#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000010.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_4000010 _journal_name_full 'Chemistry of Materials' _journal_year 2000 _chemical_formula_moiety 'Mn O18 V6, 2(C2 H10 N2)' _chemical_formula_sum 'C4 H20 Mn N4 O18 V6' _chemical_formula_weight 772.82 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' 'N' 'N' 0.0061 0.0033 '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' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.074(1) _cell_length_b 8.522(1) _cell_length_c 8.794(1) _cell_angle_alpha 77.83(1) _cell_angle_beta 63.44(1) _cell_angle_gamma 83.60(2) _cell_volume 528.96(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 379 _exptl_absorpt_coefficient_mu 3.203 _exptl_absorpt_correction_type 'empirical via \y scans' _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 2141 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.01 _reflns_number_total 1990 _reflns_number_gt 1824 _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^)+(0.0854P)^2^+0.1956P] 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 1990 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.003 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 0.5000 0.5000 0.0136(2) Uani 1 2 d S . . V2 V 0.52187(7) 0.21668(6) 0.24830(7) 0.0149(2) Uani 1 1 d . . . V3 V 0.32477(7) 0.27860(6) -0.02907(7) 0.01427(19) Uani 1 1 d . . . V4 V -0.08812(7) 0.29001(6) 0.25839(7) 0.01388(19) Uani 1 1 d . . . O1 O 0.4155(4) 0.3313(3) 0.4009(3) 0.0214(5) Uani 1 1 d . . . O2 O 0.4434(4) 0.0377(3) 0.3376(4) 0.0263(6) Uani 1 1 d . . . O3 O 0.2728(4) 0.0913(3) -0.0035(4) 0.0284(6) Uani 1 1 d . . . O4 O -0.0236(4) 0.1340(3) 0.3673(3) 0.0223(5) Uani 1 1 d . . . O5 O 0.4243(4) 0.3485(3) 0.7588(3) 0.0218(5) Uani 1 1 d . . . O6 O 0.2158(3) 0.5884(3) 0.6048(3) 0.0201(5) Uani 1 1 d . . . O7 O 0.7662(3) 0.2140(3) 0.1863(3) 0.0222(5) Uani 1 1 d . . . O8 O 0.4828(4) 0.2888(3) 0.0604(3) 0.0271(6) Uani 1 1 d . . . O9 O 0.1142(3) 0.3866(3) 0.0826(3) 0.0213(5) Uani 1 1 d . . . N1 N -0.2219(4) 0.1632(4) 0.7137(4) 0.0202(6) Uani 1 1 d . . . H1A H -0.3276 0.2043 0.7094 0.024 Uiso 1 1 d R . . H1B H -0.2483 0.0863 0.8083 0.024 Uiso 1 1 d R . . H1C H -0.1531 0.1182 0.6200 0.024 Uiso 1 1 d R . . C1 C -0.1155(5) 0.2914(4) 0.7188(5) 0.0233(7) Uani 1 1 d . . . H1D H -0.2011 0.3676 0.7854 0.028 Uiso 1 1 calc R . . H1E H -0.0452 0.3484 0.6022 0.028 Uiso 1 1 calc R . . N2 N 0.1770(4) 0.1362(4) 0.6872(4) 0.0227(6) Uani 1 1 d . . . H2A H 0.2421 0.0856 0.7444 0.027 Uiso 1 1 d R . . H2B H 0.2524 0.2010 0.5908 0.027 Uiso 1 1 d R . . H2C H 0.1344 0.0616 0.6554 0.027 Uiso 1 1 d R . . C2 C 0.0150(5) 0.2255(4) 0.7978(5) 0.0226(7) Uani 1 1 d . . . H2D H 0.0588 0.3139 0.8230 0.027 Uiso 1 1 calc R . . H2E H -0.0528 0.1547 0.9065 0.027 Uiso 1 1 calc R . . 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 0.0136(4) 0.0151(3) 0.0149(4) -0.0029(3) -0.0088(3) 0.0007(3) V2 0.0134(3) 0.0200(3) 0.0157(3) -0.0042(2) -0.0097(2) -0.0008(2) V3 0.0133(3) 0.0174(3) 0.0140(3) -0.0001(2) -0.0089(2) 0.0000(2) V4 0.0115(3) 0.0171(3) 0.0160(3) -0.0035(2) -0.0087(2) 0.0010(2) O1 0.0186(12) 0.0234(12) 0.0259(13) -0.0081(10) -0.0113(10) -0.0016(10) O2 0.0302(15) 0.0221(12) 0.0310(14) -0.0060(10) -0.0159(12) -0.0038(10) O3 0.0379(16) 0.0214(12) 0.0258(13) -0.0001(10) -0.0147(12) -0.0049(11) O4 0.0240(13) 0.0206(11) 0.0235(12) -0.0030(9) -0.0131(11) 0.0052(10) O5 0.0178(12) 0.0287(12) 0.0188(12) 0.0037(9) -0.0108(10) -0.0031(10) O6 0.0149(12) 0.0234(12) 0.0270(13) -0.0088(10) -0.0125(10) 0.0040(9) O7 0.0166(12) 0.0321(13) 0.0228(12) -0.0105(10) -0.0108(10) 0.0013(10) O8 0.0210(13) 0.0443(15) 0.0222(13) -0.0007(11) -0.0168(11) -0.0025(11) O9 0.0162(12) 0.0223(11) 0.0243(12) -0.0013(9) -0.0092(10) -0.0002(9) N1 0.0168(14) 0.0287(15) 0.0195(14) -0.0060(12) -0.0114(12) 0.0004(12) C1 0.0244(19) 0.0202(16) 0.0301(19) -0.0042(14) -0.0159(16) -0.0015(14) N2 0.0223(16) 0.0240(15) 0.0244(15) -0.0030(12) -0.0129(13) -0.0007(12) C2 0.0205(18) 0.0275(18) 0.0252(18) -0.0061(14) -0.0133(15) -0.0037(14) _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.983 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.160