# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Abrahams, Brendan F.' 'Elliott, Robert' 'Hudson, Timothy' _publ_contact_author_name 'Abrahams, Brendan F.' _publ_contact_author_email bfa@unimelb.edu.au _publ_section_title ; A new type of 3D [(MII)2(TCNQ-II)3]2- coordination network with spacious channels of hexagonal cross-section generated from TCNQH2 ; # Attachment '- rweb25e(dmso4)final.cif' data_rweb25e _database_code_depnum_ccdc_archive 'CCDC 842123' #TrackingRef '- rweb25e(dmso4)final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(DMSO)4(H2O)2][Mn2TCNQ3]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 Mn3 N12 O6 S4' _chemical_formula_weight 1125.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-31m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z' 'x, x-y, -z' '-x+y, y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z' '-x, -x+y, z' 'x-y, -y, z' _cell_length_a 13.0158(9) _cell_length_b 13.0158(9) _cell_length_c 10.8532(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1592.32(17) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min 3.9079 _cell_measurement_theta_max 72.8307 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.072 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 575 _exptl_absorpt_coefficient_mu 6.389 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 0.682 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0711 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3473 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 73.25 _reflns_number_total 1136 _reflns_number_gt 740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1982P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1136 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2809 _refine_ls_wR_factor_gt 0.2513 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _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 0.6667 0.3333 0.0000 0.0517(6) Uani 1 6 d S . . N1 N 0.5324(4) 0.3394(4) 0.1200(3) 0.0780(14) Uani 1 1 d . . . C1 C 0.4965(5) 0.3915(5) 0.1742(3) 0.0663(13) Uani 1 1 d . . . C2 C 0.4540(6) 0.4540(6) 0.2395(5) 0.0686(19) Uani 1 2 d S . . C3 C 0.4777(6) 0.4777(6) 0.3736(5) 0.0651(18) Uani 1 2 d S . . C4 C 0.4350(5) 0.5420(5) 0.4377(4) 0.0687(14) Uani 1 1 d . . . H4 H 0.3900 0.5702 0.3954 0.082 Uiso 1 1 calc R . . Mn2 Mn 0.0000 0.0000 0.0000 0.099(3) Uani 0.537(13) 12 d SP . . Mn3 Mn 0.0000 0.0000 0.2013(10) 0.078(3) Uani 0.231(6) 6 d SP . . 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 0.0659(8) 0.0659(8) 0.0232(7) 0.000 0.000 0.0329(4) N1 0.098(3) 0.117(4) 0.0346(18) -0.007(2) 0.0057(19) 0.066(3) C1 0.086(3) 0.098(4) 0.0289(18) 0.003(2) 0.0022(19) 0.056(3) C2 0.101(4) 0.101(4) 0.024(2) 0.000(2) 0.000(2) 0.065(4) C3 0.093(4) 0.093(4) 0.023(2) 0.004(2) 0.004(2) 0.056(4) C4 0.097(4) 0.097(4) 0.039(2) -0.003(2) -0.004(2) 0.069(3) Mn2 0.103(4) 0.103(4) 0.092(5) 0.000 0.000 0.0514(19) Mn3 0.064(4) 0.064(4) 0.107(8) 0.000 0.000 0.0319(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N1 2.212(4) 2_655 ? Mn1 N1 2.212(4) 6_655 ? Mn1 N1 2.212(4) 5 ? Mn1 N1 2.212(4) 3_665 ? Mn1 N1 2.212(4) 4_665 ? Mn1 N1 2.212(4) . ? N1 C1 1.158(6) . ? C1 C2 1.385(6) . ? C2 C1 1.385(6) 10 ? C2 C3 1.488(7) . ? C3 C4 1.400(5) . ? C3 C4 1.400(5) 10 ? C4 C4 1.386(9) 4_666 ? C4 H4 0.9500 . ? Mn2 Mn3 2.185(11) . ? Mn2 Mn3 2.185(11) 7 ? 