#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000330.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_5000330 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C41 H35.5 Cl2 Fe2 N6.5 O5' _chemical_formula_moiety 'C36 H28 Cl2 Fe2 N4 O5, 2.5(C2 H3 N)' _chemical_formula_weight 881.87 _cell_length_a 11.459(6) _cell_length_b 16.457(8) _cell_length_c 11.376(6) _cell_angle_alpha 92.36(3) _cell_angle_beta 105.11(3) _cell_angle_gamma 74.40(3) _cell_volume 1993.9(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 66 _cell_measurement_theta_min 11.18 _cell_measurement_theta_max 15.84 _cell_measurement_temperature 108 _exptl_crystal_colour green _exptl_crystal_description 'triangular plate' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 0.9139 _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_crystal_treatment ; The sample consisted of transparent green crystals in the mother liquor of MeCN. The crystals had formed by cooling the solution in the freezer and had a tendency to redissolve in the mother liquor when warmed to room temperature. The first two data collection attempts came to a premature end due to ice problems. A third crystal was not diffracting well and finally a triangular shaped crystal was selected and mounted using a nylon loop and a lot of silicone grease. ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 108 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16730 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_min 3.01717 _diffrn_reflns_theta_max 25.1048 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 4 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 300 _reflns_number_total 7057 _reflns_number_gt 5457 _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 Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B' Cl Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 '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' 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 7057 _refine_ls_number_parameters 509 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef -0.00000046(9) _refine_ls_extinction_method Zachariasen _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)+(.07F)^2^ _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0457 _refine_ls_goodness_of_fit_ref 1.0395 _refine_ls_shift/su_max 0.0027 _refine_diff_density_max 0.86 _refine_diff_density_min -0.56 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 Fe1 Fe 0.13732(5) 0.16190(3) 0.33672(5) 0.02176(19) Uani 1 0 . Fe2 Fe 0.29647(5) 0.22310(3) 0.18632(5) 0.01939(19) Uani 1 0 . O3 O 0.2146(2) 0.15226(15) 0.2184(2) 0.0214(9) Uani 1 0 . Cl4 Cl -0.05255(8) 0.13324(6) 0.22738(9) 0.0309(3) Uani 1 0 . Cl5 Cl 0.24562(8) 0.20622(6) -0.02830(8) 0.0241(3) Uani 1 0 . O6 O 0.0626(2) 0.29086(15) 0.3141(2) 0.0267(10) Uani 1 0 . C7 C 0.0728(3) 0.3431(2) 0.2408(3) 0.0219(13) Uani 1 0 . O8 O 0.1554(2) 0.32983(15) 0.1816(2) 0.0237(9) Uani 1 0 . C9 C -0.0208(3) 0.4278(2) 0.2217(3) 0.0232(13) Uani 1 0 . C10 C -0.0075(4) 0.4899(2) 0.1511(4) 0.0263(14) Uani 1 0 . C11 C -0.0926(4) 0.5684(2) 0.1327(4) 0.0339(16) Uani 1 0 . C12 C -0.1935(4) 0.5860(3) 0.1838(4) 0.0393(18) Uani 1 0 . C13 C -0.2087(4) 0.5242(3) 0.2534(4) 0.0416(18) Uani 1 0 . C14 C -0.1228(4) 0.4453(3) 0.2736(4) 0.0346(16) Uani 1 0 . O15 O 0.2854(2) 0.18391(17) 0.4713(2) 0.0337(10) Uani 1 0 . C16 C 0.3505(3) 0.2332(2) 0.4621(3) 0.0235(13) Uani 1 0 . O17 O 0.3644(2) 0.25763(16) 0.3642(2) 0.0274(10) Uani 1 0 . C18 C 0.4163(3) 0.2652(2) 0.5794(3) 0.0213(13) Uani 1 0 . C19 C 0.4041(3) 0.2394(2) 0.6894(3) 0.0253(14) Uani 1 0 . C20 C 0.4691(4) 0.2645(3) 0.7984(3) 0.0296(14) Uani 1 0 . C21 C 0.5462(4) 0.3175(3) 0.7970(4) 0.0334(15) Uani 1 0 . C22 C 