Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2001 data_General _journal_coden_Cambridge 1145 _audit_creation_date 'Tue April 24 2001' _audit_creation_method 'by teXsan' #--------------------------------------------------------------------------- # SUBMISSION DETAILS loop_ _publ_author_name 'Masaki Matsuda' 'Toshio Naito' 'Tamotsu Inabe' 'Noriaki Hanasaki' 'Hiroyuki Tajima' _publ_contact_author_name ' Tamotsu INABE ' _publ_contact_author_address ; Division of Chemistry Graduate School of Science Hokkaido University Sapporo 060-0810 Japan ; _publ_contact_author_email ' inabe@sci.hokudai.ac.jp' _publ_contact_author_fax ' (+81)-11-746-2557 ' _publ_contact_author_phone ' (+81)-11-706-3511 ' _publ_requested_journal ' J. Mater. Chem.' #--------------------------------------------------------------------------- data_(PTMA)x[Fe(Pc)(CN)2].yCH3CN(295K) _database_code_CSD 164082 #--------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C40.50 H26 Fe N11.50 ' _chemical_formula_moiety '?' _chemical_formula_weight 729.57 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nnm' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/2+x,1/2-y,1/2-z 1/2-x,1/2+y,1/2-z -x,-y,-z x,y,-z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,1/2+z _cell_length_a 13.9001(5) _cell_length_b 7.3319(2) _cell_length_c 16.3165(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1662.88(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 19011 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 295 #--------------------------------------------------------------------------- _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type none #--------------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3600 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 1.0005 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.0005 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 #--------------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; The stoichiometry is assumed as x=0.5 and y=1. PTMA and CH3CN are orientationally disordered, and they partially occupy the same site complementarily. Non-hydrogen atoms of PTMA and CH3CN are refined isotropically, and hydrogen atoms attached to them are not included. When one atomic site is occupied by two kinds of atoms (C and N), the site is represented by either one. Since C(11) (part of PTMA) and C(17) (part of CH3CN) are closely located, their coordinates are not refined (positions were determined by the difference synthesis). Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1979 _reflns_number_gt 1218 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.0577 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 1218 _refine_ls_number_parameters 139 _refine_ls_goodness_of_fit_ref 3.182 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_shift/su_max 0.0606 _refine_diff_density_max 0.47 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Fe' 'Fe' 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe(1) Fe 1.0000 0.0000 1.0000 0.0325(3) Uani 1.00 d S . . N(1) N 0.9635(2) 0.1731(4) 1.0833(2) 0.0321(9) Uani 1.00 d . . . N(2) N 1.0000 0.0000 1.2061(3) 0.037(1) Uani 1.00 d S . . N(3) N 0.8959(3) 0.4146(7) 1.0000 0.035(1) Uani 1.00 d S . . N(4) N 1.2173(4) 0.1104(9) 1.0000 0.060(2) Uani 1.00 d S . . N(5) N 0.5880(8) 0.328(2) 1.0000 0.105(4) Uiso 0.75 d SP . . C(1) C 0.9651(3) 0.1431(6) 1.1662(3) 0.035(1) Uani 1.00 d . . . C(2) C 0.9195(3) 0.2954(6) 1.2088(3) 0.035(1) Uani 1.00 d . . . C(3) C 0.9023(3) 0.3250(7) 1.2922(3) 0.042(1) Uani 1.00 d . . . C(4) C 0.8527(3) 0.4849(8) 1.3126(3) 0.052(1) Uani 1.00 d . . . C(5) C 0.8246(3) 0.6062(7) 1.2522(3) 0.052(2) Uani 1.00 d . . . C(6) C 0.8419(3) 0.5774(6) 1.1684(3) 0.040(1) Uani 1.00 d . . . C(7) C 0.8900(3) 0.4162(6) 1.1488(2) 0.033(1) Uani 1.00 d . . . C(8) C 0.9177(3) 0.3374(6) 1.0705(2) 0.033(1) Uani 1.00 d . . . C(9) C 1.1373(4) 0.0805(9) 1.0000 0.037(2) Uani 1.00 d S . . C(10) C 0.5000 0.5000 1.0000 0.033(4) Uiso 0.50 d SP . . C(11) C 0.4738 0.3438 1.0000 0.09(1) Uiso 0.25 d SP . . C(12) C 0.5566(9) 0.185(2) 1.0000 0.039(3) Uiso 0.50 d SP . . C(13) C 0.661(2) 0.288(4) 1.0000 0.060(8) Uiso 0.25 d SP . . C(14) C 0.662(1) 0.466(2) 1.0000 0.125(5) Uiso 0.75 d SP . . C(15) C 0.587(1) 0.599(3) 1.0000 0.016(4) Uiso 0.25 d SP . . C(16) C 0.657(1) 0.402(2) 1.0724(10) 0.038(4) Uiso 0.25 d P . . C(17) C 0.5009 0.2700 1.0000 0.111(7) Uiso 0.50 d SP . . H(3) H 0.9247 0.2392 1.3372 0.0630 Uiso 1.00 calc . . . H(4) H 0.8320 0.4707 1.3765 0.0630 Uiso 1.00 calc . . . H(5) H 0.793(3) 0.712(6) 1.267(3) 0.07(2) Uiso 1.00 calc . . . H(6) H 0.826(4) 0.660(7) 1.109(3) 0.12(2) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0362(7) 0.0372(7) 0.0242(6) 0.0049(7) 0.0000 0.0000 N(1) 0.037(2) 0.037(2) 0.022(2) 0.004(2) 0.000(1) -0.001(2) N(2) 0.047(3) 0.036(3) 0.029(3) 0.004(3) 0.0000 0.0000 N(3) 0.038(3) 0.042(3) 0.024(3) 0.004(3) 0.0000 0.0000 N(4) 0.049(3) 0.084(5) 0.047(3) -0.003(4) 0.0000 0.0000 C(1) 0.035(2) 0.038(2) 0.032(2) -0.001(2) 0.000(2) -0.002(2) C(2) 0.032(2) 0.039(3) 0.034(2) 0.000(2) 0.004(2) -0.005(2) C(3) 0.045(3) 0.050(3) 0.031(3) 0.005(3) 0.001(2) -0.002(2) C(4) 0.055(3) 0.063(3) 0.037(2) 0.006(3) 0.008(2) -0.008(3) C(5) 0.050(3) 0.053(3) 0.053(3) 0.012(3) 0.004(3) -0.012(3) C(6) 0.040(2) 0.045(3) 0.036(2) 0.004(2) 0.002(2) -0.004(3) C(7) 0.030(2) 0.039(2) 0.031(2) 0.002(2) 0.000(2) 0.000(2) C(8) 0.031(2) 0.038(2) 0.032(2) -0.001(2) 0.001(2) -0.003(2) C(9) 0.041(4) 0.046(4) 0.025(3) 0.002(3) 0.0000 0.0000 #--------------------------------------------------------------------------- _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; Since PTMA and CH3CN are orientationally disordered and partially occupy the same site complementarily, unusual geometry is included (N(5), C(10)-C(17)). ; 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 Fe(1) N(1) 1.927(3) . . yes Fe(1) N(1) 1.927(3) . 6_557 yes Fe(1) N(1) 1.927(3) . 2_755 yes Fe(1) N(1) 1.927(3) . 5_757 yes Fe(1) C(9) 1.997(6) . . yes Fe(1) C(9) 1.997(6) . 2_755 yes N(1) C(1) 1.372(5) . . yes N(1) C(8) 1.378(5) . . yes N(2) C(1) 1.327(4) . . yes N(2) C(1) 1.327(4) . 2_755 yes N(3) C(8) 1.318(5) . . yes N(3) C(8) 1.318(5) . 6_557 yes N(4) C(9) 1.134(7) . . yes N(5) C(10) 1.76(1) . . yes N(5) C(11) 1.59(1) . . yes N(5) C(12) 1.14(1) . . yes N(5) C(13) 1.06(3) . . yes N(5) C(14) 1.45(2) . . yes N(5) C(16) 1.61(2) . . yes N(5) C(16) 1.61(2) . 