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_3 _geom_angle_publ_flag N1 Mn1 N1 93.7(2) 2_655 6_655 ? N1 Mn1 N1 88.7(2) 2_655 5 ? N1 Mn1 N1 88.85(16) 6_655 5 ? N1 Mn1 N1 88.85(16) 2_655 3_665 ? N1 Mn1 N1 88.7(2) 6_655 3_665 ? N1 Mn1 N1 176.5(2) 5 3_665 ? N1 Mn1 N1 176.5(2) 2_655 4_665 ? N1 Mn1 N1 88.85(16) 6_655 4_665 ? N1 Mn1 N1 88.85(16) 5 4_665 ? N1 Mn1 N1 93.7(2) 3_665 4_665 ? N1 Mn1 N1 88.85(16) 2_655 . ? N1 Mn1 N1 176.5(2) 6_655 . ? N1 Mn1 N1 93.7(2) 5 . ? N1 Mn1 N1 88.85(16) 3_665 . ? N1 Mn1 N1 88.7(2) 4_665 . ? C1 N1 Mn1 151.3(4) . . ? N1 C1 C2 179.7(5) . . ? C1 C2 C1 117.3(5) 10 . ? C1 C2 C3 121.3(3) 10 . ? C1 C2 C3 121.3(3) . . ? C4 C3 C4 119.1(5) . 10 ? C4 C3 C2 120.5(3) . . ? C4 C3 C2 120.5(3) 10 . ? C4 C4 C3 120.5(3) 4_666 . ? C4 C4 H4 119.8 4_666 . ? C3 C4 H4 119.8 . . ? Mn3 Mn2 Mn3 180.0 . 7 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 73.25 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.892 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.098 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.008 778 175 ' ' _platon_squeeze_details ; ; # Attachment '- rweb44d(dmso4)final.cif' data_rweb44d _database_code_depnum_ccdc_archive 'CCDC 842124' #TrackingRef '- rweb44d(dmso4)final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cd(DMSO)4(H2O)2][Cd2TCNQ3]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 Cd3 N12 O6 S4' _chemical_formula_weight 1298.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-31m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-y, -x, -z' '-x+y, -x, z' 'x, x-y, -z' '-x+y, y, -z' '-x, -y, -z' 'y, -x+y, -z' 'y, x, z' 'x-y, x, -z' '-x, -x+y, z' 'x-y, -y, z' _cell_length_a 12.9515(4) _cell_length_b 12.9515(4) _cell_length_c 10.8818(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1580.78(7) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2124 _cell_measurement_theta_min 3.9379 _cell_measurement_theta_max 74.0393 _exptl_crystal_description 'hexagonal rod' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2689 _exptl_crystal_size_mid 0.0804 _exptl_crystal_size_min 0.0623 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 9.654 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_T_max 0.625 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3620 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 74.21 _reflns_number_total 1155 _reflns_number_gt 967 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0601P)^2^+0.4570P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1155 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _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 Cd1 Cd 0.3333 0.6667 0.5000 0.0759(3) Uani 1 6 d S . . N1 N 0.4820(4) 0.6740(4) 0.3758(3) 0.1079(13) Uani 1 1 d . . . C2 C 0.5581(4) 0.5581(4) 0.2564(3) 0.0777(12) Uani 1 2 d S . . C3 C 0.5287(4) 0.5287(4) 0.1258(3) 0.0761(12) Uani 1 2 d S . . C4 C 0.4614(4) 0.5663(4) 0.0615(3) 0.0876(10) Uani 1 1 d . . . H4 H 0.4334 0.6123 0.1027 0.105 Uiso 1 1 calc R . . C1 C 0.5156(4) 0.6217(4) 0.3220(3) 0.0874(10) Uani 1 1 d . . . Cd2 Cd 0.0000 0.0000 0.5000 0.0607(14) Uani 0.289(7) 12 d SP . . Cd3 Cd 0.0000 0.0000 0.3955(10) 0.252(4) Uani 0.355(3) 6 d SP . . 