Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Bishop, Michael M.' 'Lindoy, Leonard F.' 'Skelton, Brian W.' 'White, Allan H.' _publ_requested_journal 'Dalton Transactions' #============================================================================== # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Prof Leonard F. Lindoy' _publ_contact_author_address ; School of Chemistry University of Sydney School of Chemistry F11, University Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_section_title ; #<< paper title text Modification of supramolecular motifs: some effects of incorporation of metal complexes into supramolecular arrays ; _publ_section_title_footnote ; ? #<< paper footnote text ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ii20mb _database_code_CSD 170261 _audit_creation_method Xtal3.6 _audit_creation_date 01-06-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H20 N10 Ni1 O2 S4' _chemical_formula_moiety ? _chemical_formula_weight 619.4 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 7.5020(10) _cell_length_b 7.6810(10) _cell_length_c 12.061(2) _cell_angle_alpha 91.773(2) _cell_angle_beta 107.638(2) _cell_angle_gamma 113.737(2) _cell_volume 596.90(15) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4093 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 23.1 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.206 _exptl_crystal_description prism _exptl_crystal_size_max .32 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .17 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .59 _exptl_absorpt_correction_T_max .93 _diffrn_reflns_number 7043 _reflns_number_total 2943 _reflns_Friedel_coverage 0 _reflns_number_gt 2607 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.34 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .029 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_number_reflns 2607 _refine_ls_number_parameters 209 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .021 _refine_diff_density_min -.629 _refine_diff_density_max .789 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 20 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 20 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 10 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ni ? 0 1 .285 1.113 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 4 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni .00000 .00000 .00000 .01764(15) Uani ? ? 1.00000 ? ? S1 .10256(8) -.07603(7) .17173(4) .0223(2) Uani ? ? 1.00000 ? ? C2 .2799(3) .1172(3) .28440(18) .0179(7) Uani ? ? 1.00000 ? ? N21 .2900(3) .0758(3) .39179(16) .0222(6) Uani ? ? 1.00000 ? ? N3 .4137(3) .2954(2) .28082(15) .0179(6) Uani ? ? 1.00000 ? ? C4 .4247(3) .3682(3) .18263(18) .0191(7) Uani ? ? 1.00000 ? ? N41 .5789(3) .5435(3) .19819(17) .0242(7) Uani ? ? 1.00000 ? ? S5 .26597(8) .27632(8) .03635(5) .0244(2) Uani ? ? 1.00000 ? ? C11 .7623(3) .4516(3) .61188(18) .0204(7) Uani ? ? 1.00000 ? ? N11 .6224(3) .2987(3) .62311(18) .0241(7) Uani ? ? 1.00000 ? ? N12 .7464(3) .5109(3) .50247(16) .0218(6) Uani ? ? 1.00000 ? ? C13 .9130(3) .6794(3) .5083(2) .0216(7) Uani ? ? 1.00000 ? ? O13 .9364(3) .7566(2) .42286(14) .0280(6) Uani ? ? 1.00000 ? ? C13a 1.0508(3) .7399(3) .6343(2) .0219(7) Uani ? ? 1.00000 ? ? C14 1.2348(4) .9030(3) .6897(2) .0282(9) Uani ? ? 1.00000 ? ? C15 1.3275(4) .9217(4) .8108(2) .0327(9) Uani ? ? 1.00000 ? ? C16 1.2394(4) .7821(4) .8731(2) .0330(9) Uani ? ? 1.00000 ? ? C17 1.0541(4) .6188(4) .8170(2) .0274(8) Uani ? ? 1.00000 ? ? C17a .9609(3) .6008(3) .6963(2) .0216(7) Uani ? ? 1.00000 ? ? H21a .388(5) .153(4) .450(3) .035(8) Uiso ? ? 1.00000 ? ? H21b .201(4) -.031(4) .399(2) .025(7) Uiso ? ? 1.00000 ? ? H41a .681(5) .594(4) .267(3) .029(7) Uiso ? ? 1.00000 ? ? H41b .591(5) .592(4) .135(3) .035(8) Uiso ? ? 1.00000 ? ? H11 .657(5) .280(5) .687(3) .044(9) Uiso ? ? 1.00000 ? ? H12 .644(5) .447(5) .436(3) .049(9) Uiso ? ? 1.00000 ? ? H14 1.291(4) 1.000(4) .646(2) .024(7) Uiso ? ? 1.00000 ? ? H15 1.454(6) 1.034(5) .844(3) .058(10) Uiso ? ? 1.00000 ? ? H16 1.295(6) .795(5) .956(3) .055(10) Uiso ? ? 1.00000 ? ? H17 .992(4) .521(4) .861(2) .021(6) Uiso ? ? 1.00000 ? ? 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 Ni .01599(19) .0169(2) .01440(19) .00304(14) .00358(14) .00039(13) S1 .0226(3) .0165(2) .0167(2) .0018(2) .0015(2) .00103(18) C2 .0162(9) .0174(9) .0171(9) .0057(7) .0041(7) .0007(7) N21 .0219(9) .0183(9) .0170(9) .0020(7) .0035(7) .0010(7) N3 .0167(8) .0164(8) .0173(8) .0047(6) .0050(7) .0004(6) C4 .0167(9) .0183(9) .0192(9) .0050(8) .0060(8) .0012(7) N41 .0228(9) .0208(9) .0173(9) -.0006(7) .0054(7) .0016(7) S5 .0209(3) .0231(3) .0155(2) -.0016(2) .0032(2) .00202(19) C11 .0210(10) .0205(10) .0182(9) .0096(8) .0042(8) .0008(7) N11 .0275(10) .0210(9) .0193(9) .0072(8) .0064(8) .0036(7) N12 .0195(9) .0190(9) .0175(9) .0021(7) .0028(7) .0006(7) C13 .0185(10) .0192(10) .0224(10) .0049(8) .0053(8) -.0003(8) O13 .0249(8) .0257(8) .0228(8) .0011(6) .0078(6) .0032(6) C13a .0180(10) .0222(10) .0218(10) .0078(8) .0038(8) -.0019(8) C14 .0198(11) .0272(12) .0299(12) .0053(9) .0061(9) -.0046(9) C15 .0196(11) .0355(13) .0302(13) .0070(10) .0004(9) -.0124(10) C16 .0284(12) .0429(14) .0211(11) .0174(11) -.0020(9) -.0080(10) C17 .0292(12) .0313(12) .0212(11) .0159(10) .0045(9) .0001(9) C17a .0211(10) .0211(10) .0214(10) .0102(8) .0049(8) -.0017(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ni S1 . . 2.1665(6) ? Ni S5 . . 2.1636(5) ? Ni S1 . 2 2.1665(6) ? Ni S5 . 2 2.1636(5) ? S1 C2 . . 1.7349(17) ? C2 N21 . . 1.330(3) ? C2 N3 . . 1.344(2) ? N21 H21a . . .84(2) ? N21 H21b . . .85(3) ? N3 C4 . . 