# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_CoSalNO2THF #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C32 H42 Co1 N4 O7' _chemical_formula_moiety 'C32 H42 Co1 N4 O7' _chemical_formula_weight 653.64 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 10.9613(3) _cell_length_b 12.0129(3) _cell_length_c 14.1562(3) _cell_angle_alpha 106.6320(10) _cell_angle_beta 91.9720(10) _cell_angle_gamma 117.1130(10) _cell_volume 1559.81(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 690.000 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type none #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 293 _diffrn_reflns_number 52313 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_min 1.530 _diffrn_reflns_theta_max 36.404 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.483 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 12705 _refine_ls_number_restraints 0 _refine_ls_number_parameters 463 _oxford_refine_ls_R_factor_ref 0.0445 _refine_ls_wR_factor_ref 0.0438 _refine_ls_goodness_of_fit_ref 1.0108 # The values computed from all data _oxford_reflns_number_all 14974 _refine_ls_R_factor_all 0.0591 _refine_ls_wR_factor_all 0.0700 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 13217 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_gt 0.0453 _reflns_number_total 13837 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 6.60 10.1 4.68 1.09 0.00 ; _oxford_refine_ls_scale 0.10330(9) _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 # Number of reflections with Friedels Law is 950 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1005 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # TODO check _oxford_atom_site_special_shape 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Co1 Co 0.916624(14) 0.636756(13) 0.622039(10) 0.0159 1.0000 Uani . . . . . . N2 N 0.77297(11) 0.50197(10) 0.51480(7) 0.0296 1.0000 Uani . . . . . . N5 N 1.01316(9) 0.68919(10) 0.52217(7) 0.0224 1.0000 Uani . . . . . . N28 N 0.27696(10) 0.18700(12) 0.68154(9) 0.0321 1.0000 Uani . . . . . . N29 N 1.61371(10) 1.10718(10) 0.71033(8) 0.0261 1.0000 Uani . . . . . . O3 O 0.82577(8) 0.56777(7) 0.71974(5) 0.0208 1.0000 Uani . . . . . . O4 O 1.07208(7) 0.76185(8) 0.72814(5) 0.0202 1.0000 Uani . . . . . . O30 O 1.64391(10) 1.11393(12) 0.62835(8) 0.0402 1.0000 Uani . . . . . . O31 O 1.70020(9) 1.17112(9) 0.78929(8) 0.0342 1.0000 Uani . . . . . . O32 O 0.20010(11) 0.12711(14) 0.59796(9) 0.0537 1.0000 Uani . . . . . . O33 O 0.23526(10) 0.17168(12) 0.75859(9) 0.0425 1.0000 Uani . . . . . . O100 O 0.82565(8) 0.76954(8) 0.63234(7) 0.0245 1.0000 Uani . . . . . . C6 C 0.65281(14) 0.41339(12) 0.52096(8) 0.0340 1.0000 Uani . . . . . . C7 C 1.14392(11) 0.77272(12) 0.53352(8) 0.0235 1.0000 Uani . . . . . . C8 C 0.60754(11) 0.39803(10) 0.61287(7) 0.0230 1.0000 Uani . . . . . . C9 C 0.46893(12) 0.30262(11) 0.60447(8) 