# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name "Dermot O'Hare" _publ_contact_author_email DERMOT.OHARE@CHEM.OX.AC.UK _publ_section_title ; Resin-assisted Solvothermal Synthesis Metal-Organic Frameworks ; loop_ _publ_author_name "Dermot O'Hare" 'Yi Du.' 'Amber L. Thompson' # Attachment 'OHare.cif' #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 698782' #============================================================================== _audit_creation_date 08-06-16 _audit_creation_method CRYSTALS_ver_12.86 _publ_section_exptl_refinement ; The difference map indicated the presence of diffuse electron density believed to be disordered solvent, thought to be ethanol. SQUEEZE was used leaving a voids from which electron density was removed. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.042 109 8 ' ' 2 0.500 0.500 -0.044 109 8 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _oxford_structure_analysis_title 5805 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 21.1466(8) _cell_length_b 11.1836(4) _cell_length_c 4.7297(2) _cell_angle_alpha 90 _cell_angle_beta 92.8883(16) _cell_angle_gamma 90 _cell_volume 1117.13(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C36 H24 Fe1 O12 # Dc = 4.19 Fooo = 544.00 Mu = 15.43 M = 352.21 # Found Formula = C12 H6 Fe1 O4 # Dc = 1.61 FOOO = 544.00 Mu = 13.47 M = 135.01 _chemical_formula_sum 'C12 H6 Fe1 O4' _chemical_formula_moiety 'C12 H6 Fe1 O4' _chemical_compound_source . _chemical_formula_weight 270.02 _cell_measurement_reflns_used 1318 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour clear_pale_brown _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.347 # Sheldrick geometric approximatio 0.97 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 9067 _reflns_number_total 1260 _diffrn_reflns_av_R_equivalents 0.069 # Number of reflections with Friedels Law is 1260 # Number of reflections without Friedels Law is 1260 # Theoretical number of reflections is about 1267 _diffrn_reflns_theta_min 5.160 _diffrn_reflns_theta_max 27.375 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.828 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 _reflns_limit_h_min -27 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 6 _oxford_diffrn_Wilson_B_factor 1.61 _oxford_diffrn_Wilson_scale 44.15 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.88 _refine_diff_density_max 0.64 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 1259 _refine_ls_number_restraints 0 _refine_ls_number_parameters 78 _oxford_refine_ls_R_factor_ref 0.0519 _refine_ls_wR_factor_ref 0.0939 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.000219 # The values computed from all data _oxford_reflns_number_all 1259 _refine_ls_R_factor_all 0.0519 _refine_ls_wR_factor_all 0.0939 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1015 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_gt 0.0891 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 3.15P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.5000 0.08222(5) 0.7500 0.0193 1.0000 Uani S T . . . . . O2 O 0.55964(8) 0.06906(17) 1.1300(4) 0.0174 1.0000 Uani . . . . . . . C3 C 0.58418(12) 0.1495(2) 1.2934(5) 0.0183 1.0000 Uani . . . . . . . O4 O 0.56285(9) 0.18020(18) 1.5253(4) 0.0233 1.0000 Uani . . . . . . . C5 C 0.64464(12) 0.2057(2) 1.2061(5) 0.0185 1.0000 Uani . . . . . . . C6 C 0.66658(13) 0.3135(3) 1.3344(6) 0.0236 1.0000 Uani . . . . . . . C7 C 0.72307(13) 0.3613(3) 1.2630(6) 0.0232 1.0000 Uani . . . . . . . C8 C 0.76095(12) 0.3042(2) 1.0642(5) 0.0182 1.0000 Uani . . . . . . . C9 C 0.67977(12) 0.1490(3) 1.0085(5) 0.0188 1.0000 Uani . . . . . . . H61 H 0.6437 0.3523 1.4683 0.0289 1.0000 Uiso R . . . . . . H71 H 0.7361 0.4338 1.3448 0.0281 1.0000 Uiso R . . . . . . H91 H 0.6635 0.0804 0.9202 0.0225 1.0000 Uiso R . . . . . . 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 Fe1 0.0131(3) 0.0297(3) 0.0154(3) 0.0000 0.00430(19) 0.0000 O2 0.0122(8) 0.0237(10) 0.0164(9) 0.0001(8) 0.0030(7) -0.0029(7) C3 0.0137(12) 0.0231(14) 0.0183(13) 0.0015(11) 0.0021(10) -0.0012(11) O4 0.0210(10) 0.0296(11) 0.0198(10) -0.0029(8) 0.0064(8) -0.0059(8) C5 0.0153(12) 0.0257(15) 0.0146(12) 0.0016(11) 0.0023(10) -0.0046(10) C6 0.0206(14) 0.0292(15) 0.0218(14) -0.0046(12) 0.0078(11) -0.0039(12) C7 0.0217(14) 0.0248(15) 0.0233(14) -0.0044(12) 0.0044(11) -0.0081(12) C8 0.0146(12) 0.0249(14) 0.0152(13) 0.0014(10) 0.0016(10) -0.0027(10) C9 0.0164(13) 0.0224(14) 0.0176(13) -0.0004(11) 0.0006(10) -0.0059(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1851(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O2 2_657 2.2016(18) yes Fe1 . O2 6_554 2.2016(18) yes Fe1 . O2 5_656 2.1482(17) yes Fe1 . O4 1_554 2.0589(19) yes Fe1 . O4 5_657 2.0589(19) yes Fe1 . O2 . 2.1482(17) yes O2 . C3 . 1.278(3) yes C3 . O4 . 1.255(3) yes C3 . C5 . 1.501(3) yes C5 . C6 . 1.418(4) yes C5 . C9 . 1.377(4) yes C6 . C7 . 1.366(4) yes C6 . H61 . 0.924 no C7 . C8 . 1.417(4) yes C7 . H71 . 0.935 no C8 . C8 4_657 1.423(5) yes C8 . C9 4_657 1.417(4) yes C9 . H91 . 0.932 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 2_657 Fe1 . O2 6_554 79.57(9) yes O2 2_657 Fe1 . O2 5_656 80.98(6) yes O2 6_554 Fe1 . O2 5_656 92.95(6) yes O2 2_657 Fe1 . O4 1_554 159.25(7) yes O2 6_554 Fe1 . O4 1_554 83.27(7) yes O2 5_656 Fe1 . O4 1_554 88.37(7) yes O2 2_657 Fe1 . O4 5_657 83.27(7) yes O2 6_554 Fe1 . O4 5_657 159.25(7) yes O2 5_656 Fe1 . O4 5_657 95.81(7) yes O4 1_554 Fe1 . O4 5_657 115.69(12) yes O2 2_657 Fe1 . O2 . 92.95(6) yes O2 6_554 Fe1 . O2 . 80.98(6) yes O2 5_656 Fe1 . O2 . 172.14(10) yes O4 1_554 Fe1 . O2 . 95.81(7) yes O4 5_657 Fe1 . O2 . 88.37(7) yes Fe1 2_657 O2 . Fe1 . 