1.336(3) ? C4 N41 . . 1.336(2) ? C4 S5 . . 1.733(2) ? N41 H41a . . .88(3) ? N41 H41b . . .87(3) ? C11 N11 . . 1.266(3) ? C11 N12 . . 1.396(3) ? C11 C17a . . 1.484(2) ? N11 H11 . . .77(4) ? N12 C13 . . 1.371(3) ? N12 H12 . . .88(3) ? C13 O13 . . 1.228(3) ? C13 C13a . . 1.486(3) ? C13a C14 . . 1.385(3) ? C13a C17a . . 1.390(3) ? C14 C15 . . 1.388(3) ? C14 H14 . . .96(3) ? C15 C16 . . 1.390(4) ? C15 H15 . . .94(3) ? C16 C17 . . 1.392(3) ? C16 H16 . . .94(4) ? C17 C17a . . 1.386(3) ? C17 H17 . . .98(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published S1 Ni S5 . . . 95.72(2) ? S1 Ni S1 . . 2 180.0000 ? S1 Ni S5 . . 2 84.28(2) ? S5 Ni S1 . . 2 84.28(2) ? S5 Ni S5 . . 2 180.0000 ? S1 Ni S5 2 . 2 95.72(2) ? Ni S1 C2 . . . 115.23(8) ? S1 C2 N21 . . . 113.34(14) ? S1 C2 N3 . . . 130.82(17) ? N21 C2 N3 . . . 115.74(16) ? C2 N21 H21a . . . 119(2) ? C2 N21 H21b . . . 119.4(17) ? H21a N21 H21b . . . 122(3) ? C2 N3 C4 . . . 125.40(15) ? N3 C4 N41 . . . 115.83(16) ? N3 C4 S5 . . . 130.68(13) ? N41 C4 S5 . . . 113.46(17) ? C4 N41 H41a . . . 120(2) ? C4 N41 H41b . . . 117.3(16) ? H41a N41 H41b . . . 121(3) ? Ni S5 C4 . . . 117.20(7) ? N11 C11 N12 . . . 121.26(16) ? N11 C11 C17a . . . 133.3(2) ? N12 C11 C17a . . . 105.45(17) ? C11 N11 H11 . . . 110(2) ? C11 N12 C13 . . . 112.56(15) ? C11 N12 H12 . . . 124(2) ? C13 N12 H12 . . . 123(2) ? N12 C13 O13 . . . 124.37(17) ? N12 C13 C13a . . . 106.21(19) ? O13 C13 C13a . . . 129.41(17) ? C13 C13a C14 . . . 130.3(2) ? C13 C13a C17a . . . 107.71(16) ? C14 C13a C17a . . . 121.9(2) ? C13a C14 C15 . . . 117.1(2) ? C13a C14 H14 . . . 120.6(13) ? C15 C14 H14 . . . 122.3(13) ? C14 C15 C16 . . . 121.3(2) ? C14 C15 H15 . . . 114(2) ? C16 C15 H15 . . . 125(2) ? C15 C16 C17 . . . 121.5(2) ? C15 C16 H16 . . . 123(2) ? C17 C16 H16 . . . 116(2) ? C16 C17 C17a . . . 117.3(2) ? C16 C17 H17 . . . 121.2(13) ? C17a C17 H17 . . . 121.5(13) ? C11 C17a C13a . . . 108.03(18) ? C11 C17a C17 . . . 130.9(2) ? C13a C17a C17 . . . 121.02(17) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 318 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min -10 _reflns_limit_k_max 9 _reflns_limit_l_min -16 _reflns_limit_l_max 15 _reflns_number_observed ? _reflns_d_resolution_high .725 _reflns_d_resolution_low 11.291 _diffrn_reflns_av_sigmaI/netI .027 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .04 _refine_ls_wR_factor_all .044 _refine_ls_goodness_of_fit_all 1.194 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_mb1253 _database_code_CSD 170262 _audit_creation_method Xtal3.6 _audit_creation_date 01-06-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C28 H44 N14 Ni1 O10 S2' _chemical_formula_moiety ? _chemical_formula_weight 859.57 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/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 8.4180(7) _cell_length_b 14.2560(10) _cell_length_c 15.9270(10) _cell_angle_alpha 90.00000 _cell_angle_beta 103.1430(10) _cell_angle_gamma 90.00000 _cell_volume 1861.3(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4851 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 20.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .707 _exptl_crystal_description prism _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .76 _exptl_absorpt_correction_T_max .96 _diffrn_reflns_number 21986 _reflns_number_total 4777 _reflns_Friedel_coverage 0 _reflns_number_gt 3543 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.37 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .053 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .04 _refine_ls_wR_factor_ref .044 _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_number_reflns 3543 _refine_ls_number_parameters 338 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .019 _refine_diff_density_min -.359 _refine_diff_density_max .619 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 56 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 28 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ni ? 0 2 .285 1.113 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 20 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 4 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni .50000 .50000 .50000 .01675(19) Uani ? ? 1.00000 ? ? N1 .5765(2) .42557(14) .59596(12) .0204(9) Uani ? ? 1.00000 ? ? C2 .5284(3) .42013(16) .66865(14) .0186(10) Uani ? ? 1.00000 ? ? N2 .5882(3) .34952(16) .72585(14) .0254(11) Uani ? ? 1.00000 ? ? N3 .4183(2) .47683(13) .69369(11) .0191(9) Uani ? ? 1.00000 ? ? C4 .3415(3) .54370(16) .63804(14) .0193(10) Uani ? ? 1.00000 ? ? N4 .2359(3) .59853(16) .67017(14) .0249(11) Uani ? ? 1.00000 ? ? N5 .3575(2) .55612(14) .55848(12) .0189(9) Uani ? ? 1.00000 ? ? N11 .3467(2) .36474(14) .98492(12) .0196(9) Uani ? ? 1.00000 ? ? C12 .3823(3) .37103(16) .90589(14) .0194(10) Uani ? ? 1.00000 ? ? O12 .4339(2) .30357(12) .87154(10) .0240(8) Uani ? ? 1.00000 ? ? N13 .3574(2) .45772(14) .86672(13) .0201(9) Uani ? ? 1.00000 ? ? C14 .2918(3) .53520(16) .89754(14) .0198(10) Uani ? ? 1.00000 ? ? O14 .2728(2) .60912(12) .85634(10) .0271(8) Uani ? ? 1.00000 ? ? C14a .2491(3) .52297(16) .98051(14) .0183(10) Uani ? ? 1.00000 ? ? C15 .1752(3) .59658(17) 1.01660(15) .0207(11) Uani ? ? 1.00000 ? ? C16 .1328(3) .58403(16) 1.09396(14) .0209(11) Uani ? ? 1.00000 ? ? O16 .0594(2) .64996(12) 1.13450(10) .0268(9) Uani ? ? 1.00000 ? ? C161 .0368(4) .74061(19) 1.09568(18) .0287(13) Uani ? ? 1.00000 ? ? C17 .1651(3) .49645(17) 1.13781(14) .0209(10) Uani ? ? 1.00000 ? ? O17 .1161(2) .49303(12) 1.21333(10) .0265(8) Uani ? ? 1.00000 ? ? C171 .1473(4) .4079(2) 1.26216(19) .0330(15) Uani ? ? 