0.0266 1.0000 Uani . . . . . . C10 C 0.42193(10) 0.28118(11) 0.68915(8) 0.0236 1.0000 Uani . . . . . . C11 C 0.51071(10) 0.34935(11) 0.78378(8) 0.0215 1.0000 Uani . . . . . . C12 C 0.64838(10) 0.44357(10) 0.79605(7) 0.0187 1.0000 Uani . . . . . . C13 C 0.69998(10) 0.47378(9) 0.70902(7) 0.0180 1.0000 Uani . . . . . . C14 C 1.23883(10) 0.85030(10) 0.62870(8) 0.0192 1.0000 Uani . . . . . . C15 C 1.19624(9) 0.84654(10) 0.72304(7) 0.0178 1.0000 Uani . . . . . . C16 C 1.29561(10) 0.94215(10) 0.81471(8) 0.0190 1.0000 Uani . . . . . . C17 C 1.43115(10) 1.02288(10) 0.80718(8) 0.0215 1.0000 Uani . . . . . . C18 C 1.47070(10) 1.01865(10) 0.71348(9) 0.0221 1.0000 Uani . . . . . . C19 C 1.37636(10) 0.93685(10) 0.62493(8) 0.0217 1.0000 Uani . . . . . . C20 C 0.74339(12) 0.51736(12) 0.90018(8) 0.0253 1.0000 Uani . . . . . . C21 C 1.25067(10) 0.95870(11) 0.91693(8) 0.0219 1.0000 Uani . . . . . . C22 C 1.12484(12) 0.98336(14) 0.91298(9) 0.0304 1.0000 Uani . . . . . . C23 C 1.36718(12) 1.07947(13) 1.00056(9) 0.0301 1.0000 Uani . . . . . . C24 C 1.21142(13) 0.83487(12) 0.94643(9) 0.0296 1.0000 Uani . . . . . . C25 C 0.87641(13) 0.50481(13) 0.89922(11) 0.0323 1.0000 Uani . . . . . . C26 C 0.78310(18) 0.66471(15) 0.93299(10) 0.0388 1.0000 Uani . . . . . . C27 C 0.67051(17) 0.4597(2) 0.97851(11) 0.0520 1.0000 Uani . . . . . . C36 C 0.98092(13) 0.64156(15) 0.33208(9) 0.0298 1.0000 Uani . . . . . . C39 C 0.69470(14) 0.43027(13) 0.32430(8) 0.0312 1.0000 Uani . . . . . . C101 C 0.9181(7) 0.9043(8) 0.6407(6) 0.0288 0.540(10) Uani . . P . 3 . C102 C 0.8508(4) 0.9792(4) 0.7242(5) 0.0509 0.540(10) Uani . . P . 3 . C103 C 0.70633(19) 0.88347(18) 0.70167(13) 0.0444 1.0000 Uani . . . . . . C104 C 0.7060(5) 0.7485(6) 0.6816(5) 0.0347 0.540(10) Uani . . P . 3 . C105 C 0.9164(10) 0.9116(11) 0.6470(10) 0.0450 0.460(10) Uani . . P . 4 . C106 C 0.8450(5) 0.9837(4) 0.6675(5) 0.0429 0.460(10) Uani . . P . 4 . C108 C 0.7449(6) 0.7834(6) 0.7047(5) 0.0303 0.460(10) Uani . . P . 4 . C341 C 0.81973(15) 0.49523(14) 0.41571(10) 0.0187 0.687(3) Uani . . P . 1 . C342 C 0.7760(3) 0.5412(3) 0.4193(2) 0.0164 0.313(3) Uani . . P . 2 . C351 C 0.91957(14) 0.63881(16) 0.42658(10) 0.0183 0.687(3) Uani . . P . 1 . C352 C 0.9279(3) 0.5785(3) 0.4146(2) 0.0175 0.313(3) Uani . . P . 2 . C371 C 0.87021(19) 0.5814(2) 0.24097(13) 0.0283 0.687(3) Uani . . P . 1 . C372 C 0.8717(4) 0.5153(6) 0.2297(3) 0.0306 0.313(3) Uani . . P . 2 . C381 C 0.7651(2) 0.4391(2) 0.23068(12) 0.0307 0.687(3) Uani . . P . 1 . C382 C 0.7194(4) 0.4745(5) 0.2326(3) 0.0280 0.313(3) Uani . . P . 