 111.69 2.80 4 -3 0 112.99 3.00 -4 -3 0 112.89 3.40 4 3 0 110.89 3.10 -4 3 0 108.69 2.60 -4 3 0 107.69 3.30 5 -3 0 1.70 0.70 -5 -3 0 1.70 0.80 -5 -3 0 2.10 0.90 -5 3 0 0.60 0.70 5 3 0 1.30 0.70 -6 -3 0 1.00 1.00 -6 -3 0 1.40 0.90 6 -3 0 -0.60 0.60 6 3 0 0.40 0.70 -6 3 0 0.70 0.90 -7 -3 0 3.90 1.30 7 -3 0 2.70 1.00 -7 -3 0 4.50 1.10 7 3 0 3.20 1.10 -7 3 0 7.90 1.60 0 -4 0 1013.50 14.80 0 -4 0 988.60 14.90 0 -4 0 970.10 14.70 0 -4 0 1022.80 14.50 0 4 0 980.80 14.50 -1 -4 0 79.49 1.90 1 -4 0 81.69 1.70 1 -4 0 80.09 1.80 -1 -4 0 82.69 2.00 1 -4 0 83.29 1.60 -1 -4 0 81.79 1.90 -1 -4 0 82.19 1.60 1 4 0 86.39 1.90 -1 4 0 79.79 1.80 1 4 0 81.29 1.80 -1 4 0 79.59 1.90 -1 4 0 83.99 1.70 -2 -4 0 500.55 8.60 -2 -4 0 506.55 8.20 2 -4 0 506.75 8.40 -2 -4 0 501.65 8.50 -2 -4 0 510.15 8.30 2 -4 0 512.75 8.10 2 4 0 517.05 8.60 -2 4 0 515.55 8.40 2 4 0 509.15 8.20 -2 4 0 504.45 8.30 -2 4 0 503.15 7.60 -3 -4 0 759.62 12.50 -3 -4 0 753.02 12.20 3 -4 0 745.93 12.00 3 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35.50 2.80 -4 -4 8 39.00 2.60 -4 4 8 33.10 2.70 -4 4 8 39.90 2.80 -3 -4 8 14.20 1.90 -3 -4 8 13.60 1.70 -3 4 8 15.10 1.90 -3 4 8 14.60 1.50 -3 4 8 11.90 1.70 -2 -4 8 217.08 6.20 -2 -4 8 221.78 5.50 -2 4 8 216.78 5.80 -2 4 8 220.38 5.90 -1 -4 8 153.28 4.30 -1 -4 8 137.59 4.70 -1 4 8 142.89 4.40 -1 4 8 145.79 4.50 0 -4 8 252.67 6.10 0 -4 8 250.17 6.60 0 4 8 244.78 6.10 0 4 8 254.77 6.30 -1 -4 -8 30.20 1.90 1 -4 8 28.80 2.00 1 4 8 28.70 2.00 1 4 8 30.90 2.00 2 -4 8 187.88 5.40 -2 -4 -8 186.58 5.00 2 4 8 175.48 5.10 3 -4 8 66.79 3.30 3 4 8 67.89 3.10 -5 -5 8 18.00 2.40 -5 -5 8 21.40 2.50 -5 5 8 28.60 2.80 -5 5 8 24.90 2.80 -4 -5 8 5.10 1.40 -4 -5 8 9.70 1.90 -4 5 8 3.70 1.30 -4 5 8 7.00 1.60 -3 -5 8 8.00 1.60 -3 -5 8 9.60 1.50 -3 5 8 10.20 1.60 -3 5 8 11.00 1.70 -2 -5 8 10.90 1.50 -2 -5 8 10.60 1.60 -2 -5 8 10.30 1.30 -2 5 8 9.60 1.50 -2 5 8 8.00 1.30 -1 -5 8 4.40 1.20 -1 -5 8 5.20 1.00 -1 5 8 5.50 1.10 -1 5 8 6.90 1.20 0 -5 8 4.40 1.00 0 -5 8 5.20 1.20 0 -5 -8 6.90 1.20 0 5 8 6.50 1.10 0 5 8 5.60 1.10 -1 -5 -8 72.49 3.00 1 -5 8 65.39 2.90 1 5 8 66.79 2.90 1 5 8 65.29 3.00 -2 -5 -8 0.30 0.80 2 -5 8 0.60 0.80 2 5 8 -0.10 0.70 3 -5 8 0.90 0.90 3 5 8 1.80 1.00 -4 -6 8 96.19 4.40 -4 -6 8 99.19 4.10 -4 6 8 99.39 