#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308546.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308546 loop_ _publ_author_name 'Maura Pellei' 'Franco Benetollo' 'Giancarlo Gioia Lobbia' 'Simone Alidori' 'Carlo Santini' _publ_contact_author ' Carlo Santini' _publ_section_title ; The First Nitro-Substituted Heteroscorpionate Ligand ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 846 _journal_page_last 848 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '[H~2~B(3-NO~2~Tz)~2~]K]' _chemical_formula_sum 'C4 H4 B K N8 O4' _chemical_formula_weight 278.06 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.77(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.931(2) _cell_length_b 10.952(3) _cell_length_c 10.448(2) _cell_measurement_temperature 293(2) _cell_volume 1088.0(4) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al. 1999)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.920 _diffrn_measured_fraction_theta_max 0.920 _diffrn_measurement_device_type 'Philips PW1100' _diffrn_measurement_method \Q/2\Q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2524 _diffrn_reflns_theta_full 28.01 _diffrn_reflns_theta_max 28.01 _diffrn_reflns_theta_min 3.72 _exptl_absorpt_coefficient_mu 0.512 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.244 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.053 _refine_ls_extinction_coef 0.026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 2415 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.220 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0449 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.7171P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1189 _refine_ls_wR_factor_ref 0.1196 _reflns_number_gt 2379 _reflns_number_total 2415 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048562xsi20041018_025714.cif _[local]_cod_data_source_block camK _cod_database_code 4308546 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' 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 K K 0.44425(5) 0.12861(5) 0.19596(5) 0.04473(19) Uani 1 1 d . . . O1 O 0.2714(2) -0.18776(19) -0.14260(19) 0.0610(5) Uani 1 1 d . . . O2 O 0.3564(3) -0.0177(2) -0.0537(2) 0.0809(7) Uani 1 1 d . . . O3 O 0.5359(3) 0.2400(2) 0.4875(2) 0.0754(6) Uani 1 1 d . . . O4 O 0.5864(2) 0.1541(2) 0.6828(2) 0.0692(6) Uani 1 1 d . . . N1 N 0.1004(2) -0.0620(2) 0.17383(18) 0.0445(4) Uani 1 1 d . . . N2 N 0.1912(2) -0.02018(18) 0.10858(18) 0.0416(4) Uani 1 1 d . . . N3 N 0.1091(3) -0.2064(2) 0.0280(2) 0.0541(5) Uani 1 1 d . . . N4 N 0.2782(2) -0.1047(2) -0.06358(19) 0.0469(5) Uani 1 1 d . . . N5 N 0.1937(2) 0.02976(18) 0.40662(17) 0.0424(4) Uani 1 1 d . . . N6 N 0.2962(2) 0.11128(18) 0.40596(18) 0.0433(4) Uani 1 1 d . . . N7 N 0.3486(2) 0.0152(2) 0.60583(19) 0.0518(5) Uani 1 1 d . . . N8 N 