#------------------------------------------------------------------------------ #$Date: 2008-02-29 15:02:27 +0200 (Fri, 29 Feb 2008) $ #$Revision: 181 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/5000407.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_5000407 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C66 H62 B2 F8 Mo2 N12' _chemical_formula_moiety 'C46 H42 Mo2 N8 2+, 2(B F4 -), 4(C5 H5 N)' _chemical_formula_weight 1388.79 _cell_length_a 27.753(6) _cell_length_b 12.462(2) _cell_length_c 18.715(4) _cell_angle_alpha 90 _cell_angle_beta 106.509(10) _cell_angle_gamma 90 _cell_volume 6206(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 140 _cell_measurement_theta_min 9.73 _cell_measurement_theta_max 14.88 _cell_measurement_temperature 98 _exptl_crystal_colour yellow _exptl_crystal_description prism _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.4799 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 98 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5325 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.1 _diffrn_standards_interval_count 300 _reflns_number_total 4080 _reflns_number_gt 3080 _reflns_threshold_expression F>3.0\s(F) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source MO Mo -1.825 0.688 'International Tables Vol. IV (1974) Table 2.2B' F F 0.014 0.01 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 4080 _refine_ls_number_parameters 401 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.3886E-8 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.05F)^2^ _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.0575 _refine_ls_goodness_of_fit_ref 1.3587 _refine_ls_shift/su_max 0.0076 _refine_diff_density_max 0.7 _refine_diff_density_min -0.64 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_disorder_group _atom_site_disorder_assembly MO1 MO 0.78882(3) 0.26545(4) 0.51250(3) 0.0451(4) Uani 1 0 . N2 N 0.7906(3) 0.2254(5) 0.4015(3) 0.049(3) Uani 1 0 . C3 C 0.7474(4) 0.1929(5) 0.3541(4) 0.050(4) Uani 1 0 . N4 N 0.7936(3) 0.3100(4) 0.6243(3) 0.045(3) Uani 1 0 . C5 C 0.8342(4) 0.2375(6) 0.3756(4) 0.053(3) Uani 1 0 . C6 C 0.8317(4) 0.2507(6) 0.3008(4) 0.058(4) Uani 1 0 . C7 C 0.8759(4) 0.2645(7) 0.2799(5) 0.065(4) Uani 1 0 . C8 C 0.9221(4) 0.2656(7) 0.3320(6) 0.075(4) Uani 1 0 . C9 C 0.9246(4) 0.2550(8) 0.4064(6) 0.084(5) Uani 1 0 . C10 C 0.8817(4) 0.2403(7) 0.4282(4) 0.070(4) Uani 1 0 . C11 C 0.8392(4) 0.3484(6) 0.6765(4) 0.049(3) Uani 1 0 . C12 C 0.8388(3) 0.4289(6) 0.7285(4) 0.051(3) Uani 1 0 . C13 C 0.8837(4) 0.4610(7) 0.7780(4) 0.062(4) Uani 1 0 . C14 C 0.9283(5) 0.4165(9) 0.7760(5) 0.089(5) Uani 1 0 . C15 C 0.9283(4) 0.3403(9) 0.7223(5) 0.087(5) Uani 1 0 . C16 C 0.8840(4) 0.3054(7) 0.6737(4) 0.065(4) Uani 1 0 . N17 N 0.8184(3) 0.1032(5) 0.5515(3) 0.053(3) Uani 1 0 . C18 C 0.8240(4) 0.0699(6) 0.6224(4) 0.065(4) Uani 1 0 . C19 C 0.8407(4) -0.0309(7) 0.6474(5) 0.084(5) Uani 1 0 . C20 C 0.8552(5) -0.1003(7) 0.6000(6) 0.110(6) Uani 1 0 . C21 C 0.8502(5) -0.0673(7) 