#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100739.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_1100739 _publ_section_title ; Aerobic Catechol Oxidation Catalyzed through Cyclic Formation of Mn(II)- semiquinonate and Bis(m-oxo)dimanganese(III,III) Complexes ; loop_ _publ_author_name 'Yutaka Hitomi' _chemical_formula_sum 'C84 H76 B2 Mn2 N8 O2' _[local]_cod_chemical_formula_sum_orig 'C84 H76 B2 N8 Mn2 O2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1361.07 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 19.474(2) _cell_length_b 14.884(2) _cell_length_c 24.538(3) _cell_angle_alpha 90 _cell_angle_beta 105.370(3) _cell_angle_gamma 90 _cell_volume 6858.3(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13782 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 243.2 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'RICABA' _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.919 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 37881 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9847 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9847 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _reflns_number_total 7748 _reflns_number_gt 3277 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1797 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4372 _refine_ls_number_parameters 442 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 1.85 _refine_diff_density_min -0.91 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.24091(4) -0.17227(5) 0.52373(3) 0.0382(3) Uani 1.00 d . . . O(1) O 0.2229(2) -0.2927(2) 0.5360(1) 0.036(1) Uani 1.00 d . . . N(1) N 0.2584(2) -0.0298(3) 0.5153(2) 0.036(1) Uani 1.00 d . . . N(2) N 0.1333(2) -0.1163(3) 0.4684(2) 0.049(2) Uani 1.00 d . . . N(3) N 0.3492(2) -0.1397(3) 0.5863(2) 0.044(2) Uani 1.00 d . . . N(4) N 0.2024(2) -0.1239(3) 0.5894(2) 0.040(1) Uani 1.00 d . . . C(1) C 0.2144(3) -0.0024(3) 0.4574(2) 0.050(2) Uani 1.00 d . . . C(2) C 0.3350(3) -0.0189(3) 0.5198(2) 0.050(2) Uani 1.00 d . . . C(3) C 0.2364(3) 0.0217(3) 0.5594(2) 0.044(2) Uani 1.00 d . . . C(4) C 0.1399(3) -0.0326(4) 0.4528(2) 0.049(2) Uani 1.00 d . . . C(5) C 0.0795(4) 0.0215(4) 0.4312(3) 0.067(2) Uani 1.00 d . . . C(6) C 0.0155(4) -0.0142(6) 0.4297(3) 0.077(3) Uani 1.00 d . . . C(7) C 0.0073(4) -0.1011(5) 0.4449(3) 0.075(3) Uani 1.00 d . . . C(8) C 0.0693(4) -0.1494(4) 0.4643(3) 0.058(2) Uani 1.00 d . . . C(9) C 0.3763(3) -0.0616(4) 0.5743(2) 0.040(2) Uani 1.00 d . . . C(10) C 0.4370(3) -0.0251(4) 0.6124(3) 0.051(2) Uani 1.00 d . . . C(11) C 0.4687(3) -0.0704(5) 0.6598(3) 0.059(2) Uani 1.00 d . . . C(12) C 0.4402(3) -0.1500(4) 0.6720(2) 0.054(2) Uani 1.00 d . . . C(13) C 0.3806(3) -0.1834(4) 0.6326(3) 0.053(2) Uani 1.00 d . . . C(14) C 0.2043(3) -0.0351(4) 0.5986(2) 0.042(2) Uani 1.00 d . . . C(15) C 0.1824(3) 0.0036(4) 0.6421(3) 0.045(2) Uani 1.00 d . . . C(16) C 0.1540(3) -0.0516(5) 0.6743(2) 0.057(2) Uani 1.00 d . . . C(17) C 0.1509(3) -0.1428(4) 0.6644(3) 0.059(2) Uani 1.00 d . . . C(18) C 0.1751(3) -0.1763(3) 0.6217(3) 0.047(2) Uani 1.00 d . . . C(19) C 0.2739(3) 0.3213(4) 0.6601(2) 0.044(2) Uani 1.00 d . . . C(20) C 0.3072(3) 0.2395(4) 0.6555(2) 0.047(2) Uani 1.00 d . . . C(21) C 0.3798(4) 0.2296(4) 0.6670(3) 0.057(2) Uani 1.00 d . . . C(22) C 0.4236(3) 0.3018(5) 0.6839(2) 0.055(2) Uani 1.00 d . . . C(23) C 0.3938(3) 0.3835(4) 0.6883(3) 0.059(2) Uani 1.00 d . . . C(24) C 0.3201(3) 0.3931(4) 0.6777(2) 