Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Bis-ketopyrrolyl complexes of Co(II) stabilised by trimethylphosphine ligands ; _publ_contact_author_name 'Prof. Pedro Gomes' _publ_contact_author_email 'PEDRO.T.GOMES@IST.UTL.PT, SONIA.CARABINEIRO@IST.UTL.PT' loop_ _publ_author_name 'Sonia A. Carabineiro' 'Pedro T. Gomes' 'Luis F. Veiros' 'Cristina Freire' 'Laura J. Pereira' ; R.T.Henriques ; 'John E. Warren' 'Sofia I. Pascu' # Attachment 'B710162G_CCDC_642094_and_642095_revised_.cif' ###################################### ## denoted 2a in text ## ###################################### data_compound_2a_(ox037) _database_code_depnum_ccdc_archive 'CCDC 642094' _audit_creation_date 07-01-18 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.9836(10) _cell_length_b 11.3840(12) _cell_length_c 9.3690(10) _cell_angle_alpha 90 _cell_angle_beta 94.4080(10) _cell_angle_gamma 90 _cell_volume 955.33(18) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? 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' 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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 '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' _cell_formula_units_Z 2 # Given Formula = C16 H8 Co1 N2 O2 P2 # Dc = 1.32 Fooo = 418.00 Mu = 10.73 M = 190.57 # Found Formula = C16 H26 Co1 N2 O2 P2 # Dc = 1.39 FOOO = 418.00 Mu = 10.75 M = 199.64 _chemical_formula_sum 'C16 H26 Co1 N2 O2 P2' _chemical_formula_moiety 'C16 H26 Co1 N2 O2 P2' _chemical_compound_source ? _chemical_formula_weight 399.28 _cell_measurement_reflns_used 7238 _cell_measurement_theta_min 0 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.02 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 418 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_radiation_wavelength 0.68140 _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _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_ambient_temperature 120(2) _diffrn_reflns_number 7238 _reflns_number_total 1988 _diffrn_reflns_av_R_equivalents 0.059 # Number of reflections with Friedels Law is 1988 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2104 _diffrn_reflns_theta_min 3.249 _diffrn_reflns_theta_max 30.774 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.466 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.81 _refine_diff_density_max 0.82 _refine_ls_number_reflns 1612 _refine_ls_number_restraints 0 _refine_ls_number_parameters 106 #_refine_ls_R_factor_ref 0.0323 _refine_ls_wR_factor_ref 0.0389 _refine_ls_goodness_of_fit_ref 1.0896 #_reflns_number_all 1984 _refine_ls_R_factor_all 0.0392 _refine_ls_wR_factor_all 0.0411 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 1612 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_gt 0.0389 _refine_ls_shift/su_max 0.005264 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.427 0.224 0.254 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 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 _atom_site_attached_hydrogens Co1 Co 0.0000 0.0000 0.0000 0.0105 1.0000 Uani S . . . . . P1 P 0.14704(6) -0.12455(4) -0.11195(5) 0.0132 1.0000 Uani . . . . . . N1 N 0.1481(2) 0.01844(14) 0.15783(19) 0.0137 1.0000 Uani . . . . . . O1 O 0.14547(17) 0.15878(13) -0.08017(15) 0.0178 1.0000 Uani . . . . . . C1 C 0.1798(2) -0.03198(18) 