#------------------------------------------------------------------------------ #$Date: 2014-07-12 00:06:05 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120077 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/50/4115009.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_4115009 loop_ _publ_author_name 'F. Albert Cotton' 'Lee M. Daniels' 'Carlos A. Murillo' 'Daren J. Timmons' 'Chad C. Wilkinson' _publ_contact_author_address ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry Texas A&M University, P.O. Box 30012 College Station, TX 77842-3012, USA ; _publ_contact_author_email cotton@tamu.edu _publ_contact_author_fax '(979) 845 9351' _publ_contact_author_name 'F. A. Cotton' _publ_contact_author_phone '(979) 845 4432' _publ_section_title ; The Extraordinary Ability of Guanidinate Derivatives to Stabilize Higher Oxidation Numbers in Dimetal Units by Modification of Redox Potentials: Structures of Mo25+ and Mo26+ Compounds ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 9249 _journal_page_last 9256 _journal_volume 124 _journal_year 2002 _chemical_formula_sum 'C28 H48 Cl Mo2 N12' _chemical_formula_weight 780.11 _chemical_name_systematic ; ? ; _space_group_IT_number 85 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4a' _symmetry_space_group_name_H-M 'P 4/n :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.561(11) _cell_length_b 13.561(11) _cell_length_c 8.5330(3) _cell_measurement_reflns_used 198 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 20.8 _cell_measurement_theta_min 9.2 _cell_volume 1569.2(18) _computing_cell_refinement MADNES _computing_data_collection MADNES _computing_data_reduction PROCOR _computing_molecular_graphics 'XP (SIEMENS, 1996)' _computing_publication_material 'CIFTAB (SHELDRICK, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 213(2) _diffrn_measurement_device 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _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 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3778 _diffrn_reflns_theta_max 22.48 _diffrn_reflns_theta_min 2.82 _diffrn_standards_number 'none (area detector data)' _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow-orange _exptl_crystal_density_diffrn 1.651 _exptl_crystal_description block _exptl_crystal_F_000 802 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.124 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.213 _refine_ls_goodness_of_fit_obs 1.221 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1012 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.261 _refine_ls_restrained_S_obs 1.221 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_obs 0.0531 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0054P)^2^+13.7495P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1128 _refine_ls_wR_factor_obs 0.1032 _reflns_number_observed 894 _reflns_number_total 1016 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ja0266464_s2_2.cif _[local]_cod_data_source_block compound2 _[local]_cod_cif_authors_sg_H-M 'P 4/n' _cod_original_cell_volume 1569.1(18) _cod_database_code 4115009 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 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 Mo1 0.0210(5) 0.0210(5) 0.0163(8) 0.000 0.000 0.000 Mo2 0.0216(5) 0.0216(5) 0.0188(8) 0.000 0.000 0.000 N11 0.027(3) 0.022(3) 0.012(3) -0.002(3) 0.003(3) -0.003(3) N12 0.030(4) 0.017(3) 0.026(4) 0.000(3) 0.008(3) 0.006(3) C17 0.017(4) 0.013(4) 0.040(5) 0.012(4) 0.003(4) 0.002(3) N13 0.035(4) 0.021(3) 0.025(4) -0.003(3) -0.004(3) 0.003(3) C16 0.055(5) 0.041(5) 0.017(5) -0.004(4) 0.006(4) 0.009(4) C11 0.036(4) 0.026(4) 