0.045(2) Uani 1.00 d . . . C(25) C 0.1653(3) 0.4259(3) 0.6722(2) 0.037(2) Uani 1.00 d . . . C(26) C 0.1443(3) 0.5004(4) 0.6360(2) 0.045(2) Uani 1.00 d . . . C(27) C 0.1216(3) 0.5818(4) 0.6539(2) 0.051(2) Uani 1.00 d . . . C(28) C 0.1227(3) 0.5943(4) 0.7090(3) 0.046(2) Uani 1.00 d . . . C(29) C 0.1450(3) 0.5235(4) 0.7465(2) 0.047(2) Uani 1.00 d . . . C(30) C 0.1647(3) 0.4425(4) 0.7277(2) 0.040(2) Uani 1.00 d . . . C(31) C 0.1614(3) 0.2508(3) 0.6877(2) 0.040(2) Uani 1.00 d . . . C(32) C 0.2066(3) 0.2169(4) 0.7370(2) 0.048(2) Uani 1.00 d . . . C(33) C 0.1857(4) 0.1580(4) 0.7757(2) 0.055(2) Uani 1.00 d . . . C(34) C 0.1155(4) 0.1294(4) 0.7605(3) 0.058(2) Uani 1.00 d . . . C(35) C 0.0682(3) 0.1595(4) 0.7118(3) 0.061(2) Uani 1.00 d . . . C(36) C 0.0918(3) 0.2182(4) 0.6762(2) 0.041(2) Uani 1.00 d . . . C(37) C 0.1443(3) 0.3144(3) 0.5810(2) 0.031(1) Uani 1.00 d . . . C(38) C 0.0739(3) 0.3421(4) 0.5616(2) 0.049(2) Uani 1.00 d . . . C(39) C 0.0366(3) 0.3300(4) 0.5061(3) 0.049(2) Uani 1.00 d . . . C(40) C 0.0666(3) 0.2880(4) 0.4669(2) 0.051(2) Uani 1.00 d . . . C(41) C 0.1354(3) 0.2605(4) 0.4860(2) 0.050(2) Uani 1.00 d . . . C(42) C 0.1740(3) 0.2723(3) 0.5419(2) 0.043(2) Uani 1.00 d . . . B(1) B 0.1874(3) 0.3287(4) 0.6497(3) 0.036(2) Uani 1.00 d . . . H(1) H 0.2158 0.0609 0.4533 0.0603 Uiso 1.00 calc . . . H(2) H 0.2321 -0.0306 0.4291 0.0603 Uiso 1.00 calc . . . H(3) H 0.3464 -0.0475 0.4887 0.0603 Uiso 1.00 calc . . . H(4) H 0.3464 0.0432 0.5198 0.0603 Uiso 1.00 calc . . . H(5) H 0.2771 0.0518 0.5819 0.0523 Uiso 1.00 calc . . . H(6) H 0.2019 0.0647 0.5412 0.0523 Uiso 1.00 calc . . . H(7) H 0.0838 0.0808 0.4182 0.0803 Uiso 1.00 calc . . . H(8) H -0.0257 0.0225 0.4176 0.0927 Uiso 1.00 calc . . . H(9) H -0.0382 -0.1265 0.4422 0.0898 Uiso 1.00 calc . . . H(10) H 0.0657 -0.2100 0.4753 0.0701 Uiso 1.00 calc . . . H(11) H 0.4555 0.0312 0.6048 0.0613 Uiso 1.00 calc . . . H(12) H 0.5109 -0.0474 0.6849 0.0706 Uiso 1.00 calc . . . H(13) H 0.4607 -0.1812 0.7062 0.0646 Uiso 1.00 calc . . . H(14) H 0.3619 -0.2399 0.6396 0.0640 Uiso 1.00 calc . . . H(15) H 0.1870 0.0663 0.6493 0.0534 Uiso 1.00 calc . . . H(16) H 0.1361 -0.0274 0.7036 0.0681 Uiso 1.00 calc . . . H(17) H 0.1320 -0.1819 0.6874 0.0711 Uiso 1.00 calc . . . H(18) H 0.1724 -0.2391 0.6148 0.0565 Uiso 1.00 calc . . . H(19) H 0.2782 0.1881 0.6438 0.0569 Uiso 1.00 calc . . . H(20) H 0.3997 0.1723 0.6633 0.0679 Uiso 1.00 calc . . . H(21) H 0.4738 0.2953 0.6923 0.0659 Uiso 1.00 calc . . . H(22) H 0.4236 0.4346 0.6988 0.0711 Uiso 1.00 calc . . . H(23) H 0.3009 0.4503 0.6827 0.0535 Uiso 1.00 calc . . . H(24) H 0.1456 0.4951 0.5977 0.0541 Uiso 1.00 calc . . . H(25) H 0.1052 0.6286 0.6273 0.0616 Uiso 1.00 calc . . . H(26) H 0.1086 0.6500 0.7216 0.0550 Uiso 1.00 calc . . . H(27) H 0.1466 0.5308 0.7853 0.0560 Uiso 1.00 calc . . . H(28) H 0.1787 0.3953 0.7544 0.0484 Uiso 1.00 calc . . . H(29) H 0.2552 0.2344 0.7458 0.0573 Uiso 1.00 calc . . . H(30) H 0.2182 0.1394 0.8100 0.0664 Uiso 1.00 calc . . . H(31) H 0.0997 0.0882 0.7842 0.0695 Uiso 1.00 calc . . . H(32) H 0.0199 0.1405 0.7025 0.0732 Uiso 1.00 calc . . . H(33) H 0.0586 0.2370 0.6423 0.0491 Uiso 1.00 calc . . . H(34) H 0.0511 0.3697 0.5870 0.0592 Uiso 1.00 calc . . . H(35) H -0.0111 0.3510 0.4939 0.0584 Uiso 1.00 calc . . . H(36) H 0.0402 0.2791 0.4287 0.0618 Uiso 1.00 calc . . . H(37) H 0.1577 0.2325 0.4604 0.0595 Uiso 1.00 calc . . . H(38) H 0.2217 0.2513 0.5538 0.0512 Uiso 1.00 calc . . .