0.5566(4) 0.3444(3) 0.6874(4) 0.0343(15) Uani 1 0 . C23 C 0.4924(4) 0.3180(2) 0.5780(3) 0.0285(14) Uani 1 0 . N24 N 0.0688(3) 0.1639(2) 0.4977(3) 0.0303(12) Uani 1 0 . C25 C 0.0080(5) 0.2342(3) 0.5425(4) 0.0420(18) Uani 1 0 . C26 C -0.0247(5) 0.2351(3) 0.6508(4) 0.050(2) Uani 1 0 . C27 C 0.0055(5) 0.1592(4) 0.7144(4) 0.056(2) Uani 1 0 . C28 C 0.0669(4) 0.0866(3) 0.6699(4) 0.0424(17) Uani 1 0 . C29 C 0.0997(4) 0.0904(3) 0.5606(3) 0.0321(14) Uani 1 0 . C30 C 0.1709(3) 0.0153(3) 0.5087(3) 0.0317(14) Uani 1 0 . C31 C 0.1970(4) -0.0657(3) 0.5585(4) 0.0402(16) Uani 1 0 . C32 C 0.2626(4) -0.1335(3) 0.5057(4) 0.0439(17) Uani 1 0 . C33 C 0.3031(4) -0.1197(3) 0.4060(4) 0.0400(17) Uani 1 0 . C34 C 0.2794(4) -0.0374(2) 0.3621(4) 0.0323(15) Uani 1 0 . N35 N 0.2118(3) 0.02922(19) 0.4112(3) 0.0264(11) Uani 1 0 . C36 C 0.3386(4) -0.0222(2) 0.2635(4) 0.0303(15) Uani 1 0 . C37 C 0.4476(3) 0.0165(2) 0.3183(4) 0.0295(14) Uani 1 0 . N38 N 0.4827(3) 0.12785(19) 0.2055(3) 0.0217(11) Uani 1 0 . C39 C 0.5067(3) 0.0440(2) 0.2279(3) 0.0249(13) Uani 1 0 . C40 C 0.5897(3) -0.0138(2) 0.1762(4) 0.0282(14) Uani 1 0 . C41 C 0.6542(4) 0.0138(2) 0.1052(4) 0.0281(14) Uani 1 0 . C42 C 0.6398(3) 0.0991(2) 0.0942(3) 0.0269(14) Uani 1 0 . C43 C 0.5535(3) 0.1547(2) 0.1448(3) 0.0236(13) Uani 1 0 . C44 C 0.5328(3) 0.2475(2) 0.1399(3) 0.0217(13) Uani 1 0 . C45 C 0.6242(3) 0.2850(2) 0.1267(3) 0.0278(14) Uani 1 0 . C46 C 0.5965(4) 0.3721(3) 0.1234(4) 0.0342(15) Uani 1 0 . C47 C 0.4800(4) 0.4196(2) 0.1321(4) 0.0322(15) Uani 1 0 . C48 C 0.3941(4) 0.3781(2) 0.1466(3) 0.0265(14) Uani 1 0 . N49 N 0.4201(3) 0.29382(19) 0.1521(3) 0.0220(11) Uani 1 0 . C50 C -0.0949(4) 0.2770(3) -0.0129(4) 0.0431(17) Uani 1 0 . C51 C -0.1615(4) 0.3584(3) -0.0749(4) 0.0326(16) Uani 1 0 . N52 N -0.2154(4) 0.4207(3) -0.1232(4) 0.0577(18) Uani 1 0 . C53 C 0.7610(8) 0.5088(4) 0.5841(5) 0.097(3) Uani 1 0 . C54 C 0.7125(6) 0.4485(5) 0.5100(5) 0.078(3) Uani 1 0 . N55 N 0.6777(8) 0.3999(6) 0.4511(6) 0.183(5) Uani 1 0 . C56 C 0.1487(10) -0.0983(6) 0.0965(9) 0.048(2) Uiso 0.5 0 . C57 C 0.0667(11) -0.0433(7) 0.0436(10) 0.058(3) Uiso 0.5 0 . C58 C -0.0483(17) -0.0474(11) 0.0081(16) 0.112(6) Uiso 0.5 0 . H1 H 0.0613 0.4776 0.1131 0.0388 Uiso 1 0 . H2 H -0.081 0.6115 0.0839 0.0439 Uiso 1 0 . H3 H -0.2552 0.6406 0.1714 0.0508 Uiso 1 0 . H4 H -0.2759 0.5366 0.2913 0.0543 Uiso 1 0 . H5 H -0.1333 0.4021 0.3214 0.0457 Uiso 1 0 . H6 H 0.3528 0.2021 0.6885 0.0348 Uiso 1 0 . H7 H 0.4604 0.2447 0.8746 0.0391 Uiso 1 0 . H8 H 0.5907 0.3361 0.8728 0.0434 Uiso 1 0 . H9 H 0.6066 0.3823 0.6871 0.0434 Uiso 1 0 . H10 H 0.5022 0.3343 0.5018 0.039 Uiso 1 0 . H11 H -0.0144 0.2869 0.496 0.0523 Uiso 1 0 . H12 H -0.0681 0.2878 0.68 0.061 Uiso 1 0 . H13 H -0.018 0.1569 0.7884 0.0677 Uiso 1 0 . H14 H 0.0908 0.0333 0.714 0.05 Uiso 1 0 . H15 H 0.1654 -0.0746 0.6288 0.0478 Uiso 1 0 . H16 H 0.2793 -0.19 0.5363 0.0481 Uiso 1 0 . H17 H 0.3495 -0.1663 0.3691 0.0491 Uiso 1 0 . H18 H 0.3685 -0.0749 0.2258 0.0413 Uiso 1 0 . H19 H 0.2774 0.0152 0.2007 0.0413 Uiso 1 0 . H20 H 0.4184 0.0639 0.364 0.0396 Uiso 1 0 . H21 H 0.5121 -0.0251 0.3733 0.0396 Uiso 1 0 . H22 H 0.603 -0.0734 0.1896 0.0398 Uiso 1 0 . H23 H 0.7068 -0.0265 0.0651 0.0406 Uiso 1 0 . H24 H 0.6885 0.1198 0.0522 0.036 Uiso 1 0 . H25 H 0.7033 0.251 0.1172 0.0396 Uiso 1 0 . H26 H 0.6586 0.399 0.1191 0.0414 Uiso 1 0 . H27 H 0.4565 0.4804 0.1266 0.0393 Uiso 1 0 . H28 H 0.3132 0.4108 0.1526 0.0393 Uiso 1 0 . H29 H -0.0979 0.2786 0.0691 0.0502 Uiso 1 0 . H30 H -0.1291 0.2335 -0.0531 0.0502 Uiso 1 0 . H31 H -0.0074 0.2631 -0.0152 0.0502 Uiso 1 0 . H32 H 0.8519 0.4953 0.6015 0.0972 Uiso 1 0 . H33 H 0.741 0.5117 0.6618 0.0972 Uiso 1 0 . H34 H 0.7282 0.5639 0.5466 0.0972 Uiso 1 0 .