# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name S.Lapidus A.C.McConnell P.W.Stephens J.S.Miller _publ_contact_author_name 'Joel S. Miller' _publ_contact_author_email jsmiller@chem.utah.edu data_ACM2001_glass _database_code_depnum_ccdc_archive 'CCDC 806337' #TrackingRef 'web_deposit_cif_file_0_SaulLapidus_1294115939.cif' # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C6 I Mn N4 O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 I Mn N4 O' _chemical_formula_weight 325.94 _exptl_crystal_density_diffrn 2.23380 #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2c 2n' _space_group_name_H-M_alt Pnam loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' 1 'x, y, z' 2 '-x, -y, z+1/2' 3 'x+1/2, -y+1/2, -z+1/2' 4 '-x+1/2, y+1/2, -z' 5 '-x, -y, -z' 6 'x, y, -z+1/2' 7 '-x+1/2, y+1/2, z+1/2' 8 'x+1/2, -y+1/2, z' _cell_length_a 12.71226(38) _cell_length_b 9.99610(30) _cell_length_c 7.62678(23) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 969.159(50) _cell_formula_units_Z 4 _cell_measurement_temperature 300 _cell_special_details ? # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? # include if applicable _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ? # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; X16C, National Synchrotron Light Source, Brookhaven National Laboratory ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; NIST standard reference material 1976(sintered plate of Al2O3) Well-isolated 7 reflections were used to calibrate wavelength and detector zero. ; _diffrn_ambient_temperature 300 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type synchrotron _diffrn_measurement_device_type 'Huber diffractometer' _diffrn_detector 'NaI scintillation counter' _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ? # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 0.699942 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7101 _pd_meas_2theta_range_min 4.5 _pd_meas_2theta_range_max 40.0 _pd_meas_2theta_range_inc 0.005 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Molecules are defined as rigid bodies using the z-matrix function implemented in TOPAS-Academic. The same isotropic displacement parameters are assigned to all atoms within a molecule. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=9999,Rs=330 in TOPAS-Academic ; _pd_proc_ls_background_function ; 1 Pearson-Voight peaks and Chebyshev polynomial with 7 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.04999 # 4.999(%) _pd_proc_ls_prof_wR_factor 0.06329 # 6.329(%) _pd_proc_ls_prof_wR_expected 0.04909 # 4.909(%) _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ? _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_extinction_coef ? _refine_ls_number_parameters 42 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.289 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.5 _pd_proc_2theta_range_max 40.0 _pd_proc_2theta_range_inc 0.005 _pd_proc_wavelength 0.699942 _pd_block_diffractogram_id ACM2001_glass # The id used for the block containing # the powder pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection SPEC _computing_cell_refinement TOPAS-Academic _computing_data_reduction TOPAS-Academic _computing_structure_solution TOPAS-Academic _computing_structure_refinement TOPAS-Academic _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv O1 O 4 0.32799(61) 0.50518(90) 0.25 1 1.22(24) Mn1 Mn 4 0.23137(18) 0.69412(25) 0.25 1 1.723(72) I1 I 4 0.11085(10) 0.93153(15) 0.25 1 4.128(47) C1 C 4 0.53342 0.85027 0.75 1 1.50(13) C2 C 4 0.43166 0.80557 0.75 1 1.50(13) C3 C 8 0.37492 0.78065 0.59477 1 1.50(13) C4 C 8 0.59015 0.87519 0.59477 1 1.50(13) N1 N 8 0.33505 0.76314 0.46297 1 1.50(13) N2 N 8 0.63006 0.89270 0.46297 1 1.50(13) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Mn1 2.8248(28) . . yes Mn1 O1 2.2529(91) . . yes Mn1 N1 2.203(18) . . yes Mn1 N1 2.203(18) . 6_555 yes Mn1 N2 2.248(11) . 3_465 yes Mn1 N2 2.248(11) . 8_465 yes N1 C3 1.1393(64) . . yes N2 C4 1.1393(64) . . yes C1 C2 1.368(20) . . yes C1 C4 1.4085(81) . . yes C1 C4 1.4085(81) . 6_556 yes C2 C3 1.4085(81) . . yes C2 C3 1.4085(81) . 6_556 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Mn1 O1 179.81(21) . . . yes I1 Mn1 N1 93.52(25) . . . yes I1 Mn1 N2 90.77(53) . . 3_465 yes I1 Mn1 N2 90.77(53) . . 8_465 yes I1 Mn1 N1 93.52(25) . . 6_555 yes O1 Mn1 N1 86.35(29) . . . yes O1 Mn1 N2 89.36(55) . . 3_465 yes O1 Mn1 N2 89.36(55) . . 8_465 yes O1 Mn1 N1 86.35(29) . . 6_555 yes N1 Mn1 N2 175.50(42) . . 3_465 yes N1 Mn1 N2 86.0(13) . . 8_465 yes N1 Mn1 N1 95.0(16) . . 6_555 yes N2 Mn1 N2 92.6(11) 3_465 . 8_465 yes N1 Mn1 N2 86.0(13) 6_555 . 3_465 yes N1 Mn1 N2 175.50(42) 6_555 . 8_465 yes Mn1 N1 C3 164.80(16) . . . yes Mn1 N2 C4 146.44(19) 3_565 . . yes C2 C1 C4 122.81(49) . . . yes C2 C1 C4 122.81(49) . . 6_556 yes C4 C1 C4 114.39(99) . . 6_556 yes C1 C2 C3 122.81(49) . . . yes C1 C2 C3 122.81(49) . . 6_556 yes C3 C2 C3 114.39(99) . . 6_556 yes N1 C3 C2 175.27(87) . . . yes N2 C4 C1 175.27(87) . . . yes