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 Cd1 0.1019(3) 0.1019(3) 0.0239(3) 0.000 0.000 0.05093(17) N1 0.131(3) 0.168(4) 0.0389(14) -0.0194(17) 0.0037(16) 0.085(3) C2 0.103(2) 0.103(2) 0.0264(16) 0.0046(15) 0.0046(15) 0.051(3) C3 0.099(2) 0.099(2) 0.0299(16) 0.0040(15) 0.0040(15) 0.049(3) C4 0.124(3) 0.122(3) 0.0386(15) -0.0076(16) -0.0021(16) 0.078(3) C1 0.098(2) 0.125(3) 0.0289(13) 0.0011(15) 0.0053(14) 0.049(2) Cd2 0.0674(15) 0.0674(15) 0.0472(19) 0.000 0.000 0.0337(8) Cd3 0.238(4) 0.238(4) 0.279(12) 0.000 0.000 0.119(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.315(4) 2_665 ? Cd1 N1 2.315(4) 6_556 ? Cd1 N1 2.315(4) 4_565 ? Cd1 N1 2.315(4) 5_566 ? Cd1 N1 2.315(4) . ? Cd1 N1 2.315(4) 3_666 ? N1 C1 1.134(6) . ? C2 C1 1.394(5) . ? C2 C1 1.394(5) 9 ? C2 C3 1.472(5) . ? C3 C4 1.382(4) . ? C3 C4 1.382(4) 9 ? C4 C4 1.385(6) 3_665 ? Cd2 Cd3 1.137(11) . ? Cd2 Cd3 1.137(11) 7_556 ? Cd3 Cd3 2.27(2) 7_556 ? 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_3 _geom_angle_publ_flag N1 Cd1 N1 87.87(19) 2_665 6_556 ? N1 Cd1 N1 89.35(13) 2_665 4_565 ? N1 Cd1 N1 93.6(2) 6_556 4_565 ? N1 Cd1 N1 93.6(2) 2_665 5_566 ? N1 Cd1 N1 89.35(13) 6_556 5_566 ? N1 Cd1 N1 175.9(2) 4_565 5_566 ? N1 Cd1 N1 89.35(13) 2_665 . ? N1 Cd1 N1 175.9(2) 6_556 . ? N1 Cd1 N1 89.35(13) 4_565 . ? N1 Cd1 N1 87.87(19) 5_566 . ? N1 Cd1 N1 175.9(2) 2_665 3_666 ? N1 Cd1 N1 89.35(13) 6_556 3_666 ? N1 Cd1 N1 87.87(19) 4_565 3_666 ? N1 Cd1 N1 89.35(13) 5_566 3_666 ? N1 Cd1 N1 93.6(2) . 3_666 ? C1 N1 Cd1 146.8(4) . . ? C1 C2 C1 117.1(4) . 9 ? C1 C2 C3 121.4(2) . . ? C1 C2 C3 121.4(2) 9 . ? C4 C3 C4 116.7(4) . 9 ? C4 C3 C2 121.7(2) . . ? C4 C3 C2 121.7(2) 9 . ? C3 C4 C4 121.7(2) . 3_665 ? N1 C1 C2 179.5(5) . . ? Cd3 Cd2 Cd3 180.000(2) . 7_556 ? Cd2 Cd3 Cd3 0.000(1) . 7_556 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 74.21 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.478 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.057 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.018 841 209 ' ' _platon_squeeze_details ; ; # Attachment '- rweb45nZn(dmso4)final.cif' data_rweb45n _database_code_depnum_ccdc_archive 'CCDC 842125' #TrackingRef '- rweb45nZn(dmso4)final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn(DMSO)4(H2O)2][Zn2TCNQ3]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 N12 O6 S4 Zn3' _chemical_formula_weight 1157.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-31m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-y, -x, -z' '-x+y, -x, z' 'x, x-y, -z' '-x+y, y, -z' '-x, -y, -z' 'y, -x+y, -z' 'y, x, z' 'x-y, x, -z' '-x, -x+y, z' 'x-y, -y, z' _cell_length_a 12.7447(4) _cell_length_b 12.7447(4) _cell_length_c 10.7107(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1506.63(8) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 1898 _cell_measurement_theta_min 4.0019 _cell_measurement_theta_max 74.2508 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.1664 _exptl_crystal_size_mid 0.1015 _exptl_crystal_size_min 0.0695 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 590 _exptl_absorpt_coefficient_mu 3.099 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3576 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 74.42 _reflns_number_total 1098 _reflns_number_gt 944 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1709P)^2^+2.2188P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1098 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2859 _refine_ls_wR_factor_gt 