#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/5000408.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_5000408 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C36 H37 B2 F8 Mo2 N9' _chemical_formula_moiety 'C36 H37 Mo2 N9 2+, 2(B F4 -)' _chemical_formula_weight 961.24 _cell_length_a 12.027(3) _cell_length_b 17.335(5) _cell_length_c 10.341(3) _cell_angle_alpha 91.758(14) _cell_angle_beta 109.715(16) _cell_angle_gamma 80.431(13) _cell_volume 2000.5(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 46 _cell_measurement_theta_min 9.66 _cell_measurement_theta_max 10.36 _cell_measurement_temperature 103 _exptl_crystal_colour red _exptl_crystal_description prism _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.7028 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 103 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8745 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 2 _diffrn_standards_number 4 _diffrn_standards_decay_% 2.7 _diffrn_standards_interval_count 300 _reflns_number_total 7101 _reflns_number_gt 5960 _reflns_threshold_expression F>3.0\s(F) _atom_sites_solution_primary Patterson _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 7101 _refine_ls_number_parameters 488 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.4652E-6 _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 0.036 _refine_ls_wR_factor_ref 0.0352 _refine_ls_goodness_of_fit_ref 0.9546 _refine_ls_shift/su_max 0.0146 _refine_diff_density_max 0.72 _refine_diff_density_min -0.50 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 0.22803(3) 0.26086(2) 0.07935(3) 0.01229(13) Uani 1 0 . Mo2 Mo 0.39015(3) 0.25870(2) 0.03445(3) 0.01235(13) Uani 1 0 . N3 N 0.1541(3) 0.2001(2) -0.0978(3) 0.0153(13) Uani 1 0 . C4 C 0.2112(3) 0.1871(2) -0.1870(4) 0.0163(13) Uani 1 0 . N5 N 0.3203(3) 0.2053(2) -0.1565(3) 0.0150(13) Uani 1 0 . C6 C 0.0355(3) 0.1824(2) -0.1355(4) 0.0161(14) Uani 1 0 . C7 C -0.0562(4) 0.2202(2) -0.2456(4) 0.0274(14) Uani 1 0 . C8 C -0.1718(4) 0.2044(3) -0.2732(5) 0.0325(14) Uani 1 0 . C9 C -0.1950(3) 0.1514(3) -0.1921(4) 0.0270(16) Uani 1 0 . C10 C -0.1021(4) 0.1130(2) -0.0843(4) 0.0247(14) Uani 1 0 . C11 C 0.0128(3) 0.1282(2) -0.0537(4) 0.0194(14) Uani 1 0 . C12 C 0.3817(3) 0.1833(2) -0.2514(3) 0.0144(13) Uani 1 0 . C13 C 0.3853(3) 0.1083(2) -0.3044(4) 0.0199(14) Uani 1 0 . C14 C 0.4473(3) 0.0875(2) -0.3958(4) 0.0196(14) Uani 1 0 . C15 C 0.5043(3) 0.1410(2) -0.4352(4) 0.0221(14) Uani 1 0 . C16 C 0.5005(3) 0.2155(2) -0.3823(4) 0.0225(14) Uani 1 0 . C17 C 0.4405(3) 0.2367(2) -0.2909(4) 0.0196(14) Uani 1 0 . N18 N 0.2946(3) 0.1587(2) 0.2039(3) 0.0146(13) Uani 1 0 . C19 C 0.4041(3) 0.1227(2) 0.2137(4) 0.0163(13) Uani 1 0 . N20 N 0.4629(3) 0.1515(2) 0.1444(3) 0.0140(13) Uani 1 0 . C21 C 0.2318(3) 0.1255(2) 0.2783(4) 0.0174(13) Uani 1 0 . C22 C 0.1537(3) 0.1762(2) 0.3298(4) 0.0186(14) Uani 1 0 . C23 C 0.0944(3) 0.1469(2) 0.4063(4) 0.0200(14) Uani 1 0 . C24 C 0.1125(3) 0.0673(2) 0.4343(4) 0.0216(14) Uani 1 0 . C25 C 0.1856(3) 0.0166(2) 0.3783(4) 0.0222(14) Uani 1 0 . C26 C 0.2446(3) 0.0454(2) 0.3011(4) 0.0177(14) Uani 1 0 . C27 C 0.5827(3) 0.1113(2) 0.1656(4) 0.0181(14) Uani 1 0 . C28 C 0.6064(3) 0.0634(2) 0.0646(4) 0.0201(14) Uani 1 0 . C29 C 0.7218(4) 0.0247(2) 0.0853(4) 0.0230(14) Uani 1 0 . C30 C 0.8144(3) 0.0355(2) 