#------------------------------------------------------------------------------ #$Date: 2014-07-12 00:16:09 +0200 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/87/4308771.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_4308771 loop_ _publ_author_name 'Maria B. Ezhova' 'Brian O. Patrick' 'Kapila N. Sereviratne' 'Brian R. James' 'Francis J. Waller' 'Michael E. Ford' _publ_section_title ; Interactions of Rh(III)-Dihydrido-Bis(phosphine) Complexes with Semicarbazones ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1482 _journal_page_last 1491 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C10 H13 N3 O ' _chemical_formula_sum 'C10 H13 N3 O' _chemical_formula_weight 191.23 _space_group_IT_number 56 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 56 _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _audit_creation_date 2004-08-04 _audit_creation_method 'by teXsan v1.8' _cell_angle_alpha 90.000(2) _cell_angle_beta 90.000(2) _cell_angle_gamma 90.000(2) _cell_formula_units_Z 8 _cell_length_a 17.885(2) _cell_length_b 15.005(3) _cell_length_c 7.4444(8) _cell_measurement_reflns_used 9066 _cell_measurement_temperature 198.2 _cell_measurement_theta_max 30.03 _cell_measurement_theta_min 2.28 _cell_volume 1997.8(5) _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_publication_material 'teXsan (MSC, 1992-1997)' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _diffrn_ambient_temperature 198.2 _diffrn_detector_area_resol_mean 11.76 _diffrn_measured_fraction_theta_full 30.03 _diffrn_measured_fraction_theta_max 0.840 _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 _diffrn_radiation_detector CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.05027 _diffrn_reflns_av_sigmaI/netI 0.110 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 18044 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_full 0.840 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 2.28 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.7416 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour clear _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 816.00 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.31 _refine_diff_density_min -0.29 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 139 _refine_ls_number_reflns 2460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.034 _refine_ls_shift/su_max 0.0030 _refine_ls_shift/su_mean 0.0007 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)]' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all 0.0912 _refine_ls_wR_factor_ref 0.0912 _reflns_number_gt 1587 _reflns_number_total 2460 _reflns_threshold_expression I>3.00\s(I) _[local]_cod_data_source_file ic0489185si20040806_022831.cif _[local]_cod_data_source_block bj335/MBE-518 _[local]_cod_cif_authors_sg_H-M 'P c c n ' _[local]_cod_chemical_formula_sum_orig 'C10 H13 N3 O ' _cod_original_cell_volume 1998(1) _cod_database_code 4308771 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2-y, +z' '1/2+x, -y,1/2-z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2+y, -z' '1/2-x, +y,1/2+z' ' +x,1/2-y,1/2+z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom