# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_1 _audit_creation_date 2012-11-28 _audit_creation_method CRYSTALS_ver_14.43 _oxford_structure_analysis_title 'sk_762_0m in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.0611(5) _cell_length_b 16.5349(7) _cell_length_c 22.6345(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4888.2(3) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall 'P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C45 H51 Cr1 N3 P3 # Dc = 1.06 Fooo = 1644.00 Mu = 3.62 M = 778.84 # Found Formula = C45 H51 Cr1 N3 P3 # Dc = 1.06 FOOO = 1644.00 Mu = 3.62 M = 778.84 _chemical_formula_sum 'C45 H51 Cr1 N3 P3' _chemical_formula_moiety 'C45 H51 Cr1 N3 P3' _chemical_compound_source ? _chemical_formula_weight 778.84 _cell_measurement_reflns_used 9416 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 120 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_max 0.450 _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 0.362 # Sheldrick geometric approximatio 0.91 0.97 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 11530 _reflns_number_total 11530 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections without Friedels Law is 11530 # Number of reflections with Friedels Law is 6490 # Theoretical number of reflections is about 5908 _diffrn_reflns_theta_min 1.799 _diffrn_reflns_theta_max 28.011 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.011 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.40 _refine_diff_density_max 0.40 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 11530 _refine_ls_number_restraints 0 _refine_ls_number_parameters 469 _oxford_refine_ls_R_factor_ref 0.0513 _refine_ls_wR_factor_ref 0.0874 _refine_ls_goodness_of_fit_ref 0.9617 _refine_ls_shift/su_max 0.0037453 _refine_ls_shift/su_mean 0.0008402 # The values computed with all filters except I/sigma _oxford_reflns_number_all 11530 _refine_ls_R_factor_all 0.0513 _refine_ls_wR_factor_all 0.0874 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9556 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_gt 0.0841 _refine_ls_abs_structure_Flack 0.019(2) _refine_ls_abs_structure_details 'Flack (1983), 5040 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.40P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Cr1 Cr 0.69406(2) 0.316347(19) 0.676393(14) 0.0147 1.0000 Uani . . . . . . P1 P 0.54997(4) 0.24405(3) 0.60381(2) 0.0182 1.0000 Uani . . . . . . P2 P 0.78760(4) 0.40343(3) 0.58554(2) 0.0174 1.0000 Uani . . . . . . P3 P 