1.00000 ? ? C18 .2377(3) .42449(17) 1.10305(14) .0200(11) Uani ? ? 1.00000 ? ? C18a .2784(3) .43776(16) 1.02271(14) .0185(10) Uani ? ? 1.00000 ? ? O1 .1430(2) .69312(12) .43166(11) .0251(8) Uani ? ? 1.00000 ? ? S1 -.00663(8) .63051(4) .40231(4) .0252(3) Uani ? ? 1.00000 ? ? C101 -.1082(4) .6763(2) .30075(17) .0346(15) Uani ? ? 1.00000 ? ? C102 -.1472(4) .6696(3) .4637(2) .0375(16) Uani ? ? 1.00000 ? ? H1 .645(3) .3823(19) .5944(17) .023(7) Uiso ? ? 1.00000 ? ? H2a .555(3) .347(2) .7714(18) .031(8) Uiso ? ? 1.00000 ? ? H2b .674(4) .328(2) .7216(18) .032(8) Uiso ? ? 1.00000 ? ? H4a .246(3) .5962(18) .7246(17) .021(7) Uiso ? ? 1.00000 ? ? H4b .205(3) .646(2) .6441(17) .022(7) Uiso ? ? 1.00000 ? ? H5 .296(3) .6013(19) .5332(16) .025(7) Uiso ? ? 1.00000 ? ? H11 .364(3) .313(2) 1.0108(18) .035(8) Uiso ? ? 1.00000 ? ? H13 .379(3) .463(2) .8185(18) .030(8) Uiso ? ? 1.00000 ? ? H15 .146(3) .6517(18) .9848(16) .023(7) Uiso ? ? 1.00000 ? ? H161a -.008(3) .7770(18) 1.1374(15) .019(6) Uiso ? ? 1.00000 ? ? H161b -.030(3) .7373(18) 1.0369(18) .029(7) Uiso ? ? 1.00000 ? ? H161c .136(3) .768(2) 1.0910(17) .029(7) Uiso ? ? 1.00000 ? ? H171a .261(4) .391(2) 1.2731(17) .033(8) Uiso ? ? 1.00000 ? ? H171b .087(3) .357(2) 1.2290(18) .034(8) Uiso ? ? 1.00000 ? ? H171c .117(4) .419(2) 1.316(2) .044(8) Uiso ? ? 1.00000 ? ? H18 .250(3) .3644(18) 1.1277(15) .017(6) Uiso ? ? 1.00000 ? ? H101a -.045(4) .656(2) .2614(19) .040(8) Uiso ? ? 1.00000 ? ? H101b -.216(3) .6491(19) .2870(16) .029(7) Uiso ? ? 1.00000 ? ? H101c -.115(4) .743(2) .304(2) .050(10) Uiso ? ? 1.00000 ? ? H102a -.092(4) .657(2) .517(2) .065(11) Uiso ? ? 1.00000 ? ? H102b -.167(4) .739(3) .453(2) .063(11) Uiso ? ? 1.00000 ? ? H102c -.238(4) .630(2) .451(2) .053(10) Uiso ? ? 1.00000 ? ? 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 Ni .0195(2) .0179(2) .0142(2) .00135(17) .00666(15) .00055(17) N1 .0224(11) .0215(10) .0192(10) .0063(9) .0088(8) .0010(8) C2 .0200(12) .0179(11) .0180(11) -.0023(9) .0047(9) .0002(9) N2 .0284(13) .0286(12) .0223(11) .0100(10) .0124(9) .0076(9) N3 .0230(10) .0204(10) .0154(9) .0032(8) .0075(8) .0008(7) C4 .0202(12) .0187(11) .0200(11) -.0016(9) .0066(9) -.0023(9) N4 .0336(12) .0261(12) .0177(11) .0093(10) .0113(9) .0051(9) N5 .0223(10) .0189(10) .0163(9) .0040(8) .0059(8) .0025(8) N11 .0245(11) .0172(10) .0181(10) .0030(8) .0067(8) .0039(8) C12 .0186(12) .0223(12) .0180(11) -.0012(9) .0056(9) .0010(9) O12 .0316(10) .0217(9) .0207(8) .0040(7) .0101(7) .0003(7) N13 .0256(11) .0202(10) .0159(10) .0006(8) .0076(8) .0009(8) C14 .0236(12) .0193(11) .0165(11) -.0020(10) .0047(9) .0002(9) O14 .0433(11) .0200(9) .0206(8) .0034(8) .0125(8) .0028(7) C14a .0194(11) .0199(12) .0163(11) -.0012(9) .0053(9) -.0008(8) C15 .0239(12) .0176(11) .0204(11) .0006(10) .0046(9) .0024(9) C16 .0234(12) .0203(12) .0201(11) .0018(10) .0074(9) -.0018(9) O16 .0363(10) .0231(9) .0249(9) .0085(8) .0154(8) .0034(7) C161 .0369(16) .0221(13) .0303(14) .0054(12) .0138(12) .0010(11) C17 .0209(11) .0251(12) .0181(11) -.0001(10) .0072(9) .0011(10) O17 .0379(10) .0252(9) .0212(8) .0045(8) .0171(7) .0051(7) C171 .0469(19) .0294(15) .0286(14) .0070(13) .0209(13) .0087(12) C18 .0230(12) .0195(12) .0185(11) .0006(10) .0068(9) .0051(9) C18a .0170(11) .0201(11) .0182(11) -.0005(9) .0037(9) -.0017(9) O1 .0205(9) .0231(9) .0311(9) .0004(7) .0049(7) -.0060(7) S1 .0292(3) .0195(3) .0271(3) -.0026(3) .0070(3) -.0040(2) C101 .0313(16) .051(2) .0220(13) -.0065(14) .0061(12) -.0039(13) C102 .0332(17) .053(2) .0291(15) -.0169(15) .0130(13) -.0121(14) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ni N1 . . 1.8518(19) ? Ni N5 . . 1.859(2) ? Ni N1 . '3 666' 1.8518(19) ? Ni N5 . '3 666' 1.859(2) ? N1 C2 . . 1.313(3) ? N1 H1 . . .85(3) ? C2 N2 . . 1.374(3) ? C2 N3 . . 1.356(3) ? N2 H2a . . .84(3) ? N2 H2b . . .80(3) ? N3 C4 . . 1.361(3) ? C4 N4 . . 1.368(3) ? C4 N5 . . 1.316(3) ? N4 H4a . . .85(3) ? N4 H4b . . .80(3) ? N5 H5 . . .87(3) ? N11 C12 . . 1.362(3) ? N11 C18a . . 1.390(3) ? N11 H11 . . .84(3) ? C12 O12 . . 1.233(3) ? C12 N13 . . 1.379(3) ? N13 C14 . . 1.374(3) ? N13 H13 . . .83(3) ? C14 O14 . . 1.232(3) ? C14 C14a . . 1.457(3) ? C14a C15 . . 1.408(3) ? C14a C18a . . 1.383(3) ? C15 C16 . . 1.370(4) ? C15 H15 . . .94(3) ? C16 O16 . . 1.365(3) ? C16 C17 . . 1.426(3) ? O16 C161 . . 1.427(3) ? C161 H161a . . .99(3) ? C161 H161b . . .98(3) ? C161 H161c . . .94(3) ? C17 O17 . . 1.358(3) ? C17 C18 . . 1.373(3) ? O17 C171 . . 1.433(3) ? C171 H171a . . .97(3) ? C171 H171b . . .97(3) ? C171 H171c . . .96(3) ? C18 C18a . . 1.411(3) ? C18 H18 . . .94(2) ? O1 S1 . . 1.5276(17) ? S1 C101 . . 1.773(3) ? S1 C102 . . 1.787(4) ? C101 H101a . . .95(3) ? C101 H101b . . .96(3) ? C101 H101c . . .95(4) ? C102 H102a . . .89(3) ? C102 H102b . . 1.02(4) ? C102 H102c . . .93(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N1 Ni N5 . . . 88.63(9) ? N1 Ni N1 . . '3 666' 180.0000 ? N1 Ni N5 . . '3 666' 91.37(9) ? N5 Ni N1 . . '3 666' 91.38(9) ? N5 Ni N5 . . '3 666' 180.0000 ? N1 Ni N5 '3 666' . '3 666' 88.63(9) ? Ni N1 C2 . . . 129.99(17) ? Ni N1 H1 . . . 120.2(18) ? C2 N1 H1 . . . 109.4(19) ? N1 C2 N2 . . . 119.2(2) ? N1 C2 N3 . . . 126.3(2) ? N2 C2 N3 . . . 114.4(2) ? C2 N2 H2a . . . 117.1(19) ? C2 N2 H2b . . . 115(2) ? H2a N2 H2b . . . 123(3) ? C2 N3 C4 . . . 118.8(2) ? N3 C4 N4 . . . 114.2(2) ? N3 C4 N5 . . . 125.7(2) ? N4 C4 N5 . . . 120.1(2) ? C4 N4 H4a . . . 115.9(17) ? C4 N4 H4b . . . 117(2) ? H4a N4 H4b . . . 120(3) ? Ni N5 C4 . . . 130.05(16) ? Ni N5 H5 . . . 118.3(19) ? C4 N5 H5 . . . 111.4(19) ? C12 N11 C18a . . . 123.4(2) ? C12 N11 H11 . . . 117(2) ? C18a N11 H11 . . . 119(2) ? N11 C12 O12 . . . 