#------------------------------------------------------------------------------ #$Date: 2016-03-22 11:52:46 +0200 (Tue, 22 Mar 2016) $ #$Revision: 178921 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/50/4115008.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_4115008 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_paper_doi 10.1021/ja0266464 _journal_volume 124 _journal_year 2002 _chemical_compound_source synthesis _chemical_formula_sum 'C28 H48 B Cl F4 Mo2 N12' _chemical_formula_weight 866.92 _chemical_name_systematic ; ? ; _space_group_IT_number 130 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4a 2ac' _symmetry_space_group_name_H-M 'P 4/n c c :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 4 _cell_length_a 14.4878(8) _cell_length_b 14.4878(8) _cell_length_c 16.3787(9) _cell_measurement_reflns_used 4621 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 27.25 _cell_measurement_theta_min 2.48 _cell_volume 3437.8(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics XP _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 213(2) _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19881 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_min 1.99 _diffrn_standards_decay_% 0. _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_T_max 0.355 _exptl_absorpt_correction_T_min 0.294 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.675 _exptl_crystal_description block _exptl_crystal_F_000 1768 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.225 _refine_diff_density_max 1.006 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.161 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 1983 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.173 _refine_ls_restrained_S_obs 1.112 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_obs 0.0382 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1353 _refine_ls_wR_factor_obs 0.0973 _reflns_number_observed 1185 _reflns_number_total 1988 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ja0266464_s2_1.cif _cod_data_source_block compound4 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 3437.84(53) _cod_original_sg_symbol_H-M 'P 4/n c c' _cod_database_code 4115008 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+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' 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 0.0330(3) 0.0330(3) 0.0194(3) 0.000 0.000 0.000 Mo2 0.0330(3) 0.0330(3) 0.0198(3) 0.000 0.000 0.000 N1 0.040(2) 0.049(2) 0.024(2) -0.002(2) 0.001(2) 0.006(2) N2 0.040(2) 0.044(2) 0.024(2) 0.0005(15) -0.002(2) 0.002(2) N3 0.039(2) 0.059(3) 0.036(2) -0.004(2) -0.002(2) 0.013(2) C1 0.056(3) 0.071(4) 0.031(2) -0.008(2) -0.004(2) 0.020(3) C2 0.059(4) 0.099(5) 0.040(3) -0.006(3) 0.013(3) 0.020(3) C3 0.042(3) 0.092(5) 0.050(3) -0.015(3) 0.004(2) 0.015(3) C4 0.040(2) 0.038(2) 0.028(2) 0.001(2) 0.000(2) 0.002(2) C5 0.050(3) 0.076(4) 0.046(3) -0.003(3) -0.013(2) 0.016(3) C6 0.054(3) 0.070(4) 0.043(3) 0.011(3) -0.013(2) 