0.2757 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _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 Zn3 Zn 0.0000 0.0000 0.5000 0.088(4) Uani 0.294(10) 12 d SP . . Zn2 Zn 0.0000 0.0000 0.0000 0.0682(15) Uani 0.706(10) 12 d SP . . Zn1 Zn 0.3333 0.6667 0.0000 0.0396(6) Uani 1 6 d S . . N1 N 0.4684(5) 0.6648(5) 0.1155(4) 0.0724(16) Uani 1 1 d . . . C2 C 0.5526(6) 0.5526(6) 0.2374(5) 0.0538(17) Uani 1 2 d S . . C3 C 0.5255(6) 0.5255(6) 0.3718(5) 0.0515(16) Uani 1 2 d S . . C4 C 0.4588(5) 0.5664(5) 0.4358(4) 0.0572(13) Uani 1 1 d . . . H4 H 0.4296 0.6120 0.3930 0.069 Uiso 1 1 calc R . . C1 C 0.5071(5) 0.6143(6) 0.1699(4) 0.0567(13) Uani 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 Zn3 0.077(5) 0.077(5) 0.110(10) 0.000 0.000 0.038(2) Zn2 0.0669(17) 0.0669(17) 0.071(3) 0.000 0.000 0.0334(9) Zn1 0.0516(7) 0.0516(7) 0.0157(8) 0.000 0.000 0.0258(4) N1 0.087(3) 0.120(5) 0.027(2) 0.008(2) -0.003(2) 0.064(3) C2 0.076(3) 0.076(3) 0.020(3) -0.010(2) -0.010(2) 0.046(4) C3 0.070(3) 0.070(3) 0.018(3) -0.008(2) -0.008(2) 0.038(4) C4 0.084(3) 0.084(3) 0.027(2) 0.000(2) -0.005(2) 0.059(3) C1 0.069(3) 0.089(4) 0.021(2) -0.009(2) -0.0106(18) 0.046(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.130(5) 6 ? Zn1 N1 2.130(5) 2_665 ? Zn1 N1 2.130(5) 5_565 ? Zn1 N1 2.130(5) 4_565 ? Zn1 N1 2.130(5) . ? Zn1 N1 2.130(5) 3_665 ? N1 C1 1.146(7) . ? C2 C1 1.391(6) 9 ? C2 C1 1.391(6) . ? C2 C3 1.481(8) . ? C3 C4 1.381(6) 9 ? C3 C4 1.381(6) . ? C4 C4 1.412(9) 3_666 ? 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_3 _geom_angle_publ_flag N1 Zn1 N1 91.2(3) 6 2_665 ? N1 Zn1 N1 89.63(19) 6 5_565 ? N1 Zn1 N1 89.6(3) 2_665 5_565 ? N1 Zn1 N1 89.6(3) 6 4_565 ? N1 Zn1 N1 89.63(19) 2_665 4_565 ? N1 Zn1 N1 178.9(3) 5_565 4_565 ? N1 Zn1 N1 178.9(3) 6 . ? N1 Zn1 N1 89.6(2) 2_665 . ? N1 Zn1 N1 91.2(3) 5_565 . ? N1 Zn1 N1 89.63(19) 4_565 . ? N1 Zn1 N1 89.63(19) 6 3_665 ? N1 Zn1 N1 178.9(3) 2_665 3_665 ? N1 Zn1 N1 89.63(19) 5_565 3_665 ? N1 Zn1 N1 91.2(3) 4_565 3_665 ? N1 Zn1 N1 89.6(3) . 3_665 ? C1 N1 Zn1 151.4(5) . . ? C1 C2 C1 116.6(6) 9 . ? C1 C2 C3 121.5(3) 9 . ? C1 C2 C3 121.5(3) . . ? C4 C3 C4 118.6(6) 9 . ? C4 C3 C2 120.7(3) 9 . ? C4 C3 C2 120.7(3) . . ? C3 C4 C4 120.7(3) . 3_666 ? N1 C1 C2 179.0(6) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 74.42 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.484 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.125 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.067 707 185 ' ' _platon_squeeze_details ; ; # Attachment '- rweb45cfinal3.cif' data_rweb45c _database_code_depnum_ccdc_archive 'CCDC 842126' #TrackingRef '- rweb45cfinal3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Mn(bipy)3][Mn2TCNQ3].2MeOH' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H44 Mn3 N18 O2' _chemical_formula_weight 1310.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P63/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z' 'x-y, -y, -z+1/2' 'x, x-y, -z' 'y, x, -z+1/2' '-x+y, y, -z' '-x, -x+y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' 'y, x, z' '-x+y, y, z-1/2' '-x, -x+y, z' '-y, -x, z-1/2' 'x-y, -y, z' 'x, x-y, z-1/2' _cell_length_a 12.8814(3) _cell_length_b 12.8814(3) _cell_length_c 22.0591(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3169.89(12) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 3065 _cell_measurement_theta_min 3.9594 _cell_measurement_theta_max 74.3999 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 5.