0.82862(4) 0.19539(3) 0.67516(3) 0.0168 1.0000 Uani . . . . . . N1 N 0.55896(12) 0.27820(10) 0.67389(8) 0.0172 1.0000 Uani . . . . . . N2 N 0.72187(14) 0.42104(10) 0.64847(8) 0.0177 1.0000 Uani . . . . . . N3 N 0.78785(13) 0.26245(10) 0.72576(7) 0.0174 1.0000 Uani . . . . . . C1 C 0.47624(16) 0.27152(13) 0.71829(9) 0.0202 1.0000 Uani . . . . . . C2 C 0.4848(2) 0.19419(15) 0.75397(10) 0.0301 1.0000 Uani . . . . . . C3 C 0.47686(19) 0.34411(14) 0.75920(11) 0.0275 1.0000 Uani . . . . . . C4 C 0.50529(17) 0.13848(13) 0.60829(9) 0.0200 1.0000 Uani . . . . . . C5 C 0.40290(18) 0.11420(13) 0.60938(9) 0.0210 1.0000 Uani . . . . . . C6 C 0.3780(2) 0.03303(15) 0.61476(10) 0.0273 1.0000 Uani . . . . . . C7 C 0.4540(2) -0.02476(15) 0.61966(10) 0.0300 1.0000 Uani . . . . . . C8 C 0.5561(2) -0.00118(15) 0.61952(10) 0.0314 1.0000 Uani . . . . . . C9 C 0.58147(18) 0.07935(14) 0.61320(9) 0.0247 1.0000 Uani . . . . . . C10 C 0.43912(16) 0.29498(13) 0.57171(9) 0.0196 1.0000 Uani . . . . . . C11 C 0.40552(19) 0.36958(14) 0.59351(10) 0.0261 1.0000 Uani . . . . . . C12 C 0.3285(2) 0.41225(16) 0.56574(11) 0.0342 1.0000 Uani . . . . . . C13 C 0.2829(2) 0.38166(16) 0.51548(11) 0.0315 1.0000 Uani . . . . . . C14 C 0.31439(19) 0.30830(15) 0.49314(10) 0.0277 1.0000 Uani . . . . . . C15 C 0.39272(18) 0.26593(15) 0.52042(10) 0.0254 1.0000 Uani . . . . . . C16 C 0.69149(17) 0.50312(12) 0.66765(9) 0.0196 1.0000 Uani . . . . . . C17 C 0.58317(18) 0.52430(15) 0.64693(11) 0.0270 1.0000 Uani . . . . . . C18 C 0.6990(2) 0.50972(14) 0.73500(10) 0.0262 1.0000 Uani . . . . . . C19 C 0.71800(17) 0.45356(13) 0.52539(9) 0.0190 1.0000 Uani . . . . . . C20 C 0.72020(19) 0.53669(14) 0.51393(10) 0.0240 1.0000 Uani . . . . . . C21 C 0.65991(19) 0.56929(15) 0.46997(11) 0.0301 1.0000 Uani . . . . . . C22 C 0.5965(2) 0.52073(17) 0.43657(11) 0.0359 1.0000 Uani . . . . . . C23 C 0.5940(2) 0.43838(17) 0.44695(11) 0.0358 1.0000 Uani . . . . . . C24 C 0.65462(19) 0.40523(15) 0.49093(10) 0.0259 1.0000 Uani . . . . . . C25 C 0.90346(16) 0.46539(13) 0.59190(10) 0.0193 1.0000 Uani . . . . . . C26 C 0.94458(18) 0.48306(14) 0.64731(10) 0.0232 1.0000 Uani . . . . . . C27 C 1.03663(18) 0.52420(16) 0.65283(11) 0.0303 1.0000 Uani . . . . . . C28 C 1.08990(19) 0.54747(16) 0.60249(12) 0.0343 1.0000 Uani . . . . . . C29 C 1.0515(2) 0.52944(17) 0.54743(11) 0.0358 1.0000 Uani . . . . . . C30 C 0.95850(19) 0.48814(15) 0.54214(10) 0.0290 1.0000 Uani . . . . . . C31 C 0.83385(17) 0.27127(14) 0.78526(9) 0.0230 1.0000 Uani . . . . . . C32 