6_557 yes N(5) C(17) 1.28(1) . . yes C(1) C(2) 1.460(5) . . yes C(2) C(3) 1.400(5) . . yes C(2) C(7) 1.382(5) . . yes C(3) C(4) 1.400(6) . . yes C(3) H(3) 1.015 . . no C(4) C(5) 1.383(7) . . yes C(4) H(4) 1.087 . . no C(5) C(6) 1.405(6) . . yes C(5) H(5) 0.92(4) . . no C(6) C(7) 1.395(5) . . yes C(6) H(6) 1.16(5) . . no C(7) C(8) 1.454(5) . . yes C(10) C(11) 1.202 . . yes C(10) C(11) 1.202 . 2_665 yes C(10) C(15) 1.41(2) . . yes C(10) C(15) 1.41(2) . 2_665 yes C(10) C(17) 1.687 . . yes C(10) C(17) 1.687 . 2_665 yes C(11) C(12) 1.64(1) . . yes C(11) C(15) 0.95(2) . 2_665 yes C(11) C(17) 0.659 . . yes C(12) C(13) 1.64(3) . . yes C(12) C(17) 0.99(1) . . yes C(13) C(14) 1.30(3) . . yes C(13) C(16) 1.45(2) . . yes C(13) C(16) 1.45(2) . 6_557 yes C(14) C(15) 1.43(2) . . yes C(14) C(16) 1.27(2) . . yes C(14) C(16) 1.27(2) . 6_557 yes C(15) C(17) 1.56(2) . 2_665 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 N(1) Fe(1) N(1) 89.6(2) . 1_555 6_557 yes N(1) Fe(1) N(1) 90.4(2) . 1_555 2_755 yes N(1) Fe(1) N(1) 180.0 . 1_555 5_757 yes N(1) Fe(1) C(9) 93.3(2) . 1_555 1_555 yes N(1) Fe(1) C(9) 86.7(2) . 1_555 2_755 yes N(1) Fe(1) N(1) 180.0 . 6_557 2_755 yes N(1) Fe(1) N(1) 90.4(2) . 6_557 5_757 yes N(1) Fe(1) C(9) 93.3(2) . 6_557 1_555 yes N(1) Fe(1) C(9) 86.7(2) . 6_557 2_755 yes N(1) Fe(1) N(1) 89.6(2) . 2_755 5_757 yes N(1) Fe(1) C(9) 86.7(2) . 2_755 1_555 yes N(1) Fe(1) C(9) 93.3(2) . 2_755 2_755 yes N(1) Fe(1) C(9) 86.7(2) . 5_757 1_555 yes N(1) Fe(1) C(9) 93.3(2) . 5_757 2_755 yes C(9) Fe(1) C(9) 180.0 . 1_555 2_755 yes Fe(1) N(1) C(1) 125.8(3) . 1_555 1_555 yes Fe(1) N(1) C(8) 126.3(3) . 1_555 1_555 yes C(1) N(1) C(8) 107.2(3) . 1_555 1_555 yes C(1) N(2) C(1) 121.2(5) . 1_555 2_755 yes C(8) N(3) C(8) 121.7(5) . 1_555 6_557 yes C(10) N(5) C(11) 41.7(3) . 1_555 1_555 yes C(10) N(5) C(12) 113(1) . 1_555 1_555 yes C(10) N(5) C(13) 150(2) . 1_555 1_555 yes C(10) N(5) C(14) 89.7(9) . 1_555 1_555 yes C(10) N(5) C(16) 99.7(8) . 1_555 1_555 yes C(10) N(5) C(16) 99.7(8) . 1_555 6_557 yes C(10) N(5) C(17) 65.2(5) . 1_555 1_555 yes C(11) N(5) C(12) 71.6(9) . 1_555 1_555 yes C(11) N(5) C(13) 168(2) . 1_555 1_555 yes C(11) N(5) C(14) 131(1) . 1_555 1_555 yes C(11) N(5) C(16) 124.4(8) . 1_555 1_555 yes C(11) N(5) C(16) 124.4(8) . 1_555 6_557 yes C(11) N(5) C(17) 23.5(2) . 1_555 1_555 yes C(12) N(5) C(13) 96(2) . 1_555 1_555 yes C(12) N(5) C(14) 156(1) . 1_555 1_555 yes C(12) N(5) C(16) 122.6(9) . 1_555 1_555 yes C(12) N(5) C(16) 122.6(9) . 1_555 6_557 yes C(12) N(5) C(17) 48.1(8) . 1_555 1_555 yes C(13) N(5) C(14) 60(1) . 1_555 1_555 yes C(13) N(5) C(16) 61(1) . 1_555 1_555 yes C(13) N(5) C(16) 61(1) . 1_555 6_557 yes C(13) N(5) C(17) 144(2) . 1_555 1_555 yes C(14) N(5) C(16) 48.8(7) . 1_555 1_555 yes C(14) N(5) C(16) 48.8(7) . 1_555 6_557 yes C(14) N(5) C(17) 154(1) . 1_555 1_555 yes C(16) N(5) C(16) 94(1) . 1_555 6_557 yes C(16) N(5) C(17) 132.0(7) . 1_555 1_555 yes C(16) N(5) C(17) 132.0(7) . 6_557 1_555 yes N(1) C(1) N(2) 128.1(4) . 1_555 1_555 yes N(1) C(1) C(2) 109.8(4) . 1_555 1_555 yes N(2) C(1) C(2) 122.0(3) . 1_555 1_555 yes C(1) C(2) C(3) 131.0(4) . 1_555 1_555 yes C(1) C(2) C(7) 106.4(3) . 1_555 1_555 yes C(3) C(2) C(7) 122.6(4) . 1_555 1_555 yes C(2) C(3) C(4) 116.4(4) . 1_555 1_555 yes C(2) C(3) H(3) 123.7 . 1_555 1_555 no C(4) C(3) H(3) 119.9 . 1_555 1_555 no C(3) C(4) C(5) 120.6(4) . 1_555 1_555 yes C(3) C(4) H(4) 106.1 . 1_555 1_555 no C(5) C(4) H(4) 132.1 . 1_555 1_555 no C(4) C(5) C(6) 123.3(5) . 1_555 1_555 yes C(4) C(5) H(5) 119(3) . 1_555 1_555 no C(6) C(5) H(5) 117(3) . 1_555 1_555 no C(5) C(6) C(7) 115.6(4) . 1_555 1_555 yes C(5) C(6) H(6) 134(2) . 1_555 1_555 no C(7) C(6) H(6) 110(2) . 1_555 1_555 no C(2) C(7) C(6) 121.6(4) . 1_555 1_555 yes C(2) C(7) C(8) 106.8(3) . 1_555 1_555 yes C(6) C(7) C(8) 131.7(4) . 1_555 1_555 yes N(1) C(8) N(3) 127.8(4) . 1_555 1_555 yes N(1) C(8) C(7) 109.7(3) . 1_555 1_555 yes N(3) C(8) C(7) 122.4(4) . 1_555 1_555 yes Fe(1) C(9) N(4) 173.9(7) . 1_555 1_555 yes N(5) C(10) N(5) 180.0 . 1_555 2_665 yes N(5) C(10) C(11) 61.8(4) . 1_555 1_555 yes N(5) C(10) C(11) 118.2(4) . 1_555 2_665 yes N(5) C(10) C(15) 76.8(8) . 1_555 1_555 yes N(5) C(10) C(15) 103.2(8) . 1_555 2_665 yes N(5) C(10) C(17) 43.7(4) . 1_555 1_555 yes N(5) C(10) C(17) 136.3(4) . 1_555 2_665 yes N(5) C(10) C(11) 118.2(4) . 2_665 1_555 yes N(5) C(10) C(11) 61.8(4) . 2_665 2_665 yes N(5) C(10) C(15) 103.2(8) . 2_665 1_555 yes N(5) C(10) C(15) 76.8(8) . 2_665 2_665 yes N(5) C(10) C(17) 136.3(4) . 2_665 1_555 yes N(5) C(10) C(17) 43.7(4) . 2_665 2_665 yes C(11) C(10) C(11) 180.0 . 1_555 2_665 yes C(11) C(10) C(15) 138.6(8) . 1_555 1_555 yes C(11) C(10) C(15) 41.4(8) . 1_555 2_665 yes C(11) C(10) C(17) 18.0814(6) . 1_555 1_555 yes C(11) C(10) C(17) 161.9186(6) . 1_555 2_665 yes C(11) C(10) C(15) 41.4(8) . 2_665 1_555 yes C(11) C(10) C(15) 138.6(8) . 2_665 2_665 yes C(11) C(10) C(17) 161.9186(6) . 2_665 1_555 yes C(11) C(10) C(17) 18.0814(6) . 2_665 2_665 yes C(15) C(10) C(15) 180.0 . 1_555 2_665 yes C(15) C(10) C(17) 120.5(8) . 1_555 1_555 yes C(15) C(10) C(17) 59.5(8) . 1_555 2_665 yes C(15) C(10) C(17) 59.5(8) . 2_665 1_555 yes C(15) C(10) C(17) 120.5(8) . 2_665 2_665 yes C(17) C(10) C(17) 180.0 . 1_555 2_665 yes N(5) C(11) C(10) 76.5(4) . 1_555 1_555 yes N(5) C(11) C(12) 41.1(5) . 1_555 1_555 yes N(5) C(11) C(15) 157(1) . 1_555 2_665 yes N(5) C(11) C(17) 50.9(4) . 1_555 1_555 yes C(10) C(11) C(12) 117.7(4) . 1_555 1_555 yes C(10) C(11) C(15) 81(1) . 1_555 2_665 yes C(10) C(11) C(17) 127.454(2) . 1_555 1_555 yes C(12) C(11) C(15) 160(1) . 1_555 2_665 yes C(12) C(11) C(17) 9.8(4) . 1_555 1_555 yes C(15) C(11) C(17) 151(1) . 2_665 1_555 yes N(5) C(12) C(11) 67.2(9) . 1_555 1_555 yes N(5) C(12) C(13) 40(1) . 1_555 1_555 yes N(5) C(12) C(17) 73(1) . 1_555 1_555 yes C(11) C(12) C(13) 107(1) . 1_555 1_555 yes C(11) C(12) C(17) 6.5(3) . 1_555 1_555 yes C(13) C(12) C(17) 113(1) . 1_555 1_555 yes N(5) C(13) C(12) 43(1) . 1_555 1_555 yes N(5) C(13) C(14) 74(2) . 1_555 1_555 yes N(5) C(13) C(16) 78(1) . 1_555 1_555 yes N(5) C(13) C(16) 78(1) . 1_555 6_557 yes C(12) C(13) C(14) 117(2) . 1_555 1_555 yes C(12) C(13) C(16) 102(1) . 1_555 1_555 yes C(12) C(13) C(16) 102(1) . 1_555 6_557 yes C(14) C(13) C(16) 54(1) . 1_555 1_555 yes C(14) C(13) C(16) 54(1) . 