0.2861(2) 0.0175 1.0000 Uani . . . . . . C2 C 0.3074(3) 0.01909(19) 0.3570(2) 0.0210 1.0000 Uani . . . . . . C3 C 0.3563(2) 0.1049(2) 0.2675(2) 0.0200 1.0000 Uani . . . . . . C4 C 0.2566(2) 0.10333(18) 0.1441(2) 0.0148 1.0000 Uani . . . . . . C5 C 0.2462(2) 0.17161(17) 0.0185(2) 0.0161 1.0000 Uani . . . . . . C100 C 0.2081(3) -0.0685(2) -0.2793(3) 0.0298 1.0000 Uani . . . . . . C101 C 0.3203(3) -0.1720(2) -0.0154(3) 0.0280 1.0000 Uani . . . . . . C102 C 0.0635(3) -0.26396(19) -0.1670(2) 0.0225 1.0000 Uani . . . . . . H11 H 0.1232 -0.0929 0.3214 0.0252 1.0000 Uiso . . . . . . H21 H 0.3498 -0.0023 0.4469 0.0302 1.0000 Uiso . . . . . . H31 H 0.4387 0.1546 0.2844 0.0275 1.0000 Uiso . . . . . . H51 H 0.3208 0.2294 0.0077 0.0227 1.0000 Uiso . . . . . . H1001 H 0.1224 -0.0476 -0.3430 0.0549 1.0000 Uiso . . . . . . H1002 H 0.2669 -0.1272 -0.3237 0.0540 1.0000 Uiso . . . . . . H1003 H 0.2688 -0.0001 -0.2596 0.0550 1.0000 Uiso . . . . . . H1011 H 0.2969 -0.2136 0.0705 0.0492 1.0000 Uiso . . . . . . H1012 H 0.3726 -0.2220 -0.0765 0.0491 1.0000 Uiso . . . . . . H1013 H 0.3821 -0.1057 0.0111 0.0500 1.0000 Uiso . . . . . . H1021 H 0.0406 -0.3068 -0.0838 0.0401 1.0000 Uiso . . . . . . H1022 H 0.1306 -0.3071 -0.2202 0.0407 1.0000 Uiso . . . . . . H1023 H -0.0267 -0.2493 -0.2246 0.0412 1.0000 Uiso . . . . . . 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 0.0151(2) 0.0078(2) 0.0083(2) 0.00006(12) -0.00018(14) -0.00094(13) P1 0.0173(3) 0.0104(2) 0.0118(3) -0.00060(18) 0.00116(19) -0.00041(18) N1 0.0188(8) 0.0094(7) 0.0129(8) -0.0003(6) 0.0019(7) 0.0008(6) O1 0.0236(8) 0.0160(7) 0.0136(7) 0.0005(6) -0.0003(6) -0.0002(6) C1 0.0262(11) 0.0136(9) 0.0128(9) 0.0023(7) 0.0016(8) 0.0011(8) C2 0.0276(12) 0.0210(10) 0.0135(9) -0.0009(8) -0.0053(8) 0.0046(9) C3 0.0167(10) 0.0225(10) 0.0201(11) -0.0039(8) -0.0029(8) 0.0005(8) C4 0.0162(9) 0.0140(9) 0.0140(9) -0.0032(7) 0.0007(7) -0.0002(8) C5 0.0170(10) 0.0146(9) 0.0168(10) -0.0022(8) 0.0022(8) -0.0038(7) C100 0.0465(15) 0.0202(11) 0.0251(12) 0.0030(9) 0.0189(10) 0.0018(10) C101 0.0198(11) 0.0349(13) 0.0284(12) -0.0083(10) -0.0038(9) 0.0082(10) C102 0.0246(11) 0.0143(9) 0.0286(11) -0.0069(9) 0.0022(9) -0.0004(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3050(8) 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 . O1 2_555 2.3854(15) yes Co1 . N1 2_555 1.9231(18) yes Co1 . P1 2_555 2.2513(5) yes Co1 . P1 . 2.2513(5) yes Co1 . N1 . 1.9231(18) yes Co1 . O1 . 2.3854(15) yes P1 . C100 . 1.816(2) yes P1 . C101 . 1.821(2) yes P1 . C102 . 1.813(2) yes N1 . C1 . 1.342(3) yes N1 . C4 . 1.385(3) yes O1 . C5 . 1.251(3) yes C1 . C2 . 1.406(3) yes C1 . H11 . 0.936 no C2 . C3 . 1.381(3) yes C2 . H21 . 0.930 no C3 . C4 . 1.408(3) yes C3 . H31 . 0.935 no C4 . C5 . 1.407(3) yes C5 . H51 . 0.950 no C100 . H1001 . 0.967 no C100 . H1002 . 0.966 no C100 . H1003 . 0.961 no C101 . H1011 . 0.971 no C101 . H1012 . 0.956 no C101 . H1013 . 0.958 no C102 . H1021 . 0.955 no C102 . H1022 . 0.949 no C102 . H1023 . 0.953 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 O1 2_555 Co1 . N1 2_555 78.23(6) yes O1 2_555 Co1 . P1 2_555 88.58(4) yes N1 2_555 Co1 . P1 2_555 91.77(5) yes O1 2_555 Co1 . P1 . 91.42(4) yes N1 2_555 Co1 . P1 . 88.23(5) yes P1 2_555 Co1 . P1 . 179.995 yes O1 2_555 Co1 . N1 . 