O(1) 0.26166(4) 0.14183(6) -0.1508(1) 0.0292(2) 1.000 . Uani d ? N(1) 0.07344(5) 0.14719(6) -0.0281(1) 0.0224(2) 1.000 . Uani d ? N(2) 0.14983(5) 0.14522(7) -0.0085(1) 0.0243(3) 1.000 . Uani d ? N(3) 0.15596(6) 0.15244(8) -0.3166(1) 0.0319(3) 1.000 . Uani d ? C(1) -0.04980(6) 0.13535(8) 0.0776(1) 0.0223(3) 1.000 . Uani d ? C(2) -0.08001(7) 0.18964(8) -0.0565(2) 0.0287(3) 1.000 . Uani d ? C(3) -0.15621(7) 0.19050(9) -0.0884(2) 0.0356(4) 1.000 . Uani d ? C(4) -0.20361(7) 0.13712(9) 0.0111(2) 0.0360(4) 1.000 . Uani d ? C(5) -0.17453(7) 0.08208(9) 0.1427(2) 0.0329(3) 1.000 . Uani d ? C(6) -0.09838(7) 0.08180(8) 0.1769(1) 0.0276(3) 1.000 . Uani d ? C(7) 0.03187(6) 0.13276(7) 0.1103(1) 0.0207(3) 1.000 . Uani d ? C(8) 0.06131(6) 0.11106(8) 0.2955(1) 0.0242(3) 1.000 . Uani d ? C(9) 0.08785(8) 0.01458(9) 0.3109(2) 0.0365(4) 1.000 . Uani d ? C(10) 0.19295(6) 0.14692(8) -0.1610(1) 0.0219(3) 1.000 . Uani d ? H(1) -0.0464 0.2279 -0.1278 0.033 1.000 . Uiso c ? H(2) -0.1774 0.2291 -0.1837 0.041 1.000 . Uiso c ? H(3) -0.2590 0.1382 -0.0100 0.041 1.000 . Uiso c ? H(4) -0.2079 0.0433 0.2123 0.037 1.000 . Uiso c ? H(5) -0.0783 0.0430 0.2723 0.032 1.000 . Uiso c ? H(6) 0.1030 0.1511 0.3229 0.027 1.000 . Uiso c ? H(7) 0.0210 0.1212 0.3837 0.027 1.000 . Uiso c ? H(8) 0.0462 -0.0264 0.2835 0.043 1.000 . Uiso c ? H(9) 0.1284 0.0036 0.2244 0.043 1.000 . Uiso c ? H(10) 0.1060 0.0023 0.4325 0.043 1.000 . Uiso c ? H(11) 0.1734(8) 0.1401(9) 0.094(2) 0.033(4) 1.000 . Uiso d ? H(12) 0.1061(8) 0.155(1) -0.311(2) 0.036(4) 1.000 . Uiso d ? H(13) 0.1805(9) 0.154(1) -0.415(2) 0.045(4) 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.0184(5) 0.0484(6) 0.0209(4) 0.0002(4) 0.0010(3) 0.0015(3) N(1) 0.0182(5) 0.0288(5) 0.0203(4) -0.0001(4) -0.0005(3) 0.0011(4) N(2) 0.0180(5) 0.0388(6) 0.0160(4) -0.0005(4) -0.0004(3) 0.0010(4) N(3) 0.0210(5) 0.0578(8) 0.0170(5) -0.0002(5) 0.0005(3) 0.0027(4) C(1) 0.0213(6) 0.0245(6) 0.0209(5) 0.0017(4) 0.0011(4) -0.0029(4) C(2) 0.0274(6) 0.0282(7) 0.0305(6) 0.0024(5) -0.0006(4) 0.0027(5) C(3) 0.0310(7) 0.0380(8) 0.0378(6) 0.0089(6) -0.0078(5) 0.0013(5) C(4) 0.0206(7) 0.0420(8) 0.0453(7) 0.0045(6) -0.0034(5) -0.0115(6) C(5) 0.0245(7) 0.0360(8) 0.0382(6) -0.0039(5) 0.0065(5) -0.0065(5) C(6) 0.0254(6) 0.0313(7) 0.0259(5) 0.0006(5) 0.0034(4) 0.0018(5) C(7) 0.0216(6) 0.0224(6) 0.0181(5) 0.0009(4) -0.0001(4) -0.0005(4) C(8) 0.0210(6) 0.0340(7) 0.0176(5) 0.0005(5) 0.0003(4) 0.0000(4) C(9) 0.0437(8) 0.0380(8) 0.0279(6) 0.0061(6) -0.0008(5) 0.0067(5) C(10) 0.0216(6) 0.0257(6) 0.0186(5) -0.0013(5) 0.0011(4) 0.0006(4) loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 104 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(2) N(1) C(7) 119.03(9) . . . yes N(1) N(2) C(10) 118.08(9) . . . yes N(1) N(2) H(11) 125.0(9) . . . no C(10) N(2) H(11) 116.8(9) . . . no C(10) N(3) H(12) 117.1(9) . . . no C(10) N(3) H(13) 119(1) . . . no H(12) N(3) H(13) 124(1) . . . no C(2) C(1) C(6) 118.3(1) . . . yes C(2) C(1) C(7) 120.9(1) . . . yes C(6) C(1) C(7) 120.8(1) . . . yes C(1) C(2) C(3) 120.6(1) . . . yes C(1) C(2) H(1) 119.3 . . . no C(3) C(2) H(1) 120.2 . . . no C(2) C(3) C(4) 120.5(1) . . . yes