1_555 6_557 yes C(16) C(13) C(16) 109(2) . 1_555 6_557 yes N(5) C(14) C(13) 45(1) . 1_555 1_555 yes N(5) C(14) C(15) 87(1) . 1_555 1_555 yes N(5) C(14) C(16) 72(1) . 1_555 1_555 yes N(5) C(14) C(16) 72(1) . 1_555 6_557 yes C(13) C(14) C(15) 132(2) . 1_555 1_555 yes C(13) C(14) C(16) 68(1) . 1_555 1_555 yes C(13) C(14) C(16) 68(1) . 1_555 6_557 yes C(15) C(14) C(16) 101(1) . 1_555 1_555 yes C(15) C(14) C(16) 101(1) . 1_555 6_557 yes C(16) C(14) C(16) 136(2) . 1_555 6_557 yes C(10) C(15) C(11) 57.2(9) . 1_555 2_665 yes C(10) C(15) C(14) 105(1) . 1_555 1_555 yes C(10) C(15) C(17) 69.0(8) . 1_555 2_665 yes C(11) C(15) C(14) 163(1) . 2_665 1_555 yes C(11) C(15) C(17) 11.8(5) . 2_665 2_665 yes C(14) C(15) C(17) 174(1) . 1_555 2_665 yes N(5) C(16) C(13) 40(1) . 1_555 1_555 yes N(5) C(16) C(14) 58.7(10) . 1_555 1_555 yes C(13) C(16) C(14) 56(1) . 1_555 1_555 yes N(5) C(17) C(10) 71.1(5) . 1_555 1_555 yes N(5) C(17) C(11) 105.6(5) . 1_555 1_555 yes N(5) C(17) C(12) 58.2(7) . 1_555 1_555 yes N(5) C(17) C(15) 122.6(9) . 1_555 2_665 yes C(10) C(17) C(11) 34.464(1) . 1_555 1_555 yes C(10) C(17) C(12) 129.3(7) . 1_555 1_555 yes C(10) C(17) C(15) 51.5(7) . 1_555 2_665 yes C(11) C(17) C(12) 163.7(7) . 1_555 1_555 yes C(11) C(17) C(15) 17.0(7) . 1_555 2_665 yes C(12) C(17) C(15) 179.2(10) . 1_555 2_665 yes #===END data_(PTMA)x[Co(Pc)(CN)2].yCH3CN(295K) #--------------------------------------------------------------------------- _database_code_CSD 164083 # CHEMICAL DATA _chemical_formula_sum 'C40.50 H26 Co N11.50 ' _chemical_formula_moiety '?' _chemical_formula_weight 732.66 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nnm' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/2+x,1/2-y,1/2-z 1/2-x,1/2+y,1/2-z -x,-y,-z x,y,-z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,1/2+z _cell_length_a 13.8706(6) _cell_length_b 7.3498(3) _cell_length_c 16.2958(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1661.3(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 13688 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 295 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type none #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1978 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9995 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; The stoichiometry is assumed as x=0.5 and y=1. PTMA and CH3CN are orientationally disordered, and they partially occupy the same site complementarily. Non-hydrogen atoms of PTMA and CH3CN are refined isotropically, and hydrogen atoms attached to them are not included. When one atomic site is occupied by two kinds of atoms (C and N), the site is represented by either one. Since C(11) (part of PTMA) and C(17) (part of CH3CN) are closely located, their coordinates are not refined (positions were determined by the difference synthesis). Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1978 _reflns_number_gt 918 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.0460 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 918 _refine_ls_number_parameters 131 _refine_ls_goodness_of_fit_ref 2.387 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_shift/su_max 0.0019 _refine_diff_density_max 0.31 _refine_diff_density_min -0.29 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Co' 'Co' 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co(1) Co 1.0000 0.0000 1.0000 0.0311(4) Uani 1.00 d S . . N(1) N 0.9629(2) 0.1723(5) 1.0830(2) 0.029(1) Uani 1.00 d . . . N(2) N 1.0000 0.0000 1.2058(3) 0.037(2) Uani 1.00 d S . . N(3) N 0.8960(4) 0.4137(8) 1.0000 0.032(2) Uani 1.00 d S . . N(4) N 1.2142(5) 0.113(1) 1.0000 0.056(2) Uani 1.00 d S . . N(5) N 0.5890(10) 0.330(2) 1.0000 0.097(4) Uiso 0.75 d SP . . C(1) C 0.9652(3) 0.1424(7) 1.1658(3) 0.033(2) Uani 1.00 d . . . C(2) C 0.9195(3) 0.2942(8) 1.2083(3) 0.033(2) Uani 1.00 d . . . C(3) C 0.9018(4) 0.3250(8) 1.2926(3) 0.042(2) Uani 1.00 d . . . C(4) C 0.8524(4) 0.4833(10) 1.3129(3) 0.050(2) Uani 1.00 d . . . C(5) C 0.8246(4) 0.6053(8) 1.2523(4) 0.049(2) Uani 1.00 d . . . C(6) C 0.8422(4) 0.5746(8) 1.1687(3) 0.038(2) Uani 1.00 d . . . C(7) C 0.8902(3) 0.4146(8) 1.1484(3) 0.030(2) Uani 1.00 d . . . C(8) C 0.9176(3) 0.3355(7) 1.0704(3) 0.032(2) Uani 1.00 d . . . C(9) C 1.1333(6) 0.081(1) 1.0000 0.034(2) Uani 1.00 d S . . C(10) C 0.5000 0.5000 1.0000 0.040(5) Uiso 0.50 d SP . . C(11) C 0.4810 0.3305 1.0000 0.051(9) Uiso 0.25 d SP . . C(12) C 0.561(1) 0.183(2) 1.0000 0.039(4) Uiso 0.50 d SP . . C(13) C 0.662(3) 0.297(5) 1.0000 0.055(10) Uiso 0.25 d SP . . C(14) C 0.663(1) 0.465(3) 1.0000 0.123(6) Uiso 0.75 d SP . . C(15) C 0.585(2) 0.599(3) 1.0000 0.017(6) Uiso 0.25 d SP . . C(16) C 0.657(1) 0.404(3) 1.071(1) 0.035(5) Uiso 0.25 d P . . C(17) C 0.5102 0.2403 1.0000 0.094(7) Uiso 0.50 d SP . . H(3) H 0.9234 0.2374 1.3340 0.0499 Uiso 1.00 calc . . . H(4) H 0.8388 0.5092 1.3700 0.0568 Uiso 1.00 calc . . . H(5) H 0.7897 0.7176 1.2694 0.0572 Uiso 1.00 calc . . . H(6) H 0.8227 0.6623 1.1291 0.0463 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0341(9) 0.0349(8) 0.0242(7) 0.004(1) 0.0000 0.0000 N(1) 0.032(2) 0.034(2) 0.020(2) 0.005(2) 0.003(2) 0.001(2) N(2) 0.047(4) 0.035(3) 0.028(3) 0.003(4) 0.0000 0.0000 N(3) 0.038(4) 0.039(4) 0.019(3) 0.003(3) 0.0000 0.0000 N(4) 0.042(4) 0.075(5) 0.052(4) -0.001(5) 0.0000 0.0000 C(1) 0.030(3) 0.034(3) 0.035(3) 0.000(3) 0.003(3) -0.001(3) C(2) 0.029(3) 0.040(3) 0.032(3) 0.001(3) 0.004(3) -0.007(3) C(3) 0.043(4) 0.047(4) 0.036(3) 0.003(3) 0.001(3) 0.002(4) C(4) 0.056(4) 0.056(4) 0.038(3) 0.011(4) 0.005(3) -0.008(5) C(5) 0.045(3) 0.048(4) 0.054(4) 0.013(3) 0.005(3) -0.011(4) C(6) 0.039(3) 0.041(4) 0.034(3) 0.005(3) 0.000(3) 0.000(3) C(7) 0.026(3) 0.035(3) 0.028(3) 0.002(3) -0.001(3) 0.003(3) C(8) 0.032(3) 0.033(3) 0.032(3) 0.000(3) 0.004(3) -0.005(3) C(9) 0.041(5) 0.039(5) 0.023(4) 0.001(4) 0.0000 0.0000 #--------------------------------------------------------------------------- _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; Since PTMA and CH3CN are orientationally disordered and partially occupy the same site complementarily, unusual geometry is included (N(5), C(10)-C(17)). ; 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 Co(1) N(1) 1.922(4) . . yes Co(1) N(1) 1.922(4) . 6_557 yes Co(1) N(1) 1.922(4) . 2_755 yes Co(1) N(1) 1.922(4) . 5_757 yes Co(1) C(9) 1.943(8) . . yes Co(1) C(9) 1.943(8) . 