# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1352 #============================================================================== data_jgm1 #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; tris-2-methylpiridinium nitrate sulphate ; _chemical_name_common 'tripicolinium nitrate sulphate' _chemical_formula_sum C18H21N5O7S _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety [N(CH2C5H5N)3](SO4)(NO3) _chemical_formula_weight 451.45 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P213' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,-y,1/2+z' '-x,1/2+y,1/2-z' '1/2+x,1/2-y,-z' '+z,+x,+y' '1/2+z,1/2-x,-y' '1/2-z,-x,1/2+y' '-z,1/2+x,1/2-y' '+y,+z,+x' '-y,1/2+z,1/2-x' '1/2+y,1/2-z,-x' '1/2-y,-z,1/2+x' _cell_length_a 12.6301(4) _cell_length_b 12.6301(4) _cell_length_c 12.6301(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2014.8(1) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.9 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.970 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames ' _diffrn_standards_decay_% 0 _diffrn_reflns_number 11037 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.3 _diffrn_reflns_theta_max 26.9 _diffrn_reflns_reduction_process 11037 _reflns_number_total 1382 _reflns_number_observed 1346 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.01F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment refine_xyzUiso _refine_ls_extinction_method ; B-C type 1 Lorentzian isotropic (1974) ; _refine_ls_extinction_coef 278(66) _refine_ls_abs_structure_details ; refine Rogers factor for S ; _refine_ls_abs_structure_Rogers -0.80(19) _refine_ls_number_reflns 1346 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_number_constraints 24 _refine_ls_R_factor_obs 0.035 _refine_ls_wR_factor_obs 0.050 _refine_ls_goodness_of_fit_obs 3.640 _refine_ls_shift/esd_max 0.0011 _refine_ls_shift/esd_mean 0.0002 _refine_diff_density_max 0.66(8) _refine_diff_density_min -0.48(8) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy S -0.29178(4) -0.29178 -0.29178 0.0165(2) Uij 0.3333 O1 -0.2221(1) -0.2221 -0.2221 0.0177(3) Uij 0.3333 O2 -0.3322(1) -0.3787(1) -0.2256(1) 0.0218(8) Uij 1. O3 0.3399(1) 0.3292(1) 0.4547(2) 0.0414(11) Uij 1. N1 -0.0798(1) -0.0798 -0.0798 0.0158(4) Uij 0.3333 N3 0.3737(1) 0.3737 0.3737 0.0214(4) Uij 0.3333 N11 -0.2846(1) -0.0308(1) -0.1494(1) 0.0172(9) Uij 1. C12 -0.3708(2) -0.0038(2) -0.2056(2) 0.0215(11) Uij 1. C13 -0.4220(2) 0.0898(2) -0.1840(2) 0.0242(12) Uij 1. C14 -0.3796(2) 0.1555(2) -0.1067(2) 0.0256(12) Uij 1. C15 -0.2894(2) 0.1259(2) -0.0512(2) 0.0221(11) Uij 1. C16 -0.2422(2) 0.0297(2) -0.0730(2) 0.0186(11) Uij 1. C17 -0.1487(2) -0.0125(2) -0.0135(2) 0.0183(11) Uij 1. HN11 -0.266(2) -0.091(3) -0.161(2) 0.035(8) Uiso 1. H12 -0.389(2) -0.046(2) -0.263(2) 0.027(7) Uiso 1. H13 -0.487(2) 0.106(2) -0.227(2) 0.036(7) Uiso 1. H14 -0.415(2) 0.219(2) -0.093(2) 0.016(5) Uiso 1. H15 -0.270(2) 0.167(2) 0.009(2) 0.012(5) Uiso 1. H17a -0.109(2) 0.043(2) 0.024(2) 0.020(5) Uiso 1. H17b -0.179(2) -0.051(2) 0.044(2) 0.039(7) Uiso 1. 