C(2) C(3) H(2) 120.3 . . . no C(4) C(3) H(2) 119.2 . . . no C(3) C(4) C(5) 119.7(1) . . . yes C(3) C(4) H(3) 120.9 . . . no C(5) C(4) H(3) 119.5 . . . no C(4) C(5) C(6) 120.1(1) . . . yes C(4) C(5) H(4) 120.0 . . . no C(6) C(5) H(4) 119.9 . . . no C(1) C(6) C(5) 120.9(1) . . . yes C(1) C(6) H(5) 119.6 . . . no C(5) C(6) H(5) 119.5 . . . no N(1) C(7) C(1) 115.64(9) . . . yes N(1) C(7) C(8) 124.4(1) . . . yes C(1) C(7) C(8) 119.96(9) . . . yes C(7) C(8) C(9) 112.38(9) . . . yes C(7) C(8) H(6) 108.9 . . . no C(7) C(8) H(7) 108.6 . . . no C(9) C(8) H(6) 109.2 . . . no C(9) C(8) H(7) 108.9 . . . no H(6) C(8) H(7) 108.9 . . . no C(8) C(9) H(8) 109.9 . . . no C(8) C(9) H(9) 109.9 . . . no C(8) C(9) H(10) 110.5 . . . no H(8) C(9) H(9) 108.5 . . . no H(8) C(9) H(10) 108.9 . . . no H(9) C(9) H(10) 109.2 . . . no O(1) C(10) N(2) 120.53(9) . . . yes O(1) C(10) N(3) 123.4(1) . . . yes N(2) C(10) N(3) 116.1(1) . . . yes loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_a _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A N(2) H(11) O(1) 0.88(1) 2.23(1) 2.264(1) 174(1) 7 N(3) H(12) N(1) 0.89(1) 2.19(1) 2.607(1) 108(1) . N(3) H(13) O(1) 0.85 2.05 2.896(1) 173.0 7_554 N(3) H(13) N(2) 0.85 3.12 2.299(1) 133.7 7_554 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(10) 1.234(1) . . yes N(1) N(2) 1.374(1) . . yes N(1) C(7) 1.289(1) . . yes N(2) C(10) 1.372(1) . . yes N(2) H(11) 0.88(1) . . no N(3) C(10) 1.337(1) . . yes N(3) H(12) 0.89(1) . . no N(3) H(13) 0.85(2) . . no C(1) C(2) 1.397(2) . . yes C(1) C(6) 1.395(2) . . yes C(1) C(7) 1.481(2) . . yes C(2) C(3) 1.383(2) . . yes C(2) H(1) 0.99 . . no C(3) C(4) 1.382(2) . . yes C(3) H(2) 0.99 . . no C(4) C(5) 1.383(2) . . yes C(4) H(3) 1.00 . . no C(5) C(6) 1.385(2) . . yes C(5) H(4) 0.98 . . no C(6) H(5) 0.99 . . no C(7) C(8) 1.511(1) . . yes C(8) C(9) 1.528(2) . . yes C(8) H(6) 0.98 . . no C(8) H(7) 0.99 . . no C(9) H(8) 0.99 . . no C(9) H(9) 0.98 . . no C(9) H(10) 0.98 . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(3) 2.896(1) . 7 no O(1) N(2) 3.098(1) . 7_554 no O(1) C(8) 3.225(1) . 7_554 no O(1) O(1) 3.273(2) . 2 no O(1) C(10) 3.273(1) . 2 no O(1) C(9) 3.312(2) . 7_554 no N(2) N(3) 3.357(2) . 8 no N(2) C(5) 3.581(2) . 5 no N(3) C(8) 3.404(1) . 1_554 no C(4) C(5) 3.599(2) . 7_454 no C(5) C(10) 3.455(2) . 5 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O(1) C(10) N(2) N(1) . . . . -177.2(1) no N(1) N(2) C(10) N(3) . . . . 1.5(2) no N(1) C(7) C(1) C(2) . . . . -30.1(2) no N(1) C(7) C(1) C(6) . . . . 148.2(1) no N(1) C(7) C(8) C(9) . . . . -76.7(1) no N(2) N(1) C(7) C(1) . . . . -179.5(1) no N(2) N(1) C(7) C(8) . . . . -1.7(2) no C(1) C(2) C(3) C(4) . . . . -0.5(2) no C(1) C(6) C(5) C(4) . . . . -1.3(2) no C(1) C(7) C(8) C(9) . . . . 101.0(1) no C(2) C(1) C(6) C(5) . . . . 0.4(2) no C(2) C(1) C(7) C(8) . . . . 151.9(1) no C(2) C(3) C(4) C(5) . . . . -0.4(2) no C(3) C(2) C(1) C(6) . . . . 0.5(2) no C(3) C(2) C(1) C(7) . . . . 178.9(1) no C(3) C(4) C(5) C(6) . . . . 1.3(2) no C(5) C(6) C(1) C(7) . . . . -178.0(1) no C(6) C(1) C(7) C(8) . . . . -29.8(2) no C(7) N(1) N(2) C(10) . . . . 170.1(1) no _journal_paper_doi 10.1021/ic0489185