87.05(6) yes Fe1 2_657 O2 . C3 . 127.24(16) yes Fe1 . O2 . C3 . 131.36(17) yes O2 . C3 . O4 . 124.6(2) yes O2 . C3 . C5 . 117.0(2) yes O4 . C3 . C5 . 118.3(2) yes Fe1 1_556 O4 . C3 . 125.11(18) yes C3 . C5 . C6 . 120.2(2) yes C3 . C5 . C9 . 119.3(2) yes C6 . C5 . C9 . 120.4(2) yes C5 . C6 . C7 . 119.9(3) yes C5 . C6 . H61 . 121.4 no C7 . C6 . H61 . 118.7 no C6 . C7 . C8 . 121.2(3) yes C6 . C7 . H71 . 118.7 no C8 . C7 . H71 . 120.1 no C8 4_657 C8 . C7 . 118.9(3) yes C8 4_657 C8 . C9 4_657 118.9(3) yes C7 . C8 . C9 4_657 122.1(2) yes C8 4_657 C9 . C5 . 120.6(2) yes C8 4_657 C9 . H91 . 120.5 no C5 . C9 . H91 . 118.9 no _chemical_name_common . #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 698783' #============================================================================== _audit_creation_date 08-03-29 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5749 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 11.3972(2) _cell_length_b 18.9914(4) _cell_length_c 11.8255(2) _cell_angle_alpha 90 _cell_angle_beta 118.0382(7) _cell_angle_gamma 90 _cell_volume 2259.20(7) _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 -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C48 H32 Co4 N2 O16 # Dc = 1.66 Fooo = 1086.00 Mu = 15.20 M = 564.26 # Found Formula = C46 H46 Co3 N4 O14 # Dc = 1.55 FOOO = 1086.00 Mu = 11.62 M = 527.84 _chemical_formula_sum 'C46 H46 Co3 N4 O14' _chemical_formula_moiety 'C46 H46 Co3 N4 O14' _chemical_compound_source . _chemical_formula_weight 1055.69 _cell_measurement_reflns_used 5301 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_intense_purple _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 1.162 # Sheldrick geometric approximatio 0.79 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.86 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 42896 _reflns_number_total 5142 _diffrn_reflns_av_R_equivalents 0.092 # Number of reflections with Friedels Law is 5142 # Number of reflections without Friedels Law is 10295 # Theoretical number of reflections is about 5176 _diffrn_reflns_theta_min 5.177 _diffrn_reflns_theta_max 27.473 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.923 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 1.39 _oxford_diffrn_Wilson_scale 78.98 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.10 _refine_diff_density_max 1.48 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5142 _refine_ls_number_restraints 0 _refine_ls_number_parameters 304 _oxford_refine_ls_R_factor_ref 0.0798 _refine_ls_wR_factor_ref 0.1069 _refine_ls_goodness_of_fit_ref 0.8775 _refine_ls_shift/su_max 0.000479 # The values computed from all data _oxford_reflns_number_all 5142 _refine_ls_R_factor_all 0.0798 _refine_ls_wR_factor_all 0.1069 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3232 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_gt 0.0933 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.27P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Co1 Co 0.5000 0.5000 0.5000 0.0135 1.0000 Uani S . . . . . . O2 O 0.69502(16) 0.48563(9) 0.65659(17) 0.0185 1.0000 Uani . . . . . . . Co3 Co 0.68371(3) 0.494322(17) 0.83204(3) 0.0160 1.0000 Uani . . . . . . . O4 O 0.57457(16) 0.58388(9) 0.80500(17) 0.0214 1.0000 Uani . . . . . . . C5 C 0.4824(2) 0.60430(12) 0.6988(2) 0.0165 1.0000 Uani . . . . . . . O6 O 0.45694(17) 0.58075(9) 0.59015(17) 0.0219 1.0000 Uani . . . . . . . C7 C 0.3940(2) 0.66278(12) 0.7002(2) 0.0160 1.0000 Uani . . . . . . . C8 C 0.4014(2) 0.68558(13) 0.8131(2) 0.0176 1.0000 Uani . . . . . . . C9 C 0.3196(2) 0.74089(13) 0.8163(2) 0.0187 1.0000 Uani . . . . . . . C10 C 0.2262(2) 0.77173(13) 0.6994(2) 0.0167 1.0000 Uani . . . . . . . C11 C 0.2196(2) 0.74673(13) 0.5835(2) 0.0187 1.0000 Uani . . . . . . . C12 C 0.3006(2) 0.69435(13) 0.5839(2) 0.0188 1.0000 Uani . . . . . . . C13 C 0.1436(2) 0.82629(13) 0.7027(3) 0.0198 1.0000 Uani . . . . . . . C14 C 0.1531(2) 0.85066(13) 0.8160(2) 0.0190 1.0000 Uani . . . . . . . C15 C 0.0616(2) 0.90720(13) 0.8183(2) 0.0185 1.0000 Uani . . . . . . . O16 O -0.02188(17) 0.93226(9) 0.71088(17) 0.0228 1.0000 Uani . . . . . . . O17 O 0.07310(17) 0.92327(9) 0.92548(17) 0.0231 1.0000 Uani . . . . . . . C18 C 0.2487(2) 0.82029(14) 0.9320(3) 0.0247 1.0000 Uani . . . . . . . C19 C 0.3284(3) 0.76705(14) 0.9328(3) 0.0253 1.0000 Uani . . . . . . . O20 O 0.79777(17) 0.39680(9) 0.88271(18) 0.0277 1.0000 Uani . . . . . . . C21 C 0.7569(3) 0.34506(14) 0.8102(3) 0.0273 1.0000 Uani . . . . . . . N22 N 0.8159(2) 0.28285(12) 0.8367(2) 0.0284 1.0000 Uani . . . . . . . C23 C 0.9388(3) 0.27271(16) 0.9551(3) 0.0387 1.0000 Uani . . . . . . . C24 C 0.7663(3) 0.22541(17) 0.7455(3) 0.0418 1.0000 Uani . . . . . . . O25 O 0.84695(17) 0.54887(10) 0.81115(18) 0.0269 1.0000 Uani . . . . . . . C26 C 0.8043(2) 0.52043(13) 0.7037(3) 0.0197 1.0000 Uani . . . . . . . C27 C 0.8851(2) 0.52357(13) 0.6341(2) 0.0188 1.0000 Uani . . . . . . . C28 C 0.8619(2) 0.47803(14) 0.5372(3) 0.0220 1.0000 Uani . . . . . . . C29 C 0.9460(2) 0.47611(14) 0.4781(3) 0.0190 1.0000 Uani . . . . . . . C30 C 0.9257(2) 0.42795(14) 0.3788(3) 0.0233 1.0000 Uani . . . . . . . C31 C 1.0066(2) 0.42839(14) 0.3232(3) 0.0224 1.0000 Uani . . . . . . . N32 N 0.7796(2) 0.50661(11) 1.0327(2) 0.0248 1.0000 Uani . . . . . . . C33 C 0.6829(3) 0.49858(17) 1.0829(3) 0.0375 1.0000 Uani . . . . . . . C34 C 0.8554(3) 0.57311(15) 1.0774(3) 0.0341 1.0000 Uani . . . . . . . H81 H 0.4617 0.6646 0.8885 0.0221 1.0000 Uiso R . . . . . . H111 H 0.1610 0.7665 0.5052 0.0244 1.0000 Uiso R . . . . . . H121 H 0.2954 0.6788 0.5074 0.0241 1.0000 Uiso R . . . . . . H131 H 0.0817 0.8470 0.6269 0.0225 1.0000 Uiso R . . . . . . H181 H 0.2586 0.8369 