122.2(2) ? N11 C12 N13 . . . 115.8(2) ? O12 C12 N13 . . . 122.1(2) ? C12 N13 C14 . . . 126.2(2) ? C12 N13 H13 . . . 117(2) ? C14 N13 H13 . . . 116(2) ? N13 C14 O14 . . . 120.7(2) ? N13 C14 C14a . . . 115.5(2) ? O14 C14 C14a . . . 123.8(2) ? C14 C14a C15 . . . 120.3(2) ? C14 C14a C18a . . . 119.5(2) ? C15 C14a C18a . . . 120.2(2) ? C14a C15 C16 . . . 120.0(2) ? C14a C15 H15 . . . 119.4(17) ? C16 C15 H15 . . . 120.4(17) ? C15 C16 O16 . . . 125.0(2) ? C15 C16 C17 . . . 119.7(2) ? O16 C16 C17 . . . 115.3(2) ? C16 O16 C161 . . . 116.7(2) ? O16 C161 H161a . . . 102.6(15) ? O16 C161 H161b . . . 111.2(15) ? O16 C161 H161c . . . 112.3(16) ? H161a C161 H161b . . . 116(2) ? H161a C161 H161c . . . 109(2) ? H161b C161 H161c . . . 106(2) ? C16 C17 O17 . . . 113.7(2) ? C16 C17 C18 . . . 120.6(2) ? O17 C17 C18 . . . 125.6(2) ? C17 O17 C171 . . . 117.1(2) ? O17 C171 H171a . . . 111.3(17) ? O17 C171 H171b . . . 109.3(16) ? O17 C171 H171c . . . 106.5(18) ? H171a C171 H171b . . . 106(2) ? H171a C171 H171c . . . 110(2) ? H171b C171 H171c . . . 114(3) ? C17 C18 C18a . . . 119.2(2) ? C17 C18 H18 . . . 122.1(16) ? C18a C18 H18 . . . 118.3(16) ? N11 C18a C14a . . . 119.5(2) ? N11 C18a C18 . . . 120.1(2) ? C14a C18a C18 . . . 120.4(2) ? O1 S1 C101 . . . 104.89(13) ? O1 S1 C102 . . . 104.66(13) ? C101 S1 C102 . . . 98.19(15) ? S1 C101 H101a . . . 105.2(16) ? S1 C101 H101b . . . 107.1(15) ? S1 C101 H101c . . . 110.2(18) ? H101a C101 H101b . . . 112(2) ? H101a C101 H101c . . . 112(3) ? H101b C101 H101c . . . 110(3) ? S1 C102 H102a . . . 101(3) ? S1 C102 H102b . . . 108(2) ? S1 C102 H102c . . . 108(2) ? H102a C102 H102b . . . 113(3) ? H102a C102 H102c . . . 108(3) ? H102b C102 H102c . . . 117(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 900 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -21 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .725 _reflns_d_resolution_low 10.474 _diffrn_reflns_av_sigmaI/netI .078 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .064 _refine_ls_wR_factor_all .047 _refine_ls_goodness_of_fit_all 1.119 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_mb137 _database_code_CSD 170263 _audit_creation_method Xtal3.6 _audit_creation_date 01-06-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C38 H64 N18 Ni1 O4' _chemical_formula_moiety ? _chemical_formula_weight 895.74 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 7.8360(10) _cell_length_b 10.0070(10) _cell_length_c 15.239(2) _cell_angle_alpha 87.349(2) _cell_angle_beta 88.506(2) _cell_angle_gamma 69.232(2) _cell_volume 1116.1(2) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5426 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 22.1 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .495 _exptl_crystal_description needle _exptl_crystal_size_max .4 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .451 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 13119 _reflns_number_total 5499 _reflns_Friedel_coverage 0 _reflns_number_gt 4686 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.18 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .038 _refine_ls_wR_factor_ref .044 _refine_ls_goodness_of_fit_ref 1.17 _refine_ls_number_reflns 4686 _refine_ls_number_parameters 405 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .006 _refine_diff_density_min -.637 _refine_diff_density_max .654 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 38 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 64 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 18 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ni ? 0 1 .285 1.113 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni .00000 .00005 .50000 .0164(2) Uani ? ? 1.00000 ? ? N1 .2241(2) .01890(15) .47015(9) .0181(9) Uani ? ? 1.00000 ? ? C2 .2694(2) .09765(17) .40803(11) .0175(10) Uani ? ? 1.00000 ? ? O2 .42677(15) .10523(13) .39685(8) .0207(8) Uani ? ? 1.00000 ? ? N3 .1354(2) .17988(16) .34988(10) .0214(10) Uani ? ? 1.00000 ? ? C4 -.0504(2) .20469(18) .35162(11) .0203(11) Uani ? ? 1.00000 ? ? O4 -.14262(16) .29184(14) .29298(9) .0292(9) Uani ? ? 1.00000 ? ? N5 -.1156(2) .13807(15) .41338(10) .0210(10) Uani ? ? 1.00000 ? ? C11 .3035(2) .55682(17) .10554(11) .0188(10) Uani ? ? 1.00000 ? ? N12 .4217(2) .49294(15) .16884(9) .0213(10) Uani ? ? 1.00000 ? ? C13 .3792(2) .39058(18) .21677(11) .0199(11) Uani ? ? 1.00000 ? ? N13 .4918(2) .32076(18) .28136(11) .0268(11) Uani ? ? 1.00000 ? ? N14 .22910(19) .35721(15) .20528(9) .0202(9) Uani ? ? 1.00000 ? ? C15 .1233(2) .42792(18) .13823(11) .0196(11) Uani ? ? 1.00000 ? ? N15 -.0263(2) .39721(18) .12275(11) .0263(11) Uani ? ? 1.00000 ? ? N16 .1535(2) .52973(15) .08483(9) .0207(9) Uani ? ? 1.00000 ? ? C11' .3395(2) .67179(18) .05126(11) .0210(11) Uani ? ? 1.00000 ? ? C12' .5162(3) .6742(2) .04314(12) .0235(12) Uani ? ? 1.00000 ? ? C13' .5500(3) .7802(2) -.00841(13) .0288(14) Uani ? ? 1.00000 ? ? C14' .4078(3) .8850(2) -.05155(14) .0353(15) Uani ? ? 1.00000 ? ? C15' .2312(3) .8846(2) -.04255(15) .0368(15) Uani ? ? 1.00000 ? ? C16' .1968(3) .7782(2) .00838(13) .0283(13) Uani ? ? 1.00000 ? ? N0 .2424(2) .26968(16) .67426(10) .0257(11) Uani ? ? 1.00000 ? ? C011 .3627(3) .2742(3) .74994(15) .0372(16) Uani ? ? 1.00000 ? ? C012 .5474(3) .1555(3) .75298(18) .0452(19) Uani ? ? 1.00000 ? ? C021 .3395(3) .2676(2) .58635(14) .0316(14) Uani ? ? 1.00000 ? ? C022 .4096(4) .3896(3) .5691(2) .048(2) Uani ? ? 1.00000 ? ? C031 .1967(3) .1338(2) .68110(13) .0263(13) Uani ? ? 1.00000 ? ? C032 .0850(4) .1195(3) .76085(16) .0415(18) Uani ? ? 1.00000 ? ? C041 .0697(3) .4000(2) .67992(15) .0341(15) Uani ? ? 