C 0.91684(18) 0.33611(15) 0.78587(11) 0.0287 1.0000 Uani . . . . . . C33 C 0.75189(19) 0.29096(18) 0.83054(10) 0.0363 1.0000 Uani . . . . . . C34 C 0.96760(15) 0.20682(12) 0.66920(9) 0.0184 1.0000 Uani . . . . . . C35 C 1.04033(19) 0.16922(15) 0.70477(11) 0.0317 1.0000 Uani . . . . . . C36 C 1.14377(19) 0.18889(18) 0.69797(13) 0.0404 1.0000 Uani . . . . . . C37 C 1.17410(19) 0.24557(16) 0.65753(13) 0.0389 1.0000 Uani . . . . . . C38 C 1.1031(2) 0.28376(16) 0.62224(13) 0.0364 1.0000 Uani . . . . . . C39 C 1.00083(18) 0.26356(15) 0.62816(10) 0.0259 1.0000 Uani . . . . . . C40 C 0.81360(17) 0.09458(13) 0.70723(10) 0.0208 1.0000 Uani . . . . . . C41 C 0.74472(18) 0.08056(15) 0.75313(11) 0.0268 1.0000 Uani . . . . . . C42 C 0.7255(2) 0.00210(17) 0.77241(13) 0.0388 1.0000 Uani . . . . . . C43 C 0.7744(2) -0.06274(17) 0.74592(15) 0.0470 1.0000 Uani . . . . . . C44 C 0.8406(2) -0.04954(15) 0.69989(15) 0.0436 1.0000 Uani . . . . . . C45 C 0.86009(19) 0.02898(15) 0.68036(13) 0.0346 1.0000 Uani . . . . . . H11 H 0.4100 0.2700 0.6965 0.0265 1.0000 Uiso R . . . . . H21 H 0.4299 0.1909 0.7829 0.0449 1.0000 Uiso R . . . . . H22 H 0.5526 0.1927 0.7729 0.0447 1.0000 Uiso R . . . . . H23 H 0.4818 0.1472 0.7283 0.0442 1.0000 Uiso R . . . . . H31 H 0.4211 0.3392 0.7851 0.0408 1.0000 Uiso R . . . . . H32 H 0.5388 0.3490 0.7806 0.0402 1.0000 Uiso R . . . . . H33 H 0.4683 0.3920 0.7360 0.0402 1.0000 Uiso R . . . . . H51 H 0.3504 0.1530 0.6054 0.0242 1.0000 Uiso R . . . . . H61 H 0.3085 0.0150 0.6150 0.0333 1.0000 Uiso R . . . . . H71 H 0.4374 -0.0781 0.6230 0.0353 1.0000 Uiso R . . . . . H81 H 0.6068 -0.0391 0.6222 0.0362 1.0000 Uiso R . . . . . H91 H 0.6497 0.0985 0.6115 0.0310 1.0000 Uiso R . . . . . H111 H 0.4341 0.3875 0.6288 0.0317 1.0000 Uiso R . . . . . H121 H 0.3082 0.4649 0.5816 0.0425 1.0000 Uiso R . . . . . H131 H 0.2302 0.4068 0.4966 0.0374 1.0000 Uiso R . . . . . H141 H 0.2870 0.2882 0.4592 0.0323 1.0000 Uiso R . . . . . H151 H 0.4140 0.2153 0.5056 0.0306 1.0000 Uiso R . . . . . H161 H 0.7408 0.5433 0.6504 0.0232 1.0000 Uiso R . . . . . H171 H 0.5722 0.5139 0.6048 0.0398 1.0000 Uiso R . . . . . H172 H 0.5353 0.4945 0.6692 0.0404 1.0000 Uiso R . . . . . H173 H 0.5702 0.5798 0.6537 0.0393 1.0000 Uiso R . . . . . H181 H 0.7653 0.4987 0.7478 0.0377 1.0000 Uiso R . . . . . H182 H 0.6532 0.4713 0.7513 0.0376 1.0000 Uiso R . . . . . H183 H 0.6794 0.5617 0.7474 0.0370 1.0000 Uiso R . . . . . H201 H 0.7639 0.5686 0.5360 0.0272 1.0000 Uiso R . . . . . H211 H 0.6609 0.6247 