1.0082 0.0306 1.0000 Uiso R . . . . . . H191 H 0.3873 0.7475 1.0093 0.0285 1.0000 Uiso R . . . . . . H211 H 0.6767 0.3481 0.7290 0.0323 1.0000 Uiso R . . . . . . H232 H 0.9493 0.2246 0.9856 0.0554 1.0000 Uiso R . . . . . . H233 H 1.0141 0.2850 0.9392 0.0557 1.0000 Uiso R . . . . . . H231 H 0.9383 0.3032 1.0206 0.0555 1.0000 Uiso R . . . . . . H241 H 0.7596 0.1833 0.7889 0.0602 1.0000 Uiso R . . . . . . H242 H 0.8264 0.2173 0.7121 0.0606 1.0000 Uiso R . . . . . . H243 H 0.6799 0.2387 0.6731 0.0594 1.0000 Uiso R . . . . . . H281 H 0.7923 0.4472 0.5087 0.0252 1.0000 Uiso R . . . . . . H301 H 0.8555 0.3958 0.3509 0.0283 1.0000 Uiso R . . . . . . H311 H 0.9921 0.3964 0.2579 0.0269 1.0000 Uiso R . . . . . . H321 H 0.8387 0.4693 1.0645 0.0405 1.0000 Uiso R . . . . . . H331 H 0.6462 0.4509 1.0617 0.0588 1.0000 Uiso R . . . . . . H333 H 0.7277 0.5041 1.1772 0.0580 1.0000 Uiso R . . . . . . H332 H 0.6158 0.5348 1.0440 0.0586 1.0000 Uiso R . . . . . . H342 H 0.9279 0.5720 1.0541 0.0487 1.0000 Uiso R . . . . . . H341 H 0.8914 0.5751 1.1695 0.0507 1.0000 Uiso R . . . . . . H343 H 0.7911 0.6114 1.0356 0.0500 1.0000 Uiso R . . . . . . 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 Co1 0.0159(2) 0.0118(2) 0.0166(3) 0.00021(19) 0.0109(2) 0.00025(18) O2 0.0171(9) 0.0197(9) 0.0224(10) 0.0010(8) 0.0124(8) 0.0000(7) Co3 0.01655(19) 0.01529(19) 0.0189(2) -0.00004(14) 0.01058(15) 0.00003(13) O4 0.0231(9) 0.0173(9) 0.0253(11) 0.0001(8) 0.0127(8) 0.0039(7) C5 0.0186(13) 0.0116(12) 0.0237(15) 0.0013(11) 0.0137(12) 0.0010(10) O6 0.0236(9) 0.0205(9) 0.0225(10) -0.0028(8) 0.0115(8) 0.0064(8) C7 0.0186(12) 0.0119(12) 0.0187(14) -0.0019(10) 0.0099(11) -0.0004(10) C8 0.0157(12) 0.0169(13) 0.0180(14) -0.0003(11) 0.0063(11) 0.0001(10) C9 0.0201(13) 0.0203(14) 0.0196(14) -0.0051(11) 0.0125(11) -0.0017(10) C10 0.0184(12) 0.0141(12) 0.0209(13) -0.0023(11) 0.0118(11) -0.0009(10) C11 0.0218(13) 0.0206(13) 0.0161(13) 0.0010(11) 0.0108(11) 0.0047(11) C12 0.0214(13) 0.0204(13) 0.0172(13) -0.0016(11) 0.0113(11) 0.0019(10) C13 0.0187(13) 0.0185(13) 0.0213(14) 0.0022(11) 0.0087(11) 0.0054(11) C14 0.0181(13) 0.0153(13) 0.0253(15) -0.0031(11) 0.0115(11) 0.0001(10) C15 0.0193(13) 0.0152(13) 0.0255(15) -0.0049(11) 0.0144(12) -0.0040(10) O16 0.0253(10) 0.0221(10) 0.0242(11) 0.0031(8) 0.0142(9) 0.0091(8) O17 0.0259(10) 0.0220(10) 0.0248(10) -0.0020(8) 0.0148(8) 0.0073(8) C18 0.0277(14) 0.0256(15) 0.0216(15) -0.0058(12) 0.0121(12) 0.0043(12) C19 0.0240(14) 0.0274(15) 0.0199(15) -0.0021(12) 0.0064(12) 0.0095(12) O20 0.0276(10) 0.0212(10) 0.0319(12) -0.0018(9) 0.0121(9) 0.0040(8) C21 0.0265(14) 0.0267(15) 0.0274(16) 0.0014(13) 0.0116(13) 0.0053(12) N22 0.0308(13) 0.0205(12) 0.0342(14) -0.0005(11) 0.0155(11) 0.0054(10) C23 0.0394(17) 0.0289(16) 0.0420(19) 0.0014(15) 0.0145(15) 0.0099(14) C24 0.048(2) 0.0272(16) 0.047(2) -0.0071(15) 0.0191(17) 0.0073(14) O25 0.0274(10) 0.0305(11) 0.0282(11) -0.0038(9) 0.0175(9) -0.0060(9) C26 0.0188(13) 0.0181(13) 0.0239(15) 0.0020(12) 0.0115(12) 0.0024(11) C27 0.0170(12) 0.0209(13) 0.0218(14) 0.0043(11) 0.0119(11) 0.0025(11) C28 0.0168(13) 0.0217(13) 0.0271(15) 0.0028(12) 0.0101(12) 0.0000(11) C29 0.0165(12) 0.0196(13) 0.0245(15) 0.0033(12) 0.0126(11) 0.0020(11) C30 0.0192(13) 0.0226(14) 0.0307(15) -0.0016(12) 0.0139(12) -0.0036(11) C31 0.0231(13) 0.0233(14) 0.0232(14) -0.0013(12) 0.0128(12) 0.0016(11) N32 0.0265(12) 0.0228(12) 0.0254(13) 0.0000(10) 0.0125(11) 0.0013(9) C33 0.0382(17) 0.049(2) 0.0283(17) 0.0009(14) 0.0181(14) -0.0044(14) C34 0.0351(16) 0.0331(17) 0.0304(17) -0.0112(14) 0.0124(14) -0.0079(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12064(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . O2 2_666 2.1388(17) yes Co1 . O17 3_546 2.0698(16) yes Co1 . O17 4_564 2.0698(16) yes Co1 . O6 2_666 2.0544(16) yes Co1 . O2 . 2.1388(17) yes Co1 . O6 . 2.0544(16) yes O2 . Co3 . 2.1448(18) yes O2 . C26 . 1.283(3) yes Co3 . O16 3_546 2.0417(16) yes Co3 . O4 . 2.0416(17) yes Co3 . O20 . 2.1787(18) yes Co3 . O25 . 2.2424(17) yes Co3 . C26 . 2.530(3) yes Co3 . N32 . 2.108(2) yes O4 . C5 . 1.261(3) yes C5 . O6 . 1.258(3) yes C5 . C7 . 1.505(3) yes C7 . C8 . 1.368(3) yes C7 . C12 . 1.417(3) yes C8 . C9 . 1.416(3) yes C8 . H81 . 0.922 no C9 . C10 . 1.416(4) yes C9 . C19 . 1.423(3) yes C10 . C11 . 1.419(3) yes C10 . C13 . 1.413(3) yes C11 . C12 . 1.355(3) yes C11 . H111 . 0.928 no C12 . H121 . 0.927 no C13 . C14 . 1.372(3) yes C13 . H131 . 0.928 no C14 . C15 . 1.506(3) yes C14 . C18 . 1.413(4) yes C15 . O16 . 1.268(3) yes C15 . O17 . 1.249(3) yes C18 . C19 . 1.356(3) yes C18 . H181 . 0.911 no C19 . H191 . 0.914 no O20 . C21 . 1.242(3) yes C21 . N22 . 1.323(3) yes C21 . H211 . 0.967 no N22 . C23 . 1.454(4) yes N22 . C24 . 1.449(4) yes C23 . H232 . 0.968 no C23 . H233 . 0.989 no C23 . H231 . 0.970 no C24 . H241 . 0.972 no C24 . H242 . 0.951 no C24 . H243 . 0.986 no O25 . C26 . 1.250(3) yes C26 . C27 . 1.497(3) yes C27 . C31 2_766 1.423(3) yes C27 . C28 . 1.359(4) yes C28 . C29 . 1.426(3) yes C28 . H281 . 0.913 no C29 . C29 2_766 1.417(5) yes C29 . C30 . 1.419(4) yes C30 . C31 . 1.361(3) yes C30 . H301 . 0.934 no C31 . H311 . 0.934 no N32 . C33 . 1.485(4) yes N32 . C34 . 1.480(3) yes N32 . H321 . 0.926 no C33 . H331 . 0.979 no C33 . H333 . 0.990 no C33 . H332 . 0.969 no C34 . H342 . 0.986 no C34 . H341 . 0.968 no C34 . H343 . 0.985 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 2_666 Co1 . O17 3_546 89.77(6) yes O2 2_666 Co1 . O17 4_564 90.23(6) yes O17 3_546 Co1 . O17 4_564 179.994 yes O2 2_666 Co1 . O6 2_666 92.89(7) yes O17 3_546 Co1 . O6 2_666 86.42(7) yes O17 4_564 Co1 . O6 2_666 93.58(7) yes O2 2_666 Co1 . O2 . 179.995 yes O17 3_546 Co1 . O2 . 