1.00000 ? ? C042 -.0729(3) .4116(3) .61206(17) .0445(18) Uani ? ? 1.00000 ? ? H1 .316(3) -.019(2) .4985(14) .025(5) Uiso ? ? 1.00000 ? ? H3 .170(3) .225(2) .3091(13) .015(4) Uiso ? ? 1.00000 ? ? H5 -.229(3) .161(2) .4074(14) .027(5) Uiso ? ? 1.00000 ? ? H13a .464(3) .257(2) .3114(14) .027(5) Uiso ? ? 1.00000 ? ? H13b .604(3) .325(2) .2841(15) .037(6) Uiso ? ? 1.00000 ? ? H15a -.061(3) .344(3) .1602(17) .043(7) Uiso ? ? 1.00000 ? ? H15b -.083(3) .430(2) .0732(16) .035(6) Uiso ? ? 1.00000 ? ? H12' .614(3) .601(2) .0723(14) .030(6) Uiso ? ? 1.00000 ? ? H13' .664(3) .781(2) -.0134(15) .033(6) Uiso ? ? 1.00000 ? ? H14' .427(3) .958(3) -.0861(16) .046(7) Uiso ? ? 1.00000 ? ? H15' .128(4) .960(3) -.0694(17) .052(7) Uiso ? ? 1.00000 ? ? H16' .073(3) .777(2) .0150(14) .031(6) Uiso ? ? 1.00000 ? ? H011a .289(3) .271(2) .8049(16) .037(6) Uiso ? ? 1.00000 ? ? H011b .372(3) .367(3) .7391(16) .041(6) Uiso ? ? 1.00000 ? ? H012a .603(4) .167(3) .8064(19) .055(8) Uiso ? ? 1.00000 ? ? H012b .621(4) .162(3) .7026(19) .054(8) Uiso ? ? 1.00000 ? ? H012c .546(4) .060(3) .7550(18) .057(8) Uiso ? ? 1.00000 ? ? H021a .251(3) .271(2) .5410(14) .029(5) Uiso ? ? 1.00000 ? ? H021b .436(3) .174(3) .5875(15) .037(6) Uiso ? ? 1.00000 ? ? H022a .457(4) .381(3) .511(2) .064(9) Uiso ? ? 1.00000 ? ? H022b .503(4) .384(3) .6098(18) .054(8) Uiso ? ? 1.00000 ? ? H022c .314(4) .486(3) .5697(18) .054(8) Uiso ? ? 1.00000 ? ? H031a .313(3) .058(2) .6799(13) .023(5) Uiso ? ? 1.00000 ? ? H031b .135(3) .135(2) .6278(14) .026(5) Uiso ? ? 1.00000 ? ? H032a .072(4) .023(3) .764(2) .074(9) Uiso ? ? 1.00000 ? ? H032b -.040(4) .191(3) .7599(18) .056(8) Uiso ? ? 1.00000 ? ? H032c .147(4) .123(3) .8138(19) .056(8) Uiso ? ? 1.00000 ? ? H041a .104(3) .478(3) .6732(15) .039(6) Uiso ? ? 1.00000 ? ? H041b .021(3) .394(2) .7414(16) .039(6) Uiso ? ? 1.00000 ? ? H042a -.173(4) .502(3) .618(2) .069(9) Uiso ? ? 1.00000 ? ? H042b -.119(5) .330(4) .617(2) .096(12) Uiso ? ? 1.00000 ? ? H042c -.031(4) .421(3) .553(2) .077(10) Uiso ? ? 1.00000 ? ? 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 Ni .01446(15) .01906(16) .01677(16) -.00746(11) -.00103(11) .00271(11) N1 .0143(7) .0218(7) .0187(7) -.0073(5) -.0035(6) .0038(5) C2 .0165(8) .0183(7) .0177(8) -.0061(6) -.0009(6) -.0009(6) O2 .0145(6) .0266(6) .0218(6) -.0092(5) -.0014(5) .0057(5) N3 .0164(7) .0273(7) .0223(7) -.0113(6) -.0027(6) .0100(6) C4 .0169(8) .0222(8) .0230(8) -.0087(6) -.0026(6) .0024(6) O4 .0178(6) .0374(7) .0328(7) -.0124(5) -.0075(5) .0193(6) N5 .0124(7) .0255(7) .0254(8) -.0078(5) -.0028(6) .0056(6) C11 .0179(8) .0210(8) .0178(8) -.0070(6) .0007(6) -.0015(6) N12 .0189(7) .0260(7) .0205(7) -.0102(6) -.0017(6) .0026(6) C13 .0150(7) .0261(8) .0191(8) -.0079(6) .0002(6) .0002(6) N13 .0179(8) .0365(9) .0294(8) -.0151(7) -.0070(6) .0143(7) N14 .0154(7) .0261(7) .0199(7) -.0088(5) -.0017(5) .0033(6) C15 .0164(8) .0240(8) .0182(8) -.0069(6) -.0002(6) -.0011(6) N15 .0216(8) .0385(9) .0237(8) -.0172(7) -.0073(6) .0082(7) N16 .0182(7) .0243(7) .0200(7) -.0084(5) -.0021(6) .0019(5) C11' .0258(9) .0214(8) .0171(8) -.0100(7) .0005(7) -.0025(6) C12' .0253(9) .0244(9) .0224(9) -.0105(7) .0008(7) -.0034(7) C13' .0330(11) .0304(10) .0287(10) -.0183(8) .0078(8) -.0053(8) C14' .0506(13) .0287(10) .0322(11) -.0220(9) .0037(9) .0046(8) C15' .0425(12) .0290(10) .0377(12) -.0123(9) -.0060(9) .0111(9) C16' .0293(10) .0271(9) .0287(10) -.0108(8) -.0039(8) .0040(7) N0 .0236(8) .0282(8) .0279(8) -.0118(6) .0030(6) -.0087(6) C011 .0300(11) .0486(13) .0374(12) -.0168(9) .0002(9) -.0206(10) C012 .0293(11) .0642(17) .0410(13) -.0123(11) -.0047(10) -.0236(12) C021 .0319(11) .0329(10) .0335(11) -.0159(8) .0110(9) -.0066(8) C022 .0510(15) .0447(14) .0589(17) -.0301(12) .0147(14) -.0048(12) C031 .0276(10) .0284(9) .0252(9) -.0128(8) .0002(8) -.0024(7) C032 .0510(15) .0489(14) .0304(12) -.0257(12) .0059(10) .0018(10) C041 .0323(11) .0279(10) .0396(12) -.0074(8) .0064(9) -.0077(8) C042 .0372(13) .0447(14) .0394(13) .0006(10) -.0029(10) .0000(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ni N1 . . 1.8738(16) ? Ni N5 . . 1.8645(14) ? Ni N1 . '2 556' 1.8742(16) ? Ni N5 . '2 556' 1.8651(14) ? N1 C2 . . 1.325(2) ? N1 H1 . . .81(2) ? C2 O2 . . 1.269(2) ? C2 N3 . . 1.391(2) ? N3 C4 . . 1.387(2) ? N3 H3 . . .85(2) ? C4 O4 . . 1.263(2) ? C4 N5 . . 1.322(2) ? N5 H5 . . .84(2) ? C11 N12 . . 1.329(2) ? C11 N16 . . 1.344(3) ? C11 C11' . . 1.489(3) ? N12 C13 . . 1.361(2) ? C13 N13 . . 1.334(2) ? C13 N14 . . 1.349(3) ? N13 H13a . . .86(2) ? N13 H13b . . .90(3) ? N14 C15 . . 1.339(2) ? C15 N15 . . 1.342(3) ? C15 N16 . . 1.357(2) ? N15 H15a . . .87(3) ? N15 H15b . . .88(2) ? C11' C12' . . 1.396(3) ? C11' C16' . . 1.393(2) ? C12' C13' . . 1.387(3) ? C12' H12' . . .95(2) ? C13' C14' . . 1.385(3) ? C13' H13' . . .90(3) ? C14' C15' . . 1.388(4) ? C14' H14' . . .93(3) ? C15' C16' . . 1.388(3) ? C15' H15' . . .97(2) ? C16' H16' . . .98(3) ? N0 C011 . . 1.521(3) ? N0 C021 . . 1.521(3) ? N0 C031 . . 1.523(3) ? N0 C041 . . 1.514(2) ? C011 C012 . . 1.512(3) ? C011 H011a . . 1.01(2) ? C011 H011b . . .96(3) ? C012 H012a . . .97(3) ? C012 H012b . . .96(3) ? C012 H012c . . .96(3) ? C021 C022 . . 1.516(4) ? C021 H021a . . .98(2) ? C021 H021b . . .98(2) ? C022 H022a . . .94(3) ? C022 H022b . . .96(3) ? C022 H022c . . .99(2) ? C031 C032 . . 1.510(3) ? C031 H031a . . .955(18) ? C031 H031b . . .96(2) ? C032 H032a . . 1.01(4) ? C032 H032b . . .99(3) ? C032 H032c . . .96(3) ? C041 C042 . . 1.513(4) ? C041 H041a . . .91(3) ? C041 H041b . . 1.01(2) ? C042 H042a . . .98(3) ? C042 H042b . . 1.00(4) ? C042 H042c . . .96(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N1 Ni N5 . . . 