4.20 -4 6 8 99.79 4.30 -3 -6 8 30.20 2.30 -3 -6 8 28.30 2.40 -3 6 8 28.30 2.50 -3 6 8 31.70 2.30 -2 -6 8 204.78 5.90 -2 -6 8 194.68 5.50 -2 6 8 200.38 5.70 -2 6 8 206.18 5.50 -1 -6 8 42.70 2.60 -1 -6 8 45.80 2.30 -1 6 8 43.60 2.40 -1 6 8 42.30 2.50 0 -6 8 78.39 3.10 0 -6 -8 74.79 3.10 0 -6 8 80.29 3.50 0 6 8 80.09 3.20 0 6 8 77.19 3.10 -1 -6 -8 18.70 1.90 1 -6 8 20.10 1.80 1 6 8 18.20 1.80 1 6 8 19.30 1.70 2 -6 8 125.29 4.40 -2 -6 -8 127.09 4.20 2 6 8 124.19 4.10 3 -6 8 29.80 2.30 3 6 8 27.80 2.20 -4 -7 8 6.30 1.60 -4 -7 8 8.90 1.70 -4 7 8 6.40 1.60 -4 7 8 8.30 1.80 -3 -7 8 20.10 2.20 -3 -7 8 25.60 2.20 -3 7 8 23.10 2.10 -3 7 8 28.90 2.70 -2 -7 8 7.00 1.40 -2 -7 8 3.10 1.00 -2 7 8 4.60 1.20 -2 7 8 6.00 1.20 1 -7 -8 2.50 1.00 -1 -7 8 2.00 0.80 -1 -7 8 3.40 1.10 -1 7 8 3.40 0.90 -1 7 8 2.90 1.00 0 -7 8 28.10 2.10 0 -7 8 28.40 1.90 0 -7 -8 28.40 2.10 0 7 8 29.60 2.00 0 7 8 26.70 2.00 -1 -7 -8 21.10 1.80 1 -7 8 23.30 1.90 1 7 8 23.00 1.90 1 7 8 23.30 2.90 2 -7 8 0.00 0.90 -2 -7 -8 1.40 0.90 2 7 8 0.70 0.80 3 -7 8 2.20 1.00 -3 -7 -8 2.20 1.00 3 7 8 0.10 0.80 -4 -8 8 68.89 3.60 -4 -8 8 62.89 3.60 -4 8 8 69.09 3.70 -3 -8 8 66.99 3.30 -3 -8 8 64.29 3.40 -3 8 8 69.59 3.60 -2 -8 8 106.19 3.90 -2 -8 8 100.59 4.00 -2 8 8 108.19 4.20 -1 -8 8 110.49 4.10 1 -8 -8 118.19 4.00 -1 8 8 117.19 4.10 0 -8 -8 9.70 1.50 0 -8 8 8.90 1.50 0 -8 8 10.50 1.40 0 8 8 11.40 1.50 -1 -8 -8 213.08 5.90 1 -8 8 223.68 5.90 1 8 8 213.98 5.70 2 -8 8 143.39 4.80 -2 -8 -8 147.99 4.70 2 8 8 143.79 4.50 -3 -8 -8 163.68 5.00 3 -8 8 157.78 5.30 -4 -9 8 -1.30 1.00 -4 -9 8 0.50 1.20 -4 9 8 0.20 1.30 -3 -9 8 15.60 2.00 -3 -9 8 18.80 2.10 -3 9 8 14.60 2.10 -2 -9 8 1.60 1.00 -2 -9 8 0.90 0.90 -2 9 8 2.40 1.30 1 -9 -8 17.10 1.90 -1 -9 8 16.70 1.90 -1 -9 8 14.50 1.60 -1 9 8 13.80 1.80 0 -9 8 6.00 1.30 0 -9 8 6.40 1.20 0 -9 -8 8.70 1.50 0 9 8 6.90 1.30 -1 -9 -8 0.90 0.90 1 -9 8 -0.10 0.80 1 -9 8 -0.20 0.70 1 9 8 0.30 0.80 -2 -9 -8 3.70 1.20 2 -9 8 2.70 1.10 2 9 8 3.10 1.00 -3 -10 8 17.60 2.10 -3 -10 8 18.80 2.20 -3 10 8 20.00 2.50 -2 -10 8 230.18 6.10 2 -10 -8 216.88 6.00 -2 -10 8 213.48 6.10 -2 10 8 208.88 6.30 1 -10 -8 28.10 2.20 -1 -10 8 40.00 2.40 -1 -10 8 34.80 2.40 -1 10 8 34.80 2.50 0 -10 8 118.49 4.30 0 -10 -8 116.89 4.30 0 10 8 113.69 4.10 1 -10 8 55.09 2.90 -1 -10 -8 53.19 3.00 1 -10 8 51.39 2.80 1 10 8 55.09 2.80 -2 -10 -8 116.39 4.30 2 -10 8 110.39 4.30 -3 -11 8 48.90 3.00 -3 11 8 53.79 3.40 2 -11 -8 5.80 1.40 -2 -11 8 3.50 1.20 -2 -11 8 4.50 1.20 -2 11 8 -0.30 1.20 1 -11 -8 14.60 1.90 -1 -11 8 16.20 1.80 -1 -11 8 19.20 2.00 -1 11 8 15.40 2.00 0 -11 8 2.30 0.80 0 -11 8 -0.20 0.70 0 -11 -8 0.50 1.00 0 11 8 -0.40 1.00 1 -11 8 0.00 0.80 1 -11 8 1.70 0.90 -1 -11 -8 0.80 1.00 1 11 8 0.80 1.00 -2 -12 8 120.49 4.30 2 -12 -8 121.79 4.40 -2 12 8 114.19 4.70 -1 -12 8 57.69 2.90 1 -12 -8 61.09 3.20 -1 12 8 54.79 3.20 0 -12 8 79.39 3.20 0 -12 -8 80.59 3.70 0 12 8 84.09 3.70 -1 -12 -8 37.30 2.70 -1 -13 8 6.90 1.40 1 -13 -8 7.50 1.50 -1 -13 8 9.80 1.60 -1 13 8 7.10 1.60 0 -13 -8 -0.40 1.00 0 13 8 -1.30 1.00 -4 0 9 0.00 0.90 -4 0 9 -2.20 1.10 -4 0 9 -0.90 1.10 -3 0 9 -0.30 1.00 -3 0 9 1.30 1.10 -3 0 9 1.20 0.90 -2 0 9 0.70 0.80 -2 0 9 0.50 0.90 -1 0 9 -0.30 0.70 -1 0 9 0.30 0.80 0 0 9 -0.10 0.80 0 0 9 -0.70 0.70 1 0 9 -0.40 0.80 1 0 9 0.40 0.80 2 0 9 -0.60 0.90 -4 -1 9 218.58 6.30 -4 -1 9 203.78 6.80 -4 1 9 211.18 6.40 -4 1 9 224.98 6.20 -4 1 9 215.38 6.90 -3 -1 9 4.20 1.20 -3 -1 9 4.00 1.30 -3 -1 9 5.00 1.30 -3 1 9 4.70 1.10 -3 1 9 3.60 1.30 -3 1 9 4.90 1.40 -2 -1 9 78.19 3.60 -2 -1 9 83.09 3.40 -2 1 9 82.99 3.50 -2 1 9 80.79 3.70 -1 -1 9 59.69 2.90 -1 -1 9 58.99 3.20 -1 1 9 53.69 3.00 -1 1 9 56.69 2.80 0 -1 9 90.69 3.50 0 -1 9 83.99 3.80 0 1 9 91.59 3.90 0 1 9 93.39 3.60 1 -1 9 70.99 3.20 1 -1 9 71.79 3.50 1 1 9 71.59 3.40 1 1 9 68.19 3.20 2 -1 9 140.29 4.80 2 1 9 139.19 4.70 -4 -2 9 4.80 1.60 -4 -2 9 6.90 1.50 -4 2 9 5.90 1.70 -4 2 9 8.70 1.70 -4 2 9 9.10 1.80 -3 -2 9 4.60 1.20 -3 -2 9 3.10 1.20 -3 -2 9 2.80 1.30 -3 2 9 4.30 1.30 -3 2 9 4.50 1.40 -3 2 9 6.10 1.20 -2 -2 9 28.10 2.40 -2 -2 9 29.20 2.20 -2 2 9 26.10 2.20 -2 2 9 28.10 2.30 -1 -2 9 4.50 1.20 -1 -2 9 2.60 1.00 -1 2 9 3.80 1.20 -1 2 9 2.70 1.10 0 -2 9 1.70 0.90 0 -2 9 1.00 0.90 0 2 9 2.50 1.00 0 2 9 0.50 0.80 1 -2 9 0.10 0.80 1 -2 9 0.60 0.90 1 2 9 0.40 0.90 1 2 9 0.30 0.80 2 -2 9 7.70 1.50 2 2 9 8.50 1.50 -4 -3 9 107.59 4.30 -4 -3 9 93.49 4.50 -4 3 9 91.49 4.40 -4 3 9 95.69 4.30 -3 -3 9 64.19 3.60 -3 -3 9 66.39 3.30 -3 3 9 64.09 3.00 -3 3 9 68.99 3.50 -3 3 9 67.89 3.50 -2 -3 9 71.39 