90.23(6) yes O17 4_564 Co1 . O2 . 89.77(6) yes O6 2_666 Co1 . O2 . 87.11(7) yes O2 2_666 Co1 . O6 . 87.11(7) yes O17 3_546 Co1 . O6 . 93.58(7) yes O17 4_564 Co1 . O6 . 86.42(7) yes O6 2_666 Co1 . O6 . 179.994 yes O2 . Co1 . O6 . 92.89(7) yes Co1 . O2 . Co3 . 108.49(7) yes Co1 . O2 . C26 . 135.38(16) yes Co3 . O2 . C26 . 91.61(15) yes O2 . Co3 . O16 3_546 99.97(7) yes O2 . Co3 . O4 . 102.82(7) yes O16 3_546 Co3 . O4 . 91.68(7) yes O2 . Co3 . O20 . 84.33(7) yes O16 3_546 Co3 . O20 . 85.99(7) yes O4 . Co3 . O20 . 172.78(7) yes O2 . Co3 . O25 . 59.91(6) yes O16 3_546 Co3 . O25 . 159.83(7) yes O4 . Co3 . O25 . 94.23(7) yes O20 . Co3 . O25 . 90.25(7) yes O2 . Co3 . C26 . 30.46(8) yes O16 3_546 Co3 . C26 . 130.24(8) yes O4 . Co3 . C26 . 101.86(7) yes O20 . Co3 . C26 . 84.80(8) yes O25 . Co3 . C26 . 29.59(7) yes O2 . Co3 . N32 . 149.60(8) yes O16 3_546 Co3 . N32 . 105.88(8) yes O4 . Co3 . N32 . 92.26(8) yes O20 . Co3 . N32 . 81.83(8) yes O25 . Co3 . N32 . 93.15(8) yes C26 . Co3 . N32 . 120.89(8) yes Co3 . O4 . C5 . 124.95(16) yes O4 . C5 . O6 . 126.3(2) yes O4 . C5 . C7 . 117.6(2) yes O6 . C5 . C7 . 116.1(2) yes Co1 . O6 . C5 . 142.96(16) yes C5 . C7 . C8 . 120.7(2) yes C5 . C7 . C12 . 120.2(2) yes C8 . C7 . C12 . 119.1(2) yes C7 . C8 . C9 . 121.4(2) yes C7 . C8 . H81 . 118.9 no C9 . C8 . H81 . 119.6 no C8 . C9 . C10 . 118.9(2) yes C8 . C9 . C19 . 122.5(2) yes C10 . C9 . C19 . 118.6(2) yes C9 . C10 . C11 . 118.6(2) yes C9 . C10 . C13 . 118.8(2) yes C11 . C10 . C13 . 122.6(2) yes C10 . C11 . C12 . 121.0(2) yes C10 . C11 . H111 . 121.0 no C12 . C11 . H111 . 118.0 no C7 . C12 . C11 . 120.9(2) yes C7 . C12 . H121 . 119.1 no C11 . C12 . H121 . 120.0 no C10 . C13 . C14 . 121.8(2) yes C10 . C13 . H131 . 119.8 no C14 . C13 . H131 . 118.4 no C13 . C14 . C15 . 121.3(2) yes C13 . C14 . C18 . 118.7(2) yes C15 . C14 . C18 . 119.9(2) yes C14 . C15 . O16 . 116.7(2) yes C14 . C15 . O17 . 116.7(2) yes O16 . C15 . O17 . 126.6(2) yes Co3 3_556 O16 . C15 . 129.07(16) yes Co1 3_556 O17 . C15 . 137.11(17) yes C14 . C18 . C19 . 121.3(2) yes C14 . C18 . H181 . 119.9 no C19 . C18 . H181 . 118.7 no C9 . C19 . C18 . 120.8(2) yes C9 . C19 . H191 . 120.1 no C18 . C19 . H191 . 119.1 no Co3 . O20 . C21 . 120.06(17) yes O20 . C21 . N22 . 124.0(3) yes O20 . C21 . H211 . 120.8 no N22 . C21 . H211 . 115.2 no C21 . N22 . C23 . 119.9(2) yes C21 . N22 . C24 . 121.3(2) yes C23 . N22 . C24 . 118.6(2) yes N22 . C23 . H232 . 112.2 no N22 . C23 . H233 . 108.3 no H232 . C23 . H233 . 109.0 no N22 . C23 . H231 . 109.0 no H232 . C23 . H231 . 108.2 no H233 . C23 . H231 . 110.0 no N22 . C24 . H241 . 109.1 no N22 . C24 . H242 . 109.0 no H241 . C24 . H242 . 109.6 no N22 . C24 . H243 . 109.5 no H241 . C24 . H243 . 112.0 no H242 . C24 . H243 . 107.6 no Co3 . O25 . C26 . 88.06(15) yes O2 . C26 . O25 . 119.9(2) yes O2 . C26 . Co3 . 57.93(13) yes O25 . C26 . Co3 . 62.35(13) yes O2 . C26 . C27 . 120.3(2) yes O25 . C26 . C27 . 119.7(2) yes Co3 . C26 . C27 . 170.29(18) yes C26 . C27 . C31 2_766 119.1(2) yes C26 . C27 . C28 . 120.8(2) yes C31 2_766 C27 . C28 . 120.0(2) yes C27 . C28 . C29 . 121.3(2) yes C27 . C28 . H281 . 120.6 no C29 . C28 . H281 . 118.0 no C28 . C29 . C29 2_766 118.2(3) yes C28 . C29 . C30 . 122.4(2) yes C29 2_766 C29 . C30 . 119.3(3) yes C29 . C30 . C31 . 120.8(2) yes C29 . C30 . H301 . 119.5 no C31 . C30 . H301 . 119.7 no C27 2_766 C31 . C30 . 120.3(2) yes C27 2_766 C31 . H311 . 119.8 no C30 . C31 . H311 . 120.0 no Co3 . N32 . C33 . 110.41(17) yes Co3 . N32 . C34 . 113.76(17) yes C33 . N32 . C34 . 111.3(2) yes Co3 . N32 . H321 . 105.4 no C33 . N32 . H321 . 107.1 no C34 . N32 . H321 . 108.5 no N32 . C33 . H331 . 107.5 no N32 . C33 . H333 . 110.6 no H331 . C33 . H333 . 108.5 no N32 . C33 . H332 . 107.8 no H331 . C33 . H332 . 112.9 no H333 . C33 . H332 . 109.5 no N32 . C34 . H342 . 107.8 no N32 . C34 . H341 . 107.6 no H342 . C34 . H341 . 110.3 no N32 . C34 . H343 . 106.2 no H342 . C34 . H343 . 113.5 no H341 . C34 . H343 . 111.0 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C28 . H281 . O6 2_666 152 0.91 2.57 3.402(4) yes _chemical_name_common . #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 701454' #============================================================================== _audit_creation_date 08-08-19 _audit_creation_method CRYSTALS_ver_12.86 _publ_section_exptl_refinement ; The difference map indicated the presence of diffuse electron density believed to be disordered solvent. SQUEEZE was used leaving a void of 1238 \%A from which 203 e^-^ were removed. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.276 -0.119 0.776 1238 203 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _oxford_structure_analysis_title 5801 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 17.8669(6) _cell_length_b 14.1157(6) _cell_length_c 19.8394(7) _cell_angle_alpha 90 _cell_angle_beta 91.256(3) _cell_angle_gamma 90 _cell_volume 5002.4(3) _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 -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C36 H24 Cl2 N2 Ni2 O24 # Dc = 1.40 Fooo = 2088.00 Mu = 9.39 M = 1056.91 # Found Formula = C37 H35 N3 Ni3 O20 # Dc = 1.35 FOOO = 2088.00 Mu = 11.89 M = 1017.82 _chemical_formula_sum 'C37 H35 N3 Ni3 O20' _chemical_formula_moiety 'C30 H16 N Ni3 O19, C4 H12 N, C3 H7 N O' _chemical_compound_source . _chemical_formula_weight 1017.82 _cell_measurement_reflns_used 9351 _cell_measurement_theta_min 5 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_green _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 1.189 # Sheldrick geometric approximatio 0.94 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.96 