90.33(7) ? N1 Ni N1 . . '2 556' 180.0000 ? N1 Ni N5 . . '2 556' 89.69(7) ? N5 Ni N1 . . '2 556' 89.69(7) ? N5 Ni N5 . . '2 556' 180.0000 ? N1 Ni N5 '2 556' . '2 556' 90.30(7) ? Ni N1 C2 . . . 131.49(11) ? Ni N1 H1 . . . 123.1(17) ? C2 N1 H1 . . . 105.2(17) ? N1 C2 O2 . . . 125.30(14) ? N1 C2 N3 . . . 118.33(16) ? O2 C2 N3 . . . 116.37(15) ? C2 N3 C4 . . . 129.09(16) ? C2 N3 H3 . . . 115.9(13) ? C4 N3 H3 . . . 114.9(12) ? N3 C4 O4 . . . 115.52(16) ? N3 C4 N5 . . . 118.51(14) ? O4 C4 N5 . . . 125.96(16) ? Ni N5 C4 . . . 131.71(12) ? Ni N5 H5 . . . 118.6(15) ? C4 N5 H5 . . . 109.6(15) ? N12 C11 N16 . . . 127.29(17) ? N12 C11 C11' . . . 116.86(17) ? N16 C11 C11' . . . 115.85(14) ? C11 N12 C13 . . . 113.85(17) ? N12 C13 N13 . . . 117.59(18) ? N12 C13 N14 . . . 124.81(14) ? N13 C13 N14 . . . 117.58(17) ? C13 N13 H13a . . . 116.9(15) ? C13 N13 H13b . . . 120.5(14) ? H13a N13 H13b . . . 121(2) ? C13 N14 C15 . . . 115.09(16) ? N14 C15 N15 . . . 117.68(17) ? N14 C15 N16 . . . 125.40(18) ? N15 C15 N16 . . . 116.91(15) ? C15 N15 H15a . . . 120.0(18) ? C15 N15 H15b . . . 117.5(18) ? H15a N15 H15b . . . 122(3) ? C11 N16 C15 . . . 113.47(14) ? C11 C11' C12' . . . 120.37(14) ? C11 C11' C16' . . . 120.21(18) ? C12' C11' C16' . . . 119.42(18) ? C11' C12' C13' . . . 120.28(16) ? C11' C12' H12' . . . 119.4(16) ? C13' C12' H12' . . . 120.3(16) ? C12' C13' C14' . . . 120.0(2) ? C12' C13' H13' . . . 119.6(14) ? C14' C13' H13' . . . 120.3(14) ? C13' C14' C15' . . . 120.0(2) ? C13' C14' H14' . . . 121.7(15) ? C15' C14' H14' . . . 118.3(15) ? C14' C15' C16' . . . 120.23(18) ? C14' C15' H15' . . . 121.7(19) ? C16' C15' H15' . . . 118.0(18) ? C11' C16' C15' . . . 120.0(2) ? C11' C16' H16' . . . 119.0(12) ? C15' C16' H16' . . . 121.0(12) ? C011 N0 C021 . . . 111.21(17) ? C011 N0 C031 . . . 110.74(15) ? C011 N0 C041 . . . 106.97(16) ? C021 N0 C031 . . . 106.29(15) ? C021 N0 C041 . . . 111.47(14) ? C031 N0 C041 . . . 110.22(16) ? N0 C011 C012 . . . 115.0(2) ? N0 C011 H011a . . . 105.2(15) ? N0 C011 H011b . . . 101.0(15) ? C012 C011 H011a . . . 111.1(11) ? C012 C011 H011b . . . 112.4(14) ? H011a C011 H011b . . . 112(2) ? C011 C012 H012a . . . 105.6(14) ? C011 C012 H012b . . . 111.2(14) ? C011 C012 H012c . . . 115.9(16) ? H012a C012 H012b . . . 111(3) ? H012a C012 H012c . . . 107(2) ? H012b C012 H012c . . . 106(2) ? N0 C021 C022 . . . 114.9(2) ? N0 C021 H021a . . . 106.3(13) ? N0 C021 H021b . . . 103.5(14) ? C022 C021 H021a . . . 109.3(14) ? C022 C021 H021b . . . 113.2(17) ? H021a C021 H021b . . . 109(2) ? C021 C022 H022a . . . 106(2) ? C021 C022 H022b . . . 110.9(18) ? C021 C022 H022c . . . 114(2) ? H022a C022 H022b . . . 110(3) ? H022a C022 H022c . . . 105(2) ? H022b C022 H022c . . . 110(2) ? N0 C031 C032 . . . 115.30(18) ? N0 C031 H031a . . . 104.2(15) ? N0 C031 H031b . . . 104.5(14) ? C032 C031 H031a . . . 111.8(13) ? C032 C031 H031b . . . 111.7(14) ? H031a C031 H031b . . . 108.7(17) ? C031 C032 H032a . . . 110.7(17) ? C031 C032 H032b . . . 112.6(17) ? C031 C032 H032c . . . 110.7(18) ? H032a C032 H032b . . . 106(3) ? H032a C032 H032c . . . 105(2) ? H032b C032 H032c . . . 111(2) ? N0 C041 C042 . . . 115.17(19) ? N0 C041 H041a . . . 106.8(13) ? N0 C041 H041b . . . 105.0(11) ? C042 C041 H041a . . . 108.6(14) ? C042 C041 H041b . . . 111.2(15) ? H041a C041 H041b . . . 110(2) ? C041 C042 H042a . . . 109(2) ? C041 C042 H042b . . . 112(2) ? C041 C042 H042c . . . 112(2) ? H042a C042 H042b . . . 110(3) ? H042a C042 H042c . . . 102(2) ? H042b C042 H042c . . . 110(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 478 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 9.332 _diffrn_reflns_av_sigmaI/netI .043 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .048 _refine_ls_wR_factor_all .047 _refine_ls_goodness_of_fit_all 1.124 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_phtha _database_code_CSD 170264 _audit_creation_method Xtal3.6 _audit_creation_date 01-06-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H23 N11 O2' _chemical_formula_moiety ? _chemical_formula_weight 521.55 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21_1 _symmetry_space_group_name_Hall p_2yb loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-z _cell_length_a 11.089(2) _cell_length_b 8.694(2) _cell_length_c 12.364(2) _cell_angle_alpha 90.00000 _cell_angle_beta 94.446(3) _cell_angle_gamma 90.00000 _cell_volume 1188.4(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 3455 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 22.1 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .1 _exptl_crystal_description plate _exptl_crystal_size_max .50 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .62 _exptl_absorpt_correction_T_max .93 _diffrn_reflns_number 13514 _reflns_number_total 3204 _reflns_Friedel_coverage 0 _reflns_number_gt 2530 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.17 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .042 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .044 _refine_ls_goodness_of_fit_ref 1.362 _refine_ls_number_reflns 2530 _refine_ls_number_parameters 443 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .005 _refine_diff_density_min -.26 _refine_diff_density_max .251 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 52 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 46 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 22 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C11 .2085(2) .5000(5) .1998(2) .0203(14) Uani ? ? 1.00000 ? ? N12 .2350(2) .4437(5) .29958(18) .0224(12) Uani ? ? 1.00000 ? ? C13 .2772(2) .2969(5) .3015(2) .0231(15) Uani ? ? 