#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/38/2013844.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_2013844 loop_ _publ_author_name 'Kolitsch, Uwe' _publ_section_title ; RbCr^III^(C~2~O~4~)~2~·2H~2~O, Cs~2~Mg(C~2~O~4~)~2~·4H~2~O and Rb~2~Cu^II^(C~2~O~4~)~2~·2H~2~O: three new complex oxalate hydrates ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m129 _journal_page_last m133 _journal_paper_doi 10.1107/S0108270104001945 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Rb2 Cu (C2 O4)2 (H2 O)2]' _chemical_formula_moiety 'C4 H4 Cu O10 Rb2' _chemical_formula_sum 'C4 H4 Cu O10 Rb2' _chemical_formula_weight 446.55 _chemical_name_common 'Dirubidium copper(II) oxalate dihydrate' _chemical_name_systematic ; Diaquabis(\m-oxalato)copper(II)dirubidium(I) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 108.05(3) _cell_angle_beta 97.69(3) _cell_angle_gamma 97.99(3) _cell_formula_units_Z 2 _cell_length_a 7.0000(10) _cell_length_b 8.949(2) _cell_length_c 8.982(2) _cell_measurement_reflns_used 2903 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.03 _cell_measurement_theta_min 2.04 _cell_volume 520.3(2) _computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor 1997)' _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_data_reduction 'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK' _computing_molecular_graphics 'ATOMS (Dowty, 1999) and ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\y and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5809 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.43 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.436 _exptl_absorpt_correction_T_max 0.449 _exptl_absorpt_correction_T_min 0.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(HKL SCALEPACK; Otwinowski & Minor, 1997)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.850 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 422 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.709 _refine_diff_density_min -0.804 _refine_ls_extinction_coef 0.0221(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 174 _refine_ls_number_reflns 3011 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0241 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.026P)^2^+0.24P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.0590 _reflns_number_gt 2641 _reflns_number_total 3011 _reflns_threshold_expression I>2\s(I) _cod_data_source_file sk1664.cif _cod_data_source_block III _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2013844 _cod_database_fobs_code 2013844 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Rb1 0.36833(4) 0.11883(3) 0.66573(2) 0.03173(8) Uani d . 1 . . Rb Rb2 0.25523(3) 0.55140(3) 0.63007(3) 0.03259(8) Uani d . 