0.5104(2) 0.1696(2) 0.5686(2) 0.0503(5) Uani 1 1 d . . . B B 0.0603(3) 0.0130(3) 0.2851(3) 0.0527(7) Uani 1 1 d . . . C1 C 0.0539(3) -0.1708(3) 0.1238(3) 0.0585(7) Uani 1 1 d . . . C2 C 0.1903(2) -0.1110(2) 0.0253(2) 0.0399(5) Uani 1 1 d . . . C3 C 0.2276(3) -0.0254(3) 0.5261(2) 0.0511(6) Uani 1 1 d . . . C4 C 0.3831(2) 0.0980(2) 0.5265(2) 0.0399(5) Uani 1 1 d . . . H3 H -0.018(3) -0.045(3) 0.314(3) 0.059(8) Uiso 1 1 d . . . H1 H -0.014(4) -0.214(3) 0.153(3) 0.078(10) Uiso 1 1 d . . . H2 H 0.026(3) 0.105(3) 0.244(3) 0.064(9) Uiso 1 1 d . . . H4 H 0.173(3) -0.085(3) 0.547(3) 0.072(10) Uiso 1 1 d . . . 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 K 0.0530(3) 0.0488(3) 0.0337(3) 0.00690(19) 0.0146(2) 0.0018(2) O1 0.0650(12) 0.0677(12) 0.0560(11) -0.0213(9) 0.0266(9) -0.0014(9) O2 0.0909(16) 0.0980(17) 0.0704(13) -0.0343(12) 0.0498(12) -0.0428(14) O3 0.0856(15) 0.0642(13) 0.0745(14) 0.0052(11) 0.0199(12) -0.0174(11) O4 0.0609(12) 0.0842(15) 0.0507(11) -0.0118(10) -0.0026(9) 0.0095(10) N1 0.0457(10) 0.0568(12) 0.0317(9) -0.0038(8) 0.0122(7) -0.0029(9) N2 0.0449(10) 0.0473(10) 0.0337(9) -0.0041(7) 0.0130(7) -0.0004(8) N3 0.0737(14) 0.0523(12) 0.0395(10) -0.0081(9) 0.0215(10) -0.0144(10) N4 0.0441(10) 0.0598(12) 0.0371(9) -0.0079(8) 0.0122(8) -0.0024(9) N5 0.0477(10) 0.0525(11) 0.0298(8) -0.0014(8) 0.0157(7) 0.0066(8) N6 0.0545(11) 0.0462(10) 0.0301(8) 0.0016(7) 0.0135(8) 0.0051(8) N7 0.0595(12) 0.0624(13) 0.0335(9) 0.0095(9) 0.0135(9) 0.0067(10) N8 0.0573(12) 0.0467(11) 0.0450(11) -0.0097(9) 0.0117(9) 0.0075(9) B 0.0440(14) 0.076(2) 0.0394(13) -0.0106(13) 0.0140(11) 0.0047(13) C1 0.0730(17) 0.0665(17) 0.0410(12) -0.0088(11) 0.0247(12) -0.0247(14) C2 0.0420(11) 0.0476(12) 0.0287(9) -0.0031(8) 0.0082(8) 0.0001(9) C3 0.0574(14) 0.0608(15) 0.0393(12) 0.0066(11) 0.0205(10) 0.0041(12) C4 0.0480(12) 0.0433(11) 0.0289(9) -0.0006(8) 0.0119(8) 0.0119(9) 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 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' 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 O1 K N3 56.73(6) 2 2 ? O1 K N2 78.65(6) 2 . ? N3 K N2 99.00(7) 2 . ? O1 K N7 147.95(6) 2 3_656 ? N3 K N7 147.14(7) 2 3_656 ? N2 K N7 106.74(7) . 3_656 ? O1 K O2 101.17(7) 2 . ? N3 K O2 71.74(7) 2 . ? N2 K O2 54.17(5) . . ? N7 K O2 107.45(8) 3_656 . ? O1 K N6 71.86(5) 2 . ? N3 K N6 128.59(6) 2 . ? N2 K N6 68.32(5) . . ? N7 K N6 80.79(6) 3_656 . ? O2 K N6 122.03(6) . . ? O1 K O2 137.45(7) 2 3_655 ? N3 K O2 81.21(7) 2 3_655 ? N2 K O2 104.32(6) . 3_655 ? N7 K O2 72.99(7) 3_656 3_655 ? O2 K O2 54.87(8) . 3_655 ? N6 K O2 149.47(7) . 3_655 ? O1 K O1 119.05(4) 2 3_655 ? N3 K O1 71.73(7) 2 3_655 ? N2 K O1 143.99(5) . 3_655 ? N7 K O1 75.44(6) 3_656 3_655 ? O2 K O1 90.38(6) . 3_655 ? N6 K O1 144.53(6) . 