#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000201.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000201 _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_name_systematic ; poly[diaqua-(mu2-squarato-O,O')-(mu2-4,4`-bipyridine-N,N')-manganese(II)] trihyd ; _chemical_formula_sum 'C14 H18 Mn N2 O9' _chemical_formula_weight 413.24 _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.7156(12) _cell_length_b 11.5444(8) _cell_length_c 8.1738(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.536(7) _cell_angle_gamma 90.00 _cell_volume 1766.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE Imaging Plate Diffraction system' _diffrn_measurement_method 'Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 14775 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 28.06 _reflns_number_total 4026 _reflns_number_gt 3254 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.8945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4026 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 1.0000 0.5000 0.01156(10) Uani 1 2 d S . . O1 O 0.45493(5) 0.96761(9) 0.74207(13) 0.0160(2) Uani 1 1 d . . . C1 C 0.48024(7) 0.98554(11) 0.88266(18) 0.0130(3) Uani 1 1 d . . . C2 C 0.53285(7) 1.06545(11) 0.95589(17) 0.0131(3) Uani 1 1 d . . . O2 O 0.57158(6) 1.14562(9) 0.90344(13) 0.0165(2) Uani 1 1 d . . . O5 O 0.55004(6) 1.15872(9) 0.58138(15) 0.0193(2) Uani 1 1 d . . . H1 H 0.5660(15) 1.219(2) 0.529(3) 0.042(7) Uiso 1 1 d . . . H2 H 0.5626(13) 1.165(2) 0.682(4) 0.035(6) Uiso 1 1 d . . . Mn2 Mn 1.0000 0.5000 1.0000 0.01162(10) Uani 1 2 d S . . O3 O 1.03731(6) 0.54620(9) 0.75958(13) 0.0178(2) Uani 1 1 d . . . C3 C 1.01624(8) 0.51998(12) 0.61806(18) 0.0140(3) Uani 1 1 d . . . C4 C 1.03109(7) 0.56741(12) 0.45600(17) 0.0141(3) Uani 1 1 d . . . O4 O 1.06808(6) 0.65017(9) 0.40434(13) 0.0182(2) Uani 1 1 d . . . O6 O 1.04762(6) 0.65836(9) 1.08483(14) 0.0182(2) Uani 1 1 d . . . H3 H 1.0651(13) 0.718(2) 1.032(3) 0.029(5) Uiso 1 1 d . . . H4 H 1.0594(14) 0.671(2) 1.184(4) 0.036(6) Uiso 1 1 d . . . N1 N 0.59884(7) 0.90567(11) 0.59970(16) 0.0163(2) Uani 1 1 d . . . C11 C 0.71565(7) 0.78515(12) 0.73507(18) 0.0163(3) Uani 1 1 d . . . C12 C 0.64898(8) 0.73238(13) 0.7168(2) 0.0207(3) Uani 1 1 d . . . H12 H 0.6422 0.6542 0.7496 0.025 Uiso 1 1 calc R . . C13 C 0.59274(8) 0.79516(13) 0.6504(2) 0.0200(3) Uani 1 1 d . . . H13 H 0.5475 0.7584 0.6400 0.024 Uiso 1 1 calc R . . C14 C 0.66260(8) 0.95658(12) 0.6189(2) 0.0191(3) Uani 1 1 d . . . H14 H 0.6678 1.0348 0.5849 0.023 Uiso 1 1 calc R . . C15 C 0.72177(8) 0.90032(13) 0.6862(2) 0.0194(3) Uani 1 1 d . . . H15 H 0.7659 0.9401 0.6988 0.023 Uiso 1 1 calc R . . N2 N 0.89557(6) 0.59699(11) 0.92993(16) 0.0176(3) Uani 1 1 d . . . C21 C 0.77776(7) 0.72087(12) 0.80327(18) 0.0161(3) Uani 1 1 d . . . C22 C 0.83283(8) 0.77667(13) 0.8883(2) 