2_755 yes N(1) C(1) 1.368(6) . . yes N(1) C(8) 1.370(6) . . yes N(2) C(1) 1.324(5) . . yes N(2) C(1) 1.324(5) . 2_755 yes N(3) C(8) 1.318(6) . . yes N(3) C(8) 1.318(6) . 6_557 yes N(4) C(9) 1.147(8) . . yes N(5) C(10) 1.75(1) . . yes N(5) C(11) 1.50(1) . . yes N(5) C(12) 1.15(2) . . yes N(5) C(13) 1.05(4) . . yes N(5) C(14) 1.42(2) . . yes N(5) C(16) 1.59(2) . . yes N(5) C(16) 1.59(2) . 6_557 yes N(5) C(17) 1.28(1) . . yes C(1) C(2) 1.458(7) . . yes C(2) C(3) 1.414(6) . . yes C(2) C(7) 1.378(7) . . yes C(3) C(4) 1.389(8) . . yes C(3) H(3) 0.980 . . no C(4) C(5) 1.388(8) . . yes C(4) H(4) 0.969 . . no C(5) C(6) 1.402(8) . . yes C(5) H(5) 0.996 . . no C(6) C(7) 1.391(6) . . yes C(6) H(6) 0.952 . . no C(7) C(8) 1.449(7) . . yes C(10) C(11) 1.273 . . yes C(10) C(11) 1.273 . 2_665 yes C(10) C(15) 1.39(2) . . yes C(10) C(15) 1.39(2) . 2_665 yes C(11) C(12) 1.55(2) . . yes C(11) C(15) 1.06(3) . 2_665 yes C(11) C(17) 0.777 . . yes C(12) C(13) 1.64(4) . . yes C(12) C(17) 0.82(2) . . yes C(13) C(14) 1.23(4) . . yes C(13) C(16) 1.41(3) . . yes C(13) C(16) 1.41(3) . 6_557 yes C(14) C(15) 1.46(3) . . yes C(14) C(16) 1.25(2) . . yes C(14) C(16) 1.25(2) . 6_557 yes C(15) C(17) 1.78(3) . 2_665 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 N(1) Co(1) N(1) 89.4(2) . 1_555 6_557 yes N(1) Co(1) N(1) 90.6(2) . 1_555 2_755 yes N(1) Co(1) N(1) 180.0 . 1_555 5_757 yes N(1) Co(1) C(9) 93.0(2) . 1_555 1_555 yes N(1) Co(1) C(9) 87.0(2) . 1_555 2_755 yes N(1) Co(1) N(1) 180.0 . 6_557 2_755 yes N(1) Co(1) N(1) 90.6(2) . 6_557 5_757 yes N(1) Co(1) C(9) 93.0(2) . 6_557 1_555 yes N(1) Co(1) C(9) 87.0(2) . 6_557 2_755 yes N(1) Co(1) N(1) 89.4(2) . 2_755 5_757 yes N(1) Co(1) C(9) 87.0(2) . 2_755 1_555 yes N(1) Co(1) C(9) 93.0(2) . 2_755 2_755 yes N(1) Co(1) C(9) 87.0(2) . 5_757 1_555 yes N(1) Co(1) C(9) 93.0(2) . 5_757 2_755 yes C(9) Co(1) C(9) 180.0 . 1_555 2_755 yes Co(1) N(1) C(1) 125.6(4) . 1_555 1_555 yes Co(1) N(1) C(8) 126.5(3) . 1_555 1_555 yes C(1) N(1) C(8) 107.4(4) . 1_555 1_555 yes C(1) N(2) C(1) 121.0(6) . 1_555 2_755 yes C(8) N(3) C(8) 121.1(6) . 1_555 6_557 yes C(10) N(5) C(11) 45.2(4) . 1_555 1_555 yes C(10) N(5) C(12) 115(1) . 1_555 1_555 yes C(10) N(5) C(13) 148(2) . 1_555 1_555 yes C(10) N(5) C(14) 90(1) . 1_555 1_555 yes C(10) N(5) C(16) 100.2(10) . 1_555 1_555 yes C(10) N(5) C(16) 100.2(10) . 1_555 6_557 yes C(10) N(5) C(17) 76.5(7) . 1_555 1_555 yes C(11) N(5) C(12) 70(1) . 1_555 1_555 yes C(11) N(5) C(13) 166(2) . 1_555 1_555 yes C(11) N(5) C(14) 135(1) . 1_555 1_555 yes C(11) N(5) C(16) 126.4(9) . 1_555 1_555 yes C(11) N(5) C(16) 126.4(9) . 1_555 6_557 yes C(11) N(5) C(17) 31.3(3) . 1_555 1_555 yes C(12) N(5) C(13) 96(2) . 1_555 1_555 yes C(12) N(5) C(14) 153(1) . 1_555 1_555 yes C(12) N(5) C(16) 121(1) . 1_555 1_555 yes C(12) N(5) C(16) 121(1) . 1_555 6_557 yes C(12) N(5) C(17) 39.1(10) . 1_555 1_555 yes C(13) N(5) C(14) 57(2) . 1_555 1_555 yes C(13) N(5) C(16) 60(1) . 1_555 1_555 yes C(13) N(5) C(16) 60(1) . 1_555 6_557 yes C(13) N(5) C(17) 135(2) . 1_555 1_555 yes C(14) N(5) C(16) 48.5(8) . 1_555 1_555 yes C(14) N(5) C(16) 48.5(8) . 1_555 6_557 yes C(14) N(5) C(17) 167(1) . 1_555 1_555 yes C(16) N(5) C(16) 93(1) . 1_555 6_557 yes C(16) N(5) C(17) 133.2(8) . 1_555 1_555 yes C(16) N(5) C(17) 133.2(8) . 6_557 1_555 yes N(1) C(1) N(2) 128.4(5) . 1_555 1_555 yes N(1) C(1) C(2) 109.6(4) . 1_555 1_555 yes N(2) C(1) C(2) 121.9(4) . 1_555 1_555 yes C(1) C(2) C(3) 131.3(5) . 1_555 1_555 yes C(1) C(2) C(7) 106.5(4) . 1_555 1_555 yes C(3) C(2) C(7) 122.2(5) . 1_555 1_555 yes C(2) C(3) C(4) 116.8(5) . 1_555 1_555 yes C(2) C(3) H(3) 120.7 . 1_555 1_555 no C(4) C(3) H(3) 122.6 . 1_555 1_555 no C(3) C(4) C(5) 120.6(5) . 1_555 1_555 yes C(3) C(4) H(4) 119.2 . 1_555 1_555 no C(5) C(4) H(4) 120.1 . 1_555 1_555 no C(4) C(5) C(6) 122.6(5) . 1_555 1_555 yes C(4) C(5) H(5) 118.2 . 1_555 1_555 no C(6) C(5) H(5) 119.2 . 1_555 1_555 no C(5) C(6) C(7) 116.8(5) . 1_555 1_555 yes C(5) C(6) H(6) 120.1 . 1_555 1_555 no C(7) C(6) H(6) 123.1 . 1_555 1_555 no C(2) C(7) C(6) 121.0(5) . 1_555 1_555 yes C(2) C(7) C(8) 106.6(4) . 1_555 1_555 yes C(6) C(7) C(8) 132.3(5) . 1_555 1_555 yes N(1) C(8) N(3) 128.1(5) . 1_555 1_555 yes N(1) C(8) C(7) 109.9(4) . 1_555 1_555 yes N(3) C(8) C(7) 122.0(5) . 1_555 1_555 yes Co(1) C(9) N(4) 174.1(8) . 1_555 1_555 yes N(5) C(10) N(5) 180.0 . 1_555 2_665 yes N(5) C(10) C(11) 56.6(4) . 1_555 1_555 yes N(5) C(10) C(11) 123.4(4) . 1_555 2_665 yes N(5) C(10) C(15) 76(1) . 1_555 1_555 yes N(5) C(10) C(15) 103(1) . 1_555 2_665 yes N(5) C(10) C(11) 123.4(4) . 2_665 1_555 yes N(5) C(10) C(11) 56.6(4) . 2_665 2_665 yes N(5) C(10) C(15) 103(1) . 2_665 1_555 yes N(5) C(10) C(15) 76(1) . 2_665 2_665 yes C(11) C(10) C(11) 180.0 . 1_555 2_665 yes C(11) C(10) C(15) 133(1) . 1_555 1_555 yes C(11) C(10) C(15) 46(1) . 1_555 2_665 yes C(11) C(10) C(15) 46(1) . 2_665 1_555 yes C(11) C(10) C(15) 133(1) . 2_665 2_665 yes C(15) C(10) C(15) 180.0 . 1_555 2_665 yes N(5) C(11) C(10) 78.1(5) . 1_555 1_555 yes N(5) C(11) C(12) 44.3(7) . 1_555 1_555 yes N(5) C(11) C(15) 150(1) . 1_555 2_665 yes N(5) C(11) C(17) 58.5(5) . 1_555 1_555 yes C(10) C(11) C(12) 122.5(6) . 1_555 1_555 yes C(10) C(11) C(15) 72(1) . 1_555 2_665 yes C(10) C(11) C(17) 136.556(2) . 1_555 1_555 yes C(12) C(11) C(15) 164(1) . 1_555 2_665 yes C(12) C(11) C(17) 14.1(6) . 1_555 1_555 yes C(15) C(11) C(17) 150(1) . 2_665 1_555 yes N(5) C(12) C(11) 65(1) . 1_555 1_555 yes N(5) C(12) C(13) 39(1) . 1_555 1_555 yes N(5) C(12) C(17) 78(1) . 1_555 1_555 yes C(11) C(12) C(13) 104(1) . 1_555 1_555 yes C(11) C(12) C(17) 13.4(6) . 1_555 1_555 yes C(13) C(12) C(17) 118(2) . 1_555 1_555 yes N(5) C(13) C(12) 44(1) . 1_555 1_555 yes N(5) C(13) C(14) 76(2) . 1_555 1_555 yes N(5) C(13) C(16) 79(2) . 1_555 1_555 yes N(5) C(13) C(16) 79(2) . 1_555 6_557 yes C(12) C(13) C(14) 121(3) . 1_555 1_555 yes C(12) C(13) C(16) 104(1) . 1_555 1_555 yes C(12) C(13) C(16) 104(1) . 1_555 6_557 yes C(14) C(13) C(16) 55(1) . 1_555 1_555 yes C(14) C(13) C(16) 55(1) . 1_555 6_557 yes C(16) C(13) C(16) 111(2) . 1_555 6_557 yes N(5) C(14) C(13) 45(1) . 1_555 1_555 yes N(5) C(14) C(15) 86(1) . 1_555 1_555 yes N(5) C(14) C(16) 73(1) . 1_555 1_555 yes N(5) C(14) C(16) 73(1) . 1_555 6_557 yes C(13) C(14) C(15) 132(2) . 1_555 1_555 yes C(13) C(14) C(16) 68(1) . 1_555 1_555 yes C(13) C(14) C(16) 68(1) . 