Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Barlow, Stephen' 'Brunker, Tim J.' 'O'Hare, Dermot' _publ_contact_author_name 'Prof Dermot O'Hare' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email 'DERMOT.OHARE@CHEM.OX.AC.UK' _publ_section_title ; (eta5-Cyclopentadienyl)(kappa3-hydrotris(pyrazolyl)borate)cobalt(II) - The First High-Spin Cobalt Organometallic Complex ; data_tjb396 _database_code_CSD 168886 _audit_creation_date 2001-03-02T15:35:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H15 B1 Co1 N6' _chemical_formula_structural 'C15 H15 N6 B1 CO1' _chemical_formula_sum 'C14 H15 B1 Co1 N6' _chemical_formula_weight 337.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c m n' _symmetry_space_group_name_Hall '-P 2n 2ac' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x, -y-1/2, z' _cell_length_a 8.1066(3) _cell_length_b 10.3543(3) _cell_length_c 17.9336(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1505.31(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'yellow/green' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.144 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_number 3120 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0372 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 5.16 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 1791 _reflns_number_gt 1516 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.9335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0083(16) _refine_ls_number_reflns 1791 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.349 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.64158(4) 0.25 0.011969(17) 0.01885(14) Uani 1 2 d S . . C1 C 0.8262(2) 0.00991(16) 0.08737(10) 0.0217(4) Uani 1 1 d . . . H1 H 0.8731 -0.0254 0.0433 0.026 Uiso 1 1 calc R . . C2 C 0.8536(2) -0.03733(18) 0.15889(10) 0.0271(4) Uani 1 1 d . . . H2 H 0.9206 -0.1086 0.173 0.033 Uiso 1 1 calc R . . C3 C 0.7628(2) 0.04157(16) 0.20463(9) 0.0238(4) Uani 1 1 d . . . H3 H 0.7557 0.0348 0.2574 0.029 Uiso 1 1 calc R . . C4 C 0.2593(3) 0.25 0.04686(15) 0.0252(5) Uani 1 2 d S . . H4 H 0.2216 0.25 -0.0033 0.03 Uiso 1 2 calc SR . . C5 C 0.1568(3) 0.25 0.10903(16) 0.0301(6) Uani 1 2 d S . . H5 H 0.0396 0.25 0.11 0.036 Uiso 1 2 calc SR . . C6 C 0.2627(3) 0.25 0.16879(15) 0.0248(5) Uani 1 2 d S . . H6 H 0.231 0.25 0.2198 0.03 Uiso 1 2 calc SR . . C11 C 0.5717(3) 0.3186(2) -0.10612(10) 0.0417(6) Uani 1 1 d . . . H11 H 0.4793 0.3729 -0.1148 0.05 Uiso 1 1 calc R . . C12 C 0.7327(3) 0.35897(19) -0.09094(10) 0.0338(5) Uani 1 1 d . . . H12 H 0.7692 0.446 -0.0877 0.041 Uiso 1 1 calc R . . C13 C 0.8301(3) 0.25 -0.08146(14) 0.0305(6) Uani 1 2 d S . . H13 H 0.9447 0.25 -0.0703 0.037 Uiso 1 2 calc SR . . B1 B 0.5847(3) 0.25 0.18545(15) 0.0184(5) Uani 1 2 d S . . N1 N 0.72499(17) 0.11151(13) 0.08898(7) 0.0185(3) Uani 1 1 d . . . N2 N 0.68538(17) 0.13034(13) 0.16228(7) 0.0184(3) Uani 1 1 d . . . N3 N 0.4173(2) 0.25 0.06705(11) 0.0214(4) Uani 1 2 d S . . N4 N 0.4187(2) 0.25 0.14330(11) 0.0200(4) Uani 1 2 d S . . H0 H 0.564(3) 0.25 0.2450(14) 0.017(6) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0197(2) 