3.10 -2 -3 9 72.59 3.60 -2 3 9 74.69 3.40 -2 3 9 72.89 3.40 -1 -3 9 118.19 4.00 -1 -3 9 118.59 4.50 -1 3 9 119.09 4.20 -1 3 9 110.29 4.20 0 -3 9 188.78 5.80 0 -3 9 182.98 5.30 0 3 9 173.98 5.40 0 3 9 176.78 5.30 1 -3 9 1.90 1.00 1 -3 9 2.40 1.00 1 3 9 0.00 0.90 1 3 9 3.30 1.10 2 -3 9 70.69 3.40 2 3 9 74.89 3.50 -4 -4 9 7.40 1.80 -4 -4 9 9.60 1.70 -4 4 9 9.90 1.90 -4 4 9 10.30 1.90 -3 -4 9 1.90 1.00 -3 -4 9 2.50 1.30 -3 4 9 5.40 1.50 -3 4 9 5.80 1.60 -3 4 9 3.20 1.30 -2 -4 9 1.20 0.90 -2 -4 9 1.70 1.10 -2 4 9 2.10 1.10 -2 4 9 1.20 1.00 -1 -4 9 5.40 1.30 -1 -4 9 5.00 1.10 -1 4 9 6.00 1.30 -1 4 9 5.20 1.20 0 -4 9 30.30 2.20 0 -4 9 28.70 2.40 0 4 9 29.20 2.20 0 4 9 27.10 2.20 1 -4 9 7.40 1.50 1 -4 9 7.60 1.40 1 4 9 6.90 1.40 1 4 9 10.80 1.60 2 -4 9 17.70 2.00 2 4 9 21.10 2.10 -3 -5 9 35.40 2.70 -3 -5 9 33.70 2.50 -3 5 9 32.70 2.70 -3 5 9 31.60 2.50 -2 -5 9 58.79 3.30 -2 -5 9 60.59 3.00 -2 5 9 54.79 3.10 -2 5 9 58.49 3.00 -1 -5 9 67.09 3.40 -1 -5 9 73.49 3.10 -1 5 9 67.49 3.30 -1 5 9 66.79 3.20 0 -5 9 231.88 6.10 0 -5 9 233.68 6.70 0 5 9 239.38 6.40 0 5 9 232.58 6.30 1 -5 9 19.00 2.20 1 -5 9 14.20 1.80 1 5 9 18.30 2.00 1 5 9 22.20 2.10 2 -5 9 71.39 3.40 2 5 9 71.19 3.30 -3 -6 9 25.70 2.50 -3 -6 9 20.30 2.30 -3 6 9 19.70 2.40 -3 6 9 18.60 2.20 -2 -6 9 28.50 2.20 -2 -6 9 26.60 2.40 -2 6 9 27.20 2.30 -2 6 9 28.90 2.50 -1 -6 9 26.80 2.30 -1 -6 9 32.30 2.10 -1 6 9 32.80 2.40 -1 6 9 29.30 2.20 0 -6 9 33.10 2.30 0 -6 9 40.80 2.70 0 6 9 37.20 2.50 0 6 9 34.40 2.30 1 -6 9 3.10 1.10 -1 -6 -9 4.90 1.30 1 -6 9 4.80 1.30 1 6 9 4.30 1.20 1 6 9 5.60 1.30 -2 -6 -9 2.60 1.10 2 -6 9 1.70 1.00 2 6 9 1.60 1.00 -3 -7 9 51.89 3.30 -3 -7 9 52.79 3.10 -3 7 9 49.00 3.00 -3 7 9 52.39 3.40 -2 -7 9 44.70 2.70 -2 -7 9 39.20 2.80 -2 7 9 42.10 2.70 -2 7 9 39.00 2.80 -1 -7 9 16.60 2.10 -1 7 9 17.70 2.80 -1 7 9 17.20 2.00 0 -7 -9 146.09 4.80 0 -7 9 147.19 4.70 0 -7 9 140.39 5.10 0 7 9 145.39 4.80 -1 -7 -9 49.40 2.80 1 -7 9 54.99 3.10 1 -7 9 50.89 2.80 1 7 9 53.69 2.90 -3 -8 9 -0.50 1.10 -3 -8 9 -0.40 1.00 -3 8 9 -0.60 1.40 -2 -8 9 13.50 1.90 -2 -8 9 13.50 1.80 -2 8 9 13.80 2.00 -1 -8 9 1.50 0.80 -1 -8 9 0.30 0.90 -1 8 9 -0.20 1.00 0 -8 9 1.10 1.00 0 -8 -9 0.60 1.00 0 -8 9 0.60 0.90 0 8 9 0.10 0.90 -1 -8 -9 3.90 1.20 1 -8 9 3.50 1.20 1 -8 9 3.80 1.10 1 8 9 3.50 1.20 -2 -9 9 58.79 3.30 -2 -9 9 56.29 3.10 -2 9 9 54.69 3.40 1 -9 -9 15.60 2.00 -1 -9 9 14.50 1.90 -1 -9 9 13.80 1.70 -1 9 9 12.40 1.90 0 -9 -9 131.59 4.70 0 -9 9 128.79 4.80 0 9 9 128.09 4.60 -1 -10 9 1.60 0.90 -1 -10 9 1.00 0.90 1 -10 -9 0.80 1.00 -1 10 9 1.60 1.20 0 -10 9 27.90 2.40 0 -10 -9 25.20 2.70 0 10 9 27.10 2.40 -2 0 10 92.39 3.90 -2 0 10 87.79 4.20 -1 0 10 27.50 2.30 -1 0 10 31.10 2.60 0 0 10 20.90 2.40 0 0 10 14.70 1.90 1 0 10 252.87 7.50 1 0 10 257.17 8.30 -2 -1 10 0.80 1.00 -2 -1 10 0.50 1.00 -2 1 10 0.50 1.10 -2 1 10 0.80 1.00 -1 -1 10 10.30 1.60 -1 -1 10 9.70 1.80 -1 1 10 9.10 1.70 -1 1 10 9.30 1.60 0 -1 10 13.80 2.00 0 -1 10 22.40 2.20 0 1 10 16.40 1.90 0 1 10 18.70 2.20 -2 -2 10 81.19 3.60 -2 -2 10 86.19 4.10 -2 2 10 83.69 3.80 -2 2 10 77.99 3.90 -1 -2 10 19.20 2.30 -1 -2 10 15.50 1.90 -1 2 10 19.00 2.20 -1 2 10 14.70 1.90 0 -2 10 39.50 2.60 0 -2 10 38.90 2.90 0 2 10 38.90 2.80 0 2 10 36.20 2.60 -2 -3 10 4.90 1.30 -2 -3 10 4.80 1.40 -2 3 10 5.10 1.40 -2 3 10 4.00 1.30 -1 -3 10 3.70 1.20 -1 -3 10 4.40 1.40 -1 3 10 4.50 1.30 -1 3 10 6.70 1.50 0 -3 10 0.90 1.00 0 -3 10 1.20 1.00 0 3 10 0.50 1.00 0 3 10 1.10 1.00 -2 -4 10 40.60 3.20 -2 -4 10 38.50 3.40 -2 -4 10 43.80 3.00 -2 4 10 37.30 2.80 -2 4 10 44.40 2.90 -1 -4 10 91.69 4.30 -1 -4 10 86.79 3.80 -1 4 10 90.39 4.00 -1 4 10 98.89 4.10 0 -4 10 25.50 2.20 0 -4 10 24.30 2.70 0 4 10 18.00 2.10 0 4 10 21.80 2.20 -1 -5 10 3.40 1.30 -1 -5 10 3.70 1.20 -1 5 10 1.70 1.20 -1 5 10 2.70 1.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23565 _shelx_res_file ; rkdd349_0m_a.res created by SHELXL-2014/7 TITL rkdd349_0m_a.res in P2(1)/c REM Old TITL rkdd349_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.056, Rweak 0.002, Alpha 0.055, Orientation as input REM Formula found by SHELXT: C4 O10 Cu CELL 0.71073 4.8564 13.5188 6.7205 90.000 96.992 90.000 ZERR 2.000 0.0002 0.0005 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O CU N UNIT 8 16 16 2 4 TEMP -173.170 SIZE 0.278 0.278 0.434 L.S. 10 BOND $H CONF ACTA EQIV $1 -x+1, -y+1, -z+1 HTAB N1 O1_$1 EQIV $2 x, -y+3/2, z+1/2 HTAB N1 O4_$2 EQIV $3 x+1, -y+3/2, z+1/2 HTAB N1 O2_$3 EQIV $4 -x+2, -y+1, -z+1 HTAB N1 O3_$4 HTAB N1 O3 HTAB N1 O4 LIST 4 FMAP 2 PLAN 10 WGHT 