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 16260 _reflns_number_total 9586 _diffrn_reflns_av_R_equivalents 0.150 # Number of reflections with Friedels Law is 9586 # Number of reflections without Friedels Law is 9586 # Theoretical number of reflections is about 9809 _diffrn_reflns_theta_min 5.133 _diffrn_reflns_theta_max 25.977 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.198 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -21 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 1.45 _oxford_diffrn_Wilson_scale 167.96 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.16 _refine_diff_density_max 1.11 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 7206 _refine_ls_number_restraints 0 _refine_ls_number_parameters 568 _oxford_refine_ls_R_factor_ref 0.1077 _refine_ls_wR_factor_ref 0.1733 _refine_ls_goodness_of_fit_ref 0.9774 _refine_ls_shift/su_max 0.000376 # The values computed from all data _oxford_reflns_number_all 7206 _refine_ls_R_factor_all 0.1077 _refine_ls_wR_factor_all 0.1733 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4709 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_gt 0.1521 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +20.61P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ni1 Ni 0.24806(5) 0.05190(6) 0.42907(4) 0.0206 1.0000 Uani . . . . . . . O2 O 0.2384(3) 0.5102(3) 0.1681(2) 0.0266 1.0000 Uani . . . . . . . C3 C 0.2419(4) 0.4333(5) 0.1974(4) 0.0241 1.0000 Uani . . . . . . . O4 O 0.2570(3) 0.3516(3) 0.1731(2) 0.0266 1.0000 Uani . . . . . . . Ni5 Ni 0.20257(5) -0.18403(6) 0.41592(4) 0.0203 1.0000 Uani . . . . . . . O6 O 0.2633(3) -0.0854(3) 0.4666(2) 0.0225 1.0000 Uani . . . . . . . C7 C 0.3184(4) -0.1425(5) 0.4806(3) 0.0220 1.0000 Uani . . . . . . . O8 O 0.3154(3) -0.2255(3) 0.4569(2) 0.0284 1.0000 Uani . . . . . . . C9 C 0.3820(4) -0.1084(5) 0.5233(3) 0.0216 1.0000 Uani . . . . . . . C10 C 0.3676(4) -0.0333(5) 0.5685(4) 0.0317 1.0000 Uani . . . . . . . C11 C 0.4248(4) 0.0078(6) 0.6067(4) 0.0302 1.0000 Uani . . . . . . . C12 C 0.4977(4) -0.0259(6) 0.5984(4) 0.0313 1.0000 Uani . . . . . . . C13 C 0.5119(4) -0.0990(5) 0.5534(4) 0.0276 1.0000 Uani . . . . . . . C14 C 0.4539(4) -0.1410(5) 0.5159(4) 0.0260 1.0000 Uani . . . . . . . C15 C 0.5935(4) -0.1228(5) 0.5380(4) 0.0279 1.0000 Uani . . . . . . . O16 O 0.6419(3) -0.0734(3) 0.5676(2) 0.0262 1.0000 Uani . . . . . . . O17 O 0.6040(3) -0.1882(4) 0.4955(2) 0.0314 1.0000 Uani . . . . . . . Ni18 Ni 0.30263(5) 0.20592(7) 0.55638(5) 0.0268 1.0000 Uani . . . . . . . O19 O 0.2369(3) 0.0938(3) 0.5305(2) 0.0241 1.0000 Uani . . . . . . . C20 C 0.1841(4) 0.1142(5) 0.5705(4) 0.0265 1.0000 Uani . . . . . . . O21 O 0.1883(3) 0.1873(3) 0.6057(3) 0.0328 1.0000 Uani . . . . . . . C22 C 0.1216(4) 0.0440(5) 0.5760(3) 0.0228 1.0000 Uani . . . . . . . C23 C 0.0483(4) 0.0735(5) 0.5897(3) 0.0260 1.0000 Uani . . . . . . . C24 C -0.0095(4) 0.0061(5) 0.5869(3) 0.0213 1.0000 Uani . . . . . . . C25 C 0.0072(4) -0.0893(5) 0.5739(3) 0.0204 1.0000 Uani . . . . . . . C26 C 0.0799(4) -0.1176(5) 0.5635(3) 0.0216 1.0000 Uani . . . . . . . C27 C 0.1376(4) -0.0508(5) 0.5640(4) 0.0261 1.0000 Uani . . . . . . . C28 C 0.0951(4) -0.2198(5) 0.5456(4) 0.0298 1.0000 Uani . . . . . . . O29 O 0.1596(3) -0.2348(3) 0.5159(2) 0.0273 1.0000 Uani . . . . . . . O30 O 0.0506(3) -0.2814(4) 0.5578(3) 0.0540 1.0000 Uani . . . . . . . C31 C -0.0911(4) 0.0352(5) 0.5893(3) 0.0209 1.0000 Uani . . . . . . . O32 O -0.1032(3) 0.1229(3) 0.5993(2) 0.0257 1.0000 Uani . . . . . . . O33 O -0.1374(3) -0.0291(3) 0.5815(2) 0.0257 1.0000 Uani . . . . . . . O34 O 0.2488(3) 0.2799(3) 0.4839(2) 0.0307 1.0000 Uani . . . . . . . C35 C 0.2349(4) 0.2636(5) 0.4215(4) 0.0252 1.0000 Uani . . . . . . . O36 O 0.2306(3) 0.1855(3) 0.3920(2) 0.0273 1.0000 Uani . . . . . . . C37 C 0.2232(4) 0.3526(5) 0.3784(3) 0.0228 1.0000 Uani . . . . . . . C38 C 0.2072(4) 0.4377(5) 0.4113(4) 0.0265 1.0000 Uani . . . . . . . C39 C 0.2000(4) 0.5196(5) 0.3733(4) 0.0264 1.0000 Uani . . . . . . . C40 C 0.2093(4) 0.5183(5) 0.3048(4) 0.0256 1.0000 Uani . . . . . . . C41 C 0.2262(4) 0.4336(5) 0.2727(3) 0.0229 1.0000 Uani . . . . . . . C42 C 0.2328(4) 0.3510(5) 0.3109(4) 0.0246 1.0000 Uani . . . . . . . C43 C 0.1844(4) 0.6111(5) 0.4103(4) 0.0260 1.0000 Uani . . . . . . . O44 O 0.1788(3) 0.6864(3) 0.3773(2) 0.0216 1.0000 Uani . . . . . . . O45 O 0.1797(3) 0.6049(3) 0.4748(2) 0.0340 1.0000 Uani . . . . . . . O46 O 0.3489(3) 0.1396(4) 0.6397(2) 0.0381 1.0000 Uani . . . . . . . C47 C 0.4085(5) 0.0909(6) 0.6521(4) 0.0412 1.0000 Uani . . . . . . . O48 O 0.4538(4) 0.1088(6) 0.6983(4) 0.0792 1.0000 Uani . . . . . . . O49 O 0.3381(3) 0.3355(4) 0.5926(3) 0.0391 1.0000 Uani . . . . . . . C50 C 0.3629(5) 0.3914(6) 0.5503(5) 0.0455 1.0000 Uani . . . . . . . N51 N 0.3666(5) 0.4838(5) 0.5561(4) 0.0555 1.0000 Uani . . . . . . . C52 C 0.3960(6) 0.5446(8) 0.5047(5) 0.0688 1.0000 Uani . . . . . . . C53 C 0.3364(8) 0.5299(9) 0.6151(7) 0.0958 1.0000 Uani . . . . . . . N54 N 0.0626(4) 0.1714(6) 0.2247(4) 0.0513 1.0000 Uani . . . . . . . C55 C 0.1026(9) 0.2208(10) 0.1737(6) 0.0992 1.0000 Uani . . . . . . . C56 C -0.0106(7) 0.1331(10) 0.2001(9) 0.1121 1.0000 Uani . . . . . . . C57 C 0.1092(8) 0.0932(10) 0.2527(6) 0.0981 1.0000 Uani . . . . . . . C58 C 0.0481(8) 0.2407(12) 0.2824(7) 0.1157 1.0000 Uani . . . . . . . C59 C 0.0964(5) 0.7046(7) 0.2135(5) 0.0494 1.0000 Uani . . . . . . . N60 N 0.0588(5) 0.7914(6) 0.1983(4) 0.0545 1.0000 Uani . . . . . . . C61 C 0.0696(7) 0.8372(9) 0.1412(6) 0.0688 1.0000 Uani . . . . . . . O62 O 0.0404(5) 0.9149(6) 0.1252(4) 0.0936 1.0000 Uani . . . . . . . C63 C 0.0072(8) 0.8278(10) 0.2484(6) 0.0952 1.0000 Uani . . . . . . . H101 H 0.3181 -0.0101 