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 S 0.0165(3) 0.0165 0.0165 -0.0018 -0.0018 -0.0018(2) O1 0.0177(6) 0.0177 0.0177 -0.0012 -0.0012 -0.0012(5) O2 0.0199(8) 0.0229(8) 0.0227(8) -0.0052(6) -0.0029(6) 0.0001(6) O3 0.0400(11) 0.0398(11) 0.0445(11) 0.0132(8) 0.0245(9) 0.0197(8) N1 0.0158(6) 0.0158 0.0158 -0.0006 -0.0006 -0.0006(7) N3 0.0214(7) 0.0214 0.0214 0.0027 0.0027 0.0027(8) N11 0.0167(9) 0.0165(9) 0.0183(9) 0.0011(7) -0.0007(7) 0.0002(7) C12 0.0169(10) 0.0266(12) 0.0209(11) 0.0003(9) -0.0017(8) 0.0027(9) C13 0.0236(12) 0.0237(12) 0.0253(12) 0.0041(9) -0.0009(9) 0.0047(8) C14 0.0262(12) 0.0213(11) 0.0294(13) 0.0083(10) 0.0028(10) 0.0012(9) C15 0.0244(11) 0.0210(11) 0.0210(11) -0.0010(9) 0.0046(9) -0.0020(9) C16 0.0183(11) 0.0213(11) 0.0163(11) -0.0026(8) 0.0038(8) 0.0020(8) C17 0.0164(11) 0.0207(11) 0.0177(11) 0.0016(8) 0.0012(8) -0.0040(8) # 5_555 0.000000 0 0 1 0.000000 1 0 0 0.000000 0 1 0 # 9_555 0.000000 0 1 0 0.000000 0 0 1 0.000000 1 0 0 #================================= # 10. MOLECULAR GEOMETRY 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 S O1 1.524(1) . . S O2 1.471(2) . . S O2 1.471(2) . 5_555 S O2 1.471(2) . 9_555 N3 O3 1.243(2) . . N3 O3 1.243(2) . 5_555 N3 O3 1.243(2) . 9_555 N1 C17 1.477(2) . . N1 C17 1.477(2) . 5_555 N1 C17 1.477(2) . 9_555 N11 C16 1.343(3) . . N11 C12 1.344(3) . . C12 C13 1.375(3) . . C13 C14 1.389(3) . . C14 C15 1.388(3) . . C15 C16 1.381(3) . . C16 C17 1.497(3) . . N11 HN11 0.81(3) . . C12 H12 0.93(2) . . C13 H13 1.00(3) . . C14 H14 0.93(2) . . C15 H15 0.95(2) . . C17 H17b 0.95(3) . . C17 H17a 0.98(2) . . 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 O1 S O2 107.66(7) . . . O1 S O2 107.66(7) . . 5_555 O1 S O2 107.66(7) . . 9_555 O2 S O2 111.22(6) . . 5_555 O2 S O2 111.22(6) . . 9_555 O2 S O2 111.22(6) 5_555 . 9_555 O3 N3 O3 120.0(1) . . 5_555 O3 N3 O3 120.0(1) . . 9_555 O3 N3 O3 120.0(1) 5_555 . 9_555 C17 N1 C17 110.3(1) . . 5_555 C17 N1 C17 110.3(1) . . 9_555 C17 N1 C17 110.3(1) 5_555 . 