0.4642 0.0377 1.0000 Uiso R . . . . . H221 H 0.5565 0.5437 0.4066 0.0427 1.0000 Uiso R . . . . . H231 H 0.5537 0.4041 0.4248 0.0435 1.0000 Uiso R . . . . . H241 H 0.6525 0.3487 0.4981 0.0316 1.0000 Uiso R . . . . . H261 H 0.9092 0.4699 0.6815 0.0267 1.0000 Uiso R . . . . . H271 H 1.0613 0.5356 0.6896 0.0352 1.0000 Uiso R . . . . . H281 H 1.1513 0.5739 0.6072 0.0425 1.0000 Uiso R . . . . . H291 H 1.0898 0.5445 0.5139 0.0433 1.0000 Uiso R . . . . . H301 H 0.9313 0.4801 0.5045 0.0343 1.0000 Uiso R . . . . . H311 H 0.8642 0.2167 0.7962 0.0286 1.0000 Uiso R . . . . . H321 H 0.8853 0.3862 0.7758 0.0405 1.0000 Uiso R . . . . . H322 H 0.9460 0.3416 0.8258 0.0408 1.0000 Uiso R . . . . . H323 H 0.9701 0.3233 0.7572 0.0406 1.0000 Uiso R . . . . . H331 H 0.7185 0.3424 0.8201 0.0539 1.0000 Uiso R . . . . . H332 H 0.7828 0.2951 0.8699 0.0543 1.0000 Uiso R . . . . . H333 H 0.7025 0.2466 0.8301 0.0542 1.0000 Uiso R . . . . . H351 H 1.0202 0.1312 0.7334 0.0382 1.0000 Uiso R . . . . . H361 H 1.1913 0.1627 0.7214 0.0484 1.0000 Uiso R . . . . . H371 H 1.2432 0.2558 0.6525 0.0479 1.0000 Uiso R . . . . . H381 H 1.1233 0.3242 0.5957 0.0451 1.0000 Uiso R . . . . . H391 H 0.9532 0.2889 0.6045 0.0327 1.0000 Uiso R . . . . . H411 H 0.7094 0.1264 0.7704 0.0330 1.0000 Uiso R . . . . . H421 H 0.6792 -0.0051 0.8033 0.0450 1.0000 Uiso R . . . . . H431 H 0.7639 -0.1164 0.7605 0.0557 1.0000 Uiso R . . . . . H441 H 0.8740 -0.0919 0.6803 0.0515 1.0000 Uiso R . . . . . H451 H 0.9055 0.0360 0.6492 0.0401 1.0000 Uiso R . . . . . 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 Cr1 0.01218(15) 0.01550(15) 0.01632(16) 0.00040(15) -0.00123(14) -0.00120(13) P1 0.0147(3) 0.0220(3) 0.0180(3) -0.0018(2) -0.0004(2) -0.0029(2) P2 0.0189(3) 0.0169(3) 0.0163(3) -0.0007(2) -0.0010(2) -0.0002(2) P3 0.0139(3) 0.0187(3) 0.0177(2) 0.0016(2) -0.0005(2) 0.0011(2) N1 0.0120(8) 0.0208(8) 0.0188(8) -0.0029(8) -0.0023(8) -0.0018(7) N2 0.0199(9) 0.0153(9) 0.0179(9) -0.0031(7) 0.0016(7) -0.0001(8) N3 0.0151(9) 0.0198(9) 0.0172(9) -0.0005(7) -0.0015(7) 0.0013(8) C1 0.0148(10) 0.0264(12) 0.0192(11) 0.0000(10) 0.0009(9) -0.0043(9) C2 0.0351(14) 0.0323(14) 0.0231(12) 0.0002(11) 0.0038(10) -0.0074(12) C3 0.0245(13) 0.0310(13) 0.0269(13) -0.0031(11) 0.0049(10) 0.0008(10) C4 0.0237(11) 0.0213(11) 0.0151(11) -0.0042(9) -0.0004(9) -0.0015(10) C5 0.0225(11) 0.0235(12) 0.0168(11) -0.0033(10) -0.0001(9) -0.0031(10) C6 0.0316(13) 0.0346(14) 0.0157(11) -0.0006(11) 0.0009(10) -0.0102(12) C7 0.0478(16) 0.0225(12) 0.0198(12) 