2 . H61 H 0.5884 0.3529 0.4596 0.0481(9) 1.0000 Uiso R . . . . . H71 H 1.1801 0.7833 0.4745 0.0361(9) 1.0000 Uiso R . . . . . H91 H 0.4078 0.2535 0.5404 0.0393(9) 1.0000 Uiso R . . . . . H111 H 0.4748 0.3298 0.8408 0.0337(9) 1.0000 Uiso R . . . . . H171 H 1.4993 1.0831 0.8671 0.0338(9) 1.0000 Uiso R . . . . . H191 H 1.4042 0.9390 0.5621 0.0340(9) 1.0000 Uiso R . . . . . H221 H 1.0966 0.9938 0.9762 0.0454(9) 1.0000 Uiso R . . . . . H222 H 1.1501 1.0620 0.8970 0.0454(9) 1.0000 Uiso R . . . . . H223 H 1.0491 0.9101 0.8626 0.0454(9) 1.0000 Uiso R . . . . . H231 H 1.3366 1.0873 1.0631 0.0452(9) 1.0000 Uiso R . . . . . H232 H 1.4481 1.0693 1.0058 0.0452(9) 1.0000 Uiso R . . . . . H233 H 1.3904 1.1583 0.9854 0.0452(9) 1.0000 Uiso R . . . . . H241 H 1.1841 0.8467 1.0101 0.0444(9) 1.0000 Uiso R . . . . . H242 H 1.2897 0.8201 0.9504 0.0444(9) 1.0000 Uiso R . . . . . H243 H 1.1361 0.7589 0.8975 0.0444(9) 1.0000 Uiso R . . . . . H251 H 0.9343 0.5511 0.9642 0.0470(9) 1.0000 Uiso R . . . . . H252 H 0.8527 0.4135 0.8798 0.0470(9) 1.0000 Uiso R . . . . . H253 H 0.9268 0.5417 0.8523 0.0470(9) 1.0000 Uiso R . . . . . H261 H 0.8424 0.7116 0.9976 0.0560(9) 1.0000 Uiso R . . . . . H262 H 0.7008 0.6732 0.9361 0.0560(9) 1.0000 Uiso R . . . . . H263 H 0.8307 0.7032 0.8860 0.0560(9) 1.0000 Uiso R . . . . . H271 H 0.7310 0.5058 1.0424 0.0720(9) 1.0000 Uiso R . . . . . H272 H 0.6454 0.3676 0.9594 0.0720(9) 1.0000 Uiso R . . . . . H273 H 0.5881 0.4672 0.9826 0.0720(9) 1.0000 Uiso R . . . . . H361 H 1.0448 0.7318 0.3393 0.0452(9) 1.0000 Uiso R . . . . . H362 H 1.0309 0.5930 0.3240 0.0452(9) 1.0000 Uiso R . . . . . H391 H 0.6433 0.4781 0.3335 0.0461(9) 1.0000 Uiso R . . . . . H392 H 0.6317 0.3400 0.3170 0.0461(9) 1.0000 Uiso R . . . . . H1011 H 1.0112 0.9335 0.6698 0.0345(9) 0.540(10) Uiso R . P . 3 . H1012 H 0.9109 0.9203 0.5822 0.0345(9) 0.540(10) Uiso R . P . 3 . H1021 H 0.8943 1.0024 0.7910 0.0669(9) 0.540(10) Uiso R . P . 3 . H1022 H 0.8652 1.0593 0.7127 0.0669(9) 0.540(10) Uiso R . P . 3 . H1031 H 0.6636 0.9017 0.7576 0.0632(9) 1.0000 Uiso R . . . . . H1032 H 0.6579 0.8834 0.6442 0.0632(9) 1.0000 Uiso R . . . . . H1041 H 0.7155 0.7276 0.7417 0.0596(9) 0.540(10) Uiso R . P . 3 . H1042 H 0.6199 0.6723 0.6377 0.0596(9) 0.540(10) Uiso R . P . 3 . H1051 H 1.0022 0.9487 0.6928 0.0751(9) 0.460(10) Uiso R . P . 4 . H1052 H 0.9568 0.9178 0.5792 0.0751(9) 0.460(10) Uiso R . P . 4 . H1061 H 0.8986 1.0673 0.7219 0.0588(9) 0.460(10) Uiso R . P . 4 . H1062 H 0.8201 1.0014 0.6110 0.0588(9) 0.460(10) Uiso R . P . 4 . H1081 H 0.7899 0.8024 0.7683 0.0452(9) 0.460(10) Uiso R . P . 4 . H1082 H 0.6577 0.6985 0.6865 0.0452(9) 0.460(10) Uiso R . P . 4 . H3411 H 0.8688 0.4456 0.4054 0.0303(9) 0.687(3) Uiso R . P . 1 . H3421 H 0.7587 0.6142 0.4280 0.0226(9) 0.313(3) Uiso R . P . 2 . H3511 H 0.8678 0.6854 0.4330 0.0304(9) 0.687(3) Uiso R . P . 1 . H3521 H 0.9411 0.5033 0.4051 0.0240(9) 0.313(3) Uiso R . P . 2 . H3711 H 0.9113 0.5823 0.1826 0.0425(9) 0.687(3) Uiso R . P . 1 . H3712 H 0.8233 0.6329 0.2470 0.0425(9) 0.687(3) Uiso R . P . 1 . H3721 H 0.8924 0.5434 0.1724 0.0493(9) 0.313(3) Uiso R . P . 2 . H3722 H 0.8850 0.4407 0.2212 0.0493(9) 0.313(3) Uiso R . P . 