101.77(6) yes N1 2_555 Co1 . N1 . 179.994 yes P1 2_555 Co1 . N1 . 88.23(5) yes P1 . Co1 . N1 . 91.77(5) yes O1 2_555 Co1 . O1 . 179.995 yes N1 2_555 Co1 . O1 . 101.77(6) yes P1 2_555 Co1 . O1 . 91.42(4) yes P1 . Co1 . O1 . 88.58(4) yes N1 . Co1 . O1 . 78.23(6) yes Co1 . P1 . C100 . 114.07(8) yes Co1 . P1 . C101 . 117.72(8) yes C100 . P1 . C101 . 103.27(13) yes Co1 . P1 . C102 . 116.04(8) yes C100 . P1 . C102 . 101.99(11) yes C101 . P1 . C102 . 101.59(11) yes Co1 . N1 . C1 . 136.74(15) yes Co1 . N1 . C4 . 117.04(14) yes C1 . N1 . C4 . 106.21(17) yes Co1 . O1 . C5 . 103.78(12) yes N1 . C1 . C2 . 110.81(19) yes N1 . C1 . H11 . 123.4 no C2 . C1 . H11 . 125.8 no C1 . C2 . C3 . 106.96(19) yes C1 . C2 . H21 . 125.6 no C3 . C2 . H21 . 127.5 no C2 . C3 . C4 . 106.11(19) yes C2 . C3 . H31 . 127.6 no C4 . C3 . H31 . 126.3 no C3 . C4 . N1 . 109.90(18) yes C3 . C4 . C5 . 132.6(2) yes N1 . C4 . C5 . 117.45(18) yes C4 . C5 . O1 . 123.44(19) yes C4 . C5 . H51 . 118.0 no O1 . C5 . H51 . 118.6 no P1 . C100 . H1001 . 110.0 no P1 . C100 . H1002 . 109.9 no H1001 . C100 . H1002 . 109.9 no P1 . C100 . H1003 . 108.9 no H1001 . C100 . H1003 . 109.4 no H1002 . C100 . H1003 . 108.8 no P1 . C101 . H1011 . 109.0 no P1 . C101 . H1012 . 108.7 no H1011 . C101 . H1012 . 110.6 no P1 . C101 . H1013 . 110.6 no H1011 . C101 . H1013 . 109.1 no H1012 . C101 . H1013 . 108.9 no P1 . C102 . H1021 . 109.0 no P1 . C102 . H1022 . 109.7 no H1021 . C102 . H1022 . 110.5 no P1 . C102 . H1023 . 108.8 no H1021 . C102 . H1023 . 108.9 no H1022 . C102 . H1023 . 109.8 no #===END ###################################### ## denoted 2b in text ## ###################################### data_compound_2b_(js0409) _database_code_depnum_ccdc_archive 'CCDC 642095' _audit_creation_date 06-11-24 _audit_creation_method CRYSTALS_ver_12.82 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.0704(5) _cell_length_b 10.0296(5) _cell_length_c 13.2877(8) _cell_angle_alpha 90 _cell_angle_beta 92.070(3) _cell_angle_gamma 90 _cell_volume 1074.84(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? 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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 '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' _cell_formula_units_Z 2 # Given Formula = C23 H39 Co1 N1 P2 # Dc = 1.39 Fooo = 450.00 Mu = 9.56 M = 225.22 # Found Formula = C18 H30 Co1 N2 O2 P2 # Dc = 1.22 FOOO = 450.00 Mu = 9.48 M = 197.67 _chemical_formula_sum 'C18 H30 Co1 N2 O2 P2' _chemical_formula_moiety 'C18 H30 Co1 N2 O2 P2' _chemical_compound_source ? _chemical_formula_weight 395.33 # Structure does not match formula _cell_measurement_reflns_used 5291 _cell_measurement_theta_min 1 _cell_measurement_theta_max 26 _cell_measurement_temperature 180 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 0.948 # Sheldrick geometric approximatio 0.75 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.83 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT. Nonius (1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement '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 180 _diffrn_reflns_number 5493 _reflns_number_total 2102 _diffrn_reflns_av_R_equivalents 0.070 # Number of reflections with Friedels Law is 2102 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2130 _diffrn_reflns_theta_min 