3_655 ? O2 K O1 40.77(5) 3_655 3_655 ? O1 K O3 84.72(7) 2 . ? N3 K O3 118.33(7) 2 . ? N2 K O3 120.03(6) . . ? N7 K O3 64.99(7) 3_656 . ? O2 K O3 169.87(7) . . ? N6 K O3 51.76(6) . . ? O2 K O3 125.19(7) 3_655 . ? O1 K O3 93.94(6) 3_655 . ? O1 K O4 124.70(5) 2 3_656 ? N3 K O4 149.34(6) 2 3_656 ? N2 K O4 56.22(5) . 3_656 ? N7 K O4 50.53(6) 3_656 3_656 ? O2 K O4 78.47(6) . 3_656 ? N6 K O4 63.28(5) . 3_656 ? O2 K O4 87.66(7) 3_655 3_656 ? O1 K O4 116.25(6) 3_655 3_656 ? O3 K O4 91.41(6) . 3_656 ? O1 K N4 128.00(5) 2 3_655 ? N3 K N4 72.63(6) 2 3_655 ? N2 K N4 123.49(5) . 3_655 ? N7 K N4 76.20(6) 3_656 3_655 ? O2 K N4 70.81(6) . 3_655 ? N6 K N4 156.41(5) . 3_655 ? O2 K N4 20.53(5) 3_655 3_655 ? O1 K N4 20.68(5) 3_655 3_655 ? O3 K N4 112.10(6) . 3_655 ? O4 K N4 104.47(6) 3_656 3_655 ? N4 O1 K 123.15(15) . 2_545 ? N4 O1 K 95.22(14) . 3_655 ? K O1 K 141.09(7) 2_545 3_655 ? N4 O2 K 121.07(15) . . ? N4 O2 K 97.79(16) . 3_655 ? K O2 K 125.13(8) . 3_655 ? N8 O3 K 111.34(16) . . ? N8 O4 K 113.21(17) . 3_656 ? C1 N1 N2 108.11(19) . . ? C1 N1 B 128.9(2) . . ? N2 N1 B 123.0(2) . . ? C2 N2 N1 101.41(18) . . ? C2 N2 K 117.98(14) . . ? N1 N2 K 132.03(13) . . ? C2 N3 C1 99.8(2) . . ? C2 N3 K 116.63(14) . 2_545 ? C1 N3 K 140.80(18) . 2_545 ? O2 N4 O1 123.5(2) . . ? O2 N4 C2 118.1(2) . . ? O1 N4 C2 118.3(2) . . ? O2 N4 K 61.68(13) . 3_655 ? O1 N4 K 64.10(13) . 3_655 ? C2 N4 K 163.28(15) . 3_655 ? C3 N5 N6 108.3(2) . . ? C3 N5 B 129.2(2) . . ? N6 N5 B 122.5(2) . . ? C4 N6 N5 102.05(18) . . ? C4 N6 K 112.72(15) . . ? N5 N6 K 125.22(13) . . ? C3 N7 C4 100.68(19) . . ? C3 N7 K 126.14(18) . 3_656 ? C4 N7 K 123.40(16) . 3_656 ? O3 N8 O4 124.7(3) . . ? O3 N8 C4 117.9(2) . . ? O4 N8 C4 117.4(2) . . ? N5 B N1 109.11(19) . . ? N1 C1 N3 112.7(2) . . ? N1 C1 C2 72.72(16) . . ? N3 C1 C2 40.00(13) . . ? N2 C2 N3 118.0(2) . . ? N2 C2 N4 119.8(2) . . ? N3 C2 N4 122.2(2) . . ? N2 C2 C1 77.76(15) . . ? N3 C2 C1 40.21(13) . . ? N4 C2 C1 162.42(19) . . ? N7 C3 N5 111.9(2) . . ? N6 C4 N7 117.0(2) . . ? N6 C4 N8 120.5(2) . . ? N7 C4 N8 122.5(2) . . ? 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 K O1 2.873(2) 2 ? K N3 2.882(2) 2 ? K N2 2.912(2) . ? K N7 2.923(2) 3_656 ? K O2 2.970(2) . ? K N6 2.979(2) . ? K O2 3.049(2) 3_655 ? K O1 3.100(2) 3_655 ? K O3 3.162(3) . ? K O4 3.392(3) 3_656 ? K N4 3.432(2) 3_655 ? O1 N4 1.217(3) . ? O1 K 2.873(2) 2_545 ? O1 K 3.100(2) 3_655 ? O2 N4 1.215(3) . ? O2 K 3.049(2) 3_655 ? O3 N8 1.224(3) . ? O4 N8 1.226(3) . ? O4 K 3.392(3) 3_656 ? N1 C1 1.330(4) . ? N1 N2 1.357(3) . ? N1 B 1.566(3) . ? N2 C2 1.319(3) . ? N3 C2 1.325(3) . ? N3 C1 1.331(3) . ? N3 K 2.882(2) 2_545 ? N4 C2 1.449(3) . ? N4 K 3.432(2) 3_655 ? N5 C3 1.339(3) . ? N5 N6 1.356(3) . ? N5 B 1.559(3) . ? N6 C4 1.313(3) . ? N7 C3 1.325(4) . ? N7 C4 1.339(3) . ? N7 K 2.923(2) 3_656 ? N8 C4 1.445(3) . ? C1 C2 2.031(3) . ? _journal_paper_doi 10.1021/ic048562x