2 . H3811 H 0.8116 0.3879 0.2220 0.0461(9) 0.687(3) Uiso R . P . 1 . H3812 H 0.6940 0.4030 0.1726 0.0461(9) 0.687(3) Uiso R . P . 1 . H3821 H 0.6984 0.5443 0.2376 0.0438(9) 0.313(3) Uiso R . P . 2 . H3822 H 0.6607 0.4009 0.1721 0.0438(9) 0.313(3) Uiso R . P . 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 Co1 0.01531(5) 0.01606(5) 0.01537(5) 0.00742(4) 0.00532(4) 0.00552(4) N2 0.0333(5) 0.0226(4) 0.0137(3) 0.0070(3) 0.0046(3) -0.0023(4) N5 0.0156(3) 0.0357(5) 0.0190(3) 0.0152(3) 0.0059(3) 0.0113(3) N28 0.0177(4) 0.0355(5) 0.0384(5) 0.0238(4) 0.0019(4) 0.0029(4) N29 0.0173(3) 0.0228(4) 0.0381(5) 0.0128(4) 0.0124(3) 0.0077(3) O3 0.0195(3) 0.0184(3) 0.0166(3) 0.0076(2) 0.0040(2) 0.0020(2) O4 0.0143(3) 0.0244(3) 0.0198(3) 0.0107(3) 0.0060(2) 0.0055(2) O30 0.0240(4) 0.0488(6) 0.0427(5) 0.0244(5) 0.0173(4) 0.0077(4) O31 0.0189(3) 0.0283(4) 0.0412(5) 0.0054(4) 0.0077(3) 0.0036(3) O32 0.0255(4) 0.0627(7) 0.0440(6) 0.0326(6) -0.0087(4) -0.0092(5) O33 0.0231(4) 0.0540(6) 0.0439(5) 0.0308(5) 0.0108(4) 0.0049(4) O100 0.0200(3) 0.0210(3) 0.0329(4) 0.0089(3) 0.0085(3) 0.0103(3) C6 0.0339(6) 0.0261(5) 0.0156(4) 0.0069(4) 0.0014(4) -0.0064(4) C7 0.0171(4) 0.0358(5) 0.0217(4) 0.0167(4) 0.0079(3) 0.0119(4) C8 0.0228(4) 0.0194(4) 0.0170(4) 0.0084(3) 0.0025(3) 0.0013(3) C9 0.0230(4) 0.0234(4) 0.0222(4) 0.0118(4) 0.0000(3) 0.0004(4) C10 0.0163(4) 0.0245(4) 0.0272(5) 0.0153(4) 0.0038(3) 0.0038(3) C11 0.0181(4) 0.0254(4) 0.0233(4) 0.0143(3) 0.0063(3) 0.0087(3) C12 0.0180(4) 0.0210(4) 0.0178(4) 0.0103(3) 0.0050(3) 0.0078(3) C13 0.0179(4) 0.0169(3) 0.0170(3) 0.0079(3) 0.0041(3) 0.0054(3) C14 0.0153(3) 0.0228(4) 0.0226(4) 0.0118(3) 0.0082(3) 0.0090(3) C15 0.0147(3) 0.0200(4) 0.0208(4) 0.0098(3) 0.0067(3) 0.0083(3) C16 0.0144(3) 0.0195(4) 0.0231(4) 0.0075(3) 0.0068(3) 0.0079(3) C17 0.0161(4) 0.0192(4) 0.0271(4) 0.0074(3) 0.0075(3) 0.0070(3) C18 0.0150(4) 0.0203(4) 0.0315(5) 0.0114(4) 0.0106(3) 0.0070(3) C19 0.0176(4) 0.0235(4) 0.0281(4) 0.0141(4) 0.0112(3) 0.0097(3) C20 0.0234(4) 0.0286(5) 0.0181(4) 0.0117(4) 0.0037(3) 0.0057(4) C21 0.0162(4) 0.0237(4) 0.0217(4) 0.0065(3) 0.0056(3) 0.0069(3) C22 0.0235(5) 0.0403(6) 0.0281(5) 0.0075(4) 0.0100(4) 0.0180(5) C23 0.0234(5) 0.0287(5) 0.0261(5) 0.0018(4) 0.0057(4) 0.0071(4) C24 0.0280(5) 0.0288(5) 0.0250(5) 0.0115(4) 0.0042(4) 0.0068(4) C25 0.0241(5) 0.0276(5) 0.0381(6) 0.0146(5) -0.0057(4) 0.0058(4) C26 0.0489(8) 0.0334(6) 0.0255(5) 0.0000(5) 0.0030(5) 0.0192(6) C27 0.0362(7) 0.0713(11) 0.0236(5) 0.0266(7) 0.0020(5) 0.0003(7) C36 0.0258(5) 0.0481(7) 0.0218(4) 0.0207(5) 0.0105(4) 0.0176(5) C39 0.0364(6) 0.0285(5) 0.0162(4) 0.0081(4) 0.0031(4) 0.0056(4) C101 0.023(2) 0.020(2) 0.043(2) 0.0080(15) -0.0037(16) 0.0137(18) C102 0.0415(15) 0.0364(15) 0.060(3) -0.0145(16) -0.0147(16) 0.0263(13) C103 0.0538(9) 0.0560(9) 0.0440(8) 0.0162(7) 0.0153(7) 0.0432(8) C104 0.0269(19) 0.040(2) 0.056(3) 0.029(2) 0.0230(17) 0.0237(17) C105 