0.0198(3) Uani 1 1 d . . . H22 H 0.8314 0.8581 0.9044 0.024 Uiso 1 1 calc R . . C23 C 0.88961(8) 0.71247(13) 0.9491(2) 0.0205(3) Uani 1 1 d . . . H23 H 0.9264 0.7520 1.0076 0.025 Uiso 1 1 calc R . . C24 C 0.84224(8) 0.54346(13) 0.8492(2) 0.0195(3) Uani 1 1 d . . . H24 H 0.8450 0.4619 0.8357 0.023 Uiso 1 1 calc R . . C25 C 0.78322(8) 0.60105(13) 0.7845(2) 0.0195(3) Uani 1 1 d . . . H25 H 0.7469 0.5592 0.7279 0.023 Uiso 1 1 calc R . . O7 O 0.68427(7) 0.36861(12) 0.73740(18) 0.0296(3) Uani 1 1 d . . . H5 H 0.6427(17) 0.381(3) 0.743(4) 0.047(8) Uiso 1 1 d . . . H6 H 0.706(3) 0.332(4) 0.815(6) 0.117(17) Uiso 1 1 d . . . O8 O 0.75185(7) 0.25064(13) 0.48861(16) 0.0292(3) Uani 1 1 d . . . H7 H 0.783(4) 0.285(6) 0.409(8) 0.17(2) Uiso 1 1 d . . . H8 H 0.723(3) 0.291(5) 0.580(7) 0.136(19) Uiso 1 1 d . . . O9 O 0.82028(7) 0.13145(13) 0.74035(18) 0.0302(3) Uani 1 1 d . . . H9 H 0.8639(17) 0.120(2) 0.740(3) 0.045(7) Uiso 1 1 d . . . H10 H 0.803(3) 0.168(5) 0.676(6) 0.119(18) Uiso 1 1 d . . . 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 Mn1 0.01452(16) 0.01083(15) 0.00930(17) 0.00098(9) -0.00137(10) 0.00131(9) O1 0.0186(5) 0.0197(5) 0.0097(5) -0.0009(4) -0.0006(4) -0.0033(4) C1 0.0157(6) 0.0115(6) 0.0118(7) -0.0005(4) 0.0002(5) 0.0016(5) C2 0.0162(6) 0.0119(6) 0.0112(7) -0.0011(4) -0.0005(5) 0.0013(5) O2 0.0229(5) 0.0138(5) 0.0127(5) 0.0002(4) 0.0003(4) -0.0051(4) O5 0.0313(6) 0.0134(5) 0.0131(6) 0.0016(4) -0.0053(4) -0.0036(4) Mn2 0.01468(16) 0.01136(15) 0.00881(17) 0.00097(9) -0.00106(10) 0.00066(9) O3 0.0235(5) 0.0205(5) 0.0095(5) -0.0007(4) -0.0004(4) -0.0064(4) C3 0.0177(6) 0.0132(6) 0.0112(7) -0.0004(5) -0.0001(5) -0.0003(5) C4 0.0203(6) 0.0117(6) 0.0102(7) -0.0003(4) 0.0001(5) 0.0002(5) O4 0.0279(5) 0.0142(5) 0.0125(5) 0.0000(4) 0.0011(4) -0.0075(4) O6 0.0287(6) 0.0134(5) 0.0124(6) 0.0014(4) -0.0045(4) -0.0039(4) N1 0.0177(6) 0.0152(5) 0.0160(6) 0.0024(4) -0.0010(4) 0.0021(4) C11 0.0161(6) 0.0171(7) 0.0156(7) 0.0024(5) -0.0009(5) 0.0030(5) C12 0.0205(7) 0.0150(6) 0.0266(9) 0.0053(5) -0.0038(5) -0.0006(5) C13 0.0166(6) 0.0173(7) 0.0261(8) 0.0041(5) -0.0043(5) -0.0009(5) C14 0.0191(7) 0.0150(6) 0.0232(8) 0.0047(5) 0.0004(5) 0.0010(5) C15 0.0156(6) 0.0167(6) 0.0259(8) 0.0037(5) -0.0006(5) -0.0003(5) N2 0.0171(6) 0.0168(6) 0.0189(7) 0.0023(4) -0.0007(4) 0.0024(4) C21 0.0141(6) 0.0171(7) 0.0172(7) 0.0034(5) 0.0001(5) 0.0024(5) C22 0.0187(7) 0.0148(6) 0.0259(8) 0.0002(5) -0.0029(5) 0.0018(5) C23 0.0190(7) 0.0184(7) 0.0242(8) -0.0005(5) -0.0048(5) 0.0010(5) C24 0.0208(7) 0.0158(7) 0.0219(8) 0.0010(5) -0.0031(5) 0.0025(5) C25 0.0185(7) 0.0177(7) 0.0222(8) 0.0004(5) -0.0042(5) 0.0012(5) O7 0.0231(6) 0.0349(7) 0.0309(7) 0.0010(5) -0.0010(5) 0.0069(5) O8 0.0256(6) 0.0386(7) 0.0233(7) -0.0016(5) -0.0018(5) 0.0003(5) O9 0.0221(6) 0.0354(7) 0.0331(8) 0.0031(5) -0.0002(5) 0.0030(5)