2.525 _diffrn_reflns_theta_max 26.074 _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.292 _diffrn_measured_fraction_theta_full 0.964 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.26 _refine_diff_density_max 0.28 _refine_ls_number_reflns 1305 _refine_ls_number_restraints 0 _refine_ls_number_parameters 115 #_refine_ls_R_factor_ref 0.0350 _refine_ls_wR_factor_ref 0.0382 _refine_ls_goodness_of_fit_ref 1.1132 #_reflns_number_all 2092 _refine_ls_R_factor_all 0.0744 _refine_ls_wR_factor_all 0.0596 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 1305 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0382 _refine_ls_shift/su_max 0.001620 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.465 0.757E-01 0.268 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. (27), 435-435 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. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437 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 _atom_site_attached_hydrogens Co1 Co 0.0000 0.0000 0.0000 0.0257 1.0000 Uani S . . . . . N1 N -0.0426(3) -0.1568(2) -0.07970(19) 0.0270 1.0000 Uani . . . . . . P1 P -0.17926(10) -0.06673(9) 0.11588(6) 0.0298 1.0000 Uani . . . . . . O1 O 0.1913(3) -0.1497(2) 0.06901(17) 0.0339 1.0000 Uani . . . . . . C1 C -0.1473(4) -0.1917(3) -0.1560(2) 0.0309 1.0000 Uani . . . . . . C2 C -0.1229(4) -0.3235(4) -0.1847(3) 0.0362 1.0000 Uani . . . . . . C3 C 0.0030(4) -0.3728(3) -0.1222(3) 0.0355 1.0000 Uani . . . . . . C4 C 0.0530(4) -0.2681(3) -0.0577(2) 0.0270 1.0000 Uani . . . . . . C5 C 0.1760(4) -0.2570(3) 0.0213(2) 0.0300 1.0000 Uani . . . . . . C6 C 0.2916(4) -0.3710(4) 0.0450(3) 0.0434 1.0000 Uani . . . . . . C100 C -0.0901(5) -0.0807(5) 0.2426(3) 0.0542 1.0000 Uani . . . . . . C101 C -0.3548(5) 0.0423(4) 0.1345(3) 0.0539 1.0000 Uani . . . . . . C102 C -0.2776(6) -0.2276(4) 0.0968(4) 0.0639 1.0000 Uani . . . . . . H11 H -0.2267 -0.1340 -0.1863 0.0373 1.0000 Uiso . . . . . . H21 H -0.1812 -0.3680 -0.2363 0.0444 1.0000 Uiso . . . . . . H31 H 0.0476 -0.4592 -0.1231 0.0430 1.0000 Uiso . . . . . . H61 H 0.2364 -0.4545 0.0391 0.0655 1.0000 Uiso . . . . . . H62 H 0.3387 -0.3632 0.1124 0.0655 1.0000 Uiso . . . . . . H63 H 0.3785 -0.3704 -0.0008 0.0656 1.0000 Uiso . . . . . . H1001 H 0.0002 -0.1435 0.2416 0.0810 1.0000 Uiso . . . . . . H1002 H -0.1719 -0.1118 0.2883 0.0810 1.0000 Uiso . . . . . . H1003 H -0.0490 0.0052 0.2637 0.0809 1.0000 Uiso . . . . . . H1011 H -0.4165 0.0531 0.0720 0.0814 1.0000 Uiso . . . . . . H1012 H -0.4249 0.0065 0.1839 0.0807 1.0000 Uiso . . . . . . H1013 H -0.3124 0.1272 0.1572 0.0812 1.0000 Uiso . . . . . . H1021 H -0.3365 -0.2282 0.0329 0.0969 1.0000 Uiso . . . . . . H1022 H -0.3519 -0.2449 0.1504 0.0966 1.0000 Uiso . . . . . . H1023 H -0.1915 -0.2941 0.0975 0.0968 1.0000 Uiso . . . . . . 