0.029(3) 0.019(3) 0.077(6) 0.021(3) 0.008(3) 0.002(2) C106 0.049(2) 0.0283(14) 0.061(3) 0.0163(17) 0.017(2) 0.0253(14) C108 0.0227(19) 0.030(2) 0.044(2) 0.0177(17) 0.0155(16) 0.0142(15) C341 0.0217(6) 0.0206(6) 0.0147(5) 0.0072(4) 0.0052(4) 0.0100(5) C342 0.0149(11) 0.0243(13) 0.0130(10) 0.0094(9) 0.0048(8) 0.0100(10) C351 0.0168(5) 0.0221(7) 0.0168(5) 0.0099(5) 0.0039(4) 0.0080(5) C352 0.0200(12) 0.0204(14) 0.0150(11) 0.0087(10) 0.0057(9) 0.0103(11) C371 0.0283(8) 0.0401(10) 0.0193(6) 0.0165(7) 0.0067(5) 0.0152(7) C372 0.0248(16) 0.047(3) 0.0187(14) 0.0139(16) 0.0066(12) 0.0144(17) C381 0.0362(9) 0.0376(9) 0.0152(6) 0.0081(6) 0.0040(6) 0.0159(8) C382 0.0217(15) 0.045(2) 0.0167(13) 0.0138(13) 0.0055(11) 0.0137(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . N2 . 1.8736(10) yes Co1 . N5 . 1.8763(8) yes Co1 . O3 . 1.8947(7) yes Co1 . O4 . 1.9015(7) yes Co1 . O100 . 2.2106(8) yes N2 . C6 . 1.2877(15) yes N2 . C341 . 1.5030(16) yes N5 . C7 . 1.2915(13) yes N5 . C351 . 1.4558(16) yes N28 . O32 . 1.2324(15) yes N28 . O33 . 1.2269(15) yes N28 . C10 . 1.4479(14) yes N29 . O30 . 1.2324(14) yes N29 . O31 . 1.2289(15) yes N29 . C18 . 1.4501(13) yes O3 . C13 . 1.2913(11) yes O4 . C15 . 1.2958(11) yes O100 . C101 . 1.432(8) yes O100 . C104 . 1.460(5) yes C6 . C8 . 1.4393(15) yes C6 . H61 . 0.954 no C7 . C14 . 1.4378(15) yes C7 . H71 . 0.954 no C8 . C9 . 1.3994(15) yes C8 . C13 . 1.4364(14) yes C9 . C10 . 1.3664(15) yes C9 . H91 . 0.954 no C10 . C11 . 1.4029(15) yes C11 . C12 . 1.3787(14) yes C11 . H111 . 0.953 no C12 . C13 . 1.4445(13) yes C12 . C20 . 1.5323(14) yes C14 . C15 . 1.4359(13) yes C14 . C19 . 1.4019(13) yes C15 . C16 . 1.4487(14) yes C16 . C17 . 1.3842(13) yes C16 . C21 . 1.5328(14) yes C17 . C18 . 1.4039(15) yes C17 . H171 . 0.956 no C18 . C19 . 1.3732(16) yes C19 . H191 . 0.953 no C20 . C25 . 1.5327(18) yes C20 . C26 . 1.5335(19) yes C20 . C27 . 1.5311(17) yes C21 . C22 . 1.5394(16) yes C21 . C23 . 1.5367(15) yes C21 . C24 . 1.5353(16) yes C22 . H221 . 0.950 no C22 . H222 . 0.953 no C22 . H223 . 0.952 no C23 . H231 . 0.952 no C23 . H232 . 0.952 no C23 . H233 . 0.953 no C24 . H241 . 0.952 no C24 . H242 . 0.955 no C24 . H243 . 0.952 no C25 . H251 . 0.950 no C25 . H252 . 0.953 no C25 . H253 . 0.955 no C26 . H261 . 0.953 no C26 . H262 . 0.954 no C26 . H263 . 0.953 no C27 . H271 . 0.950 no C27 . H272 . 0.959 no C27 . H273 . 0.950 no C36 . C351 . 1.5198(17) yes C36 . C371 . 1.489(2) yes C36 . H361 . 0.957 no C36 . H362 . 0.954 no C39 . C341 . 1.5769(19) yes C39 . C381 . 1.562(2) yes C39 . H391 . 0.960 no C39 . H392 . 0.955 no C101 . C102 . 1.675(10) yes C101 . H1011 . 0.947 no C101 . H1012 . 0.910 no C102 . C103 . 1.424(4) yes C102 . H1021 . 0.947 no C102 . H1022 . 0.965 no C103 . C104 . 1.562(5) yes C103 . H1031 . 0.956 no C103 . H1032 . 0.956 no C104 . H1041 . 0.968 no C104 . H1042 . 0.981 no C105 . C106 . 