9_555 C12 N11 C16 123.9(2) . . . N11 C12 C13 119.6(2) . . . C12 C13 C14 118.2(2) . . . C13 C14 C15 120.7(2) . . . C14 C15 C16 119.4(2) . . . N11 C16 C15 118.1(2) . . . N11 C16 C17 118.2(2) . . . C15 C16 C17 123.6(2) . . . N1 C17 C16 112.6(2) . . . C16 N11 HN11 123.2(20) . . . C12 N11 HN11 112.3(20) . . . N11 C12 H12 118.1(15) . . . C13 C12 H12 121.9(15) . . . C12 C13 H13 116.7(15) . . . C14 C13 H13 125.2(15) . . . C15 C14 H14 122.6(13) . . . C13 C14 H14 116.8(13) . . . C16 C15 H15 121.7(13) . . . C14 C15 H15 117.9(13) . . . H17a C17 H17b 101.5(20) . . . N1 C17 H17b 112.0(18) . . . C16 C17 H17b 104.4(15) . . . N1 C17 H17a 112.4(13) . . . C16 C17 H17a 113.0(13) . . . loop_ _publ_manuscript_incl_extra_item '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA N11 HN11 O1 0.81(3) 1.91(3) 2.702(2) 166(3) #================================== data_jgm2 #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; bis-tri(2-pyridylmethyl)aminecalcium diperchlorate ; _chemical_name_common ; bis-tripicolylaminecalcium perchlorate ; _chemical_formula_sum C36H36N8O8Cl2Ca _chemical_formula_structural [Ca(C18H18N4)2](ClO4)2 _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_weight 819.715 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '1 P21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,1/2+y,1/2-z' '-x,-y,-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 9.7069(5) _cell_length_b 10.8978(5) _cell_length_c 18.3622(9) _cell_angle_alpha 90.0 _cell_angle_beta 103.411(1) _cell_angle_gamma 90.0 _cell_volume 1889.5(1) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.4 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.924 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames ' _diffrn_standards_decay_% 0 _diffrn_reflns_number 12025 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 28.4 _diffrn_reflns_reduction_process 12025 _reflns_number_total 4561 _reflns_number_observed 3903 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method ; B-C type 1 Lorentzian isotropic (1974) ; _refine_ls_extinction_coef 110(26) _refine_ls_number_reflns 3903 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.029 _refine_ls_wR_factor_obs 0.051 _refine_ls_goodness_of_fit_obs 1.757 _refine_ls_shift/esd_max 0.00093 _refine_ls_shift/esd_mean 0.00007 _refine_diff_density_max 0.34(5) _refine_diff_density_min -0.44(5) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Ca 0.00000 0.00000 0.50000 0.0130(2) Uij 0.5 Cl 0.37954(3) 0.53722(3) 0.64587(2) 0.0186(2) Uij 1.0 O1 0.37003(11) 0.41750(9) 0.67681(6) 0.0263(6) Uij 1.0 O2 0.23973(12) 0.58182(12) 0.61354(7) 0.0419(7) Uij 1.0 O3 0.45807(14) 0.52912(10) 0.58866(7) 0.0388(7) Uij 1.0 O4 0.45011(12) 0.61881(10) 0.70461(6) 0.0364(7) Uij 1.0 N1 0.07037(11) 0.21710(9) 0.55531(6) 0.0152(5) Uij 1.0 N11 0.08139(11) 0.15383(10) 0.41204(6) 0.0176(6) Uij 1.0 N21 0.20630(12) 0.00437(10) 0.61863(6) 0.0176(6) Uij 1.0 N31 -0.19700(11) 0.11685(10) 0.54383(6) 0.0187(6) Uij 1.0 C12 0.07257(14) 0.12777(13) 0.33936(8) 0.0218(7) Uij 