1 . . Rb Cu1 0.0000 0.0000 0.0000 0.02151(9) Uani d S 1 . . Cu Cu2 0.5000 0.5000 0.0000 0.02131(10) Uani d S 1 . . Cu C1 0.1311(3) 0.3660(2) 0.0004(2) 0.0194(4) Uani d . 1 . . C C2 0.2251(3) 0.4665(2) 0.1773(2) 0.0199(4) Uani d . 1 . . C C3 0.2628(3) 0.1559(3) 0.2745(2) 0.0238(4) Uani d . 1 . . C C4 0.0562(3) 0.1520(3) 0.3179(2) 0.0246(4) Uani d . 1 . . C O1 -0.0331(2) 0.2808(2) -0.03125(19) 0.0312(4) Uani d . 1 . . O O2 0.2361(2) 0.37932(19) -0.10198(17) 0.0239(3) Uani d . 1 . . O O3 0.1293(2) 0.4699(2) 0.28201(19) 0.0313(4) Uani d . 1 . . O O4 0.4047(2) 0.53626(19) 0.19850(17) 0.0238(3) Uani d . 1 . . O O5 0.4100(3) 0.2198(2) 0.3775(2) 0.0392(4) Uani d . 1 . . O O6 0.2631(2) 0.0892(2) 0.12515(17) 0.0260(3) Uani d . 1 . . O O7 0.0398(3) 0.2196(2) 0.45588(19) 0.0373(4) Uani d . 1 . . O O8 -0.0872(2) 0.0760(2) 0.20220(18) 0.0268(3) Uani d . 1 . . O OW9 0.5727(3) 0.2387(3) 0.0175(2) 0.0358(4) Uani d . 1 . . O OW10 0.7878(3) 0.1353(2) 0.6452(2) 0.0351(4) Uani d . 1 . . O H1 0.848(6) 0.171(4) 0.595(4) 0.054(11) Uiso d . 1 . . H H2 0.842(5) 0.180(4) 0.739(4) 0.053(10) Uiso d . 1 . . H H3 0.502(7) 0.175(5) 0.039(5) 0.075(14) Uiso d . 1 . . H H4 0.689(6) 0.219(5) 0.016(4) 0.065(11) Uiso d . 1 . . H 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 Rb1 0.03486(14) 0.03152(13) 0.02394(13) 0.00059(9) 0.00844(9) 0.00374(9) Rb2 0.02269(12) 0.03945(14) 0.03162(13) -0.00294(9) -0.00095(9) 0.01260(10) Cu1 0.01680(17) 0.0273(2) 0.01724(18) -0.00022(14) 0.00411(12) 0.00445(13) Cu2 0.01554(17) 0.0286(2) 0.01555(17) -0.00190(14) 0.00433(12) 0.00349(13) C1 0.0171(9) 0.0206(9) 0.0209(9) 0.0036(7) 0.0042(7) 0.0074(7) C2 0.0208(9) 0.0204(9) 0.0202(9) 0.0045(8) 0.0059(7) 0.0083(7) C3 0.0240(10) 0.0244(10) 0.0220(10) -0.0027(8) 0.0033(8) 0.0098(8) C4 0.0292(11) 0.0215(10) 0.0218(10) 0.0000(8) 0.0067(8) 0.0068(8) O1 0.0199(8) 0.0371(9) 0.0325(9) -0.0047(7) 0.0047(6) 0.0103(7) O2 0.0186(7) 0.0298(8) 0.0194(7) 0.0001(6) 0.0039(5) 0.0047(6) O3 0.0298(9) 0.0395(10) 0.0257(8) 0.0027(7) 0.0148(7) 0.0101(7) O4 0.0207(7) 0.0294(8) 0.0186(7) 0.0012(6) 0.0056(5) 0.0051(6) O5 0.0310(9) 0.0504(11) 0.0270(9) -0.0154(8) -0.0041(7) 0.0137(8) O6 0.0177(7) 0.0344(8) 0.0223(8) -0.0008(6) 0.0042(6) 0.0064(6) O7 0.0473(11) 0.0377(10) 0.0224(8) 0.0000(8) 0.0151(7) 0.0037(7) O8 0.0229(8) 0.0326(8) 0.0226(7) 0.0004(6) 0.0075(6) 0.0070(6) OW9 0.0298(10) 0.0414(11) 0.0443(11) 0.0130(8) 0.0152(8) 0.0195(8) OW10 0.0381(10) 0.0332(9) 0.0281(10) -0.0047(8) 0.0057(8) 0.0070(7) 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' Rb Rb -0.9393 2.9676 '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 _geom_angle_publ_flag O6 Cu1 O6 2 . 180.00(9) yes O6 Cu1 O8 2 . 94.73(7) yes O6 Cu1 O8 . . 85.27(7) yes O6 Cu1 O8 2 2 85.27(7) ? O6 Cu1 O8 . 