Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kuang-Lieh Lu' 'Wei-Hsien Hou' 'Hsiu-Mei Lin' 'Yen-Hsiang Liu' 'Huang-Chun Wu' _publ_contact_author_name 'Prof Kuang-Lieh Lu' _publ_contact_author_address ; Institute of Chemistry, Academia Sinica Nankang Taipei 115 TAIWAN ; _publ_contact_author_email 'LU@CHEM.SINICA.EDU.TW' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Crystal engineering toward intersecting channels in a interpenetrated diamondoid network based on a net-to-net H-bonding interaction ; data_1 _database_code_CSD 192958 _audit_creation_date 2002-11-05T10:06:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_formula_sum 'C12 H11 Cd N4 O4.50' _chemical_formula_moiety 'C12 H10 Cd N4 O4, 0.5(H2O)' _chemical_formula_weight 395.65 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Tetragonal _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.569(3) _cell_length_b 18.569(3) _cell_length_c 23.042(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7945(2) _cell_formula_units_Z 16 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 49743 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_special_details ; The crystalline sample of 1 was kept in a desiccator at room temperature for 15 h, and a single crystal of 1 was selected and mounted on the glass fiber for crystallographic analysis. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7675 _exptl_absorpt_correction_T_max 0.8776 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0076997 _diffrn_orient_matrix_ub_12 -0.0282498 _diffrn_orient_matrix_ub_13 -0.0363489 _diffrn_orient_matrix_ub_21 -0.0101107 _diffrn_orient_matrix_ub_22 0.0457508 _diffrn_orient_matrix_ub_23 -0.0214768 _diffrn_orient_matrix_ub_31 0.0524548 _diffrn_orient_matrix_ub_32 0.0046718 _diffrn_orient_matrix_ub_33 -0.0094752 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_number 21094 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 27.61 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 4485 _reflns_number_gt 3424 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. Due to the disorder nature of the solvent water molecule, the assignment of H atoms of the water molecules is not attempted. The framework of 1 contains solvent accessible volume. ; _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^)+(0.0685P)^2^+95.4501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0021(3) _refine_ls_number_reflns 4485 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.2154 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.015 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.5224(5) 0.8448(5) 0.7696(4) 0.063(2) Uani 1 1 d . . . C2 