1.0 C13 0.15330(16) 0.18602(14) 0.29668(8) 0.0266(8) Uij 1.0 C14 0.24809(16) 0.27578(14) 0.32983(9) 0.0282(8) Uij 1.0 C15 0.25719(15) 0.30510(12) 0.40459(8) 0.0236(7) Uij 1.0 C16 0.17202(13) 0.24235(12) 0.44360(7) 0.0171(7) Uij 1.0 C17 0.18704(13) 0.26835(12) 0.52562(8) 0.0188(7) Uij 1.0 C22 0.29818(14) -0.08836(12) 0.64064(8) 0.0209(7) Uij 1.0 C23 0.41050(15) -0.08225(13) 0.70272(8) 0.0242(7) Uij 1.0 C24 0.43052(15) 0.02519(13) 0.74419(8) 0.0252(8) Uij 1.0 C25 0.33701(14) 0.12165(12) 0.72256(7) 0.0207(7) Uij 1.0 C26 0.22581(13) 0.10755(12) 0.66031(7) 0.0165(6) Uij 1.0 C27 0.11617(14) 0.20715(11) 0.63737(7) 0.0172(6) Uij 1.0 C32 -0.31418(14) 0.06417(12) 0.55732(8) 0.0221(7) Uij 1.0 C33 -0.42150(14) 0.12941(14) 0.57735(8) 0.0259(8) Uij 1.0 C34 -0.40856(15) 0.25529(14) 0.58412(9) 0.0283(8) Uij 1.0 C35 -0.28915(15) 0.31132(13) 0.57035(9) 0.0257(8) Uij 1.0 C36 -0.18522(13) 0.23972(12) 0.55097(7) 0.0179(7) Uij 1.0 C37 -0.05456(14) 0.29748(11) 0.53404(8) 0.0192(7) Uij 1.0 H12 0.00763 0.06628 0.31623 0.0261 Uiso 1.0 H13 0.14380 0.16476 0.24558 0.0319 Uiso 1.0 H14 0.30580 0.31658 0.30213 0.0339 Uiso 1.0 H15 0.32058 0.36699 0.42863 0.0283 Uiso 1.0 H17a 0.27365 0.23375 0.55273 0.0225 Uiso 1.0 H17b 0.18912 0.35473 0.53273 0.0225 Uiso 1.0 H22 0.28523 -0.16187 0.61206 0.0251 Uiso 1.0 H23 0.47243 -0.15015 0.71657 0.0290 Uiso 1.0 H24 0.50718 0.03259 0.78681 0.0302 Uiso 1.0 H25 0.34890 0.19635 0.74997 0.0249 Uiso 1.0 H27a 0.03629 0.18861 0.65705 0.0207 Uiso 1.0 H27b 0.15565 0.28330 0.65711 0.0207 Uiso 1.0 H32 -0.32339 -0.02245 0.55279 0.0266 Uiso 1.0 H33 -0.50249 0.08861 0.58628 0.0311 Uiso 1.0 H34 -0.48050 0.30273 0.59801 0.0339 Uiso 1.0 H35 -0.27858 0.39791 0.57415 0.0309 Uiso 1.0 H37a -0.07211 0.31375 0.48187 0.0230 Uiso 1.0 H37b -0.03538 0.37231 0.56102 0.0230 Uiso 1.0 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 Ca 0.0120(2) 0.0125(2) 0.0143(2) -0.0016(1) 0.0025(1) -0.0015(1) Cl 0.0222(2) 0.0142(2) 0.0199(2) -0.0009(1) 0.0059(1) 0.0008(1) O1 0.0310(6) 0.0179(5) 0.0277(6) -0.0047(4) 0.0022(4) 0.0053(4) O2 0.0373(7) 0.0481(7) 0.0362(7) 0.0210(6) 0.0003(5) 0.0097(6) O3 0.0516(8) 0.0345(6) 0.0405(7) -0.0081(5) 0.0313(6) -0.0044(5) O4 0.0429(7) 0.0277(6) 0.0407(7) -0.0158(5) 0.0141(5) -0.0168(5) N1 0.0134(5) 0.0150(5) 0.0166(6) -0.0002(4) 0.0024(4) 0.0002(4) N11 0.0164(6) 0.0182(5) 0.0172(5) -0.0016(4) 0.0021(4) 0.0016(4) N21 0.0168(6) 0.0166(5) 0.0185(6) -0.0013(4) 0.0025(4) -0.0003(4) N31 0.0159(5) 0.0182(5) 0.0217(6) 0.0004(4) 0.0037(4) -0.0024(4) C12 0.0209(7) 0.0252(7) 0.0183(7) -0.0018(5) 0.0027(5) 0.0006(5) C13 0.0258(8) 0.0358(8) 0.0191(7) 0.0000(6) 0.0071(6) 0.0029(6) C14 0.0251(8) 0.0335(8) 0.0289(8) -0.0031(6) 0.0121(6) 0.0075(6) C15 