0.5725 0.0363 1.0000 Uiso R . . . . . . H121 H 0.5384 0.0017 0.6236 0.0382 1.0000 Uiso R . . . . . . H141 H 0.4634 -0.1920 0.4851 0.0339 1.0000 Uiso R . . . . . . H231 H 0.0379 0.1371 0.6006 0.0302 1.0000 Uiso R . . . . . . H251 H -0.0319 -0.1351 0.5728 0.0280 1.0000 Uiso R . . . . . . H271 H 0.1873 -0.0710 0.5563 0.0311 1.0000 Uiso R . . . . . . H381 H 0.2030 0.4397 0.4588 0.0289 1.0000 Uiso R . . . . . . H401 H 0.2040 0.5745 0.2793 0.0312 1.0000 Uiso R . . . . . . H421 H 0.2452 0.2938 0.2892 0.0311 1.0000 Uiso R . . . . . . H522 H 0.3639 0.6008 0.4988 0.1042 1.0000 Uiso R . . . . . . H523 H 0.4471 0.5665 0.5180 0.1042 1.0000 Uiso R . . . . . . H521 H 0.3989 0.5105 0.4613 0.1041 1.0000 Uiso R . . . . . . H533 H 0.3603 0.5907 0.6237 0.1400 1.0000 Uiso R . . . . . . H531 H 0.3440 0.4903 0.6549 0.1401 1.0000 Uiso R . . . . . . H532 H 0.2828 0.5415 0.6096 0.1401 1.0000 Uiso R . . . . . . H551 H 0.1535 0.2332 0.1894 0.1450 1.0000 Uiso R . . . . . . H552 H 0.0776 0.2797 0.1636 0.1452 1.0000 Uiso R . . . . . . H553 H 0.1038 0.1813 0.1338 0.1452 1.0000 Uiso R . . . . . . H562 H -0.0406 0.1102 0.2369 0.1591 1.0000 Uiso R . . . . . . H563 H -0.0368 0.1813 0.1756 0.1591 1.0000 Uiso R . . . . . . H561 H -0.0015 0.0793 0.1696 0.1591 1.0000 Uiso R . . . . . . H573 H 0.0789 0.0543 0.2815 0.1551 1.0000 Uiso R . . . . . . H571 H 0.1507 0.1196 0.2803 0.1551 1.0000 Uiso R . . . . . . H572 H 0.1288 0.0574 0.2167 0.1550 1.0000 Uiso R . . . . . . H581 H 0.0214 0.2108 0.3179 0.1480 1.0000 Uiso R . . . . . . H583 H 0.0949 0.2659 0.2995 0.1481 1.0000 Uiso R . . . . . . H582 H 0.0179 0.2937 0.2647 0.1480 1.0000 Uiso R . . . . . . H592 H 0.1203 0.7078 0.2613 0.0742 1.0000 Uiso R . . . . . . H591 H 0.1374 0.6936 0.1784 0.0743 1.0000 Uiso R . . . . . . H593 H 0.0584 0.6491 0.2112 0.0743 1.0000 Uiso R . . . . . . H611 H 0.1030 0.8100 0.1082 0.0863 1.0000 Uiso R . . . . . . H632 H -0.0124 0.8904 0.2355 0.1460 1.0000 Uiso R . . . . . . H631 H 0.0316 0.8337 0.2917 0.1460 1.0000 Uiso R . . . . . . H633 H -0.0361 0.7857 0.2529 0.1461 1.0000 Uiso R . . . . . . H501 H 0.3800 0.3653 0.5093 0.0575 1.0000 Uiso R . . . . . . 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 Ni1 0.0226(5) 0.0114(5) 0.0277(5) -0.0011(4) 0.0006(4) 0.0004(4) O2 0.031(3) 0.016(3) 0.033(3) 0.000(2) 0.001(2) -0.003(2) C3 0.015(4) 0.026(5) 0.031(4) 0.004(3) 0.004(3) 0.000(3) O4 0.036(3) 0.012(3) 0.032(3) 0.002(2) 0.009(2) 0.001(2) Ni5 0.0221(5) 0.0107(5) 0.0282(5) 0.0002(4) 0.0006(4) 0.0006(4) O6 0.025(3) 0.015(3) 0.028(3) 0.002(2) 0.002(2) 0.000(2) C7 0.027(4) 0.012(4) 0.027(4) 0.003(3) 0.005(3) 0.004(3) O8 0.027(3) 0.021(3) 0.038(3) 0.001(2) 0.003(2) 0.004(2) C9 0.028(4) 0.014(4) 0.023(4) -0.005(3) -0.001(3) -0.004(3) C10 0.028(5) 0.027(5) 0.041(5) -0.003(4) -0.002(4) 0.005(4) C11 0.028(5) 0.028(4) 0.035(4) 0.001(4) -0.007(4) 0.006(4) C12 0.026(5) 0.039(5) 0.028(4) -0.003(4) -0.003(3) 0.000(4) C13 0.030(5) 0.022(4) 0.032(4) 0.003(3) 0.004(4) 0.007(4) C14 0.025(4) 0.020(4) 0.032(4) -0.001(3) -0.002(3) 0.000(3) C15 0.028(5) 0.021(4) 0.034(4) 0.012(4) 0.006(4) -0.004(4) O16 0.023(3) 0.021(3) 0.035(3) -0.001(2) 0.003(2) -0.004(2) O17 0.030(3) 0.028(3) 0.037(3) -0.009(3) 0.003(2) 0.004(2) Ni18 0.0298(6) 0.0194(5) 0.0313(5) -0.0024(4) 0.0003(4) 0.0000(4) O19 0.023(3) 0.021(3) 0.028(3) -0.003(2) 0.002(2) 0.004(2) C20 0.022(4) 0.015(4) 0.042(5) -0.001(3) 0.001(4) -0.004(3) O21 0.035(3) 0.018(3) 0.046(3) -0.008(3) 0.004(3) 0.000(2) C22 0.024(4) 0.017(4) 0.028(4) 0.002(3) 0.001(3) 0.002(3) C23 0.034(5) 0.016(4) 0.028(4) -0.006(3) -0.002(3) 0.002(3) C24 0.018(4) 0.019(4) 0.027(4) 0.003(3) -0.001(3) 0.006(3) C25 0.026(4) 0.014(4) 0.021(4) 0.000(3) 0.001(3) 0.001(3) C26 0.030(4) 0.013(4) 0.022(4) 0.002(3) 0.007(3) 0.003(3) C27 0.018(4) 0.027(4) 0.033(4) -0.002(3) -0.001(3) 0.005(4) C28 0.033(5) 0.018(4) 0.039(5) -0.003(3) 0.001(4) 0.006(4) O29 0.032(3) 0.018(3) 0.032(3) -0.001(2) 0.007(2) 0.005(2) O30 0.051(4) 0.016(3) 0.097(5) -0.007(3) 0.034(4) -0.006(3) C31 0.016(4) 0.024(5) 0.023(4) 0.003(3) -0.001(3) 0.003(4) O32 0.027(3) 0.020(3) 0.031(3) 0.000(2) 0.001(2) 0.004(2) O33 0.020(3) 0.016(3) 0.042(3) 0.001(2) -0.001(2) 0.002(2) O34 0.043(3) 0.018(3) 0.031(3) 0.000(2) -0.002(2) 0.004(2) C35 0.033(5) 0.012(4) 0.031(5) 0.000(3) 0.005(3) 0.005(3) O36 0.039(3) 0.011(3) 0.033(3) -0.003(2) 0.006(2) 0.001(2) C37 0.029(4) 0.015(4) 0.026(4) -0.002(3) 0.006(3) 0.000(3) C38 0.035(5) 0.014(4) 0.030(4) 0.002(3) -0.002(3) -0.001(3) C39 0.032(5) 0.014(4) 0.034(5) 0.000(3) -0.002(3) -0.001(3) C40 0.034(5) 0.013(4) 0.029(4) -0.001(3) 0.003(3) 0.001(3) C41 0.031(4) 0.010(4) 0.028(4) -0.002(3) 0.001(3) 0.001(3) C42 0.026(4) 0.016(4) 0.032(4) -0.006(3) 0.001(3) 0.002(3) C43 0.031(5) 0.014(4) 0.033(5) -0.006(3) 0.001(3) -0.007(3) O44 0.030(3) 0.008(2) 0.027(3) 0.004(2) -0.001(2) 0.002(2) O45 0.058(4) 0.018(3) 0.025(3) -0.003(2) 0.005(3) 0.003(3) O46 0.046(4) 0.041(4) 0.027(3) -0.006(3) -0.004(3) 0.011(3) C47 0.035(5) 0.040(5) 0.049(6) -0.008(4) 0.005(4) 0.004(5) O48 0.071(5) 0.083(6) 0.082(5) -0.049(4) -0.039(4) 0.031(4) O49 0.036(3) 0.027(3) 0.054(4) -0.007(3) -0.003(3) -0.007(3) C50 0.038(5) 0.023(5) 0.075(7) -0.010(5) -0.004(5) -0.012(4) N51 0.056(5) 0.036(5) 0.074(6) -0.004(4) -0.005(4) 0.006(4) C52 0.076(8) 0.056(7) 0.075(8) 0.023(6) 0.002(6) -0.012(6) C53 0.124(12) 0.053(8) 0.113(11) -0.016(7) 0.043(9) -0.016(8) N54 0.045(5) 0.066(6) 0.042(4) 0.012(4) -0.007(4) 0.001(4) C55 0.132(13) 0.093(10) 0.073(8) 0.001(7) 0.028(8) -0.036(9) C56 0.066(9) 0.086(10) 0.182(15) -0.004(10) -0.054(9) -0.008(8) C57 0.092(10) 0.126(12) 0.077(8) 0.042(8) -0.003(7) 0.051(9) C58 0.090(11) 0.164(16) 0.091(10) 0.032(11) -0.038(8) -0.046(11) C59 0.048(6) 0.051(6) 0.048(5) -0.004(5) -0.004(4) 0.005(5) N60 0.059(5) 0.058(5) 0.046(5) -0.003(4) -0.005(4) 0.020(4) C61 0.068(8) 0.076(9) 0.062(7) -0.001(6) -0.008(6) -0.004(7) O62 0.116(7) 0.074(6) 0.090(6) 0.025(5) -0.002(5) 0.035(5) C63 0.114(11) 0.099(11) 0.073(8) -0.001(7) 0.023(8) 0.028(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.07936(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . O2 3_545 2.036(5) yes Ni1 . O33 2_556 2.009(5) yes Ni1 . O16 2_656 1.989(5) yes Ni1 . O6 . 