C 0.5540(5) 0.8334(6) 0.8212(4) 0.072(3) Uani 1 1 d . . . H2A H 0.53 0.821 0.8551 0.087 Uiso 1 1 calc R . . C3 C 0.6376(4) 0.8561(5) 0.7639(4) 0.058(2) Uani 1 1 d . . . H3A H 0.6833 0.8637 0.7485 0.07 Uiso 1 1 calc R . . C4 C 0.4464(5) 0.8388(5) 0.7514(4) 0.065(2) Uani 1 1 d . . . H4A H 0.4119 0.8329 0.7803 0.078 Uiso 1 1 calc R . . C5 C 0.4241(5) 0.8410(5) 0.6970(4) 0.061(2) Uani 1 1 d . . . H5A H 0.4584 0.8473 0.6681 0.073 Uiso 1 1 calc R . . C6 C 0.3485(5) 0.8342(5) 0.6796(4) 0.0562(19) Uani 1 1 d . . . C7 C 0.7198(5) 0.6076(5) 0.9492(4) 0.062(2) Uani 1 1 d . . . C8 C 0.7097(6) 0.6783(5) 0.9527(4) 0.071(2) Uani 1 1 d . . . H8A H 0.7028 0.7032 0.9873 0.085 Uiso 1 1 calc R . . C9 C 0.7201(5) 0.6572(5) 0.8633(4) 0.066(2) Uani 1 1 d . . . H9A H 0.7226 0.6628 0.8233 0.08 Uiso 1 1 calc R . . C10 C 0.7209(5) 0.5530(5) 0.9937(4) 0.069(2) Uani 1 1 d . . . H10A H 0.722 0.5696 1.0318 0.083 Uiso 1 1 calc R . . C11 C 0.7207(5) 0.4823(6) 0.9872(4) 0.072(2) Uani 1 1 d . . . H11A H 0.7227 0.4633 0.9499 0.087 Uiso 1 1 calc R . . C12 C 0.7172(5) 0.4320(6) 1.0376(5) 0.068(2) Uani 1 1 d . . . Cd1 Cd 0.71538(3) 0.82941(3) 0.87880(3) 0.0559(3) Uani 1 1 d . . . N1 N 0.5767(4) 0.8583(4) 0.7322(3) 0.0594(17) Uani 1 1 d . . . H1A H 0.5732 0.8667 0.6956 0.071 Uiso 1 1 calc R . . N2 N 0.6262(4) 0.8427(4) 0.8162(3) 0.0578(16) Uani 1 1 d . . . N3 N 0.7260(4) 0.5939(4) 0.8905(3) 0.0680(19) Uani 1 1 d . . . H3B H 0.7324 0.5526 0.8745 0.082 Uiso 1 1 calc R . . N4 N 0.7106(4) 0.7099(4) 0.8995(3) 0.0645(18) Uani 1 1 d . . . O1 O 0.7043(4) 0.3663(4) 1.0267(3) 0.081(2) Uani 1 1 d . . . O2 O 0.7239(4) 0.4555(4) 1.0883(3) 0.0743(18) Uani 1 1 d . . . O3 O 0.3367(3) 0.8311(4) 0.6259(3) 0.0719(17) Uani 1 1 d . . . O4 O 0.2987(3) 0.8322(4) 0.7146(3) 0.079(2) Uani 1 1 d . . . O91 O 0.5 0.75 1.0106(15) 0.216(13) Uani 1 2 d S . . 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 C1 0.057(5) 0.066(5) 0.067(5) 0.001(4) -0.003(4) -0.002(4) C2 0.057(5) 0.102(8) 0.059(5) 0.005(5) -0.010(4) -0.006(5) C3 0.043(4) 0.067(5) 0.065(5) 0.002(4) -0.007(4) -0.002(4) C4 0.046(4) 0.080(6) 0.070(6) 0.003(5) 0.000(4) 0.002(4) C5 0.055(5) 0.063(5) 0.064(5) 0.003(4) 0.000(4) 0.003(4) C6 0.053(5) 0.056(5) 0.059(5) 0.001(4) 0.002(4) 0.003(4) C7 0.068(5) 0.060(5) 0.058(5) 0.005(4) 0.001(4) 0.002(4) C8 0.094(7) 0.065(6) 0.054(5) -0.003(4) 0.008(5) 0.000(5) C9 0.072(6) 0.065(5) 0.062(5) 0.010(4) 0.009(4) 0.008(4) C10 0.074(6) 0.069(6) 0.064(5) 0.005(4) 0.002(4) 0.006(5) C11 0.076(6) 0.076(6) 0.065(5) 0.010(5) -0.003(5) -0.002(5) C12 0.055(5) 0.075(6) 0.073(6) 0.007(5) -0.010(4) -0.004(4) Cd1 0.0526(4) 0.0572(4) 0.0580(4) 0.0019(3) -0.0043(3) 0.0013(3) N1 