0.0212(7) 0.0212(7) 0.0289(8) -0.0034(5) 0.0069(6) 0.0037(6) C16 0.0151(6) 0.0154(6) 0.0206(7) 0.0003(5) 0.0034(5) 0.0019(5) C17 0.0162(6) 0.0174(6) 0.0214(7) -0.0050(5) 0.0017(5) 0.0000(5) C22 0.0221(7) 0.0161(6) 0.0236(7) -0.0003(5) 0.0031(5) -0.0002(5) C23 0.0216(7) 0.0219(7) 0.0273(8) 0.0026(5) 0.0022(6) 0.0068(6) C24 0.0218(7) 0.0278(7) 0.0219(7) -0.0026(6) -0.0033(6) 0.0030(6) C25 0.0210(7) 0.0208(6) 0.0189(7) -0.0045(5) 0.0017(5) -0.0014(5) C26 0.0158(6) 0.0163(6) 0.0181(6) -0.0036(5) 0.0053(5) 0.0004(5) C27 0.0172(6) 0.0170(6) 0.0163(6) -0.0015(5) 0.0016(5) -0.0026(5) C32 0.0182(7) 0.0208(6) 0.0275(7) -0.0003(5) 0.0056(5) -0.0027(6) C33 0.0165(7) 0.0334(8) 0.0288(8) 0.0000(6) 0.0073(5) -0.0027(6) C34 0.0189(7) 0.0319(8) 0.0344(8) 0.0058(6) 0.0071(6) -0.0096(7) C35 0.0203(7) 0.0212(7) 0.0336(8) 0.0042(5) 0.0019(6) -0.0066(6) C36 0.0163(6) 0.0190(6) 0.0167(6) 0.0015(5) 0.0004(5) -0.0009(5) C37 0.0178(7) 0.0143(6) 0.0240(7) 0.0018(5) 0.0018(5) 0.0016(5) #================================= # 10. MOLECULAR GEOMETRY 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 Ca N11 2.576(1) . . Ca N11 2.576(1) . 3_556 Ca N31 2.577(1) . . Ca N31 2.577(1) . 3_556 Ca N21 2.595(1) . . Ca N21 2.595(1) . 3_556 Ca N1 2.603(1) . . Ca N1 2.603(1) . 3_556 Cl O1 1.434(1) . . Cl O2 1.434(1) . . Cl O3 1.437(1) . . Cl O4 1.442(1) . . N1 C17 1.476(2) . . N1 C27 1.473(2) . . N1 C37 1.473(2) . . N11 C12 1.348(2) . . N11 C16 1.343(2) . . N21 C22 1.346(2) . . N21 C26 1.349(2) . . N31 C32 1.347(2) . . N31 C36 1.348(2) . . C12 C13 1.384(2) . . C13 C14 1.383(2) . . C14 C15 1.392(2) . . C15 C16 1.393(2) . . C16 C17 1.506(2) . . C22 C23 1.384(2) . . C23 C24 1.386(2) . . C24 C25 1.385(2) . . C25 C26 1.387(2) . . C26 C27 1.510(2) . . C32 C33 1.380(2) . . C33 C34 1.381(2) . . C34 C35 1.384(2) . . C35 C36 1.386(2) . . C36 C37 1.511(2) . . C12 H12 0.950 . . C13 H13 0.950 . . C14 H14 0.950 . . C15 H15 0.950 . . C17 H17a 0.950 . . C17 H17b 0.950 . . C22 H22 0.950 . . C23 H23 0.950 . . C24 H24 0.950 . . C25 H25 0.950 . . C27 H27a 0.950 . . C27 H27b 0.950 . . C32 H32 0.950 . . C33 H33 0.950 . . C34 H34 0.950 . . C35 H35 0.950 . . C37 H37a 0.950 . . C37 H37b 0.950 . . 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 N1 Ca N1 180.00 . . 3_556 N1 Ca N11 64.03(3) . . . N1 Ca N11 115.97(3) 3_556 . . N1 Ca N21 64.80(3) . . . N1 Ca N21 115.20(3) 3_556 . . N1 Ca N31 64.88(3) . . . N1 Ca N31 115.12(3) 3_556 . . N11 Ca N11 180.00 . . 3_556 N11 Ca N21 103.01(3) . . . N11 Ca N21 76.99(3) 3_556 . . N11 Ca N31 103.41(3) . . . N11 Ca N31 76.59(3) 3_556 . . N21 Ca N21 180.00 . . 3_556 N21 Ca N31 102.29(4) . . . N21 Ca N31 77.71(4) 3_556 . . N31 Ca N31 180.00 . . 