#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000383.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_4000383 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C6 H7 Mn N9 O' _chemical_formula_weight 276.15 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/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 11.300(2) _cell_length_b 10.077(2) _cell_length_c 10.122(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.22(3) _cell_angle_gamma 90.00 _cell_volume 1088.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7212 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.47 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.886 _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_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method 'Oscillation' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7212 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2393 _reflns_number_gt 1570 _reflns_threshold_expression >2sigma(I) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.' MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381 USA.' for the Solution of Crystal Structure, University of Gottingen, Germany.' for the Solution of Crystal Structure, University of Gottingen, Germany.' for the Refinement of Crystal Structure, University of Gottingen, Germany.' 4.2 for MSDOS (1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.' for the refinement of Crystal Structure, University of Gottingen, Germany.' _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^)+(0.0237P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(13) _refine_ls_number_reflns 2393 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _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 Mn Mn 0.52693(3) 0.10839(3) 0.38266(3) 0.03141(9) Uani 1 1 d . . . O O 0.85526(13) -0.04321(15) 0.29784(18) 0.0587(5) Uani 1 1 d . . . N1 N 0.65081(14) -0.01951(15) 0.30472(18) 0.0370(4) Uani 1 1 d . . . H1 H 0.6241 -0.0935 0.2633 0.044 Uiso 1 1 calc R . . N2 N 0.71032(15) 0.22698(15) 0.40496(18) 0.0393(4) Uani 1 1 d . . . N3 N 0.95228(19) 0.3248(2) 0.4560(3) 0.0711(6) Uani 1 1 d . . . N4 N 0.61998(14) 0.02455(16) 0.59910(18) 0.0388(4) Uani 1 1 d . . . N5 N 0.73024(16) 0.00222(17) 0.63677(19) 0.0462(4) Uani 1 1 d . . . N6 N 0.83629(17) -0.0174(3) 0.6704(2) 0.0826(8) Uani 1 1 d . . . N7 N 0.41734(16) 0.17320(17) 0.17086(19) 0.0453(4) Uani 1 1 d . . . N8 N 0.44474(14) 0.19332(15) 0.07082(18) 0.0346(4) Uani 1 1 d . . . N9 N 0.46795(17) 0.21192(17) -0.03243(19) 0.0482(5) Uani 1 1 d . . . C1 C 0.8370(2) -0.1772(2) 0.2504(3) 0.0711(8) Uani 1 1 d . . . H1A H 0.9122 -0.2098 0.2374 0.107 Uiso 1 1 calc R . . H1B H 0.7692 -0.1813 0.1632 0.107 Uiso 1 1 calc R . . H1C H 0.8172 -0.2308 0.3187 0.107 Uiso 1 1 calc R . . C2 C 0.76103(18) 0.01965(19) 0.3230(2) 0.0386(5) Uani 1 1 d . . . C3 C 0.79984(18) 0.15478(19) 0.3794(2) 0.0388(5) Uani 1 1 d . . . C4 C 0.9195(2) 0.2033(2) 0.4054(3) 0.0560(6) Uani 1 1 d . . . H4 H 0.9791 0.1496 0.3870 0.067 Uiso 1 1 calc R . . C5 C 0.8623(2) 0.3965(2) 0.4791(3) 0.0707(8) Uani 1 1 d . . . H5 H 0.8809 0.4823 0.5136 0.085 Uiso 1 1 calc R . . C6 C 0.7420(2) 0.3487(2) 0.4538(3) 0.0554(6) Uani 1 1 d . . . H6 H 0.6823 0.4029 0.4715 0.066 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 Mn 0.03530(15) 0.03182(14) 0.03224(16) 0.00323(15) 0.01807(11) 0.00053(16) O 0.0444(8) 0.0520(9) 0.0922(14) -0.0185(9) 0.0395(9) -0.0032(8) N1 0.0374(9) 0.0330(9) 0.0446(11) -0.0096(8) 0.0188(8) -0.0055(8) N2 0.0460(9) 0.0319(9) 0.0478(11) -0.0009(8) 0.0257(8) -0.0055(8) N3 0.0592(12) 0.0578(13) 0.104(2) -0.0147(13) 0.0370(13) -0.0240(11) N4 0.0330(9) 0.0454(10) 0.0395(11) 0.0108(8) 0.0141(8) -0.0016(8) N5 0.0443(11) 0.0528(11) 0.0420(12) 0.0096(9) 0.0150(9) -0.0050(9) N6 0.0388(11) 0.115(2) 0.089(2) 0.0273(15) 0.0149(12) 0.0056(13) N7 0.0554(10) 0.0518(10) 0.0361(12) 0.0112(8) 0.0250(9) 0.0077(9) N8 0.0361(9) 0.0288(9) 0.0381(11) 0.0000(7) 0.0112(8) -0.0004(7) N9 0.0693(12) 0.0469(10) 0.0377(12) 0.0002(8) 0.0301(9) -0.0108(9) C1 0.0566(14) 0.0591(16) 0.108(2) -0.0252(16) 0.0419(15) 0.0016(13) C2 0.0389(11) 0.0413(12) 0.0420(13) -0.0009(9) 0.0217(10) -0.0010(10) C3 0.0405(10) 0.0353(10) 0.0466(14) 0.0022(9) 0.0222(10) -0.0067(9) C4 0.0471(12) 0.0494(14) 0.0789(19) -0.0064(12) 0.0309(12) -0.0121(11) C5 0.0775(17) 0.0462(13) 0.097(2) -0.0216(15) 0.0409(16) -0.0295(15) C6 0.0651(14) 0.0375(12) 0.0754(19) -0.0088(11) 0.0393(13) -0.0119(11)