0.2031(4) 0.0271(14) Uani 1 0 . C31 C 0.7913(3) 0.0848(3) 0.3021(4) 0.0259(14) Uani 1 0 . C32 C 0.6759(3) 0.1228(2) 0.2837(4) 0.0200(14) Uani 1 0 . N33 N 0.1129(3) 0.3645(2) -0.0357(3) 0.0174(13) Uani 1 0 . C34 C 0.0516(3) 0.4141(2) -0.1074(4) 0.0208(14) Uani 1 0 . C35 C -0.0257(4) 0.4775(3) -0.2011(4) 0.0320(16) Uani 1 0 . N36 N 0.2539(3) 0.3307(2) 0.2633(3) 0.0174(13) Uani 1 0 . C37 C 0.2617(3) 0.3631(2) 0.3632(4) 0.0179(14) Uani 1 0 . C38 C 0.2708(3) 0.4022(2) 0.4920(4) 0.0206(14) Uani 1 0 . N39 N 0.3510(3) 0.3726(2) -0.0694(3) 0.0167(13) Uani 1 0 . C40 C 0.3325(3) 0.4349(2) -0.1103(4) 0.0199(14) Uani 1 0 . C41 C 0.3053(4) 0.5156(2) -0.1615(5) 0.0334(16) Uani 1 0 . N42 N 0.4875(3) 0.3174(2) 0.2175(3) 0.0182(13) Uani 1 0 . C43 C 0.5406(3) 0.3505(2) 0.3079(4) 0.0176(14) Uani 1 0 . C44 C 0.6076(4) 0.3928(2) 0.4231(4) 0.0257(14) Uani 1 0 . N45 N 0.6000(3) 0.2588(2) 0.0158(3) 0.0230(13) Uani 1 0 . C46 C 0.6978(4) 0.2653(2) 0.0464(4) 0.0201(14) Uani 1 0 . C47 C 0.8233(4) 0.2739(3) 0.0896(5) 0.0316(18) Uani 1 0 . B48 B -0.0412(4) 0.3625(3) 0.4581(5) 0.024(2) Uani 1 0 . F49 F 0.0042(2) 0.3647(2) 0.3508(2) 0.0337(11) Uani 1 0 . F50 F -0.1077(2) 0.43477(10) 0.4664(3) 0.0358(13) Uani 1 0 . F51 F -0.1166(2) 0.3064(2) 0.4312(3) 0.0375(13) Uani 1 0 . F52 F 0.0519(2) 0.3442(2) 0.5812(3) 0.0381(11) Uani 1 0 . B53 B 0.3533(5) 0.5556(3) 0.2156(5) 0.029(2) Uani 1 0 . F54 F 0.2443(3) 0.5761(3) 0.1134(3) 0.0806(18) Uani 1 0 . F55 F 0.4310(3) 0.5136(2) 0.1555(3) 0.0485(14) Uani 1 0 . F56 F 0.3418(2) 0.50948(10) 0.3157(2) 0.0376(11) Uani 1 0 . F57 F 0.3996(5) 0.6199(2) 0.2726(4) 0.099(3) Uani 1 0 . H1 H 0.1747 0.1648 -0.2727 0.0287 Uiso 1 0 . H2 H -0.0409 0.2566 -0.3019 0.0386 Uiso 1 0 . H3 H -0.2355 0.2302 -0.3488 0.044 Uiso 1 0 . H4 H -0.2743 0.1416 -0.2107 0.0398 Uiso 1 0 . H5 H -0.1174 0.0754 -0.0302 0.0366 Uiso 1 0 . H6 H 0.076 0.1022 0.0222 0.032 Uiso 1 0 . H7 H 0.3458 0.0716 -0.2783 0.0321 Uiso 1 0 . H8 H 0.4505 0.0363 -0.4314 0.0332 Uiso 1 0 . H9 H 0.5459 0.1268 -0.4981 0.0353 Uiso 1 0 . H10 H 0.5395 0.2523 -0.4092 0.0342 Uiso 1 0 . H11 H 0.439 0.2877 -0.2546 0.0322 Uiso 1 0 . H12 H 0.4395 0.0767 0.2699 0.0284 Uiso 1 0 . H13 H 0.1415 0.2309 0.312 0.0307 Uiso 1 0 . H14 H 0.041 0.1816 0.4397 0.0328 Uiso 1 0 . H15 H 0.0754 0.0476 0.4912 0.0327 Uiso 1 0 . H16 H 0.1952 -0.0383 0.3932 0.0336 Uiso 1 0 . H17 H 0.2943 0.0102 0.2634 0.0302 Uiso 1 0 . H18 H 0.5437 0.0572 -0.0185 0.0318 Uiso 1 0 . H19 H 0.7373 -0.0096 0.0177 0.0358 Uiso 1 0 . H20 H 0.8935 0.0093 0.2163 0.0385 Uiso 1 0 . H21 H 0.855 0.0927 0.3832 0.0374 Uiso 1 0 . H22 H 0.6606 0.1568 0.3518 0.0322 Uiso 1 0 . H23 H 0.0047 0.525 -0.175 0.0446 Uiso 1 0 . H24 H -0.0278 0.4659 -0.2921 0.0446 Uiso 1 0 . H25 H -0.1043 0.483 -0.1969 0.0446 Uiso 1 0 . H26 H 0.3514 0.4089 0.5379 0.0337 Uiso 1 0 . H27 H 0.2206 0.4519 0.4737 0.0337 Uiso 1 0 . H28 H 0.2464 0.3713 0.5484 0.0337 Uiso 1 0 . H29 H 0.374 0.5297 -0.1743 0.0449 Uiso 1 0 . H30 H 0.2411 0.5207 -0.2467 0.0449 Uiso 1 0 . H31 H 0.2829 0.5492 -0.0969 0.0449 Uiso 1 0 . H32 H 0.6018 0.3741 0.5056 0.0374 Uiso 1 0 . H33 H 0.6893 0.3849 0.429 0.0374 Uiso 1 0 . H34 H 0.5758 0.447 0.4101 0.0374 Uiso 1 0 . H35 H 0.872 0.2237 0.1092 0.0449 Uiso 1 0 . H36 H 0.8378 0.2993 0.0181 0.0449 Uiso 1 0 . H37 H 0.8421 0.3044 0.1697 0.0449 Uiso 1 0 . _cod_database_code 5000408