2 94.73(7) ? O8 Cu1 O8 . 2 180.00(9) yes O6 Cu1 O1 2 2 90.62(7) yes O6 Cu1 O1 . 2 89.38(7) yes O8 Cu1 O1 . 2 92.83(7) yes O8 Cu1 O1 2 2 87.17(7) yes O6 Cu1 O1 2 . 89.38(7) ? O6 Cu1 O1 . . 90.62(7) ? O8 Cu1 O1 . . 87.17(7) ? O8 Cu1 O1 2 . 92.83(7) ? O1 Cu1 O1 2 . 180.00(7) ? O4 Cu2 O4 . 2_665 180.00(10) yes O4 Cu2 O2 . . 85.75(7) yes O4 Cu2 O2 2_665 . 94.25(7) yes O4 Cu2 O2 . 2_665 94.25(7) ? O4 Cu2 O2 2_665 2_665 85.75(7) ? O2 Cu2 O2 . 2_665 180.0 yes O4 Cu2 OW9 . . 88.69(7) yes O4 Cu2 OW9 2_665 . 91.31(7) yes O2 Cu2 OW9 . . 85.22(7) yes O2 Cu2 OW9 2_665 . 94.78(7) yes O4 Cu2 OW9 . 2_665 91.31(7) ? O4 Cu2 OW9 2_665 2_665 88.69(7) ? O2 Cu2 OW9 . 2_665 94.78(7) ? O2 Cu2 OW9 2_665 2_665 85.22(7) ? OW9 Cu2 OW9 . 2_665 180.0 ? O1 C1 O2 . . 124.87(19) no O1 C1 C2 . . 119.80(18) no O2 C1 C2 . . 115.33(17) no O3 C2 O4 . . 125.8(2) no O3 C2 C1 . . 119.68(19) no O4 C2 C1 . . 114.50(17) no O5 C3 O6 . . 124.8(2) no O5 C3 C4 . . 120.60(19) no O6 C3 C4 . . 114.56(18) no O7 C4 O8 . . 125.1(2) no O7 C4 C3 . . 119.5(2) no O8 C4 C3 . . 115.43(18) no H3 OW9 H4 . . 113(4) ? H1 OW10 H2 . . 107(4) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rb1 OW10 . 2.953(2) yes Rb1 OW10 2_656 2.954(2) yes Rb1 O2 1_556 2.9575(18) yes Rb1 O5 . 3.0304(19) yes Rb1 O8 2_556 3.0450(18) yes Rb1 O4 2_666 3.054(2) yes Rb1 OW9 1_556 3.073(2) yes Rb1 O7 . 3.181(2) yes Rb1 O5 2_656 3.533(2) yes Rb2 O3 2_566 2.9024(17) yes Rb2 O5 2_666 2.912(2) yes Rb2 O3 . 2.9586(19) yes Rb2 O7 . 2.964(2) yes Rb2 O4 2_666 2.9901(17) yes Rb2 OW9 2_666 3.109(2) yes Rb2 O2 1_556 3.2414(17) yes Rb2 O7 2_566 3.285(2) yes Rb2 O5 . 3.536(2) no Cu1 O6 2 1.9429(17) yes Cu1 O6 . 1.9429(17) no Cu1 O8 . 1.9444(16) yes Cu1 O8 2 1.9444(16) no Cu1 O1 2 2.6512(19) yes Cu1 O1 . 2.6512(19) no Cu2 O4 . 1.9363(15) yes Cu2 O4 2_665 1.9363(15) no Cu2 O2 . 1.9487(16) yes Cu2 O2 2_665 1.9487(16) no Cu2 OW9 . 2.508(2) yes Cu2 OW9 2_665 2.508(2) no C1 O1 . 1.232(3) no C1 O2 . 1.274(2) no C1 C2 . 1.561(3) no C2 O3 . 1.221(3) no C2 O4 . 1.285(3) no C3 O5 . 1.224(3) no C3 O6 . 1.289(3) no C3 C4 . 1.546(3) no C4 O7 . 1.228(3) no C4 O8 . 1.282(3) no OW9 H3 . 0.79(5) no OW9 H4 . 0.86(4) no OW10 H1 . 0.76(4) no OW10 H2 . 0.82(4) no 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 OW9 H3 O6 . 0.79(5) 2.08(5) 2.824(3) 156(4) yes OW9 H4 O1 1_655 0.86(4) 2.08(4) 2.843(3) 147(4) yes OW10 H1 O7 1_655 0.76(4) 2.05(4) 2.793(3) 166(4) yes OW10 H2 O1 1_656 0.82(4) 1.99(4) 2.817(3) 177(4) 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 _geom_torsion_publ_flag O1 C1 C2 O3 -5.7(3) no O2 C1 C2 O3 174.8(2) no O1 C1 C2 O4 172.38(19) no O2 C1 C2 O4 -7.1(3) no O5 C3 C4 O7 3.1(3) no O6 C3 C4 O7 -176.3(2) no O5 C3 C4 O8 -177.1(2) no O6 C3 C4 O8 3.5(3) no