1.00000 ? ? N13 .2999(3) .2320(5) .3997(2) .0299(15) Uani ? ? 1.00000 ? ? N14 .2970(2) .2117(5) .21470(18) .0243(13) Uani ? ? 1.00000 ? ? C15 .2664(2) .2791(5) .1194(2) .0233(15) Uani ? ? 1.00000 ? ? N15 .2785(3) .2005(5) .0289(2) .0316(15) Uani ? ? 1.00000 ? ? N16 .2206(2) .4244(5) .10705(19) .0233(12) Uani ? ? 1.00000 ? ? C11' .1584(2) .6591(5) .1895(2) .0226(15) Uani ? ? 1.00000 ? ? C12' .1626(3) .7587(5) .2783(3) .0286(16) Uani ? ? 1.00000 ? ? C13' .1162(3) .9067(5) .2669(3) .0320(17) Uani ? ? 1.00000 ? ? C14' .0647(3) .9566(5) .1685(3) .0301(17) Uani ? ? 1.00000 ? ? C15' .0581(3) .8591(6) .0800(3) .0351(18) Uani ? ? 1.00000 ? ? C16' .1054(3) .7116(5) .0903(2) .0297(17) Uani ? ? 1.00000 ? ? C21 .1915(2) .2890(5) .6993(2) .0210(14) Uani ? ? 1.00000 ? ? N22 .2185(2) .3461(5) .79853(18) .0221(12) Uani ? ? 1.00000 ? ? C23 .2615(2) .4925(5) .8012(2) .0221(15) Uani ? ? 1.00000 ? ? N23 .2864(3) .5584(4) .8972(2) .0298(15) Uani ? ? 1.00000 ? ? N24 .2808(2) .5760(5) .71249(18) .0244(13) Uani ? ? 1.00000 ? ? C25 .2526(3) .5072(5) .6172(2) .0243(15) Uani ? ? 1.00000 ? ? N25 .2719(3) .5844(5) .5266(2) .0315(15) Uani ? ? 1.00000 ? ? N26 .2059(2) .3635(5) .60552(18) .0228(12) Uani ? ? 1.00000 ? ? C21' .1416(2) .1305(5) .6900(2) .0215(14) Uani ? ? 1.00000 ? ? C22' .1349(3) .0378(5) .7808(2) .0254(16) Uani ? ? 1.00000 ? ? C23' .0909(3) -.1121(5) .7705(3) .0294(16) Uani ? ? 1.00000 ? ? C24' .0525(3) -.1694(5) .6691(3) .0292(17) Uani ? ? 1.00000 ? ? C25' .0558(3) -.0773(5) .5784(3) .0317(17) Uani ? ? 1.00000 ? ? C26' .1005(3) .0723(5) .5887(2) .0270(16) Uani ? ? 1.00000 ? ? C31 .4232(2) .9349(5) .8235(2) .0270(15) Uani ? ? 1.00000 ? ? O31 .4061(2) .8791(4) .91167(16) .0360(12) Uani ? ? 1.00000 ? ? N32 .3961(2) .8627(4) .72471(19) .0265(13) Uani ? ? 1.00000 ? ? C33 .4114(2) .9600(5) .6387(2) .0247(15) Uani ? ? 1.00000 ? ? O33 .38471(18) .9280(4) .54322(15) .0303(11) Uani ? ? 1.00000 ? ? C33a .4623(2) 1.1063(5) .6863(2) .0233(14) Uani ? ? 1.00000 ? ? C34 .4943(2) 1.2410(5) .6378(3) .0290(15) Uani ? ? 1.00000 ? ? C35 .5353(3) 1.3601(5) .7062(3) .0327(17) Uani ? ? 1.00000 ? ? C36 .5447(3) 1.3438(5) .8183(3) .0333(17) Uani ? ? 1.00000 ? ? C37 .5127(3) 1.2069(5) .8667(3) .0297(16) Uani ? ? 1.00000 ? ? C37a .4709(2) 1.0888(5) .7986(2) .0242(14) Uani ? ? 1.00000 ? ? H13a .326(3) .133(4) .402(3) .042(10) Uiso ? ? 1.00000 ? ? H13b .282(3) .280(4) .457(3) .024(8) Uiso ? ? 1.00000 ? ? H15a .308(3) .105(5) .034(3) .055(12) Uiso ? ? 1.00000 ? ? H15b .256(3) .243(4) -.033(3) .033(10) Uiso ? ? 1.00000 ? ? H12' .201(2) .722(3) .347(2) .018(7) Uiso ? ? 1.00000 ? ? H13' .120(2) .970(4) .330(2) .023(8) Uiso ? ? 1.00000 ? ? H14' .033(3) 1.061(4) .160(3) .045(10) Uiso ? ? 1.00000 ? ? H15' .023(3) .895(4) .005(3) .038(9) Uiso ? ? 1.00000 ? ? H16' .100(2) .648(3) .027(2) .022(8) Uiso ? ? 1.00000 ? ? H23a .310(3) .657(4) .902(3) .042(10) Uiso ? ? 1.00000 ? ? H23b .266(3) .517(4) .962(3) .041(10) Uiso ? ? 1.00000 ? ? H25a .308(3) .674(5) .532(3) .054(12) Uiso ? ? 1.00000 ? ? H25b .254(3) .548(5) .464(3) .049(12) Uiso ? ? 1.00000 ? ? H22' .159(3) .082(3) .855(2) .025(8) Uiso ? ? 1.00000 ? ? H23' .086(2) -.173(4) .837(2) .030(8) Uiso ? ? 1.00000 ? ? H24' .024(3) -.277(4) .667(2) .035(9) Uiso ? ? 1.00000 ? ? H25' .030(2) -.116(3) .509(3) .027(9) Uiso ? ? 1.00000 ? ? H26' .106(2) .133(3) .519(2) .025(8) Uiso ? ? 1.00000 ? ? H32 .355(4) .771(5) .723(3) .072(13) Uiso ? ? 1.00000 ? ? H34 .485(2) 1.259(3) .562(2) .021(7) Uiso ? ? 1.00000 ? ? H35 .554(3) 1.448(4) .671(3) .040(9) Uiso ? ? 1.00000 ? ? H36 .566(3) 1.430(5) .867(3) .056(11) Uiso ? ? 1.00000 ? ? H37 .519(3) 1.20(2) .948(2) .035(9) Uiso ? ? 1.00000 ? ? 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 C11 .0211(14) .0222(15) .0179(16) -.0055(11) .0023(11) .0023(12) N12 .0266(12) .0217(13) .0187(13) -.0015(11) .0005(9) -.0002(10) C13 .0238(14) .0242(16) .0211(17) -.0031(11) .0009(11) .0000(12) N13 .0467(16) .0257(15) .0173(15) .0066(12) .0024(12) -.0014(12) N14 .0332(13) .0236(13) .0160(13) .0012(10) .0018(10) -.0008(10) C15 .0243(14) .0243(15) .0212(17) -.0027(12) .0020(12) .0003(12) N15 .0487(17) .0272(16) .0187(15) .0067(13) .0016(12) .0003(13) N16 .0296(12) .0234(13) .0169(13) -.0006(10) .0011(9) .0005(11) C11' .0219(14) .0248(15) .0214(16) -.0032(12) .0035(11) .0016(12) C12' .0356(17) .0291(17) .0201(17) -.0011(13) -.0040(13) .0022(13) C13' .0395(18) .0267(16) .0299(18) -.0003(13) .0019(14) -.0069(14) C14' .0326(17) .0260(17) .032(2) .0045(13) .0026(13) .0050(14) C15' .043(2) .0360(19) .0255(18) .0113(16) .0008(14) .0084(16) C16' .0391(18) .0307(18) .0191(16) .0048(14) .0011(13) -.0025(14) C21 .0219(13) .0202(15) .0208(16) .0029(11) .0016(11) .0003(12) N22 .0269(13) .0209(12) .0186(13) .0008(10) .0013(9) -.0005(11) C23 .0279(15) .0206(15) .0178(16) .0023(11) .0011(11) .0003(12) N23 .0498(17) .0230(15) .0169(14) -.0041(12) .0033(12) -.0000(12) N24 .0356(14) .0206(13) .0171(13) .0023(10) .0018(10) -.0010(10) C25 .0321(16) .0204(15) .0201(17) .0019(12) .0006(12) .0005(12) N25 .0563(19) .0239(14) .0141(15) -.0042(14) .0008(12) .0009(12) N26 .0290(13) .0208(12) .0182(13) .0013(10) -.0007(9) .0000(11) C21' .0211(14) .0204(14) .0231(17) .0032(11) .0028(11) -.0015(12) C22' .0294(16) .0270(16) .0196(17) -.0020(12) .0005(12) -.0003(12) C23' .0362(17) .0266(17) .0257(17) -.0042(13) .0035(13) .0017(14) C24' .0294(16) .0247(17) .034(2) -.0044(13) .0054(13) -.0011(14) C25' .0341(17) .0319(17) .0284(19) -.0081(15) -.0014(13) -.0052(16) C26' .0312(16) .0282(17) .0214(17) -.0032(13) .0008(12) -.0007(14) C31 .0298(16) .0265(16) .0239(16) .0022(13) -.0030(12) .0032(13) O31 .0525(13) .0327(12) .0222(11) -.0048(10) -.0016(9) .0064(10) N32 .0368(14) .0221(12) .0209(13) -.0016(11) .0039(10) .0001(10) C33 .0241(14) .0262(15) .0245(17) .0046(11) .0070(11) -.0008(13) O33 .0398(12) .0302(11) .0211(11) .0015(9) .0040(9) -.0035(9) C33a .0202(14) .0266(15) .0233(16) .0027(11) .0025(11) -.0016(12) C34 .0262(15) .0335(16) .0278(17) -.0009(12) .0047(12) .0044(14) C35 .0302(17) .0281(16) .040(2) -.0052(13) .0028(13) .0051(15) C36 .0303(16) .0320(17) .038(2) -.0037(14) .0029(14) -.0073(16) C37 .0293(16) .0345(17) .0248(16) -.0017(13) -.0013(13) -.0042(14) C37a .0205(14) .0279(14) .0240(16) .0018(11) -.0004(11) .0012(12) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published C11 N12 . . 