0.013(3) C7 0.042(3) 0.056(3) 0.031(2) -0.002(2) -0.005(2) 0.002(2) B 0.054(4) 0.054(4) 0.039(6) 0.000 0.000 -0.005(8) F1 0.114(4) 0.164(6) 0.136(5) -0.022(4) -0.070(4) -0.014(3) Cl1 0.0478(8) 0.0478(8) 0.0319(11) 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 0.7500 -0.2500 0.57110(4) 0.0284(2) Uani 1 d S Mo2 Mo 0.7500 -0.2500 0.43848(4) 0.0286(2) Uani 1 d S N1 N 0.6193(3) -0.1888(3) 0.5747(2) 0.0376(9) Uani 1 d . N2 N 0.6108(3) -0.2078(3) 0.4350(2) 0.0361(9) Uani 1 d . N3 N 0.4814(3) -0.1528(3) 0.5065(2) 0.0449(10) Uani 1 d . C1 C 0.5773(4) -0.1465(4) 0.6473(3) 0.0528(14) Uani 1 d . H1A H 0.5806(4) -0.0792(4) 0.6429(3) 0.063 Uiso 1 calc R H1B H 0.6116(4) -0.1653(4) 0.6961(3) 0.063 Uiso 1 calc R C2 C 0.4790(4) -0.1758(5) 0.6551(3) 0.066(2) Uani 1 d . H2A H 0.4518(4) -0.1491(5) 0.7046(3) 0.079 Uiso 1 calc R H2B H 0.4751(4) -0.2432(5) 0.6590(3) 0.079 Uiso 1 calc R C3 C 0.4269(4) -0.1422(5) 0.5802(3) 0.061(2) Uani 1 d . H3A H 0.3694(4) -0.1773(5) 0.5746(3) 0.074 Uiso 1 calc R H3B H 0.4108(4) -0.0770(5) 0.5873(3) 0.074 Uiso 1 calc R C4 C 0.5691(3) -0.1838(3) 0.5054(2) 0.0352(9) Uani 1 d . C5 C 0.4295(4) -0.1274(4) 0.4333(3) 0.057(2) Uani 1 d . H5A H 0.4037(4) -0.0654(4) 0.4402(3) 0.068 Uiso 1 calc R H5B H 0.3781(4) -0.1706(4) 0.4258(3) 0.068 Uiso 1 calc R C6 C 0.4907(4) -0.1292(4) 0.3584(3) 0.0556(15) Uani 1 d . H6A H 0.4527(4) -0.1314(4) 0.3089(3) 0.067 Uiso 1 calc R H6B H 0.5288(4) -0.0734(4) 0.3564(3) 0.067 Uiso 1 calc R C7 C 0.5513(3) -0.2135(4) 0.3628(3) 0.0433(12) Uani 1 d . H7A H 0.5129(3) -0.2691(4) 0.3659(3) 0.052 Uiso 1 calc R H7B H 0.5894(3) -0.2176(4) 0.3135(3) 0.052 Uiso 1 calc R B B 0.2500 -0.2500 0.2500 0.049(3) Uani 1 d S F1 F 0.3256(4) -0.2504(4) 0.2961(4) 0.138(2) Uani 1 d . Cl1 Cl 0.7500 -0.2500 0.25635(12) 0.0425(5) 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 '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 N1 Mo1 N1 89.954(5) . 3_545 y N1 Mo1 N1 176.8(2) . 2_645 y N1 Mo1 Mo2 91.60(9) . . y N2 Mo2 N2 89.959(5) . 3_545 y N2 Mo2 N2 176.9(2) . 2_645 y N2 Mo2 Mo1 91.53(9) . . y C4 N1 C1 115.8(4) . . ? C4 N1 Mo1 119.1(3) . . ? C1 N1 Mo1 125.0(3) . . ? C4 N2 C7 116.2(4) . . ? C4 N2 Mo2 118.8(3) . . ? C7 N2 Mo2 124.6(3) . . ? C4 N3 C3 124.0(4) . . ? C4 N3 C5 123.9(4) . . ? C3 N3 C5 112.1(4) . . ? N1 C1 C2 110.3(4) . . ? C1 C2 C3 108.2(5) . . ? N3 C3 C2 111.6(4) . . ? N2 C4 N3 121.4(4) . . ? N2 C4 N1 117.6(4) . . ? N3 C4 N1 120.9(4) . . ? N3 C5 C6 111.1(4) . . ? C7 C6 C5 108.4(4) . . ? N2 C7 C6 109.7(4) . . ? F1 B F1 109.2(5) 8 2_545 ? F1 B F1 110.9(6) 8 7_545 ? F1 B F1 108.4(5) 2_545 7_545 ? Mo2 Cl1 Mo1 180.0 . 13 ? 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 2.1722(9) . y Mo1 N1 2.092(4) . y Mo2 N2 2.108(4) . y N1 C4 1.350(5) . ? N1 C1 1.469(5) . ? N2 C4 1.347(5) . ? N2 C7 1.466(5) . ? N3 C4 1.347(6) . ? N3 C3 1.450(6) . ? N3 C5 1.462(6) . ? C1 C2 1.493(8) . ? C2 C3 1.520(8) . ? C5 C6 1.514(7) . ? C6 C7 1.506(7) . ? B F1 1.330(4) 8 ? Cl1 Mo1 3.034(2) 13 y Mo2 Cl1 2.983(2) . y