2.091(5) yes Ni1 . O19 . 2.110(5) yes Ni1 . O36 . 2.046(5) yes O2 . C3 . 1.232(8) yes C3 . O4 . 1.280(8) yes C3 . C41 . 1.525(10) yes O4 . Ni5 3_555 1.987(5) yes Ni5 . O44 1_545 2.025(5) yes Ni5 . O32 2_556 1.992(5) yes Ni5 . O6 . 2.020(5) yes Ni5 . O8 . 2.236(5) yes Ni5 . O29 . 2.259(5) yes O6 . C7 . 1.299(8) yes C7 . O8 . 1.262(8) yes C7 . C9 . 1.483(10) yes C9 . C10 . 1.415(10) yes C9 . C14 . 1.376(10) yes C10 . C11 . 1.386(11) yes C10 . H101 . 0.949 no C11 . C12 . 1.401(11) yes C11 . C47 . 1.512(11) yes C12 . C13 . 1.391(10) yes C12 . H121 . 0.956 no C13 . C14 . 1.395(10) yes C13 . C15 . 1.533(10) yes C14 . H141 . 0.962 no C15 . O16 . 1.247(9) yes C15 . O17 . 1.267(9) yes O17 . Ni18 2_656 1.996(5) yes Ni18 . O19 . 2.030(5) yes Ni18 . O21 . 2.299(5) yes Ni18 . O34 . 2.006(5) yes Ni18 . O46 . 2.057(5) yes Ni18 . O49 . 2.060(5) yes O19 . C20 . 1.281(8) yes C20 . O21 . 1.246(8) yes C20 . C22 . 1.498(10) yes C22 . C23 . 1.407(10) yes C22 . C27 . 1.390(10) yes C23 . C24 . 1.404(10) yes C23 . H231 . 0.943 no C24 . C25 . 1.405(9) yes C24 . C31 . 1.518(9) yes C25 . C26 . 1.378(10) yes C25 . H251 . 0.952 no C26 . C27 . 1.397(10) yes C26 . C28 . 1.512(10) yes C27 . H271 . 0.948 no C28 . O29 . 1.324(9) yes C28 . O30 . 1.206(9) yes C31 . O32 . 1.272(8) yes C31 . O33 . 1.236(8) yes O34 . C35 . 1.278(8) yes C35 . O36 . 1.250(8) yes C35 . C37 . 1.531(10) yes C37 . C38 . 1.399(10) yes C37 . C42 . 1.355(10) yes C38 . C39 . 1.386(10) yes C38 . H381 . 0.948 no C39 . C40 . 1.372(10) yes C39 . C43 . 1.515(10) yes C40 . C41 . 1.391(9) yes C40 . H401 . 0.946 no C41 . C42 . 1.394(10) yes C42 . H421 . 0.943 no C43 . O44 . 1.251(8) yes C43 . O45 . 1.287(8) yes O46 . C47 . 1.286(10) yes C47 . O48 . 1.236(10) yes O49 . C50 . 1.241(10) yes C50 . N51 . 1.310(11) yes C50 . H501 . 0.950 no N51 . C52 . 1.441(12) yes N51 . C53 . 1.452(13) yes C52 . H522 . 0.986 no C52 . H523 . 0.993 no C52 . H521 . 0.989 no C53 . H533 . 0.972 no C53 . H531 . 0.976 no C53 . H532 . 0.975 no N54 . C55 . 1.432(13) yes N54 . C56 . 1.488(14) yes N54 . C57 . 1.482(13) yes N54 . C58 . 1.531(17) yes C55 . H551 . 0.971 no C55 . H552 . 0.963 no C55 . H553 . 0.969 no C56 . H562 . 0.970 no C56 . H563 . 0.954 no C56 . H561 . 0.985 no C57 . H573 . 0.967 no C57 . H571 . 0.985 no C57 . H572 . 0.950 no C58 . H581 . 0.958 no C58 . H583 . 0.964 no C58 . H582 . 0.982 no C59 . N60 . 1.426(11) yes C59 . H592 . 1.033 no C59 . H591 . 1.032 no C59 . H593 . 1.038 no N60 . C61 . 1.321(13) yes N60 . C63 . 1.464(13) yes C61 . O62 . 1.253(13) yes C61 . H611 . 0.975 no C63 . H632 . 0.983 no C63 . H631 . 0.959 no C63 . H633 . 0.981 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 3_545 Ni1 . O33 2_556 89.5(2) yes O2 3_545 Ni1 . O16 2_656 86.4(2) yes O33 2_556 Ni1 . O16 2_656 175.9(2) yes O2 3_545 Ni1 . O6 . 92.98(18) yes O33 2_556 Ni1 . O6 . 90.52(19) yes O16 2_656 Ni1 . O6 . 90.51(19) yes O2 3_545 Ni1 . O19 . 178.5(2) yes O33 2_556 Ni1 . O19 . 91.78(19) yes O16 2_656 Ni1 . O19 . 92.27(19) yes O6 . Ni1 . O19 . 86.26(18) yes O2 3_545 Ni1 . O36 . 86.89(19) yes O33 2_556 Ni1 . O36 . 88.2(2) yes O16 2_656 Ni1 . O36 . 90.8(2) yes O6 . Ni1 . O36 . 178.7(2) yes O19 . Ni1 . O36 . 93.89(19) yes Ni1 3_555 O2 . C3 . 134.0(5) yes O2 . C3 . O4 . 128.7(6) yes O2 . C3 . C41 . 116.7(6) yes O4 . C3 . C41 . 114.6(6) yes C3 . O4 . Ni5 3_555 130.2(4) yes O44 1_545 Ni5 . O32 2_556 98.93(19) yes O44 1_545 Ni5 . O4 3_545 88.26(18) yes O32 2_556 Ni5 . O4 3_545 95.5(2) yes O44 1_545 Ni5 . O6 . 156.51(19) yes O32 2_556 Ni5 . O6 . 104.1(2) yes O4 3_545 Ni5 . O6 . 93.77(19) yes O44 1_545 Ni5 . O8 . 94.65(19) yes O32 2_556 Ni5 . O8 . 164.33(19) yes O4 3_545 Ni5 . O8 . 92.7(2) yes O6 . Ni5 . O8 . 61.90(19) yes O44 1_545 Ni5 . O29 . 88.47(18) yes O32 2_556 Ni5 . O29 . 87.24(18) yes O4 3_545 Ni5 . O29 . 176.02(18) yes O6 . Ni5 . O29 . 88.33(18) yes O8 . Ni5 . O29 . 85.33(18) yes Ni1 . O6 . Ni5 . 113.4(2) yes Ni1 . O6 . C7 . 138.1(4) yes Ni5 . O6 . C7 . 94.3(4) yes O6 . C7 . O8 . 118.1(7) yes O6 . C7 . C9 . 119.2(6) yes O8 . C7 . C9 . 122.7(6) yes Ni5 . O8 . C7 . 85.6(4) yes C7 . C9 . C10 . 117.3(7) yes C7 . C9 . C14 . 122.4(6) yes C10 . C9 . C14 . 120.1(7) yes C9 . C10 . C11 . 121.2(7) yes C9 . C10 . H101 . 119.6 no C11 . C10 . H101 . 119.2 no C10 . C11 . C12 . 118.1(7) yes C10 . C11 . C47 . 120.1(7) yes C12 . C11 . C47 . 121.7(7) yes C11 . C12 . C13 . 120.7(7) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 119.5 no C12 . C13 . C14 . 120.9(7) yes C12 . C13 . C15 . 118.5(7) yes C14 . C13 . C15 . 120.0(7) yes C13 . C14 . C9 . 119.0(7) yes C13 . C14 . H141 . 121.2 no C9 . C14 . H141 . 119.8 no C13 . C15 . O16 . 115.9(7) yes C13 . C15 . O17 . 116.5(7) yes O16 . C15 . O17 . 127.6(7) yes C15 . O16 . Ni1 2_656 140.8(5) yes C15 . O17 . Ni18 2_656 124.9(5) yes O17 2_656 Ni18 . O19 . 104.9(2) yes O17 2_656 Ni18 . O21 . 165.0(2) yes O19 . Ni18 . O21 . 60.29(18) yes O17 2_656 Ni18 . O34 . 95.1(2) yes O19 . Ni18 . O34 . 87.6(2) yes O21 . Ni18 . O34 . 87.0(2) yes O17 2_656 Ni18 . O46 . 91.8(2) yes O19 . Ni18 . O46 . 93.9(2) yes O21 . Ni18 . O46 . 87.2(2) yes O34 . Ni18 . O46 . 172.3(2) yes O17 2_656 Ni18 . O49 . 92.2(2) yes O19 . Ni18 . O49 . 162.2(2) yes O21 . Ni18 . O49 . 