1.338(4) ? C11 N16 . . 1.338(4) ? C11 C11' . . 1.492(6) ? N12 C13 . . 1.359(6) ? C13 N13 . . 1.345(4) ? C13 N14 . . 1.336(4) ? N13 H13a . . .91(4) ? N13 H13b . . .85(3) ? N14 C15 . . 1.336(4) ? C15 N15 . . 1.327(5) ? C15 N16 . . 1.366(6) ? N15 H15a . . .90(4) ? N15 H15b . . .87(3) ? C11' C12' . . 1.397(5) ? C11' C16' . . 1.395(4) ? C12' C13' . . 1.388(6) ? C12' H12' . . .97(3) ? C13' C14' . . 1.374(5) ? C13' H13' . . .96(3) ? C14' C15' . . 1.381(5) ? C14' H14' . . .98(4) ? C15' C16' . . 1.388(6) ? C15' H15' . . 1.03(3) ? C16' H16' . . .95(3) ? C21 N22 . . 1.336(4) ? C21 N26 . . 1.349(4) ? C21 C21' . . 1.486(6) ? N22 C23 . . 1.358(6) ? C23 N23 . . 1.327(4) ? C23 N24 . . 1.346(4) ? N23 H23a . . .90(4) ? N23 H23b . . .92(4) ? N24 C25 . . 1.336(4) ? C25 N25 . . 1.337(5) ? C25 N26 . . 1.356(6) ? N25 H25a . . .88(4) ? N25 H25b . . .85(4) ? C21' C22' . . 1.389(5) ? C21' C26' . . 1.394(4) ? C22' C23' . . 1.393(6) ? C22' H22' . . 1.01(3) ? C23' C24' . . 1.386(5) ? C23' H23' . . .98(3) ? C24' C25' . . 1.381(5) ? C24' H24' . . .99(3) ? C25' C26' . . 1.394(6) ? C25' H25' . . .94(3) ? C26' H26' . . 1.01(3) ? C31 O31 . . 1.221(4) ? C31 N32 . . 1.386(4) ? C31 C37a . . 1.480(6) ? N32 C33 . . 1.380(5) ? N32 H32 . . .92(4) ? C33 O33 . . 1.226(4) ? C33 C33a . . 1.494(5) ? C33a C34 . . 1.376(6) ? C33a C37a . . 1.392(4) ? C34 C35 . . 1.391(6) ? C34 H34 . . .95(3) ? C35 C36 . . 1.389(5) ? C35 H35 . . .91(4) ? C36 C37 . . 1.391(6) ? C36 H36 . . .98(4) ? C37 C37a . . 1.384(5) ? C37 H37 . . 1.00(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N12 C11 N16 . . . 125.5(4) ? N12 C11 C11' . . . 118.1(3) ? N16 C11 C11' . . . 116.3(3) ? C11 N12 C13 . . . 114.2(3) ? N12 C13 N13 . . . 116.7(3) ? N12 C13 N14 . . . 125.8(3) ? N13 C13 N14 . . . 117.5(4) ? C13 N13 H13a . . . 117(2) ? C13 N13 H13b . . . 120(2) ? H13a N13 H13b . . . 122(3) ? C13 N14 C15 . . . 114.7(4) ? N14 C15 N15 . . . 118.9(4) ? N14 C15 N16 . . . 124.8(3) ? N15 C15 N16 . . . 116.3(3) ? C15 N15 H15a . . . 118(2) ? C15 N15 H15b . . . 119(2) ? H15a N15 H15b . . . 123(3) ? C11 N16 C15 . . . 114.8(3) ? C11 C11' C12' . . . 121.2(3) ? C11 C11' C16' . . . 120.5(3) ? C12' C11' C16' . . . 118.3(4) ? C11' C12' C13' . . . 120.4(3) ? C11' C12' H12' . . . 117.6(17) ? C13' C12' H12' . . . 122.0(17) ? C12' C13' C14' . . . 120.6(3) ? C12' C13' H13' . . . 117.0(17) ? C14' C13' H13' . . . 122.5(18) ? C13' C14' C15' . . . 120.0(4) ? C13' C14' H14' . . . 121(2) ? C15' C14' H14' . . . 119(2) ? C14' C15' C16' . . . 119.8(3) ? C14' C15' H15' . . . 121.4(19) ? C16' C15' H15' . . . 118.7(19) ? C11' C16' C15' . . . 120.9(3) ? C11' C16' H16' . . . 121.7(18) ? C15' C16' H16' . . . 117.4(17) ? N22 C21 N26 . . . 125.3(4) ? N22 C21 C21' . . . 118.1(3) ? N26 C21 C21' . . . 116.5(3) ? C21 N22 C23 . . . 115.1(3) ? N22 C23 N23 . . . 118.3(3) ? N22 C23 N24 . . . 124.2(3) ? N23 C23 N24 . . . 117.4(4) ? C23 N23 H23a . . . 121(2) ? C23 N23 H23b . . . 124(2) ? H23a N23 H23b . . . 113(3) ? C23 N24 C25 . . . 115.9(4) ? N24 C25 N25 . . . 118.2(4) ? N24 C25 N26 . . . 124.6(3) ? N25 C25 N26 . . . 117.2(3) ? C25 N25 H25a . . . 119(2) ? C25 N25 H25b . . . 123(3) ? H25a N25 H25b . . . 119(4) ? C21 N26 C25 . . . 114.9(3) ? C21 C21' C22' . . . 121.2(3) ? C21 C21' C26' . . . 120.0(3) ? C22' C21' C26' . . . 118.7(4) ? C21' C22' C23' . . . 120.6(3) ? C21' C22' H22' . . . 118.9(18) ? C23' C22' H22' . . . 120.4(17) ? C22' C23' C24' . . . 120.0(3) ? C22' C23' H23' . . . 118.3(18) ? C24' C23' H23' . . . 121.7(18) ? C23' C24' C25' . . . 120.1(4) ? C23' C24' H24' . . . 116.4(17) ? C25' C24' H24' . . . 123.5(17) ? C24' C25' C26' . . . 119.9(3) ? C24' C25' H25' . . . 120(2) ? C26' C25' H25' . . . 119.9(19) ? C21' C26' C25' . . . 120.7(3) ? C21' C26' H26' . . . 122.5(17) ? C25' C26' H26' . . . 116.8(17) ? O31 C31 N32 . . . 124.7(4) ? O31 C31 C37a . . . 128.9(3) ? N32 C31 C37a . . . 106.4(3) ? C31 N32 C33 . . . 111.8(3) ? C31 N32 H32 . . . 119(2) ? C33 N32 H32 . . . 127(2) ? N32 C33 O33 . . . 124.6(4) ? N32 C33 C33a . . . 106.4(3) ? O33 C33 C33a . . . 128.9(3) ? C33 C33a C34 . . . 130.9(3) ? C33 C33a C37a . . . 107.2(3) ? C34 C33a C37a . . . 121.9(3) ? C33a C34 C35 . . . 116.9(3) ? C33a C34 H34 . . . 124.3(17) ? C35 C34 H34 . . . 118.7(17) ? C34 C35 C36 . . . 121.8(4) ? C34 C35 H35 . . . 115(2) ? C36 C35 H35 . . . 124(2) ? C35 C36 C37 . . . 121.0(4) ? C35 C36 H36 . . . 122(2) ? C37 C36 H36 . . . 117(2) ? C36 C37 C37a . . . 117.2(3) ? C36 C37 H37 . . . 117(9) ? C37a C37 H37 . . . 125(9) ? C31 C37a C33a . . . 107.9(3) ? C31 C37a C37 . . . 130.6(3) ? C33a C37a C37 . . . 121.3(4) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 544 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min -16 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 12.296 _diffrn_reflns_av_sigmaI/netI .064 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .06 _refine_ls_wR_factor_all .046 _refine_ls_goodness_of_fit_all 1.251 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end