0.026300 0.197100 FVAR 0.61973 CU1 4 0.000000 0.500000 0.000000 10.50000 0.00454 0.00426 = 0.01054 0.00048 -0.00113 -0.00002 O1 3 0.326145 0.447795 0.158852 11.00000 0.00649 0.00626 = 0.01059 0.00078 -0.00105 0.00025 O2 3 0.154368 0.628337 0.073374 11.00000 0.00680 0.00596 = 0.01532 -0.00018 -0.00258 0.00045 O3 3 0.723924 0.502530 0.326215 11.00000 0.00836 0.00993 = 0.01359 -0.00054 -0.00329 0.00114 O4 3 0.529484 0.693883 0.250659 11.00000 0.01252 0.00750 = 0.01605 -0.00138 -0.00347 -0.00163 C1 1 0.493027 0.515729 0.230638 11.00000 0.00710 0.00640 = 0.00806 0.00035 0.00129 0.00071 C2 1 0.390722 0.623081 0.183430 11.00000 0.00744 0.00703 = 0.00940 0.00000 0.00052 0.00090 N1 5 0.951318 0.673946 0.578545 11.00000 0.00995 0.00753 = 0.01102 0.00039 -0.00070 -0.00166 H1 2 0.840089 0.672251 0.661851 11.00000 0.02042 H2 2 1.027438 0.731869 0.581531 11.00000 0.01871 H3 2 1.071969 0.628529 0.607098 11.00000 0.02331 H4 2 0.849298 0.664326 0.467695 11.00000 0.02930 HKLF 4 REM rkdd349_0m_a.res in P2(1)/c REM R1 = 0.0179 for 1537 Fo > 4sig(Fo) and 0.0204 for all 1672 data REM 86 parameters refined using 0 restraints END WGHT 0.0263 0.1971 REM Highest difference peak 0.370, deepest hole -0.513, 1-sigma level 0.096 Q1 1 0.4338 0.5689 0.2035 11.00000 0.05 0.37 Q2 1 0.2686 0.6297 0.1350 11.00000 0.05 0.29 Q3 1 0.4817 0.6600 0.2042 11.00000 0.05 0.25 Q4 1 0.4184 0.7116 0.4975 11.00000 0.05 0.24 Q5 1 0.1499 0.6714 -0.1514 11.00000 0.05 0.23 Q6 1 0.3451 0.7396 0.4220 11.00000 0.05 0.22 Q7 1 0.7451 0.6874 0.1779 11.00000 0.05 0.21 Q8 1 0.4854 0.7303 -0.0076 11.00000 0.05 0.21 Q9 1 0.2381 0.4622 0.1265 11.00000 0.05 0.21 Q10 1 0.6132 0.5055 0.2737 11.00000 0.05 0.21 ; _shelx_res_checksum 66019 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Cu Cu1 0 0.5 0 0.00661(5) Uani d 1 O O1 0.32614(14) 0.44779(5) 0.15885(10) 0.00795(12) Uani d 1 O O2 0.15437(14) 0.62834(5) 0.07337(11) 0.00968(13) Uani d 1 O O3 0.72392(16) 0.50253(5) 0.32622(12) 0.01101(14) Uani d 1 O O4 0.52948(15) 0.69388(5) 0.25066(12) 0.01245(14) Uani d 1 C C1 0.4930(2) 0.51573(7) 0.23064(14) 0.00716(15) Uani d 1 C C2 0.39072(19) 0.62308(7) 0.18343(14) 0.00800(15) Uani d 1 N N1 0.95132(18) 0.67395(6) 0.57854(13) 0.00966(14) Uani d 1 H H1 0.840(3) 0.6723(13) 