1_555 6_557 yes C(15) C(14) C(16) 101(1) . 1_555 1_555 yes C(15) C(14) C(16) 101(1) . 1_555 6_557 yes C(16) C(14) C(16) 137(2) . 1_555 6_557 yes C(10) C(15) C(11) 60(1) . 1_555 2_665 yes C(10) C(15) C(14) 105(1) . 1_555 1_555 yes C(10) C(15) C(17) 73(1) . 1_555 2_665 yes C(11) C(15) C(14) 166(2) . 2_665 1_555 yes C(11) C(15) C(17) 12.3(6) . 2_665 2_665 yes C(14) C(15) C(17) 178(1) . 1_555 2_665 yes N(5) C(16) C(13) 40(1) . 1_555 1_555 yes N(5) C(16) C(14) 58(1) . 1_555 1_555 yes C(13) C(16) C(14) 55(1) . 1_555 1_555 yes N(5) C(17) C(11) 90.3(6) . 1_555 1_555 yes N(5) C(17) C(12) 62(1) . 1_555 1_555 yes N(5) C(17) C(15) 107.1(9) . 1_555 2_665 yes C(11) C(17) C(12) 152(1) . 1_555 1_555 yes C(11) C(17) C(15) 16.8(8) . 1_555 2_665 yes C(12) C(17) C(15) 169(1) . 1_555 2_665 yes #===END data_(PTMA)x[Fe(Pc)(CN)2].yCH3CN(123K) #--------------------------------------------------------------------------- _database_code_CSD 157358 # CHEMICAL DATA _chemical_formula_sum 'C40.50 H26 Fe N11.50 ' _chemical_formula_moiety '?' _chemical_formula_weight 729.57 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nnm' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/2+x,1/2-y,1/2-z 1/2-x,1/2+y,1/2-z -x,-y,-z x,y,-z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,1/2+z _cell_length_a 13.850(1) _cell_length_b 7.2494(4) _cell_length_c 16.155(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1622.1(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 17140 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type none #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1930 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 0 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; The stoichiometry is assumed as x=0.5 and y=1. PTMA and CH3CN are orientationally disordered, and they partially occupy the same site complementarily. Non-hydrogen atoms of PTMA and CH3CN are refined isotropically, and hydrogen atoms attached to them are not included. When one atomic site is occupied by two kinds of atoms (C and N), the site is represented by either one. Since C(11) (part of PTMA) and C(17) (part of CH3CN) are closely located, their coordinates are not refined (positions were determined by the difference synthesis). Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1930 _reflns_number_gt 1326 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.0534 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1326 _refine_ls_number_parameters 131 _refine_ls_goodness_of_fit_ref 2.943 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_shift/su_max 0.0555 _refine_diff_density_max 0.87 _refine_diff_density_min -0.53 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Fe' 'Fe' 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe(1) Fe 1.0000 0.0000 1.0000 0.0190(3) Uani 1.00 d S . . N(1) N 0.9635(2) 0.1752(4) 1.0842(2) 0.0174(7) Uani 1.00 d . . . N(2) N 1.0000 0.0000 1.2079(2) 0.021(1) Uani 1.00 d S . . N(3) N 0.8959(3) 0.4189(6) 1.0000 0.019(1) Uani 1.00 d S . . N(4) N 1.2195(3) 0.1073(7) 1.0000 0.033(1) Uani 1.00 d S . . N(6) N 0.5842(6) 0.333(1) 1.0000 0.061(2) Uiso 0.75 d SP . . C(1) C 0.9651(2) 0.1454(5) 1.1679(2) 0.0199(8) Uani 1.00 d . . . C(2) C 0.9196(2) 0.2991(5) 1.2106(2) 0.0190(9) Uani 1.00 d . . . C(3) C 0.9020(2) 0.3294(5) 1.2942(2) 0.0241(10) Uani 1.00 d . . . C(4) C 0.8524(2) 0.4898(6) 1.3144(2) 0.0292(9) Uani 1.00 d . . . C(5) C 0.8232(3) 0.6148(5) 1.2542(2) 0.0294(10) Uani 1.00 d . . . C(6) C 0.8416(2) 0.5838(5) 1.1701(2) 0.0225(9) Uani 1.00 d . . . C(7) C 0.8899(2) 0.4214(5) 1.1501(2) 0.0186(8) Uani 1.00 d . . . C(8) C 0.9176(2) 0.3411(5) 1.0715(2) 0.0194(9) Uani 1.00 d . . . C(9) C 1.1380(4) 0.0783(7) 1.0000 0.021(1) Uani 1.00 d S . . C(10) C 0.5000 0.5000 1.0000 0.024(3) Uiso 0.50 d SP . . C(11) C 0.4991 0.3160 1.0000 0.042(6) Uiso 0.25 d SP . . C(12) C 0.5609(8) 0.189(1) 1.0000 0.027(3) Uiso 0.50 d SP . . C(13) C 0.660(1) 0.291(3) 1.0000 0.015(4) Uiso 0.25 d SP . . C(14) C 0.6645(8) 0.467(2) 1.0000 0.083(4) Uiso 0.75 d SP . . C(15) C 0.587(1) 0.605(2) 1.0000 0.005(3) Uiso 0.25 d SP . . C(16) C 0.6580(8) 0.402(2) 1.0717(7) 0.088(4) Uiso 0.50 d P . . C(17) C 0.4996 0.2266 1.0000 0.076(5) Uiso 0.50 d SP . . H(3) H 0.9233 0.2424 1.3359 0.0272 Uiso 1.00 calc . . . H(4) H 0.8376 0.5141 1.3711 0.0334 Uiso 1.00 calc . . . H(5) H 0.7889 0.7272 1.2710 0.0341 Uiso 1.00 calc . . . H(6) H 0.8229 0.6705 1.1290 0.0261 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0227(5) 0.0211(5) 0.0131(5) 0.0025(6) 0.0000 0.0000 N(1) 0.020(1) 0.019(1) 0.013(1) 0.001(1) 0.000(1) -0.001(1) N(2) 0.026(2) 0.021(2) 0.017(2) -0.003(2) 0.0000 0.0000 N(3) 0.021(2) 0.025(2) 0.012(2) 0.001(2) 0.0000 0.0000 N(4) 0.033(3) 0.046(3) 0.019(2) 0.001(3) 0.0000 0.0000 C(1) 0.020(2) 0.022(2) 0.018(2) -0.002(2) -0.002(1) -0.001(2) C(2) 0.015(2) 0.022(2) 0.020(2) 0.000(1) 0.003(1) -0.002(2) C(3) 0.026(2) 0.028(2) 0.018(2) 0.004(2) 0.000(2) 0.002(2) C(4) 0.034(2) 0.036(2) 0.018(2) 0.006(2) 0.007(1) -0.002(2) C(5) 0.033(2) 0.029(2) 0.026(2) 0.010(2) 0.003(2) -0.006(2) C(6) 0.021(2) 0.023(2) 0.023(2) 0.001(2) -0.001(2) 0.005(2) C(7) 0.017(2) 0.022(2) 0.017(2) -0.001(2) 0.000(1) 0.001(2) C(8) 0.017(2) 0.021(2) 0.021(2) 0.001(1) 0.002(1) 0.000(2) C(9) 0.027(3) 0.024(3) 0.011(2) 0.002(3) 0.0000 0.0000 #--------------------------------------------------------------------------- _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; Since PTMA and CH3CN are orientationally disordered and partially occupy the same site complementarily, unusual geometry is included (N(5), C(10)-C(17)). ; 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 Fe(1) N(1) 1.929(3) . . yes Fe(1) N(1) 1.929(3) . 6_557 yes Fe(1) N(1) 1.929(3) . 2_755 yes Fe(1) N(1) 1.929(3) . 5_757 yes Fe(1) C(9) 1.995(5) . . yes Fe(1) C(9) 1.995(5) . 2_755 yes N(1) C(1) 1.369(4) . . yes N(1) C(8) 1.376(4) . . yes N(2) C(1) 1.327(4) . . yes N(2) C(1) 1.327(4) . 2_755 yes N(3) C(8) 1.320(4) . . yes N(3) C(8) 1.320(4) . 6_557 yes N(4) C(9) 1.148(6) . . yes N(6) C(10) 1.682(8) . . yes N(6) C(11) 1.184(8) . . yes N(6) C(12) 1.09(1) . . yes N(6) C(13) 1.09(2) . . yes N(6) C(14) 1.48(1) . . yes N(6) C(16) 1.62(1) . . yes N(6) C(16) 1.62(1) . 