#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/38/2013843.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_2013843 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_volume 60 _journal_year 2004 _chemical_formula_iupac '[Cs2 Mg (C2 O4)2 (H2 O)4]' _chemical_formula_moiety 'C4 H8 Cs2 Mg O12' _chemical_formula_sum 'C4 H8 Cs2 Mg O12' _chemical_formula_weight 538.23 _chemical_name_common 'Dicaesium magnesium oxalate tetrahydrate' _chemical_name_systematic ; Tetraaquabis(\m-oxalato)magnesium(II)dicaesium(I) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 128.61(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.045(3) _cell_length_b 7.3680(10) _cell_length_c 13.588(3) _cell_measurement_reflns_used 2059 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.03 _cell_measurement_theta_min 2.04 _cell_volume 1333.5(7) _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 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 0.0090 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 3719 _diffrn_reflns_theta_full 29.97 _diffrn_reflns_theta_max 29.97 _diffrn_reflns_theta_min 3.16 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.569 _exptl_absorpt_correction_T_max 0.573 _exptl_absorpt_correction_T_min 0.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(HKL SCALEPACK; Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.681 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.680 _refine_diff_density_min -0.732 _refine_ls_extinction_coef 0.00120(11) _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 1.095 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 1935 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0182 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.009P)^2^+2.37P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0395 _reflns_number_gt 1773 _reflns_number_total 1935 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1664.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2013843 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Cs 0.152825(10) 0.316641(18) 0.107435(12) 0.03296(6) Uani d . 1 . . Cs Mg 0.0000 0.33317(11) 0.2500 0.02091(18) Uani d S 1 . . Mg C1 0.12842(14) 0.1839(3) 0.49764(18) 0.0241(4) Uani d . 1 . . C C2 0.15869(13) 0.0878(2) 0.42361(18) 0.0233(4) Uani d . 1 . . C O1 0.06078(11) 0.30331(18) 0.43747(13) 0.0269(3) Uani d . 1 . . O O2 0.17076(12) 0.1346(3) 0.60756(14) 0.0400(4) Uani d . 1 . . O O3 0.22516(12) -0.0283(2) 0.47684(15) 0.0377(4) Uani d . 1 . . O O4 0.10857(11) 0.13669(19) 0.30969(13) 0.0273(3) Uani d . 1 . . O OW5 0.09999(13) 0.5245(2) 0.28078(17) 0.0355(4) Uani d . 1 . . O OW6 -0.03594(13) 0.1615(2) -0.15258(16) 0.0343(3) Uani d . 1 . . O H1 0.083(3) 0.628(5) 0.252(3) 0.056(9) Uiso d . 1 . . H H2 0.153(3) 0.529(5) 0.347(3) 0.069(11) Uiso d . 1 . . H H3 -0.077(2) 0.161(4) -0.137(3) 0.051(9) Uiso d . 1 . . H H4 -0.053(2) 0.083(4) -0.196(3) 0.042(8) 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 Cs 0.03167(9) 0.03670(9) 0.02957(9) -0.00206(5) 0.01865(7) -0.00134(5) Mg 0.0214(4) 0.0205(4) 0.0192(4) 0.000 0.0119(4) 0.000 C1 0.0212(9) 0.0290(9) 0.0204(9) -0.0024(7) 0.0122(8) -0.0027(7) C2 0.0205(8) 0.0238(8) 0.0231(9) -0.0010(7) 0.0125(7) -0.0013(7) O1 0.0286(7) 0.0295(7) 0.0231(7) 0.0049(5) 0.0164(6) -0.0004(5) O2 0.0354(8) 0.0587(10) 0.0221(7) 0.0106(8) 0.0160(7) 0.0084(7) O3 0.0315(8) 0.0420(9) 0.0309(8) 0.0158(7) 0.0152(7) 0.0046(7) O4 0.0309(7) 0.0277(7) 0.0230(7) 0.0052(6) 0.0167(6) 0.0011(5) OW5 0.0258(8) 0.0288(8) 0.0343(9) -0.0035(6) 0.0101(7) 0.0068(7) OW6 0.0405(9) 0.0304(8) 0.0340(9) -0.0048(7) 0.0242(8) -0.0055(7) 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 Cs O2 7_556 3.104(2) yes Cs O3 4 3.1486(16) yes Cs OW6 . 3.155(2) yes Cs O1 2 3.2962(16) yes Cs O1 6_565 3.3338(15) yes Cs O2 6 3.339(2) yes Cs OW5 . 3.3694(19) yes Cs O3 6 3.4514(18) yes Cs O4 . 3.5309(15) yes Mg OW5 2 2.0439(17) yes Mg OW5 . 2.0439(17) no Mg O4 2 2.0748(16) yes Mg O4 . 2.0748(16) no Mg O1 2 2.0778(16) yes Mg O1 . 2.0778(16) no C1 O2 . 1.240(2) yes C1 O1 . 1.263(2) yes C1 C2 . 1.558(3) yes C2 O3 . 1.231(2) yes C2 O4 . 1.267(2) yes OW5 H1 . 0.82(4) no OW5 H2 . 0.78(4) no OW6 H3 . 0.84(3) no OW6 H4 . 0.74(3) no 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 OW5 Mg OW5 . 2 92.77(11) no OW5 Mg O4 . 2 171.00(6) no OW5 Mg O4 2 2 88.56(7) no OW5 Mg O4 . . 88.56(7) no OW5 Mg O4 2 . 171.00(6) no O4 Mg O4 2 . 91.51(9) no OW5 Mg O1 . 2 92.18(7) no OW5 Mg O1 2 2 96.20(7) no O4 Mg O1 2 2 78.82(6) no O4 Mg O1 . 2 92.64(7) no OW5 Mg O1 . . 96.20(7) no OW5 Mg O1 2 . 92.18(7) no O4 Mg O1 2 . 92.64(7) no O4 Mg O1 . . 78.82(6) no O1 Mg O1 2 . 167.84(9) no O2 C1 O1 . . 126.41(19) yes O2 C1 C2 . . 117.79(17) yes O1 C1 C2 . . 115.78(16) yes O3 C2 O4 . . 125.94(18) yes O3 C2 C1 . . 119.39(17) yes O4 C2 C1 . . 114.65(16) yes Mg OW5 H1 . . 123(2) no Cs OW5 H1 . . 105(2) no Mg OW5 H2 . . 119(3) no Cs OW5 H2 . . 101(2) no H1 OW5 H2 . . 108(3) no Cs OW6 H3 . . 98(2) no Cs OW6 H4 . . 142(2) no H3 OW6 H4 . . 103(3) 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 OW5 H1 OW6 5_565 0.82(4) 1.88(4) 2.684(2) 166(3) yes OW5 H2 O3 7_556 0.78(4) 1.96(4) 2.735(3) 170(3) yes OW6 H3 O2 2 0.84(3) 1.89(3) 2.729(2) 174(3) yes OW6 H4 O4 5 0.74(3) 2.02(3) 2.760(2) 174(3) yes