3_556 Ca N1 C17 110.75(7) . . . Ca N1 C27 108.78(7) . . . Ca N1 C37 108.16(7) . . . Ca N11 C12 121.70(9) . . . Ca N11 C16 117.54(8) . . . Ca N21 C22 124.52(8) . . . Ca N21 C26 118.11(8) . . . Ca N31 C32 124.48(8) . . . Ca N31 C36 117.97(8) . . . O1 Cl O2 109.30(7) . . . O2 Cl O3 109.26(8) . . . O2 Cl O4 109.90(7) . . . O1 Cl O3 109.12(7) . . . O1 Cl O4 109.12(7) . . . O3 Cl O4 110.13(7) . . . C27 N1 C37 110.5(1) . . . C17 N1 C27 109.3(1) . . . C17 N1 C37 109.4(1) . . . C12 N11 C16 117.6(1) . . . C22 N21 C26 117.3(1) . . . C32 N31 C36 117.5(1) . . . N11 C12 C13 123.3(1) . . . C12 C13 C14 118.8(1) . . . C13 C14 C15 118.7(1) . . . C14 C15 C16 119.0(1) . . . N11 C16 C15 122.6(1) . . . N11 C16 C17 117.9(1) . . . C15 C16 C17 119.4(1) . . . N1 C17 C16 113.2(1) . . . N21 C22 C23 123.5(1) . . . C22 C23 C24 118.5(1) . . . C23 C24 C25 119.0(1) . . . C24 C25 C26 119.0(1) . . . N21 C26 C25 122.7(1) . . . N21 C26 C27 116.3(1) . . . C25 C26 C27 120.9(1) . . . N1 C27 C26 111.4(1) . . . N31 C32 C33 123.5(1) . . . C32 C33 C34 118.5(1) . . . C33 C34 C35 119.0(1) . . . C34 C35 C36 119.3(1) . . . N31 C36 C35 122.3(1) . . . N31 C36 C37 116.7(1) . . . C35 C36 C37 120.9(1) . . . N1 C37 C36 112.1(1) . . . N11 C12 H12 118.3 . . . C13 C12 H12 118.3 . . . C14 C13 H13 120.6 . . . C12 C13 H13 120.6 . . . C13 C14 H14 120.7 . . . C15 C14 H14 120.7 . . . C14 C15 H15 120.5 . . . C16 C15 H15 120.5 . . . H17a C17 H17b 109.5 . . . N1 C17 H17a 108.5 . . . C16 C17 H17a 108.5 . . . N1 C17 H17b 108.5 . . . C16 C17 H17b 108.5 . . . N21 C22 H22 118.3 . . . C23 C22 H22 118.3 . . . C22 C23 H23 120.8 . . . C24 C23 H23 120.8 . . . C25 C24 H24 120.5 . . . C23 C24 H24 120.5 . . . C24 C25 H25 120.5 . . . C26 C25 H25 120.5 . . . H27a C27 H27b 109.5 . . . N1 C27 H27a 109.0 . . . C26 C27 H27a 109.0 . . . N1 C27 H27b 109.0 . . . C26 C27 H27b 109.0 . . . N31 C32 H32 118.3 . . . C33 C32 H32 118.3 . . . C32 C33 H33 120.7 . . . C34 C33 H33 120.7 . . . C33 C34 H34 120.5 . . . C35 C34 H34 120.5 . . . C34 C35 H35 120.4 . . . C36 C35 H35 120.4 . . . H37a C37 H37b 109.5 . . . N1 C37 H37a 108.8 . . . C36 C37 H37a 108.8 . . . N1 C37 H37b 108.8 . . . C36 C37 H37b 108.8 . . . N11 N1 N21 94.07(5) . . . N11 N1 N31 94.12(4) . . . N21 N1 N31 92.76(4) . . . N1 N11 N21 94.42(4) . . 3_556 N1 N11 N31 94.49(4) . . 3_556 N21 N11 N31 77.83(4) 3_556 . 3_556 N1 N21 N11 93.73(4) . . 3_556 N1 N21 N31 92.62(4) . . 3_556 N11 N21 N31 77.47(4) 3_556 . 3_556 N1 N31 N11 94.41(4) . . 3_556 N1 N31 N21 93.22(4) . . 3_556 N11 N31 N21 77.90(4) 3_556 . 3_556 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N1 N11 2.746(2) . . N1 N21 2.785(2) . . N1 N31 2.779(2) . . N11 N21 3.218(2) . 3_556 N11 N31 3.193(2) . 3_556 N21 N31 3.244(2) . 3_556