0.054(4) 0.065(4) 0.059(4) 0.008(3) -0.003(3) -0.004(3) N2 0.053(4) 0.064(4) 0.057(4) 0.005(3) -0.002(3) 0.001(3) N3 0.074(5) 0.059(4) 0.071(5) -0.003(4) 0.002(4) 0.009(4) N4 0.073(5) 0.062(4) 0.058(4) -0.001(3) 0.008(4) 0.006(3) O1 0.110(6) 0.060(4) 0.073(4) 0.010(3) -0.018(4) 0.003(4) O2 0.084(5) 0.074(4) 0.065(4) 0.011(3) -0.016(3) -0.012(3) O3 0.061(4) 0.099(5) 0.056(4) -0.003(3) 0.001(3) 0.002(3) O4 0.054(4) 0.121(6) 0.063(4) 0.002(4) 0.003(3) 0.003(4) O91 0.121(14) 0.118(14) 0.41(4) 0 0 0.021(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.343(13) . ? C1 N1 1.349(11) . ? C1 C4 1.475(12) . ? C2 N2 1.357(11) . ? C2 H2A 0.93 . ? C3 N2 1.248(11) . ? C3 N1 1.347(10) . ? C3 H3A 0.93 . ? C4 C5 1.321(12) . ? C4 H4A 0.93 . ? C5 C6 1.465(12) . ? C5 H5A 0.93 . ? C6 O4 1.228(10) . ? C6 O3 1.258(10) . ? C7 C8 1.330(13) . ? C7 N3 1.380(11) . ? C7 C10 1.442(12) . ? C8 N4 1.358(12) . ? C8 H8A 0.93 . ? C9 N4 1.297(12) . ? C9 N3 1.336(12) . ? C9 H9A 0.93 . ? C10 C11 1.320(14) . ? C10 H10A 0.93 . ? C11 C12 1.493(13) . ? C11 H11A 0.93 . ? C12 O2 1.254(12) . ? C12 O1 1.268(12) . ? Cd1 N2 2.211(7) . ? Cd1 O3 2.256(7) 10_657 ? Cd1 N4 2.272(8) . ? Cd1 O1 2.291(7) 14_557 ? Cd1 O2 2.466(7) 14_557 ? N1 H1A 0.86 . ? N3 H3B 0.86 . ? 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 C2 C1 N1 105.5(8) . . ? C2 C1 C4 131.0(9) . . ? N1 C1 C4 123.3(8) . . ? C1 C2 N2 109.7(9) . . ? C1 C2 H2A 125.2 . . ? N2 C2 H2A 125.2 . . ? N2 C3 N1 112.7(8) . . ? N2 C3 H3A 123.7 . . ? N1 C3 H3A 123.7 . . ? C5 C4 C1 124.5(9) . . ? C5 C4 H4A 117.7 . . ? C1 C4 H4A 117.7 . . ? C4 C5 C6 123.9(8) . . ? C4 C5 H5A 118 . . ? C6 C5 H5A 118 . . ? O4 C6 O3 120.9(8) . . ? O4 C6 C5 123.0(8) . . ? O3 C6 C5 116.1(8) . . ? C8 C7 N3 104.6(8) . . ? C8 C7 C10 130.8(9) . . ? N3 C7 C10 124.5(8) . . ? C7 C8 N4 111.7(8) . . ? C7 C8 H8A 124.1 . . ? N4 C8 H8A 124.1 . . ? N4 C9 N3 111.9(8) . . ? N4 C9 H9A 124.1 . . ? N3 C9 H9A 124.1 . . ? C11 C10 C7 128.1(10) . . ? C11 C10 H10A 115.9 . . ? C7 C10 H10A 115.9 . . ? C10 C11 C12 122.3(10) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? O2 C12 O1 122.6(9) . . ? O2 C12 C11 120.2(9) . . ? O1 C12 C11 117.2(9) . . ? O2 C12 Cd1 65.4(5) . 14_547 ? O1 C12 Cd1 57.4(5) . 14_547 ? C11 C12 Cd1 173.9(8) . 14_547 ? N2 Cd1 O3 135.7(2) . 10_657 ? N2 Cd1 N4 102.5(3) . . ? O3 Cd1 N4 93.6(3) 10_657 . ? N2 Cd1 O1 121.3(3) . 14_557 ? O3 Cd1 O1 97.5(3) 10_657 14_557 ? N4 Cd1 O1 95.1(3) . 14_557 ? N2 Cd1 O2 98.2(3) . 14_557 ? O3 Cd1 O2 86.4(3) 10_657 14_557 ? N4 Cd1 O2 150.0(3) . 14_557 ? O1 Cd1 O2 55.3(2) 14_557 14_557 ? N2 Cd1 C12 113.3(3) . 14_557 ? O3 Cd1 C12 90.7(3) 10_657 14_557 ? N4 Cd1 C12 122.5(3) . 