1.392(12) yes C105 . H1051 . 0.957 no C105 . H1052 . 1.079 no C106 . H1061 . 0.967 no C106 . H1062 . 0.946 no C108 . H1081 . 0.926 no C108 . H1082 . 0.982 no C341 . C351 . 1.521(2) yes C341 . H3411 . 0.956 no C342 . C352 . 1.524(4) yes C342 . H3421 . 0.954 no C351 . H3511 . 0.953 no C352 . H3521 . 0.952 no C371 . C381 . 1.524(3) yes C371 . H3711 . 0.954 no C371 . H3712 . 0.957 no C372 . C382 . 1.517(6) yes C372 . H3721 . 0.960 no C372 . H3722 . 0.948 no C381 . H3811 . 0.949 no C381 . H3812 . 0.956 no C382 . H3821 . 0.950 no C382 . H3822 . 0.969 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 . Co1 . N5 . 85.26(4) yes N2 . Co1 . O3 . 93.48(4) yes N5 . Co1 . O3 . 173.07(4) yes N2 . Co1 . O4 . 173.73(5) yes N5 . Co1 . O4 . 93.57(4) yes O3 . Co1 . O4 . 86.94(3) yes N2 . Co1 . O100 . 91.50(5) yes N5 . Co1 . O100 . 92.41(4) yes O3 . Co1 . O100 . 94.44(3) yes O4 . Co1 . O100 . 94.70(3) yes Co1 . N2 . C6 . 126.73(8) yes Co1 . N2 . C341 . 111.66(8) yes C6 . N2 . C341 . 121.17(10) yes Co1 . N5 . C7 . 127.26(8) yes Co1 . N5 . C351 . 112.18(7) yes C7 . N5 . C351 . 120.05(9) yes O32 . N28 . O33 . 122.77(11) yes O32 . N28 . C10 . 118.51(11) yes O33 . N28 . C10 . 118.72(11) yes O30 . N29 . O31 . 122.68(10) yes O30 . N29 . C18 . 118.62(10) yes O31 . N29 . C18 . 118.69(10) yes Co1 . O3 . C13 . 128.92(6) yes Co1 . O4 . C15 . 128.83(6) yes Co1 . O100 . C101 . 117.6(3) yes Co1 . O100 . C104 . 119.0(2) yes C101 . O100 . C104 . 115.7(4) yes N2 . C6 . C8 . 125.39(10) yes N2 . C6 . H61 . 117.4 no C8 . C6 . H61 . 117.2 no N5 . C7 . C14 . 124.66(9) yes N5 . C7 . H71 . 117.6 no C14 . C7 . H71 . 117.7 no C6 . C8 . C9 . 116.87(9) yes C6 . C8 . C13 . 122.21(9) yes C9 . C8 . C13 . 120.90(9) yes C8 . C9 . C10 . 119.21(10) yes C8 . C9 . H91 . 120.4 no C10 . C9 . H91 . 120.4 no N28 . C10 . C9 . 119.45(10) yes N28 . C10 . C11 . 119.06(10) yes C9 . C10 . C11 . 121.49(9) yes C10 . C11 . C12 . 121.58(9) yes C10 . C11 . H111 . 119.1 no C12 . C11 . H111 . 119.4 no C11 . C12 . C13 . 118.51(9) yes C11 . C12 . C20 . 120.74(9) yes C13 . C12 . C20 . 120.73(8) yes C12 . C13 . C8 . 118.18(8) yes C12 . C13 . O3 . 119.61(8) yes C8 . C13 . O3 . 122.21(8) yes C7 . C14 . C15 . 123.07(8) yes C7 . C14 . C19 . 115.80(9) yes C15 . C14 . C19 . 121.04(9) yes C14 . C15 . O4 . 122.03(9) yes C14 . C15 . C16 . 118.36(8) yes O4 . C15 . C16 . 119.61(8) yes C15 . C16 . C17 . 118.18(9) yes C15 . C16 . C21 . 121.09(8) yes C17 . C16 . C21 . 120.65(9) yes C16 . C17 . C18 . 121.49(10) yes C16 . C17 . H171 . 119.2 no C18 . C17 . H171 . 119.3 no N29 . C18 . C17 . 118.98(10) yes N29 . C18 . C19 . 119.21(9) yes C17 . C18 . C19 . 121.76(9) yes C14 . C19 . C18 . 118.80(9) yes C14 . C19 . H191 . 120.7 no C18 . C19 . H191 . 120.5 no C12 . C20 . C25 . 110.98(10) yes C12 . C20 . C26 . 109.59(10) yes C25 . C20 . C26 . 109.40(10) yes C12 . C20 . C27 . 111.29(10) yes C25 . C20 . C27 . 