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83160 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.39 (release 18-08-2010 CrysAlis171 .NET) (compiled Aug 18 2010,17:42:00) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7375 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 74.57 _reflns_number_total 1202 _reflns_number_gt 962 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.2000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1202 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0990 _refine_ls_wR_factor_ref 0.3385 _refine_ls_wR_factor_gt 0.3149 _refine_ls_goodness_of_fit_ref 1.501 _refine_ls_restrained_S_all 1.501 _refine_ls_shift/su_max 0.000 _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 0.6667 0.3333 0.0000 0.0466(7) Uani 1 6 d S . . N1 N 0.5270(3) 0.3340(3) 0.05824(12) 0.0720(11) Uani 1 1 d . . . C1 C 0.4326(4) 0.4326(4) 0.18588(19) 0.0532(12) Uani 1 2 d S . . C2 C 0.4823(3) 0.3748(3) 0.08583(12) 0.0542(10) Uani 1 1 d . . . C3 C 0.4289(4) 0.4289(4) 0.1193(2) 0.0510(11) Uani 1 2 d S . . C7 C 0.3803(4) 0.4870(4) 0.21835(13) 0.0614(11) Uani 1 1 d . . . H1 H 0.3439 0.5247 0.1972 0.074 Uiso 1 1 calc R . . Mn3 Mn 0.0000 0.0000 0.0311(4) 0.109(3) Uani 0.50 6 d SP . . 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 0.0645(8) 0.0645(8) 0.0107(9) 0.000 0.000 0.0322(4) N1 0.094(2) 0.106(3) 0.0188(14) 0.0003(14) 0.0062(13) 0.052(2) C1 0.073(2) 0.073(2) 0.0188(19) 0.0037(15) 0.0037(15) 0.040(2) C2 0.070(2) 0.072(2) 0.0181(14) 0.0019(13) 0.0042(12) 0.0335(17) C3 0.070(2) 0.070(2) 0.0201(18) 0.0059(15) 0.0059(15) 0.041(2) C7 0.093(3) 0.084(2) 0.0210(18) 0.0021(14) -0.0012(15) 0.055(2) Mn3 0.0774(15) 0.0774(15) 0.172(8) 0.000 0.000 0.0387(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N1 2.215(4) 3_655 ? Mn1 N1 2.215(4) 11_655 ? Mn1 N1 2.215(4) 5_665 ? Mn1 N1 2.215(4) 9 ? Mn1 N1 2.215(4) . ? Mn1 N1 2.215(4) 7_665 ? N1 C2 1.131(5) . ? C1 C7 1.389(4) 19 ? C1 C7 1.389(4) . ? C1 C3 1.470(6) . ? C2 C3 1.408(4) . ? C3 C2 1.408(4) 19 ? C7 C7 1.396(6) 16_556 ? C7 H1 0.9500 . ? Mn3 Mn3 1.374(18) 13 ? 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_3 _geom_angle_publ_flag N1 Mn1 N1 90.56(18) 3_655 11_655 ? N1 Mn1 N1 89.73(12) 3_655 5_665 ? N1 Mn1 N1 89.99(18) 11_655 5_665 ? N1 Mn1 N1 89.99(18) 3_655 9 ? N1 Mn1 N1 89.73(12) 11_655 9 ? N1 Mn1 N1 179.60(19) 5_665 9 ? N1 Mn1 N1 89.73(12) 3_655 . ? N1 Mn1 N1 179.60(19) 11_655 . ? N1 Mn1 N1 89.73(12) 5_665 . ? N1 Mn1 N1 90.56(18) 9 . ? N1 Mn1 N1 179.60(19) 3_655 7_665 ? N1 Mn1 N1 89.73(12) 11_655 7_665 ? N1 Mn1 N1 90.56(18) 5_665 7_665 ? N1 Mn1 N1 89.73(12) 9 7_665 ? N1 Mn1 N1 89.99(18) . 7_665 ? C2 N1 Mn1 156.5(3) . . ? C7 C1 C7 117.9(4) 19 . ? C7 C1 C3 121.1(2) 19 . ? C7 C1 C3 121.1(2) . . ? N1 C2 C3 178.2(4) . . ? C2 C3 C2 116.8(4) . 19 ? C2 C3 C1 121.58(19) . . ? C2 C3 C1 121.58(19) 19 . ? C1 C7 C7 121.1(2) . 16_556 ? C1 C7 H1 119.5 . . ? C7 C7 H1 119.5 16_556 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 74.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.819 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.139 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.202 1627 338 ' ' _platon_squeeze_details ; ;