14_557 ? O1 Cd1 C12 27.8(3) 14_557 14_557 ? O2 Cd1 C12 27.5(3) 14_557 14_557 ? C3 N1 C1 106.1(8) . . ? C3 N1 H1A 127 . . ? C1 N1 H1A 127 . . ? C3 N2 C2 106.0(7) . . ? C3 N2 Cd1 121.6(6) . . ? C2 N2 Cd1 132.2(6) . . ? C9 N3 C7 106.9(8) . . ? C9 N3 H3B 126.5 . . ? C7 N3 H3B 126.5 . . ? C9 N4 C8 104.8(8) . . ? C9 N4 Cd1 126.6(6) . . ? C8 N4 Cd1 127.7(6) . . ? C12 O1 Cd1 94.8(6) . 14_547 ? C12 O2 Cd1 87.1(6) . 14_547 ? C6 O3 Cd1 102.9(5) . 10_557 ? # #===END data_1a _database_code_CSD 192959 _audit_creation_date 2002-10-08T17:32:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H10 Cd1 N4 O4' _chemical_formula_sum 'C12 H10 Cd N4 O4' _chemical_formula_weight 386.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.569(3) _cell_length_b 18.569(3) _cell_length_c 23.042(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7945(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.31 _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_factor_muR 0.518 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 2 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.6399 _exptl_absorpt_correction_T_max 0.7239 _exptl_absorpt_correction_T_ave 0.5676 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.035367 _diffrn_orient_matrix_ub_12 0.024166 _diffrn_orient_matrix_ub_13 0.02741 _diffrn_orient_matrix_ub_21 -0.03253 _diffrn_orient_matrix_ub_22 0.034365 _diffrn_orient_matrix_ub_23 -0.004692 _diffrn_orient_matrix_ub_31 -0.024315 _diffrn_orient_matrix_ub_32 -0.010887 _diffrn_orient_matrix_ub_33 0.046138 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.018 _diffrn_standards_decay_corr_min 0.968 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 9 1 0 8 2 -4 8 0 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_number 3546 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _reflns_number_total 3331 _reflns_number_gt 2124 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1558P)^2^+23.2024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00059(15) _refine_ls_number_reflns 3331 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.248 _refine_ls_wR_factor_gt 0.2156 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.058 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.211 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.71571(3) 0.82877(4) 0.87897(3) 0.0545(4) Uani 1 1 d . . . N1 N 0.5770(4) 0.8589(4) 0.7329(3) 0.0555(18) Uani 1 1 d . . . H1A H 0.5735 0.8678 0.6964 0.067 Uiso 1 1 calc R . . N2 N 0.6266(4) 0.8437(4) 0.8171(3) 0.0584(19) Uani 1 1 d . . . N3 N 0.7264(4) 0.5939(4) 0.8907(3) 0.064(2) Uani 1 1 d . . . H3B H 0.7325 0.5527 0.8743 0.077 Uiso 1 1 calc R . . N4 N 0.7110(4) 0.7107(4) 0.8993(3) 