106.87(12) yes C26 . C20 . C27 . 108.65(13) yes C16 . C21 . C22 . 109.75(9) yes C16 . C21 . C23 . 111.70(8) yes C22 . C21 . C23 . 106.63(9) yes C16 . C21 . C24 . 111.08(9) yes C22 . C21 . C24 . 109.47(9) yes C23 . C21 . C24 . 108.10(10) yes C21 . C22 . H221 . 110.1 no C21 . C22 . H222 . 109.6 no H221 . C22 . H222 . 109.2 no C21 . C22 . H223 . 109.7 no H221 . C22 . H223 . 109.3 no H222 . C22 . H223 . 109.0 no C21 . C23 . H231 . 110.0 no C21 . C23 . H232 . 109.9 no H231 . C23 . H232 . 109.1 no C21 . C23 . H233 . 109.7 no H231 . C23 . H233 . 109.1 no H232 . C23 . H233 . 109.1 no C21 . C24 . H241 . 110.1 no C21 . C24 . H242 . 109.9 no H241 . C24 . H242 . 108.8 no C21 . C24 . H243 . 110.0 no H241 . C24 . H243 . 109.1 no H242 . C24 . H243 . 108.8 no C20 . C25 . H251 . 110.1 no C20 . C25 . H252 . 110.0 no H251 . C25 . H252 . 109.2 no C20 . C25 . H253 . 109.9 no H251 . C25 . H253 . 109.0 no H252 . C25 . H253 . 108.8 no C20 . C26 . H261 . 110.3 no C20 . C26 . H262 . 109.7 no H261 . C26 . H262 . 108.9 no C20 . C26 . H263 . 110.1 no H261 . C26 . H263 . 109.0 no H262 . C26 . H263 . 108.8 no C20 . C27 . H271 . 110.3 no C20 . C27 . H272 . 109.8 no H271 . C27 . H272 . 108.8 no C20 . C27 . H273 . 109.7 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 108.8 no C351 . C36 . C371 . 111.64(11) yes C351 . C36 . H361 . 108.9 no C371 . C36 . H361 . 109.6 no C351 . C36 . H362 . 109.3 no C371 . C36 . H362 . 108.8 no H361 . C36 . H362 . 108.6 no C341 . C39 . C381 . 104.83(12) yes C341 . C39 . H391 . 110.8 no C381 . C39 . H391 . 110.9 no C341 . C39 . H392 . 111.2 no C381 . C39 . H392 . 111.0 no H391 . C39 . H392 . 108.2 no O100 . C101 . C102 . 98.6(5) yes O100 . C101 . H1011 . 112.3 no C102 . C101 . H1011 . 108.6 no O100 . C101 . H1012 . 113.0 no C102 . C101 . H1012 . 110.0 no H1011 . C101 . H1012 . 113.3 no C101 . C102 . C103 . 103.3(3) yes C101 . C102 . H1021 . 111.6 no C103 . C102 . H1021 . 113.2 no C101 . C102 . H1022 . 108.9 no C103 . C102 . H1022 . 111.3 no H1021 . C102 . H1022 . 108.4 no C102 . C103 . C104 . 103.8(2) yes C102 . C103 . H1031 . 110.2 no C104 . C103 . H1031 . 111.4 no C102 . C103 . H1032 . 111.7 no C104 . C103 . H1032 . 111.2 no H1031 . C103 . H1032 . 108.5 no C103 . C104 . O100 . 101.7(3) yes C103 . C104 . H1041 . 114.1 no O100 . C104 . H1041 . 112.0 no C103 . C104 . H1042 . 112.8 no O100 . C104 . H1042 . 111.0 no H1041 . C104 . H1042 . 105.5 no O100 . C105 . C106 . 112.3(7) yes O100 . C105 . H1051 . 111.8 no C106 . C105 . H1051 . 115.1 no O100 . C105 . H1052 . 107.7 no C106 . C105 . H1052 . 109.8 no H1051 . C105 . H1052 . 99.2 no C103 . C106 . C105 . 101.7(4) yes C103 . C106 . H1061 . 110.4 no C105 . C106 . H1061 . 111.8 no C103 . C106 . H1062 . 111.6 no C105 . C106 . H1062 . 112.8 no H1061 . C106 . H1062 . 108.4 no C103 . C108 . O100 . 110.4(4) yes C103 . C108 . H1081 . 111.4 no O100 . C108 . H1081 . 111.7 no C103 . C108 . H1082 . 