0.5271(5) 0.099(5) Uani 1 0 . C22 C 0.8319(4) 0.0329(6) 0.5057(4) 0.075(4) Uani 1 0 . N23 N 0.7928(3) 0.4403(4) 0.4863(3) 0.049(3) Uani 1 0 . C24 C 0.7973(4) 0.4753(6) 0.4198(4) 0.061(4) Uani 1 0 . C25 C 0.8002(4) 0.5817(6) 0.4022(4) 0.071(5) Uani 1 0 . C26 C 0.7979(5) 0.6581(6) 0.4531(5) 0.090(5) Uani 1 0 . C27 C 0.7925(5) 0.6238(6) 0.5207(5) 0.089(5) Uani 1 0 . C28 C 0.7910(4) 0.5174(6) 0.5344(4) 0.070(4) Uani 1 0 . B29 B 0.7905(5) -0.0988(7) 0.3095(5) 0.058(5) Uani 1 0 . F30 F 0.7591(2) -0.1120(4) 0.3545(3) 0.081(3) Uani 1 0 . F31 F 0.8271(3) -0.0281(5) 0.3407(3) 0.105(3) Uani 1 0 . F32 F 0.7627(3) -0.0593(7) 0.2431(3) 0.141(4) Uani 1 0 . F33 F 0.8097(3) -0.1935(5) 0.2969(4) 0.127(4) Uani 1 0 . N34 N 0.9357(4) 0.6837(10) 0.6044(6) 0.107(5) Uani 1 0 . C35 C 0.9326(5) 0.5036(10) 0.5609(7) 0.100(6) Uani 1 0 . C36 C 0.9319(5) 0.5772(12) 0.6128(7) 0.108(7) Uani 1 0 . C37 C 0.9396(5) 0.7120(10) 0.5378(8) 0.112(7) Uani 1 0 . C38 C 0.9351(8) 0.5357(16) 0.4947(9) 0.156(10) Uani 1 0 . C39 C 0.9399(8) 0.6430(17) 0.4830(8) 0.171(11) Uani 1 0 . C40 C 0.9705(13) 0.159(2) 0.5966(17) 0.084(10) Uiso 0.460822 0 . C41 C 0.9847(15) 0.109(3) 0.671(2) 0.110(10) Uiso 0.372678 0 . C42 C 1.023(2) 0.027(5) 0.704(3) 0.250(19) Uiso 0.427493 0 . C43 C 1.0550(8) 0.0292(16) 0.6206(12) 0.058(5) Uiso 0.455469 0 . C44 C 1.0203(10) 0.011(2) 0.5625(15) 0.092(8) Uiso 0.442758 0 . C45 C 0.9749(9) 0.0672(18) 0.5477(12) 0.077(6) Uiso 0.464276 0 . C46 C 0.9617(9) 0.1263(17) 0.6049(13) 0.086(8) Uiso 0.653222 0 . C47 C 1.0081(8) 0.1867(15) 0.6192(10) 0.104(5) Uiso 0.720856 0 . C48 C 1.0531(6) 0.1314(13) 0.6382(8) 0.079(4) Uiso 0.68909 0 . C49 C 1.0528(8) 0.0303(17) 0.6605(12) 0.107(6) Uiso 0.653597 0 . C50 C 1.0020(16) -0.021(3) 0.642(2) 0.104(11) Uiso 0.328287 0 . C51 C 0.9613(15) 0.057(3) 0.624(2) 0.149(13) Uiso 0.479521 0 . H1 H 0.7475 0.1713 0.3035 0.062 Uiso 1 0 . H2 H 0.7999 0.2507 0.2625 0.0742 Uiso 1 0 . H3 H 0.8746 0.2734 0.2276 0.0806 Uiso 1 0 . H4 H 0.9536 0.275 0.3172 0.093 Uiso 1 0 . H5 H 0.957 0.2568 0.4437 0.0989 Uiso 1 0 . H6 H 0.8841 0.2318 0.4804 0.0826 Uiso 1 0 . H7 H 0.8068 0.4616 0.7292 0.0698 Uiso 1 0 . H8 H 0.8831 0.5163 0.8143 0.0688 Uiso 1 0 . H9 H 0.9595 0.4369 0.8132 0.1049 Uiso 1 0 . H10 H 0.9605 0.3116 0.718 0.1022 Uiso 1 0 . H11 H 0.884 0.2504 0.637 0.0747 Uiso 1 0 . H12 H 0.8139 0.1191 0.657 0.0835 Uiso 1 0 . H13 H 0.8437 -0.0527 0.6984 0.0904 Uiso 1 0 . H14 H 0.8684 -0.171 0.6169 0.1125 Uiso 1 0 . H15 H 0.8612 -0.113 0.4926 0.1009 Uiso 1 0 . H16 H 0.8278 0.0557 0.4545 0.0878 Uiso 1 0 . H17 H 0.799 0.4224 0.3828 0.0629 Uiso 1 0 . H18 H 0.805 0.6023 0.3543 0.0731 Uiso 1 0 . H19 H 0.7977 0.7339 0.4414 0.0955 Uiso 1 0 . H20 H 0.7903 0.6757 0.5583 0.0937 Uiso 1 0 . H21 H 0.7883 0.4955 0.5828 0.0879 Uiso 1 0 . H22 H 0.9283 0.4264 0.5716 0.1156 Uiso 1 0 . H23 H 0.9315 0.5515 0.6617 0.113 Uiso 1 0 . H24 H 0.9419 0.7904 0.5274 0.1309 Uiso 1 0 . H25 H 0.9333 0.4851 0.4559 0.1688 Uiso 1 0 . H26 H 0.9435 0.6674 0.4356 0.1758 Uiso 1 0 .