#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000008.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_4000008 _journal_name_full 'Chemistry of Materials' _journal_year 2000 _chemical_formula_moiety 'F Mn O9 V3, C2 H10 N2' _chemical_formula_sum 'C2 H10 F Mn N2 O9 V3' _chemical_formula_weight 432.88 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.805(3) _cell_length_b 7.485(1) _cell_length_c 21.038(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2331.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Bar _exptl_crystal_colour Orange-red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.467 _exptl_crystal_density_method ? _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 3.443 _exptl_absorpt_correction_type 'empirical via \y scans' _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.95 _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_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2115 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2043 _reflns_number_observed 1429 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2026 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_all 0.1351 _refine_ls_wR_factor_obs 0.1004 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 1.214 _refine_ls_restrained_S_obs 1.089 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.24791(7) 0.74356(12) 0.49035(4) 0.0120(2) Uani 1 d . . V1 V 0.34156(7) 0.55386(14) 0.73640(5) 0.0167(3) Uani 1 d . . V2 V 0.39023(6) 0.52105(13) 0.88926(4) 0.0108(2) Uani 1 d . . V3 V 0.38460(6) 0.50742(13) 0.59221(4) 0.0111(2) Uani 1 d . . F1 F 0.1888(2) 0.4925(5) 0.4941(2) 0.0202(7) Uani 1 d . . O1 O 0.3140(3) 0.6737(6) 0.5783(2) 0.0174(9) Uani 1 d . . O2 O 0.3689(3) 0.3479(6) 0.5397(2) 0.0174(9) Uani 1 d . . O3 O 0.3626(3) 0.4079(6) 0.6675(2) 0.0242(11) Uani 1 d . . O4 O 0.2338(3) 0.5879(7) 0.7443(2) 0.0327(12) Uani 1 d . . O5 O 0.3905(3) 0.7432(6) 0.7217(2) 0.0313(12) Uani 1 d . . O6 O 0.3873(3) 0.4555(6) 0.8088(2) 0.0250(10) Uani 1 d . . O7 O 0.3587(3) 0.3463(5) 0.9318(2) 0.0180(9) Uani 1 d . . O8 O 0.5015(3) 0.5877(6) 0.9093(2) 0.0197(10) Uani 1 d . . O9 O 0.3205(3) 0.6927(6) 0.9013(2) 0.0173(9) Uani 1 d . . N1 N 0.3774(3) 0.0237(7) 0.6258(3) 0.0215(12) Uani 1 d . . H1A H 0.3654(3) -0.0717(7) 0.6505(3) 0.026 Uiso 1 d R . H1B H 0.3426(3) 0.0209(7) 0.5908(3) 0.026 Uiso 1 d R . H1C H 0.3651(3) 0.1249(7) 0.6472(3) 0.026 Uiso 1 d R . N2 N 0.6305(3) 0.0351(7) 0.6483(3) 0.0213(12) Uani 1 d . . H2A H 0.6622(3) 0.0559(7) 0.6841(3) 0.026 Uiso 1 d R . H2B H 0.6415(3) 0.1212(7) 0.6195(3) 0.026 Uiso 1 d R . H2C H 0.6465(3) -0.0708(7) 0.6314(3) 0.026 Uiso 1 d R . C1 C 0.4750(4) 0.0197(8) 0.6073(3) 0.0170(13) Uani 1 d . . H1D H 0.4866(4) 0.1205(8) 0.5803(3) 0.020 Uiso 1 d R . H1E H 0.4898(4) -0.0872(8) 0.5844(3) 0.020 Uiso 1 d R . C2 C 0.5333(4) 0.0335(9) 0.6657(3) 0.0210(14) Uani 1 d . . H2D H 0.5197(4) 0.1423(9) 0.6879(3) 0.025 Uiso 1 d R . H2E H 0.5199(4) -0.0651(9) 0.6933(3) 0.025 Uiso 1 d 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 0.0131(4) 0.0116(4) 0.0113(4) 0.0001(4) 0.0002(4) 0.0008(3) V1 0.0175(5) 0.0215(5) 0.0112(5) 0.0004(4) -0.0001(4) 0.0002(4) V2 0.0093(4) 0.0137(5) 0.0096(5) 0.0011(4) 0.0004(3) 0.0007(4) V3 0.0094(4) 0.0135(5) 0.0104(5) 0.0006(4) -0.0016(3) 0.0003(4) F1 0.017(2) 0.013(2) 0.031(2) -0.001(2) 0.0050(14) 0.000(2) O1 0.013(2) 0.019(2) 0.020(2) 0.000(2) -0.006(2) 0.004(2) O2 0.021(2) 0.021(2) 0.011(2) -0.002(2) -0.004(2) -0.002(2) O3 0.033(3) 0.024(2) 0.015(2) 0.004(2) 0.002(2) 0.000(2) O4 0.023(2) 0.050(3) 0.025(3) 0.006(2) 0.003(2) 0.003(2) O5 0.032(3) 0.028(3) 0.034(3) 0.005(2) 0.002(2) -0.006(2) O6 0.034(2) 0.028(3) 0.014(2) -0.003(2) -0.005(2) 0.007(2) O7 0.019(2) 0.016(2) 0.019(2) 0.001(2) 0.005(2) -0.003(2) O8 0.014(2) 0.017(2) 0.028(3) -0.001(2) 0.000(2) 0.001(2) O9 0.012(2) 0.023(2) 0.017(2) 0.000(2) 0.004(2) 0.004(2) N1 0.016(3) 0.016(3) 0.033(3) 0.003(2) -0.007(2) -0.002(2) N2 0.023(3) 0.022(3) 0.019(3) 0.001(2) 0.000(2) -0.001(2) C1 0.018(3) 0.015(3) 0.018(3) 0.003(3) -0.002(2) 0.001(3) C2 0.017(3) 0.033(4) 0.013(3) -0.001(3) 0.005(2) 0.002(3) _refine_diff_density_max 0.600 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.146