0.02324(19) 0.0136(2) 0 -0.00001(13) 0 C1 0.0209(8) 0.0200(8) 0.0243(9) -0.0024(7) 0.0035(7) 0.0016(7) C2 0.0260(9) 0.0242(9) 0.0312(10) 0.0056(7) -0.0010(7) 0.0064(8) C3 0.0258(9) 0.0259(9) 0.0199(9) 0.0057(7) -0.0020(7) 0.0012(8) C4 0.0225(12) 0.0202(11) 0.0330(15) 0 -0.0058(11) 0 C5 0.0177(13) 0.0240(13) 0.0487(17) 0 0.0024(12) 0 C6 0.0204(12) 0.0214(11) 0.0326(14) 0 0.0077(11) 0 C11 0.0373(11) 0.0702(15) 0.0175(9) 0.0079(9) 0.0009(8) 0.0252(11) C12 0.0521(13) 0.0312(10) 0.0180(9) 0.0032(7) 0.0057(9) -0.0046(10) C13 0.0256(13) 0.0487(17) 0.0173(13) 0 0.0036(10) 0 B1 0.0210(13) 0.0188(12) 0.0152(13) 0 0.0033(11) 0 N1 0.0208(7) 0.0186(6) 0.0162(7) -0.0013(5) 0.0013(6) -0.0005(6) N2 0.0217(7) 0.0199(7) 0.0135(7) 0.0013(5) 0.0016(5) 0.0002(6) N3 0.0198(10) 0.0247(10) 0.0197(10) 0 -0.0018(8) 0 N4 0.0189(10) 0.0204(9) 0.0207(10) 0 0.0041(8) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N3 2.069(2) . ? Co N1 2.1026(13) . ? Co N1 2.1026(13) 8_565 ? Co C13 2.268(3) . ? Co C12 2.2859(18) 8_565 ? Co C12 2.2859(18) . ? Co C11 2.3045(18) 8_565 ? Co C11 2.3045(18) . ? C1 N1 1.334(2) . ? C1 C2 1.391(2) . ? C2 C3 1.372(2) . ? C3 N2 1.347(2) . ? C4 N3 1.331(3) . ? C4 C5 1.391(4) . ? C5 C6 1.373(4) . ? C6 N4 1.345(3) . ? C11 C12 1.397(3) . ? C11 C11 1.421(5) 8_565 ? C12 C13 1.388(3) . ? C13 C12 1.388(3) 8_565 ? B1 N2 1.541(2) 8_565 ? B1 N2 1.541(2) . ? B1 N4 1.543(3) . ? N1 N2 1.3672(18) . ? N3 N4 1.367(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co N1 88.22(5) . . ? N3 Co N1 88.22(5) . 8_565 ? N1 Co N1 86.00(7) . 8_565 ? N3 Co C13 160.89(9) . . ? N1 Co C13 105.58(6) . . ? N1 Co C13 105.58(6) 8_565 . ? N3 Co C12 132.03(7) . 8_565 ? N1 Co C12 95.15(6) . 8_565 ? N1 Co C12 139.73(7) 8_565 8_565 ? C13 Co C12 35.48(6) . 8_565 ? N3 Co C12 132.03(7) . . ? N1 Co C12 139.73(7) . . ? N1 Co C12 95.15(6) 8_565 . ? C13 Co C12 35.48(6) . . ? C12 Co C12 59.16(10) 8_565 . ? N3 Co C11 102.87(7) . 8_565 ? N1 Co C11 118.19(7) . 8_565 ? N1 Co C11 153.25(7) 8_565 8_565 ? C13 Co C11 59.12(8) . 8_565 ? C12 Co C11 35.44(8) 8_565 8_565 ? C12 Co C11 59.31(7) . 8_565 ? N3 Co C11 102.87(7) . . ? N1 Co C11 153.25(7) . . ? N1 Co C11 118.19(7) 8_565 . ? C13 Co C11 59.12(8) . . ? C12 Co C11 59.31(7) 8_565 . ? C12 Co C11 35.44(8) . . ? C11 Co C11 35.92(12) 8_565 . ? N1 C1 C2 110.84(15) . . ? C3 C2 C1 104.84(15) . . ? N2 C3 C2 108.61(14) . . ? N3 C4 C5 110.9(2) . . ? C6 C5 C4 104.6(2) . . ? N4 C6 C5 108.8(2) . . ? C12 C11 C11 107.40(12) . 8_565 ? C12 C11 Co 71.55(10) . . ? C11 C11 Co 72.04(6) 8_565 . ? C13 C12 C11 108.20(19) . . ? C13 C12 Co 71.56(13) . . ? C11 C12 Co 73.01(11) . . ? C12 C13 C12 108.8(3) 8_565 . ? C12 C13 Co 72.96(13) 8_565 . ? C12 C13 Co 72.96(13) . . ? N2 B1 N2 107.04(19) 8_565 . ? N2 B1 N4 109.26(13) 8_565 . ? N2 B1 N4 109.26(13) . . ? C1 N1 N2 106.11(13) . . ? C1 N1 Co 136.15(11) . . ? N2 N1 Co 117.31(10) . . ? C3 N2 N1 109.59(13) . . ? C3 N2 B1 130.04(15) . . ? N1 N2 B1 119.89(14) . . ? C4 N3 N4 106.3(2) . . ? C4 N3 Co 135.70(17) . . ? N4 N3 Co 118.02(14) . . ? C6 N4 N3 109.4(2) . . ? C6 N4 B1 130.8(2) . . ? N3 N4 B1 119.83(18) . . ?