0.0601(19) Uani 1 1 d . . . O1 O 0.7059(4) 0.3654(4) 1.0260(3) 0.081(2) Uani 1 1 d . . . O2 O 0.7252(4) 0.4544(4) 1.0876(3) 0.0708(18) Uani 1 1 d . . . O3 O 0.3365(4) 0.8315(4) 0.6257(3) 0.071(2) Uani 1 1 d . . . O4 O 0.2979(4) 0.8325(5) 0.7160(3) 0.077(2) Uani 1 1 d . . . C1 C 0.5207(5) 0.8444(5) 0.7696(4) 0.058(2) Uani 1 1 d . . . C2 C 0.5533(5) 0.8341(6) 0.8218(4) 0.070(3) Uani 1 1 d . . . H2A H 0.5294 0.8223 0.8559 0.084 Uiso 1 1 calc R . . C3 C 0.6378(5) 0.8571(5) 0.7630(4) 0.059(2) Uani 1 1 d . . . H3A H 0.6832 0.8647 0.747 0.071 Uiso 1 1 calc R . . C4 C 0.4462(5) 0.8381(5) 0.7520(4) 0.064(2) Uani 1 1 d . . . H4A H 0.412 0.8315 0.7809 0.077 Uiso 1 1 calc R . . C5 C 0.4236(5) 0.8410(5) 0.6983(4) 0.060(2) Uani 1 1 d . . . H5A H 0.4577 0.8478 0.6692 0.073 Uiso 1 1 calc R . . C6 C 0.3478(5) 0.8342(5) 0.6810(4) 0.057(2) Uani 1 1 d . . . C7 C 0.7214(5) 0.6064(5) 0.9492(4) 0.056(2) Uani 1 1 d . . . C8 C 0.7119(6) 0.6793(5) 0.9529(4) 0.067(3) Uani 1 1 d . . . H8A H 0.7066 0.7043 0.9876 0.08 Uiso 1 1 calc R . . C9 C 0.7202(6) 0.6569(6) 0.8640(4) 0.068(3) Uani 1 1 d . . . H9A H 0.7222 0.6621 0.8239 0.082 Uiso 1 1 calc R . . C10 C 0.7223(5) 0.5527(5) 0.9935(4) 0.064(2) Uani 1 1 d . . . H10A H 0.7233 0.5693 1.0316 0.077 Uiso 1 1 calc R . . C11 C 0.7218(5) 0.4823(5) 0.9867(5) 0.067(3) Uani 1 1 d . . . H11A H 0.7247 0.4639 0.9492 0.081 Uiso 1 1 calc R . . C12 C 0.7171(5) 0.4309(6) 1.0359(5) 0.066(3) 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 Cd1 0.0515(5) 0.0573(5) 0.0548(6) 0.0019(3) -0.0053(3) 0.0020(3) N1 0.055(4) 0.066(5) 0.045(4) 0.001(3) -0.003(3) -0.002(3) N2 0.049(4) 0.069(5) 0.057(5) 0.003(4) -0.005(3) -0.004(4) N3 0.079(6) 0.059(5) 0.056(5) 0.003(4) 0.007(4) 0.013(4) N4 0.071(5) 0.057(5) 0.052(5) 0.005(4) 0.007(4) 0.011(4) O1 0.110(6) 0.058(5) 0.075(5) -0.003(4) -0.026(4) -0.004(4) O2 0.088(5) 0.069(4) 0.056(4) 0.002(3) -0.009(4) -0.008(3) O3 0.051(4) 0.108(6) 0.055(4) 0.000(4) -0.001(3) 0.000(4) O4 0.050(4) 0.121(6) 0.058(4) 0.001(4) 0.009(3) 0.001(4) C1 0.057(5) 0.064(6) 0.055(6) 0.000(4) -0.001(4) 0.002(4) C2 0.054(6) 0.097(8) 0.060(6) 0.009(5) 0.008(5) 0.003(5) C3 0.051(5) 0.063(6) 0.065(6) 0.009(4) -0.006(4) -0.007(4) C4 0.048(5) 0.085(7) 0.059(6) 0.006(5) 0.001(4) 0.007(4) C5 0.052(5) 0.062(6) 0.068(6) 0.004(4) 0.002(5) 0.002(4) C6 0.051(5) 0.059(5) 0.063(6) 0.002(4) -0.004(4) 0.002(4) C7 0.056(5) 0.060(5) 0.052(5) -0.003(4) 0.001(4) 0.002(4) C8 0.097(8) 0.060(6) 0.043(5) -0.003(4) 0.005(5) -0.007(5) C9 0.074(7) 0.076(7) 0.054(6) 0.009(5) 0.008(5) 0.008(5) C10 0.069(6) 0.067(6) 0.056(6) 0.009(5) -0.004(5) 0.003(5) C11 0.071(7) 0.063(6) 0.067(6) 0.009(5) -0.009(5) 0.010(5) C12 