0.662(3) 0.020(4) Uiso d 1 H H2 1.027(3) 0.7319(13) 0.582(3) 0.019(4) Uiso d 1 H H3 1.072(4) 0.6285(14) 0.607(3) 0.023(4) Uiso d 1 H H4 0.849(4) 0.6643(14) 0.468(3) 0.029(5) Uiso d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.00454(8) 0.00426(8) 0.01054(8) -0.00002(5) -0.00113(5) 0.00048(5) O1 0.0065(3) 0.0063(3) 0.0106(3) 0.0002(2) -0.0011(2) 0.0008(2) O2 0.0068(3) 0.0060(3) 0.0153(3) 0.0005(2) -0.0026(2) -0.0002(2) O3 0.0084(3) 0.0099(3) 0.0136(3) 0.0011(2) -0.0033(2) -0.0005(2) O4 0.0125(3) 0.0075(3) 0.0160(3) -0.0016(2) -0.0035(2) -0.0014(2) C1 0.0071(3) 0.0064(3) 0.0081(3) 0.0007(3) 0.0013(3) 0.0003(3) C2 0.0074(3) 0.0070(4) 0.0094(3) 0.0009(3) 0.0005(3) 0.0000(3) N1 0.0100(3) 0.0075(3) 0.0110(3) -0.0017(3) -0.0007(3) 0.0004(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O2 Cu1 O2 3_565 . 180.00(4) O2 Cu1 O1 3_565 3_565 85.44(3) O2 Cu1 O1 . 3_565 94.56(3) O2 Cu1 O1 3_565 . 94.57(3) O2 Cu1 O1 . . 85.43(3) O1 Cu1 O1 3_565 . 180.0 C1 O1 Cu1 . . 112.64(6) C2 O2 Cu1 . . 112.83(6) O3 C1 O1 . . 125.83(9) O3 C1 C2 . . 119.23(8) O1 C1 C2 . . 114.91(8) O4 C2 O2 . . 125.44(9) O4 C2 C1 . . 120.44(8) O2 C2 C1 . . 114.12(8) H1 N1 H2 . . 108.8(16) H1 N1 H3 . . 108.4(16) H2 N1 H3 . . 111.5(16) H1 N1 H4 . . 103.3(16) H2 N1 H4 . . 111.1(16) H3 N1 H4 . . 113.3(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cu1 O2 3_565 1.9301(7) Cu1 O2 . 1.9301(7) Cu1 O1 3_565 1.9326(7) Cu1 O1 . 1.9326(7) O1 C1 . 1.2798(11) O2 C2 . 1.2895(12) O3 C1 . 1.2355(12) O4 C2 . 1.2249(12) C1 C2 . 1.5541(13) N1 H1 . 0.824(17) N1 H2 . 0.865(18) N1 H3 . 0.854(19) N1 H4 . 0.85(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O1 3_666 0.824(17) 2.230(17) 2.8667(11) 134.2(16) yes N1 H1 O4 4_576 0.824(17) 2.475(17) 3.0503(12) 127.8(15) yes N1 H2 O2 4_676 0.865(18) 1.991(18) 2.8507(11) 172.5(16) yes N1 H3 O3 3_766 0.854(19) 2.053(19) 2.8884(11) 165.7(17) yes N1 H4 O3 . 0.85(2) 2.43(2) 3.0015(11) 124.7(16) yes N1 H4 O4 . 0.85(2) 2.04(2) 2.8330(12) 155.1(18) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion Cu1 O1 C1 O3 -175.08(8) Cu1 O1 C1 C2 2.83(9) Cu1 O2 C2 O4 -179.39(8) Cu1 O2 C2 C1 -0.18(10) O3 C1 C2 O4 -4.51(14) O1 C1 C2 O4 177.43(9) O3 C1 C2 O2 176.24(9) O1 C1 C2 O2 -1.82(12) _cod_database_fobs_code 2241944