6_557 yes N(6) C(17) 1.402(8) . . yes C(1) C(2) 1.455(4) . . yes C(2) C(3) 1.390(4) . . yes C(2) C(7) 1.382(4) . . yes C(3) C(4) 1.389(5) . . yes C(3) H(3) 0.969 . . no C(4) C(5) 1.390(5) . . yes C(4) H(4) 0.956 . . no C(5) C(6) 1.401(5) . . yes C(5) H(5) 0.981 . . no C(6) C(7) 1.391(4) . . yes C(6) H(6) 0.950 . . no C(7) C(8) 1.447(5) . . yes C(10) C(11) 1.334 . . yes C(10) C(11) 1.334 . 2_665 yes C(10) C(15) 1.42(2) . . yes C(10) C(15) 1.42(2) . 2_665 yes C(11) C(12) 1.26(1) . . yes C(11) C(15) 1.32(2) . 2_665 yes C(11) C(17) 0.648 . . yes C(12) C(13) 1.56(2) . . yes C(12) C(17) 0.89(1) . . yes C(13) C(14) 1.28(2) . . yes C(13) C(16) 1.41(2) . . yes C(13) C(16) 1.41(2) . 6_557 yes C(14) C(15) 1.47(2) . . yes C(14) C(16) 1.25(1) . . yes C(14) C(16) 1.25(1) . 6_557 yes C(15) C(17) 1.71(2) . 2_665 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 N(1) Fe(1) N(1) 89.7(2) . 1_555 6_557 yes N(1) Fe(1) N(1) 90.3(2) . 1_555 2_755 yes N(1) Fe(1) N(1) 180.0 . 1_555 5_757 yes N(1) Fe(1) C(9) 93.7(1) . 1_555 1_555 yes N(1) Fe(1) C(9) 86.3(1) . 1_555 2_755 yes N(1) Fe(1) N(1) 180.0 . 6_557 2_755 yes N(1) Fe(1) N(1) 90.3(2) . 6_557 5_757 yes N(1) Fe(1) C(9) 93.7(1) . 6_557 1_555 yes N(1) Fe(1) C(9) 86.3(1) . 6_557 2_755 yes N(1) Fe(1) N(1) 89.7(2) . 2_755 5_757 yes N(1) Fe(1) C(9) 86.3(1) . 2_755 1_555 yes N(1) Fe(1) C(9) 93.7(1) . 2_755 2_755 yes N(1) Fe(1) C(9) 86.3(1) . 5_757 1_555 yes N(1) Fe(1) C(9) 93.7(1) . 5_757 2_755 yes C(9) Fe(1) C(9) 180.0 . 1_555 2_755 yes Fe(1) N(1) C(1) 126.0(2) . 1_555 1_555 yes Fe(1) N(1) C(8) 126.3(2) . 1_555 1_555 yes C(1) N(1) C(8) 107.0(3) . 1_555 1_555 yes C(1) N(2) C(1) 121.7(4) . 1_555 2_755 yes C(8) N(3) C(8) 122.1(4) . 1_555 6_557 yes C(10) N(6) C(11) 52.0(3) . 1_555 1_555 yes C(10) N(6) C(12) 119.0(9) . 1_555 1_555 yes C(10) N(6) C(13) 150(1) . 1_555 1_555 yes C(10) N(6) C(14) 92.6(7) . 1_555 1_555 yes C(10) N(6) C(16) 102.3(6) . 1_555 1_555 yes C(10) N(6) C(16) 102.3(6) . 1_555 6_557 yes C(10) N(6) C(17) 79.4(4) . 1_555 1_555 yes C(11) N(6) C(12) 66.9(8) . 1_555 1_555 yes C(11) N(6) C(13) 157(1) . 1_555 1_555 yes C(11) N(6) C(14) 144.7(9) . 1_555 1_555 yes C(11) N(6) C(16) 131.1(5) . 1_555 1_555 yes C(11) N(6) C(16) 131.1(5) . 1_555 6_557 yes C(11) N(6) C(17) 27.4(2) . 1_555 1_555 yes C(12) N(6) C(13) 90(1) . 1_555 1_555 yes C(12) N(6) C(14) 148(1) . 1_555 1_555 yes C(12) N(6) C(16) 118.7(7) . 1_555 1_555 yes C(12) N(6) C(16) 118.7(7) . 1_555 6_557 yes C(12) N(6) C(17) 39.5(7) . 1_555 1_555 yes C(13) N(6) C(14) 57(1) . 1_555 1_555 yes C(13) N(6) C(16) 58.8(7) . 1_555 1_555 yes C(13) N(6) C(16) 58.8(7) . 1_555 6_557 yes C(13) N(6) C(17) 130(1) . 1_555 1_555 yes C(14) N(6) C(16) 47.4(5) . 1_555 1_555 yes C(14) N(6) C(16) 47.4(5) . 1_555 6_557 yes C(14) N(6) C(17) 172.1(8) . 1_555 1_555 yes C(16) N(6) C(16) 91.0(9) . 1_555 6_557 yes C(16) N(6) C(17) 134.1(5) . 1_555 1_555 yes C(16) N(6) C(17) 134.1(5) . 6_557 1_555 yes N(1) C(1) N(2) 127.8(3) . 1_555 1_555 yes N(1) C(1) C(2) 109.9(3) . 1_555 1_555 yes N(2) C(1) C(2) 122.4(3) . 1_555 1_555 yes C(1) C(2) C(3) 131.1(3) . 1_555 1_555 yes C(1) C(2) C(7) 106.6(3) . 1_555 1_555 yes C(3) C(2) C(7) 122.3(3) . 1_555 1_555 yes C(2) C(3) C(4) 116.6(3) . 1_555 1_555 yes C(2) C(3) H(3) 121.3 . 1_555 1_555 no C(4) C(3) H(3) 122.1 . 1_555 1_555 no C(3) C(4) C(5) 121.7(3) . 1_555 1_555 yes C(3) C(4) H(4) 119.1 . 1_555 1_555 no C(5) C(4) H(4) 119.2 . 1_555 1_555 no C(4) C(5) C(6) 121.4(3) . 1_555 1_555 yes C(4) C(5) H(5) 119.3 . 1_555 1_555 no C(6) C(5) H(5) 119.4 . 1_555 1_555 no C(5) C(6) C(7) 116.7(3) . 1_555 1_555 yes C(5) C(6) H(6) 121.4 . 1_555 1_555 no C(7) C(6) H(6) 121.9 . 1_555 1_555 no C(2) C(7) C(6) 121.4(3) . 1_555 1_555 yes C(2) C(7) C(8) 106.4(3) . 1_555 1_555 yes C(6) C(7) C(8) 132.2(3) . 1_555 1_555 yes N(1) C(8) N(3) 127.5(3) . 1_555 1_555 yes N(1) C(8) C(7) 110.1(3) . 1_555 1_555 yes N(3) C(8) C(7) 122.4(3) . 1_555 1_555 yes Fe(1) C(9) N(4) 174.0(5) . 1_555 1_555 yes N(6) C(10) N(6) 180.0 . 1_555 2_665 yes N(6) C(10) C(11) 44.4(3) . 1_555 1_555 yes N(6) C(10) C(11) 135.6(3) . 1_555 2_665 yes N(6) C(10) C(15) 78.5(7) . 1_555 1_555 yes N(6) C(10) C(15) 101.5(7) . 1_555 2_665 yes N(6) C(10) C(11) 135.6(3) . 2_665 1_555 yes N(6) C(10) C(11) 44.4(3) . 2_665 2_665 yes N(6) C(10) C(15) 101.5(7) . 2_665 1_555 yes N(6) C(10) C(15) 78.5(7) . 2_665 2_665 yes C(11) C(10) C(11) 180.0 . 1_555 2_665 yes C(11) C(10) C(15) 122.9(6) . 1_555 1_555 yes C(11) C(10) C(15) 57.1(6) . 1_555 2_665 yes C(11) C(10) C(15) 57.1(6) . 2_665 1_555 yes C(11) C(10) C(15) 122.9(6) . 2_665 2_665 yes C(15) C(10) C(15) 180.0 . 1_555 2_665 yes N(6) C(11) C(10) 83.6(4) . 1_555 1_555 yes N(6) C(11) C(12) 52.9(5) . 1_555 1_555 yes N(6) C(11) C(15) 148.4(8) . 1_555 2_665 yes N(6) C(11) C(17) 95.3(4) . 1_555 1_555 yes C(10) C(11) C(12) 136.5(5) . 1_555 1_555 yes C(10) C(11) C(15) 64.8(7) . 1_555 2_665 yes C(10) C(11) C(17) 178.8780(1) . 1_555 1_555 yes C(12) C(11) C(15) 158.7(8) . 1_555 2_665 yes C(12) C(11) C(17) 42.4(5) . 1_555 1_555 yes C(15) C(11) C(17) 116.3(7) . 2_665 1_555 yes N(6) C(12) C(11) 60.1(7) . 1_555 1_555 yes N(6) C(12) C(13) 44.6(9) . 1_555 1_555 yes N(6) C(12) C(17) 89(1) . 1_555 1_555 yes C(11) C(12) C(13) 104(1) . 1_555 1_555 yes C(11) C(12) C(17) 29.3(4) . 1_555 1_555 yes C(13) C(12) C(17) 133(1) . 1_555 1_555 yes N(6) C(13) C(12) 44.4(9) . 1_555 1_555 yes N(6) C(13) C(14) 76(1) . 1_555 1_555 yes N(6) C(13) C(16) 79(1) . 1_555 1_555 yes N(6) C(13) C(16) 79(1) . 1_555 6_557 yes C(12) C(13) C(14) 121(1) . 1_555 1_555 yes C(12) C(13) C(16) 104.7(10) . 1_555 1_555 yes C(12) C(13) C(16) 104.7(10) . 1_555 6_557 yes C(14) C(13) C(16) 55.3(8) . 1_555 1_555 yes C(14) C(13) C(16) 55.3(8) . 1_555 6_557 yes C(16) C(13) C(16) 110(1) . 1_555 6_557 yes N(6) C(14) C(13) 45.9(9) . 1_555 1_555 yes N(6) C(14) C(15) 84.0(9) . 1_555 1_555 yes N(6) C(14) C(16) 72.3(8) . 1_555 1_555 yes N(6) C(14) C(16) 72.3(8) . 1_555 6_557 yes C(13) C(14) C(15) 129(1) . 1_555 1_555 yes C(13) C(14) C(16) 67.6(8) . 1_555 1_555 yes C(13) C(14) C(16) 67.6(8) . 1_555 6_557 yes C(15) C(14) C(16) 101.8(9) . 1_555 1_555 yes C(15) C(14) C(16) 101.8(9) . 1_555 6_557 yes C(16) C(14) C(16) 134(1) . 1_555 6_557 yes C(10) C(15) C(11) 58.1(6) . 1_555 2_665 yes C(10) C(15) C(14) 104(1) . 1_555 1_555 yes C(10) C(15) C(17) 77.9(7) . 1_555 2_665 yes C(11) C(15) C(14) 162(1) . 2_665 1_555 yes C(11) C(15) C(17) 19.9(3) . 2_665 2_665 yes C(14) C(15) C(17) 177(1) . 1_555 2_665 yes N(6) C(16) C(13) 41.5(8) . 1_555 1_555 yes N(6) C(16) C(14) 60.3(8) . 1_555 1_555 yes C(13) C(16) C(14) 57.1(10) . 