0.0038(10) -0.0026(11) -0.0089(12) C8 0.0395(15) 0.0318(14) 0.0229(12) 0.0045(11) -0.0055(11) 0.0072(12) C9 0.0241(12) 0.0312(13) 0.0188(11) -0.0019(10) -0.0029(9) 0.0006(10) C10 0.0167(10) 0.0259(12) 0.0161(10) 0.0011(9) -0.0004(8) -0.0058(9) C11 0.0291(13) 0.0253(12) 0.0237(12) -0.0049(10) -0.0091(10) -0.0012(10) C12 0.0402(15) 0.0288(13) 0.0335(14) -0.0047(12) -0.0074(12) 0.0090(12) C13 0.0289(14) 0.0410(15) 0.0247(12) 0.0042(12) -0.0060(11) 0.0056(12) C14 0.0287(13) 0.0369(13) 0.0174(10) 0.0016(11) -0.0056(10) -0.0047(12) C15 0.0289(13) 0.0280(13) 0.0193(11) -0.0042(10) 0.0006(10) -0.0010(11) C16 0.0219(11) 0.0155(9) 0.0215(11) -0.0025(9) 0.0007(10) -0.0011(9) C17 0.0246(12) 0.0262(13) 0.0303(13) -0.0075(11) -0.0017(10) 0.0063(10) C18 0.0303(13) 0.0234(11) 0.0249(12) -0.0071(10) 0.0006(11) 0.0021(11) C19 0.0195(11) 0.0222(11) 0.0151(10) -0.0019(9) 0.0023(9) 0.0009(9) C20 0.0283(13) 0.0229(11) 0.0207(11) -0.0009(10) -0.0016(10) -0.0017(10) C21 0.0343(14) 0.0270(13) 0.0290(13) 0.0094(11) -0.0021(11) 0.0003(11) C22 0.0357(15) 0.0410(16) 0.0309(14) 0.0098(13) -0.0138(12) 0.0006(13) C23 0.0371(15) 0.0380(15) 0.0323(14) 0.0043(12) -0.0176(12) -0.0066(12) C24 0.0296(13) 0.0234(12) 0.0248(12) 0.0012(11) -0.0023(10) -0.0026(11) C25 0.0170(10) 0.0187(10) 0.0221(11) -0.0001(10) -0.0008(9) -0.0012(9) C26 0.0201(11) 0.0312(13) 0.0183(11) -0.0025(10) -0.0014(9) 0.0007(10) C27 0.0224(12) 0.0419(15) 0.0268(12) -0.0092(12) -0.0049(10) -0.0009(11) C28 0.0199(12) 0.0458(16) 0.0373(14) -0.0022(13) -0.0023(11) -0.0088(12) C29 0.0274(13) 0.0507(17) 0.0293(13) 0.0040(13) 0.0076(11) -0.0101(13) C30 0.0260(13) 0.0416(15) 0.0192(11) -0.0005(11) 0.0001(10) -0.0069(12) C31 0.0221(11) 0.0286(12) 0.0182(11) 0.0001(10) -0.0059(9) -0.0001(10) C32 0.0247(13) 0.0323(14) 0.0291(13) -0.0044(11) -0.0073(10) -0.0025(11) C33 0.0319(13) 0.0590(17) 0.0179(12) -0.0085(13) -0.0004(10) -0.0085(12) C34 0.0149(10) 0.0195(10) 0.0209(11) -0.0032(9) -0.0004(9) 0.0016(8) C35 0.0274(13) 0.0271(13) 0.0408(15) -0.0006(12) -0.0056(12) 0.0049(11) C36 0.0218(13) 0.0387(15) 0.0607(18) -0.0053(15) -0.0132(12) 0.0100(13) C37 0.0158(11) 0.0335(14) 0.0675(19) -0.0147(15) 0.0040(12) -0.0005(11) C38 0.0284(14) 0.0307(14) 0.0500(17) -0.0026(13) 0.0153(13) -0.0044(12) C39 0.0211(11) 0.0279(13) 0.0288(13) -0.0012(11) 0.0030(10) 0.0018(10) C40 0.0171(10) 0.0190(10) 0.0264(11) 0.0073(9) -0.0046(9) -0.0023(10) C41 0.0220(12) 0.0305(13) 0.0278(13) 0.0080(11) -0.0051(10) -0.0041(10) C42 0.0296(14) 0.0436(16) 0.0433(16) 0.0172(14) -0.0073(12) -0.0161(13) C43 0.0343(16) 0.0281(14) 0.079(2) 0.0235(16) -0.0220(16) -0.0103(12) C44 0.0303(14) 0.0190(12) 0.082(2) -0.0011(14) -0.0110(15) 0.0030(11) C45 0.0258(13) 0.0271(13) 0.0509(16) -0.0019(14) 0.0023(13) 0.0033(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.100594(16) 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 Cr1 . P1 . 