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 0.0273(3) 0.0256(3) 0.0240(3) -0.0001(3) -0.0016(2) -0.0030(3) N1 0.0275(14) 0.0264(13) 0.0269(14) 0.0003(11) -0.0026(11) -0.0029(11) P1 0.0296(4) 0.0309(4) 0.0289(4) 0.0014(4) 0.0013(3) -0.0042(4) O1 0.0337(12) 0.0375(13) 0.0301(12) -0.0014(10) -0.0049(10) -0.0026(10) C1 0.0259(16) 0.0377(18) 0.0288(17) -0.0027(13) -0.0016(13) -0.0016(13) C2 0.0295(17) 0.043(2) 0.0359(18) -0.0119(15) -0.0002(15) -0.0079(14) C3 0.0362(19) 0.0319(18) 0.0390(19) -0.0067(15) 0.0072(15) -0.0020(15) C4 0.0261(16) 0.0296(16) 0.0254(15) 0.0007(13) 0.0033(13) -0.0037(13) C5 0.0297(16) 0.0336(17) 0.0270(16) 0.0068(14) 0.0043(13) -0.0019(14) C6 0.0352(19) 0.043(2) 0.051(2) 0.0069(17) -0.0068(16) 0.0016(16) C100 0.048(2) 0.082(3) 0.0327(19) 0.017(2) 0.0008(17) -0.009(2) C101 0.046(2) 0.059(3) 0.058(2) 0.017(2) 0.0205(19) 0.0139(18) C102 0.068(3) 0.052(3) 0.073(3) -0.012(2) 0.032(3) -0.027(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3232(8) 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 . O1 2_555 2.319(2) yes Co1 . N1 2_555 1.920(2) yes Co1 . P1 2_555 2.2523(8) yes Co1 . N1 . 1.920(2) yes Co1 . P1 . 2.2523(8) yes Co1 . O1 . 2.319(2) yes N1 . C1 . 1.343(4) yes N1 . C4 . 1.382(4) yes P1 . C100 . 1.812(4) yes P1 . C101 . 1.814(4) yes P1 . C102 . 1.812(4) yes O1 . C5 . 1.253(4) yes C1 . C2 . 1.392(5) yes C1 . H11 . 0.943 no C2 . C3 . 1.381(5) yes C2 . H21 . 0.932 no C3 . C4 . 1.405(4) yes C3 . H31 . 0.939 no C4 . C5 . 1.422(4) yes C5 . C6 . 1.501(5) yes C6 . H61 . 0.950 no C6 . H62 . 0.964 no C6 . H63 . 0.945 no C100 . H1001 . 0.964 no C100 . H1002 . 0.965 no C100 . H1003 . 0.961 no C101 . H1011 . 0.959 no C101 . H1012 . 0.952 no C101 . H1013 . 0.962 no C102 . H1021 . 0.958 no C102 . H1022 . 0.964 no C102 . H1023 . 0.963 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 O1 2_555 Co1 . N1 2_555 77.95(9) yes O1 2_555 Co1 . P1 2_555 88.41(6) yes N1 2_555 Co1 . P1 2_555 91.55(8) yes O1 2_555 Co1 . N1 . 102.05(9) yes N1 2_555 Co1 . N1 . 179.994 yes P1 2_555 Co1 . N1 . 88.45(8) yes O1 2_555 Co1 . P1 . 91.59(6) yes N1 2_555 Co1 . P1 . 88.45(8) yes P1 2_555 Co1 . P1 . 179.995 yes N1 . Co1 . P1 . 91.55(8) yes O1 2_555 Co1 . O1 . 179.995 yes N1 2_555 Co1 . O1 . 102.05(9) yes P1 2_555 Co1 . O1 . 91.59(6) yes N1 . Co1 . O1 . 77.95(9) yes P1 . Co1 . O1 . 88.41(6) yes Co1 . N1 . C1 . 136.5(2) yes Co1 . N1 . C4 . 117.2(2) yes C1 . N1 . C4 . 106.2(3) yes Co1 . P1 . C100 . 114.50(13) yes Co1 . P1 . C101 . 116.01(13) yes C100 . P1 . C101 . 101.9(2) yes Co1 . P1 . C102 . 117.25(15) yes C100 . P1 . C102 . 102.6(2) yes C101 . P1 . C102 . 102.5(2) yes Co1 . O1 . C5 . 107.7(2) yes N1 . C1 . C2 . 111.3(3) yes N1 . C1 . H11 . 124.1 no C2 . C1 . H11 . 124.5 no C1 . C2 . C3 . 106.4(3) yes C1 . C2 . H21 . 125.8 no C3 . C2 . H21 . 127.8 no C2 . C3 . C4 . 106.8(3) yes C2 . C3 . H31 . 126.6 no C4 . C3 . H31 . 126.6 no C3 . C4 . N1 . 109.2(3) yes C3 . C4 . C5 . 133.3(3) yes N1 . C4 . C5 . 117.5(3) yes C4 . C5 . O1 . 119.6(3) yes C4 . C5 . C6 . 120.5(3) yes O1 . C5 . C6 . 119.9(3) yes C5 . C6 . H61 . 111.6 no C5 . C6 . H62 . 110.8 no H61 . C6 . H62 . 108.4 no C5 . C6 . H63 . 109.3 no H61 . C6 . H63 . 108.0 no H62 . C6 . H63 . 108.7 no P1 . C100 . H1001 . 108.3 no P1 . C100 . H1002 . 110.6 no H1001 . C100 . H1002 . 109.4 no P1 . C100 . H1003 . 108.9 no H1001 . C100 . H1003 . 109.7 no H1002 . C100 . H1003 . 110.0 no P1 . C101 . H1011 . 109.5 no P1 . C101 . H1012 . 110.7 no H1011 . C101 . H1012 . 109.7 no P1 . C101 . H1013 . 107.8 no H1011 . C101 . H1013 . 109.8 no H1012 . C101 . H1013 . 109.3 no P1 . C102 . H1021 . 109.3 no P1 . C102 . H1022 . 109.8 no H1021 . C102 . H1022 . 110.6 no P1 . C102 . H1023 . 107.7 no H1021 . C102 . H1023 . 109.8 no H1022 . C102 . H1023 . 109.6 no #===END