1_555 1_555 yes N(6) C(17) C(11) 57.3(3) . 1_555 1_555 yes N(6) C(17) C(12) 51.1(7) . 1_555 1_555 yes N(6) C(17) C(15) 101.1(6) . 1_555 2_665 yes C(11) C(17) C(12) 108.3(7) . 1_555 1_555 yes C(11) C(17) C(15) 43.8(5) . 1_555 2_665 yes C(12) C(17) C(15) 152.2(9) . 1_555 2_665 yes #===END data_(PTMA)x[Co(Pc)(CN)2].y(acetone)(113K) #--------------------------------------------------------------------------- _database_code_CSD 157359 # CHEMICAL DATA _chemical_formula_sum 'C41.5 H30 Co N10.5 O ' _chemical_formula_moiety '?' _chemical_formula_weight 749.72 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nnm' _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/2+x,1/2-y,1/2-z 1/2-x,1/2+y,1/2-z -x,-y,-z x,y,-z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,1/2+z _cell_length_a 13.6682(5) _cell_length_b 7.3102(2) _cell_length_c 16.3705(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1635.7(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 14898 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 113 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type none #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15650 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; The stoichiometry is assumed as x=0.5 and y=1. PTMA is orientationally disordered, and PTMA and acetone partially occupy the same site complementarily. Non-hydrogen atoms of PTMA and acetone are refined isotropically, and hydrogen atoms attached to them are not included. When one atomic site is occupied by two kinds of atoms (C and N), the site is represented by either one. Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1950 _reflns_number_gt 1060 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0530 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1060 _refine_ls_number_parameters 135 _refine_ls_goodness_of_fit_ref 1.343 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0012 _refine_diff_density_max 0.30 _refine_diff_density_min -0.33 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Co' 'Co' 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 1.0000 0.0000 1.0000 0.0207(3) Uani 1.00 d S . . O(1) O 0.5108(9) 0.247(2) 1.0000 0.052(3) Uiso 0.50 d SP . . N(1) N 0.9625(2) 0.1733(4) 1.0835(2) 0.0214(8) Uani 1.00 d . . . N(2) N 1.0000 0.0000 1.2060(2) 0.023(1) Uani 1.00 d S . . N(3) N 0.8950(3) 0.4163(6) 1.0000 0.022(1) Uani 1.00 d S . . N(4) N 1.2181(4) 0.1114(8) 1.0000 0.035(1) Uani 1.00 d S . . N(5) N 0.5875(6) 0.345(1) 1.0000 0.054(2) Uiso 0.75 d SP . . C(1) C 0.9651(3) 0.1442(5) 1.1662(2) 0.0221(9) Uani 1.00 d . . . C(2) C 0.9198(2) 0.2964(5) 1.2084(2) 0.0206(9) Uani 1.00 d . . . C(3) C 0.9024(3) 0.3270(6) 1.2909(2) 0.0244(10) Uani 1.00 d . . . C(4) C 0.8524(3) 0.4882(7) 1.3114(2) 0.0288(10) Uani 1.00 d . . . C(5) C 0.8232(3) 0.6108(5) 1.2511(2) 0.027(1) Uani 1.00 d . . . C(6) C 0.8406(3) 0.5802(6) 1.1685(2) 0.0246(9) Uani 1.00 d . . . C(7) C 0.8896(3) 0.4180(5) 1.1487(2) 0.0217(9) Uani 1.00 d . . . C(8) C 0.9169(3) 0.3383(5) 1.0707(2) 0.0214(10) Uani 1.00 d . . . C(9) C 1.1358(4) 0.0796(8) 1.0000 0.024(1) Uani 1.00 d S . . C(10) C 0.5000 0.5000 1.0000 0.031(4) Uiso 0.50 d SP . . C(11) C 0.472(2) 0.347(3) 1.0000 0.024(5) Uiso 0.25 d SP . . C(12) C 0.558(1) 0.168(2) 1.0000 0.043(3) Uiso 0.50 d SP . . C(13) C 0.655(2) 0.273(4) 1.0000 0.036(6) Uiso 0.25 d SP . . C(14) C 0.664(2) 0.475(3) 1.0000 0.029(5) Uiso 0.25 d SP . . C(15) C 0.589(2) 0.592(3) 1.0000 0.019(5) Uiso 0.25 d SP . . C(16) C 0.6424(6) 0.397(1) 1.0762(4) 0.062(2) Uiso 0.75 d P . . H(1) H 0.8217 0.6727 1.1221 0.0450 Uiso 1.00 calc . . . H(2) H 0.7884 0.7168 1.2652 0.0450 Uiso 1.00 calc . . . H(3) H 0.8333 0.4792 1.3759 0.0450 Uiso 1.00 calc . . . H(4) H 0.9259 0.2398 1.3324 0.0450 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0223(5) 0.0263(5) 0.0135(5) 0.0014(6) 0.0000 0.0000 N(1) 0.022(2) 0.027(2) 0.015(1) 0.003(1) -0.001(1) 0.001(1) N(2) 0.025(2) 0.029(2) 0.016(2) 0.003(3) 0.0000 0.0000 N(3) 0.021(2) 0.028(2) 0.019(2) 0.003(2) 0.0000 0.0000 N(4) 0.029(3) 0.055(4) 0.021(3) 0.001(3) 0.0000 0.0000 C(1) 0.021(2) 0.028(2) 0.018(2) -0.005(2) -0.002(1) 0.000(2) C(2) 0.016(2) 0.026(2) 0.020(2) -0.002(2) 0.000(2) -0.002(2) C(3) 0.023(2) 0.031(2) 0.018(2) 0.000(2) 0.000(2) 0.000(2) C(4) 0.027(2) 0.039(2) 0.020(2) 0.000(2) 0.004(2) -0.001(2) C(5) 0.020(2) 0.038(2) 0.024(2) 0.006(2) 0.001(2) -0.005(2) C(6) 0.021(2) 0.031(2) 0.022(2) 0.000(2) 0.000(2) 0.002(2) C(7) 0.017(2) 0.027(2) 0.021(2) -0.002(2) 0.000(2) 0.002(2) C(8) 0.019(2) 0.025(2) 0.020(2) -0.002(2) -0.001(1) -0.001(2) C(9) 0.033(3) 0.027(3) 0.011(2) 0.002(3) 0.0000 0.0000 #--------------------------------------------------------------------------- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; Since orientationally disordered PTMA and acetone partially occupy the same site complementarily, unusual geometry is included (O(1), N(5), C(10)-C(16)). ; 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 Co N(1) 1.932(3) . . yes Co N(1) 1.932(3) . 6_557 yes Co N(1) 1.932(3) . 2_755 yes Co N(1) 1.932(3) . 5_757 yes Co C(9) 1.945(6) . . yes Co C(9) 1.945(6) . 2_755 yes O(1) N(5) 1.27(1) . . yes O(1) C(11) 0.90(2) . . yes O(1) C(12) 0.86(2) . . yes O(1) C(15) 1.80(2) . 2_665 yes N(1) C(1) 1.372(4) . . yes N(1) C(8) 1.374(5) . . yes N(2) C(1) 1.327(4) . . yes N(2) C(1) 1.327(4) . 2_755 yes N(3) C(8) 1.324(4) . . yes N(3) C(8) 1.324(4) . 6_557 yes N(4) C(9) 1.149(7) . . yes N(5) C(10) 1.646(9) . . yes N(5) C(11) 1.58(2) . . yes N(5) C(12) 1.36(2) . . yes N(5) C(13) 1.07(3) . . yes N(5) C(14) 1.42(2) . . yes N(5) C(15) 1.81(2) . . yes N(5) C(16) 1.506(9) . . yes N(5) C(16) 1.506(9) . 6_557 yes C(1) C(2) 1.449(5) . . yes C(2) C(3) 1.390(5) . . yes C(2) C(7) 1.385(5) . . yes C(3) C(4) 1.403(6) . . yes C(3) H(4) 0.985 . . no C(4) C(5) 1.392(6) . . yes C(4) H(3) 1.088 . . no C(5) C(6) 1.391(6) . . yes C(5) H(2) 0.937 . . no C(6) C(7) 1.400(5) . . yes C(6) H(1) 1.049 . . no C(7) C(8) 1.452(5) . . yes C(10) C(11) 1.18(2) . . yes C(10) C(11) 1.18(2) . 2_665 yes C(10) C(15) 1.39(2) . . yes C(10) C(15) 1.39(2) . 2_665 yes C(11) C(12) 1.76(3) . . yes C(11) C(15) 0.94(3) . 2_665 yes C(12) C(13) 1.54(3) . . yes C(13) C(14) 1.48(3) . . yes C(13) C(16) 1.55(2) . . yes C(13) C(16) 1.55(2) . 6_557 yes C(14) C(15) 1.34(3) . . yes C(14) C(16) 1.40(1) . . yes C(14) C(16) 1.40(1) . 