0.015(4) 0.005(3) 0.001(3) -0.003(3) C12 0.045(5) 0.044(5) 0.016(4) 0.007(4) 0.000(4) 0.007(4) C13 0.050(5) 0.033(5) 0.024(5) 0.010(4) -0.001(4) 0.012(4) C15 0.039(5) 0.044(5) 0.029(5) -0.014(4) -0.005(4) 0.004(4) C14 0.062(6) 0.017(4) 0.030(5) -0.001(4) 0.005(4) -0.002(4) Cl1 0.0294(13) 0.0294(13) 0.065(3) 0.000 0.000 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags Mo1 Mo 0.2500 0.2500 0.00817(15) 0.0194(4) Uani 1 d S Mo2 Mo 0.2500 0.2500 -0.2412(2) 0.0207(4) Uani 1 d S N11 N 0.3041(4) 0.1033(4) 0.0200(7) 0.0203(14) Uani 1 d . N12 N 0.3028(4) 0.1015(4) -0.2505(7) 0.0243(15) Uani 1 d . C17 C 0.3177(5) 0.0542(5) -0.1147(10) 0.023(2) Uani 1 d . N13 N 0.3461(4) -0.0444(4) -0.1146(8) 0.0267(15) Uani 1 d . C16 C 0.3284(6) 0.0496(6) -0.3914(10) 0.038(2) Uani 1 d . H16A H 0.4002(6) 0.0500(6) -0.4043(10) 0.045 Uiso 1 calc R H16B H 0.2993(6) 0.0834(6) -0.4817(10) 0.045 Uiso 1 calc R C11 C 0.3157(6) 0.0498(5) 0.1660(9) 0.026(2) Uani 1 d . H11A H 0.2539(6) 0.0158(5) 0.1909(9) 0.031 Uiso 1 calc R H11B H 0.3293(6) 0.0968(5) 0.2507(9) 0.031 Uiso 1 calc R C12 C 0.3971(6) -0.0236(6) 0.1580(9) 0.035(2) Uani 1 d . H12A H 0.4013(6) -0.0595(6) 0.2574(9) 0.042 Uiso 1 calc R H12B H 0.4599(6) 0.0104(6) 0.1408(9) 0.042 Uiso 1 calc R C13 C 0.3783(6) -0.0946(6) 0.0267(9) 0.036(2) Uani 1 d . H13A H 0.4389(6) -0.1314(6) 0.0044(9) 0.043 Uiso 1 calc R H13B H 0.3277(6) -0.1420(6) 0.0590(9) 0.043 Uiso 1 calc R C15 C 0.2924(6) -0.0551(6) -0.3870(10) 0.037(2) Uani 1 d . H15A H 0.2208(6) -0.0566(6) -0.3717(10) 0.045 Uiso 1 calc R H15B H 0.3078(6) -0.0884(6) -0.4860(10) 0.045 Uiso 1 calc R C14 C 0.3424(7) -0.1053(5) -0.2556(9) 0.036(2) Uani 1 d . H14A H 0.3075(7) -0.1668(5) -0.2318(9) 0.044 Uiso 1 calc R H14B H 0.4098(7) -0.1223(5) -0.2872(9) 0.044 Uiso 1 calc R Cl1 Cl 0.2500 0.2500 -0.6034(6) 0.0413(11) Uani 1 d S 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 N11 Mo1 N11 89.87(2) . 4 y N11 Mo1 N11 89.87(2) . 3 ? N11 Mo1 N11 174.5(3) 4 3 ? N11 Mo1 N11 174.5(3) . 2 y N11 Mo1 N11 89.87(2) 4 2 ? N11 Mo1 N11 89.87(2) 3 2 ? N11 Mo1 Mo2 92.7(2) . . y N11 Mo1 Mo2 92.7(2) 4 . ? N11 Mo1 Mo2 92.7(2) 3 . ? N11 Mo1 Mo2 92.7(2) 2 . ? Mo1 Mo2 N12 92.1(2) . 4 ? Mo1 Mo2 N12 92.1(2) . . y N12 Mo2 N12 89.921(13) 4 . ? Mo1 Mo2 N12 92.1(2) . 3 ? N12 Mo2 N12 175.8(3) 4 3 ? N12 Mo2 N12 89.922(13) . 3 y Mo1 Mo2 N12 92.1(2) . 2 y N12 Mo2 N12 89.922(13) 4 2 ? N12 Mo2 N12 175.8(3) . 2 y N12 Mo2 N12 89.921(13) 3 2 y Mo1 Mo2 Cl1 180.0 . . ? N12 Mo2 Cl1 87.9(2) 4 . y N12 Mo2 Cl1 87.9(2) . . ? N12 Mo2 Cl1 87.9(2) 3 . ? N12 Mo2 Cl1 87.9(2) 2 . ? C17 N11 C11 118.2(6) . . ? C17 N11 Mo1 118.2(5) . . ? C11 N11 Mo1 123.2(5) . . ? C17 N12 C16 116.9(6) . . ? C17 N12 Mo2 118.0(5) . . ? C16 N12 Mo2 125.0(5) . . ? N12 C17 N11 118.9(6) . . y N12 C17 N13 120.1(7) . . ? N11 C17 N13 121.0(7) . . ? C17 N13 C13 122.3(6) . . ? C17 N13 C14 122.2(6) . . ? C13 N13 C14 115.4(6) . . ? N12 C16 C15 111.3(7) . . ? N11 C11 C12 112.1(6) . . ? C11 C12 C13 109.8(7) . . ? N13 C13 C12 111.7(6) . . ? C14 C15 C16 107.8(7) . . ? N13 C14 C15 112.4(6) . . ? Mo2 Cl1 Mo1 180.0 . 1_554 ? 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 Mo1 Mo2 2.128(2) . y Mo1 N11 2.122(6) . y Mo1 N11 2.122(6) 4 ? Mo1 N11 2.122(6) 3 ? Mo1 N11 2.123(6) 2 ? Mo2 N12 2.139(6) 4 ? Mo2 N12 2.139(6) . y Mo2 N12 2.139(6) 3 ? Mo2 N12 2.139(6) 2 ? Mo2 Cl1 3.091(6) . y N11 C17 1.341(10) . ? N11 C11 1.450(9) . ? N12 C17 1.340(10) . ? N12 C16 1.436(10) . ? C17 N13 1.392(8) . ? N13 C13 1.451(10) . ? N13 C14 1.460(10) . ? C16 C15 1.502(11) . ? C11 C12 1.487(11) . ? C12 C13 1.499(11) . ? C15 C14 1.477(12) . ? Cl1 Mo1 3.314(6) 1_554 y _journal_paper_doi 10.1021/ja0266464