0.051(5) 0.074(7) 0.072(7) 0.014(5) -0.002(5) -0.003(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N2 2.201(7) . ? Cd1 N4 2.244(8) . ? Cd1 O3 2.246(7) 10_657 ? Cd1 O1 2.301(8) 14_557 ? Cd1 O2 2.462(7) 14_557 ? N1 C3 1.326(11) . ? N1 C1 1.372(12) . ? N1 H1A 0.86 . ? N2 C3 1.287(12) . ? N2 C2 1.377(12) . ? N3 C9 1.327(13) . ? N3 C7 1.372(12) . ? N3 H3B 0.86 . ? N4 C9 1.301(13) . ? N4 C8 1.366(12) . ? O1 C12 1.254(12) . ? O2 C12 1.278(12) . ? O3 C6 1.292(11) . ? O4 C6 1.229(11) . ? C1 C2 1.360(13) . ? C1 C4 1.445(13) . ? C2 H2A 0.93 . ? C3 H3A 0.93 . ? C4 C5 1.306(13) . ? C4 H4A 0.93 . ? C5 C6 1.469(13) . ? C5 H5A 0.93 . ? C7 C8 1.367(13) . ? C7 C10 1.429(13) . ? C8 H8A 0.93 . ? C9 H9A 0.93 . ? C10 C11 1.315(14) . ? C10 H10A 0.93 . ? C11 C12 1.485(14) . ? C11 H11A 0.93 . ? 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 N2 Cd1 N4 103.2(3) . . ? N2 Cd1 O3 135.7(3) . 10_657 ? N4 Cd1 O3 94.1(3) . 10_657 ? N2 Cd1 O1 121.3(3) . 14_557 ? N4 Cd1 O1 95.0(3) . 14_557 ? O3 Cd1 O1 96.8(3) 10_657 14_557 ? N2 Cd1 O2 97.9(3) . 14_557 ? N4 Cd1 O2 149.6(3) . 14_557 ? O3 Cd1 O2 85.5(3) 10_657 14_557 ? O1 Cd1 O2 55.1(2) 14_557 14_557 ? N2 Cd1 C12 112.7(3) . 14_557 ? N4 Cd1 C12 121.9(3) . 14_557 ? O3 Cd1 C12 90.6(3) 10_657 14_557 ? O1 Cd1 C12 27.2(3) 14_557 14_557 ? O2 Cd1 C12 27.9(3) 14_557 14_557 ? C3 N1 C1 108.7(8) . . ? C3 N1 H1A 125.6 . . ? C1 N1 H1A 125.6 . . ? C3 N2 C2 105.1(8) . . ? C3 N2 Cd1 122.0(6) . . ? C2 N2 Cd1 132.5(7) . . ? C9 N3 C7 107.4(9) . . ? C9 N3 H3B 126.3 . . ? C7 N3 H3B 126.3 . . ? C9 N4 C8 103.7(8) . . ? C9 N4 Cd1 127.9(7) . . ? C8 N4 Cd1 127.3(6) . . ? C12 O1 Cd1 95.7(6) . 14_547 ? C12 O2 Cd1 87.7(6) . 14_547 ? C6 O3 Cd1 102.2(6) . 10_557 ? C2 C1 N1 103.5(8) . . ? C2 C1 C4 131.5(9) . . ? N1 C1 C4 124.9(8) . . ? C1 C2 N2 110.7(9) . . ? C1 C2 H2A 124.7 . . ? N2 C2 H2A 124.7 . . ? N2 C3 N1 112.0(9) . . ? N2 C3 H3A 124 . . ? N1 C3 H3A 124 . . ? C5 C4 C1 124.8(9) . . ? C5 C4 H4A 117.6 . . ? C1 C4 H4A 117.6 . . ? C4 C5 C6 124.2(9) . . ? C4 C5 H5A 117.9 . . ? C6 C5 H5A 117.9 . . ? O4 C6 O3 121.6(9) . . ? O4 C6 C5 123.2(9) . . ? O3 C6 C5 115.3(9) . . ? C8 C7 N3 103.9(8) . . ? C8 C7 C10 130.4(9) . . ? N3 C7 C10 125.7(9) . . ? N4 C8 C7 111.5(8) . . ? N4 C8 H8A 124.2 . . ? C7 C8 H8A 124.2 . . ? N4 C9 N3 113.5(9) . . ? N4 C9 H9A 123.2 . . ? N3 C9 H9A 123.2 . . ? C11 C10 C7 127.5(10) . . ? C11 C10 H10A 116.2 . . ? C7 C10 H10A 116.2 . . ? C10 C11 C12 123.3(10) . . ? C10 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? O1 C12 O2 121.4(10) . . ? O1 C12 C11 119.6(10) . . ? O2 C12 C11 119.0(10) . . ? O1 C12 Cd1 57.0(5) . 14_547 ? O2 C12 Cd1 64.4(5) . 14_547 ? C11 C12 Cd1 175.2(8) . 14_547 ?