102.8(2) yes O34 . Ni18 . O49 . 85.8(2) yes O46 . Ni18 . O49 . 90.5(2) yes Ni1 . O19 . Ni18 . 113.2(2) yes Ni1 . O19 . C20 . 137.8(5) yes Ni18 . O19 . C20 . 95.6(4) yes O19 . C20 . O21 . 119.8(7) yes O19 . C20 . C22 . 117.2(6) yes O21 . C20 . C22 . 122.9(6) yes Ni18 . O21 . C20 . 84.3(4) yes C20 . C22 . C23 . 121.1(6) yes C20 . C22 . C27 . 117.9(6) yes C23 . C22 . C27 . 120.9(7) yes C22 . C23 . C24 . 118.6(6) yes C22 . C23 . H231 . 121.0 no C24 . C23 . H231 . 120.4 no C23 . C24 . C25 . 119.9(6) yes C23 . C24 . C31 . 121.4(6) yes C25 . C24 . C31 . 118.3(6) yes C24 . C25 . C26 . 120.6(7) yes C24 . C25 . H251 . 119.8 no C26 . C25 . H251 . 119.6 no C25 . C26 . C27 . 120.1(6) yes C25 . C26 . C28 . 119.0(7) yes C27 . C26 . C28 . 120.7(7) yes C26 . C27 . C22 . 119.8(7) yes C26 . C27 . H271 . 119.3 no C22 . C27 . H271 . 120.9 no C26 . C28 . O29 . 114.8(7) yes C26 . C28 . O30 . 121.3(7) yes O29 . C28 . O30 . 123.9(7) yes Ni5 . O29 . C28 . 131.1(5) yes C24 . C31 . O32 . 115.7(6) yes C24 . C31 . O33 . 116.0(6) yes O32 . C31 . O33 . 128.3(6) yes C31 . O32 . Ni5 2_556 123.4(5) yes C31 . O33 . Ni1 2_556 141.7(5) yes Ni18 . O34 . C35 . 132.8(5) yes O34 . C35 . O36 . 128.5(6) yes O34 . C35 . C37 . 114.4(6) yes O36 . C35 . C37 . 117.1(6) yes C35 . O36 . Ni1 . 129.5(5) yes C35 . C37 . C38 . 118.1(6) yes C35 . C37 . C42 . 121.3(6) yes C38 . C37 . C42 . 120.4(7) yes C37 . C38 . C39 . 118.7(7) yes C37 . C38 . H381 . 120.8 no C39 . C38 . H381 . 120.5 no C38 . C39 . C40 . 121.0(7) yes C38 . C39 . C43 . 117.6(6) yes C40 . C39 . C43 . 121.3(6) yes C39 . C40 . C41 . 119.9(7) yes C39 . C40 . H401 . 120.4 no C41 . C40 . H401 . 119.7 no C3 . C41 . C40 . 119.9(6) yes C3 . C41 . C42 . 121.0(6) yes C40 . C41 . C42 . 119.0(6) yes C41 . C42 . C37 . 120.9(6) yes C41 . C42 . H421 . 119.0 no C37 . C42 . H421 . 120.0 no C39 . C43 . O44 . 118.9(6) yes C39 . C43 . O45 . 116.2(6) yes O44 . C43 . O45 . 124.9(6) yes C43 . O44 . Ni5 1_565 123.8(4) yes Ni18 . O46 . C47 . 135.5(5) yes C11 . C47 . O46 . 118.0(8) yes C11 . C47 . O48 . 118.0(8) yes O46 . C47 . O48 . 124.0(8) yes Ni18 . O49 . C50 . 116.1(5) yes O49 . C50 . N51 . 126.2(9) yes O49 . C50 . H501 . 117.3 no N51 . C50 . H501 . 116.4 no C50 . N51 . C52 . 123.3(9) yes C50 . N51 . C53 . 119.9(9) yes C52 . N51 . C53 . 116.8(9) yes N51 . C52 . H522 . 110.1 no N51 . C52 . H523 . 110.2 no H522 . C52 . H523 . 108.0 no N51 . C52 . H521 . 110.7 no H522 . C52 . H521 . 109.2 no H523 . C52 . H521 . 108.5 no N51 . C53 . H533 . 111.6 no N51 . C53 . H531 . 110.4 no H533 . C53 . H531 . 108.1 no N51 . C53 . H532 . 111.5 no H533 . C53 . H532 . 107.4 no H531 . C53 . H532 . 107.7 no C55 . N54 . C56 . 113.1(10) yes C55 . N54 . C57 . 110.0(10) yes C56 . N54 . C57 . 109.5(10) yes C55 . N54 . C58 . 108.2(10) yes C56 . N54 . C58 . 108.4(10) yes C57 . N54 . C58 . 107.4(9) yes N54 . C55 . H551 . 109.9 no N54 . C55 . H552 . 109.4 no H551 . C55 . H552 . 109.8 no N54 . C55 . H553 . 108.6 no H551 . C55 . H553 . 109.1 no H552 . C55 . H553 . 110.1 no N54 . C56 . H562 . 111.7 no N54 . C56 . H563 . 109.0 no H562 . C56 . H563 . 110.4 no N54 . C56 . H561 . 109.0 no H562 . C56 . H561 . 107.9 no H563 . C56 . H561 . 108.8 no N54 . C57 . H573 . 109.1 no N54 . C57 . H571 . 109.7 no H573 . C57 . H571 . 108.1 no N54 . C57 . H572 . 109.2 no H573 . C57 . H572 . 111.2 no H571 . C57 . H572 . 109.5 no N54 . C58 . H581 . 111.3 no N54 . C58 . H583 . 109.8 no H581 . C58 . H583 . 110.2 no N54 . C58 . H582 . 108.8 no H581 . C58 . H582 . 108.7 no H583 . C58 . H582 . 108.0 no N60 . C59 . H592 . 109.9 no N60 . C59 . H591 . 108.9 no H592 . C59 . H591 . 109.9 no N60 . C59 . H593 . 109.6 no H592 . C59 . H593 . 109.2 no H591 . C59 . H593 . 109.3 no C59 . N60 . C61 . 121.7(9) yes C59 . N60 . C63 . 117.3(9) yes C61 . N60 . C63 . 121.0(10) yes N60 . C61 . O62 . 125.3(11) yes N60 . C61 . H611 . 119.1 no O62 . C61 . H611 . 115.6 no N60 . C63 . H632 . 111.5 no N60 . C63 . H631 . 111.0 no H632 . C63 . H631 . 107.8 no N60 . C63 . H633 . 111.1 no H632 . C63 . H633 . 106.9 no H631 . C63 . H633 . 108.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C10 . H101 . O19 . 143 0.95 2.21 3.027(12) yes C27 . H271 . O6 . 137 0.95 2.27 3.035(12) yes C52 . H521 . O62 3_545 155 0.99 2.45 3.378(12) yes C55 . H551 . O4 . 140 0.97 2.52 3.319(12) yes C56 . H561 . O62 1_545 161 0.99 2.60 3.547(12) yes C58 . H582 . O48 4_454 164 0.98 2.21 3.163(12) yes C59 . H592 . O44 . 171 1.03 2.52 3.548(12) yes C63 . H631 . O32 2_566 170 0.96 2.56 3.511(12) yes #============================================================================== # start Validation Reply Form #============================================================================== _vrf_PLAT601_1 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 110.00 A**3. RESPONSE: The difference map indicated the presence of diffuse electron density believed to be disordered solvent, thought to be ethanol. SQUEEZE was used leaving a voids from which electron density was removed. ; _vrf_RINTA01_3 ; PROBLEM: The value of Rint is greater than 0.15. RESPONSE: The data are very weak, so the R(int) is high at high angle. ; _vrf_PLAT220_5801 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.80 Ratio RESPONSE: The network includes coordinated DMF solvent, which exhibits a high degree of thermal motion in the terminal methyl groups. In addition there are a some uncoordinated carboxylate groups which vibrate more than those held in place with covalent bonds. ; #============================================================================== # end Validation Reply Form #============================================================================== _chemical_name_common .