106.8 no O100 . C108 . H1082 . 107.4 no H1081 . C108 . H1082 . 108.8 no C39 . C341 . N2 . 112.87(11) yes C39 . C341 . C351 . 110.74(11) yes N2 . C341 . C351 . 104.94(11) yes C39 . C341 . H3411 . 109.4 no N2 . C341 . H3411 . 109.2 no C351 . C341 . H3411 . 109.5 no N2 . C342 . C39 . 115.8(2) yes N2 . C342 . C352 . 96.06(19) yes C39 . C342 . C352 . 104.8(2) yes N2 . C342 . H3421 . 113.1 no C39 . C342 . H3421 . 112.8 no C352 . C342 . H3421 . 112.8 no C341 . C351 . C36 . 108.88(12) yes C341 . C351 . N5 . 103.46(11) yes C36 . C351 . N5 . 118.81(11) yes C341 . C351 . H3511 . 108.3 no C36 . C351 . H3511 . 108.7 no N5 . C351 . H3511 . 108.3 no C342 . C352 . C36 . 112.9(2) yes C342 . C352 . N5 . 104.2(2) yes C36 . C352 . N5 . 108.2(2) yes C342 . C352 . H3521 . 110.6 no C36 . C352 . H3521 . 110.4 no N5 . C352 . H3521 . 110.4 no C36 . C371 . C381 . 110.04(15) yes C36 . C371 . H3711 . 109.9 no C381 . C371 . H3711 . 109.9 no C36 . C371 . H3712 . 109.1 no C381 . C371 . H3712 . 109.4 no H3711 . C371 . H3712 . 108.5 no C36 . C372 . C382 . 113.0(3) yes C36 . C372 . H3721 . 108.1 no C382 . C372 . H3721 . 107.4 no C36 . C372 . H3722 . 110.2 no C382 . C372 . H3722 . 109.2 no H3721 . C372 . H3722 . 108.8 no C371 . C381 . C39 . 112.57(14) yes C371 . C381 . H3811 . 108.9 no C39 . C381 . H3811 . 108.8 no C371 . C381 . H3812 . 108.7 no C39 . C381 . H3812 . 108.7 no H3811 . C381 . H3812 . 109.0 no C39 . C382 . C372 . 104.1(3) yes C39 . C382 . H3821 . 111.6 no C372 . C382 . H3821 . 113.1 no C39 . C382 . H3822 . 110.3 no C372 . C382 . H3822 . 109.8 no H3821 . C382 . H3822 . 107.9 no _iucr_refine_instruction_details_constraints ; # # Punched on 02/07/13 at 02:36:28 # #LIST 12 BLOCK SCALE X'S CO(1,U'S) UNTIL C(382) EQUIV H(61, U[ISO]) UNTIL H(3822) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) H ( 223,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) H ( 263,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) H ( 273,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S) RIDE C ( 101,X'S) H (1011,X'S) H (1012,X'S) RIDE C ( 102,X'S) H (1021,X'S) H (1022,X'S) RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) RIDE C ( 104,X'S) H (1041,X'S) H (1042,X'S) RIDE C ( 105,X'S) H (1051,X'S) H (1052,X'S) RIDE C ( 106,X'S) H (1061,X'S) H (1062,X'S) RIDE C ( 108,X'S) H (1081,X'S) H (1082,X'S) RIDE C ( 341,X'S) H (3411,X'S) RIDE C ( 342,X'S) H (3421,X'S) RIDE C ( 351,X'S) H (3511,X'S) RIDE C ( 352,X'S) H (3521,X'S) RIDE C ( 371,X'S) H (3711,X'S) H (3712,X'S) RIDE C ( 372,X'S) H (3721,X'S) H (3722,X'S) RIDE C ( 381,X'S) H (3811,X'S) H (3812,X'S) RIDE C ( 382,X'S) H (3821,X'S) H (3822,X'S) EQUIV PART(1,OCC) PART (2,OCC) WEIGHT -1 PART(2,OCC) EQUIV PART(3,OCC) PART (4,OCC) WEIGHT -1 PART(4,OCC) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 02/07/13 at 02:36:28 # #LIST 16 NO END ; _database_code_depnum_ccdc_archive 'CCDC 948259'