6_557 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 N(1) Co N(1) 90.0(2) . 1_555 6_557 yes N(1) Co N(1) 90.0(2) . 1_555 2_755 yes N(1) Co N(1) 180.0 . 1_555 5_757 yes N(1) Co C(9) 93.2(1) . 1_555 1_555 yes N(1) Co C(9) 86.8(1) . 1_555 2_755 yes N(1) Co N(1) 180.0 . 6_557 2_755 yes N(1) Co N(1) 90.0(2) . 6_557 5_757 yes N(1) Co C(9) 93.2(1) . 6_557 1_555 yes N(1) Co C(9) 86.8(1) . 6_557 2_755 yes N(1) Co N(1) 90.0(2) . 2_755 5_757 yes N(1) Co C(9) 86.8(1) . 2_755 1_555 yes N(1) Co C(9) 93.2(1) . 2_755 2_755 yes N(1) Co C(9) 86.8(1) . 5_757 1_555 yes N(1) Co C(9) 93.2(1) . 5_757 2_755 yes C(9) Co C(9) 180.0 . 1_555 2_755 yes N(5) O(1) C(11) 91(1) . 1_555 1_555 yes N(5) O(1) C(12) 76(1) . 1_555 1_555 yes N(5) O(1) C(15) 104(1) . 1_555 2_665 yes C(11) O(1) C(12) 168(2) . 1_555 1_555 yes C(11) O(1) C(15) 13(1) . 1_555 2_665 yes C(12) O(1) C(15) 178(1) . 1_555 2_665 yes Co N(1) C(1) 126.1(3) . 1_555 1_555 yes Co N(1) C(8) 126.1(2) . 1_555 1_555 yes C(1) N(1) C(8) 107.3(3) . 1_555 1_555 yes C(1) N(2) C(1) 121.3(4) . 1_555 2_755 yes C(8) N(3) C(8) 121.9(5) . 1_555 6_557 yes O(1) N(5) C(10) 77.8(7) . 1_555 1_555 yes O(1) N(5) C(11) 34.9(9) . 1_555 1_555 yes O(1) N(5) C(12) 38.3(7) . 1_555 1_555 yes O(1) N(5) C(13) 115(1) . 1_555 1_555 yes O(1) N(5) C(14) 172(1) . 1_555 1_555 yes O(1) N(5) C(15) 124(1) . 1_555 1_555 yes O(1) N(5) C(16) 123.7(4) . 1_555 1_555 yes O(1) N(5) C(16) 123.7(4) . 1_555 6_557 yes C(10) N(5) C(11) 42.9(9) . 1_555 1_555 yes C(10) N(5) C(12) 116.0(9) . 1_555 1_555 yes C(10) N(5) C(13) 166(1) . 1_555 1_555 yes C(10) N(5) C(14) 94(1) . 1_555 1_555 yes C(10) N(5) C(15) 47.2(7) . 1_555 1_555 yes C(10) N(5) C(16) 100.8(5) . 1_555 1_555 yes C(10) N(5) C(16) 100.8(5) . 1_555 6_557 yes C(11) N(5) C(12) 73(1) . 1_555 1_555 yes C(11) N(5) C(13) 150(1) . 1_555 1_555 yes C(11) N(5) C(14) 137(1) . 1_555 1_555 yes C(11) N(5) C(15) 90(1) . 1_555 1_555 yes C(11) N(5) C(16) 119.8(5) . 1_555 1_555 yes C(11) N(5) C(16) 119.8(5) . 1_555 6_557 yes C(12) N(5) C(13) 77(1) . 1_555 1_555 yes C(12) N(5) C(14) 149(1) . 1_555 1_555 yes C(12) N(5) C(15) 163(1) . 1_555 1_555 yes C(12) N(5) C(16) 113.0(6) . 1_555 1_555 yes C(12) N(5) C(16) 113.0(6) . 1_555 6_557 yes C(13) N(5) C(14) 71(1) . 1_555 1_555 yes C(13) N(5) C(15) 119(1) . 1_555 1_555 yes C(13) N(5) C(16) 72.1(8) . 1_555 1_555 yes C(13) N(5) C(16) 72.1(8) . 1_555 6_557 yes C(14) N(5) C(15) 47(1) . 1_555 1_555 yes C(14) N(5) C(16) 57.3(4) . 1_555 1_555 yes C(14) N(5) C(16) 57.3(4) . 1_555 6_557 yes C(15) N(5) C(16) 75.0(6) . 1_555 1_555 yes C(15) N(5) C(16) 75.0(6) . 1_555 6_557 yes C(16) N(5) C(16) 111.9(8) . 1_555 6_557 yes N(1) C(1) N(2) 128.1(3) . 1_555 1_555 yes N(1) C(1) C(2) 109.9(3) . 1_555 1_555 yes N(2) C(1) C(2) 122.0(3) . 1_555 1_555 yes C(1) C(2) C(3) 131.4(4) . 1_555 1_555 yes C(1) C(2) C(7) 106.5(3) . 1_555 1_555 yes C(3) C(2) C(7) 122.1(4) . 1_555 1_555 yes C(2) C(3) C(4) 116.8(3) . 1_555 1_555 yes C(2) C(3) H(4) 120.6 . 1_555 1_555 no C(4) C(3) H(4) 122.5 . 1_555 1_555 no C(3) C(4) C(5) 120.7(3) . 1_555 1_555 yes C(3) C(4) H(3) 107.3 . 1_555 1_555 no C(5) C(4) H(3) 131.2 . 1_555 1_555 no C(4) C(5) C(6) 122.5(4) . 1_555 1_555 yes C(4) C(5) H(2) 120.2 . 1_555 1_555 no C(6) C(5) H(2) 117.3 . 1_555 1_555 no C(5) C(6) C(7) 116.3(4) . 1_555 1_555 yes C(5) C(6) H(1) 123.9 . 1_555 1_555 no C(7) C(6) H(1) 119.8 . 1_555 1_555 no C(2) C(7) C(6) 121.5(3) . 1_555 1_555 yes C(2) C(7) C(8) 106.7(3) . 1_555 1_555 yes C(6) C(7) C(8) 131.8(4) . 1_555 1_555 yes N(1) C(8) N(3) 127.8(3) . 1_555 1_555 yes N(1) C(8) C(7) 109.6(3) . 1_555 1_555 yes N(3) C(8) C(7) 122.6(3) . 1_555 1_555 yes Co C(9) N(4) 174.2(6) . 1_555 1_555 yes N(5) C(10) N(5) 180.0 . 1_555 2_665 yes N(5) C(10) C(11) 65(1) . 1_555 1_555 yes N(5) C(10) C(11) 114(1) . 1_555 2_665 yes N(5) C(10) C(15) 72.4(9) . 1_555 1_555 yes N(5) C(10) C(15) 107.6(9) . 1_555 2_665 yes N(5) C(10) C(11) 114(1) . 2_665 1_555 yes N(5) C(10) C(11) 65(1) . 2_665 2_665 yes N(5) C(10) C(15) 107.6(9) . 2_665 1_555 yes N(5) C(10) C(15) 72.4(9) . 2_665 2_665 yes C(11) C(10) C(11) 180.0000(1) . 1_555 2_665 yes C(11) C(10) C(15) 137(1) . 1_555 1_555 yes C(11) C(10) C(15) 42(1) . 1_555 2_665 yes C(11) C(10) C(15) 42(1) . 2_665 1_555 yes C(11) C(10) C(15) 137(1) . 2_665 2_665 yes C(15) C(10) C(15) 180.0 . 1_555 2_665 yes O(1) C(11) N(5) 53(1) . 1_555 1_555 yes O(1) C(11) C(10) 125(2) . 1_555 1_555 yes O(1) C(11) C(12) 5(1) . 1_555 1_555 yes O(1) C(11) C(15) 154(3) . 1_555 2_665 yes N(5) C(11) C(10) 71(1) . 1_555 1_555 yes N(5) C(11) C(12) 47.6(9) . 1_555 1_555 yes N(5) C(11) C(15) 152(2) . 1_555 2_665 yes C(10) C(11) C(12) 119(1) . 1_555 1_555 yes C(10) C(11) C(15) 80(2) . 1_555 2_665 yes C(12) C(11) C(15) 159(2) . 1_555 2_665 yes O(1) C(12) N(5) 65(1) . 1_555 1_555 yes O(1) C(12) C(11) 6(1) . 1_555 1_555 yes O(1) C(12) C(13) 108(1) . 1_555 1_555 yes N(5) C(12) C(11) 59(1) . 1_555 1_555 yes N(5) C(12) C(13) 42(1) . 1_555 1_555 yes C(11) C(12) C(13) 101(1) . 1_555 1_555 yes N(5) C(13) C(12) 59(1) . 1_555 1_555 yes N(5) C(13) C(14) 65(1) . 1_555 1_555 yes N(5) C(13) C(16) 67(1) . 1_555 1_555 yes N(5) C(13) C(16) 67(1) . 1_555 6_557 yes C(12) C(13) C(14) 124(2) . 1_555 1_555 yes C(12) C(13) C(16) 101(1) . 1_555 1_555 yes C(12) C(13) C(16) 101(1) . 1_555 6_557 yes C(14) C(13) C(16) 55.0(9) . 1_555 1_555 yes C(14) C(13) C(16) 55.0(9) . 1_555 6_557 yes C(16) C(13) C(16) 106(1) . 1_555 6_557 yes N(5) C(14) C(13) 43(1) . 1_555 1_555 yes N(5) C(14) C(15) 81(1) . 1_555 1_555 yes N(5) C(14) C(16) 64.6(9) . 1_555 1_555 yes N(5) C(14) C(16) 64.6(9) . 1_555 6_557 yes C(13) C(14) C(15) 124(2) . 1_555 1_555 yes C(13) C(14) C(16) 65.1(10) . 1_555 1_555 yes C(13) C(14) C(16) 65.1(10) . 1_555 6_557 yes C(15) C(14) C(16) 95(1) . 1_555 1_555 yes C(15) C(14) C(16) 95(1) . 1_555 6_557 yes C(16) C(14) C(16) 125(1) . 1_555 6_557 yes O(1) C(15) N(5) 130(1) . 2_665 1_555 yes O(1) C(15) C(10) 69.8(9) . 2_665 1_555 yes O(1) C(15) C(11) 12(1) . 2_665 2_665 yes O(1) C(15) C(14) 178(1) . 2_665 1_555 yes N(5) C(15) C(10) 60.4(9) . 1_555 1_555 yes N(5) C(15) C(11) 117(2) . 1_555 2_665 yes N(5) C(15) C(14) 50(1) . 1_555 1_555 yes C(10) C(15) C(11) 57(1) . 1_555 2_665 yes C(10) C(15) C(14) 111(1) . 1_555 1_555 yes C(11) C(15) C(14) 168(2) . 2_665 1_555 yes N(5) C(16) C(13) 40.7(9) . 1_555 1_555 yes N(5) C(16) C(14) 58.1(9) . 1_555 1_555 yes C(13) C(16) C(14) 59(1) . 1_555 1_555 yes #===END