2.7695(6) yes Cr1 . P2 . 2.7919(6) yes Cr1 . P3 . 2.6626(6) yes Cr1 . N1 . 1.8748(16) yes Cr1 . N2 . 1.8782(17) yes Cr1 . N3 . 1.8824(17) yes P1 . N1 . 1.6879(18) yes P1 . C4 . 1.843(2) yes P1 . C10 . 1.826(2) yes P2 . N2 . 1.6885(18) yes P2 . C19 . 1.835(2) yes P2 . C25 . 1.833(2) yes P3 . N3 . 1.6807(18) yes P3 . C34 . 1.830(2) yes P3 . C40 . 1.829(2) yes N1 . C1 . 1.480(3) yes N2 . C16 . 1.479(3) yes N3 . C31 . 1.482(3) yes C1 . C2 . 1.517(3) yes C1 . C3 . 1.516(3) yes C1 . H11 . 0.996 no C2 . H21 . 0.973 no C2 . H22 . 0.983 no C2 . H23 . 0.972 no C3 . H31 . 0.939 no C3 . H32 . 0.946 no C3 . H33 . 0.956 no C4 . C5 . 1.397(3) yes C4 . C9 . 1.399(3) yes C5 . C6 . 1.386(3) yes C5 . H51 . 0.943 no C6 . C7 . 1.382(4) yes C6 . H61 . 0.956 no C7 . C8 . 1.390(4) yes C7 . H71 . 0.911 no C8 . C9 . 1.379(3) yes C8 . H81 . 0.913 no C9 . H91 . 0.947 no C10 . C11 . 1.399(3) yes C10 . C15 . 1.395(3) yes C11 . C12 . 1.380(3) yes C11 . H111 . 0.930 no C12 . C13 . 1.380(3) yes C12 . H121 . 0.978 no C13 . C14 . 1.377(3) yes C13 . H131 . 0.910 no C14 . C15 . 1.385(3) yes C14 . H141 . 0.910 no C15 . H151 . 0.943 no C16 . C17 . 1.531(3) yes C16 . C18 . 1.531(3) yes C16 . H161 . 1.005 no C17 . H171 . 0.979 no C17 . H172 . 0.941 no C17 . H173 . 0.946 no C18 . H181 . 0.931 no C18 . H182 . 0.947 no C18 . H183 . 0.940 no C19 . C20 . 1.399(3) yes C19 . C24 . 1.390(3) yes C20 . C21 . 1.378(3) yes C20 . H201 . 0.924 no C21 . C22 . 1.379(3) yes C21 . H211 . 0.925 no C22 . C23 . 1.382(4) yes C22 . H221 . 0.937 no C23 . C24 . 1.385(3) yes C23 . H231 . 0.922 no C24 . H241 . 0.950 no C25 . C26 . 1.395(3) yes C25 . C30 . 1.388(3) yes C26 . C27 . 1.387(3) yes C26 . H261 . 0.928 no C27 . C28 . 1.389(3) yes C27 . H271 . 0.911 no C28 . C29 . 1.376(4) yes C28 . H281 . 0.920 no C29 . C30 . 1.399(3) yes C29 . H291 . 0.943 no C30 . H301 . 0.933 no C31 . C32 . 1.525(3) yes C31 . C33 . 1.517(3) yes C31 . H311 . 1.016 no C32 . H321 . 0.953 no C32 . H322 . 0.986 no C32 . H323 . 0.975 no C33 . H331 . 0.985 no C33 . H332 . 0.980 no C33 . H333 . 0.977 no C34 . C35 . 1.392(3) yes C34 . C39 . 1.390(3) yes C35 . C36 . 1.398(4) yes C35 . H351 . 0.940 no C36 . C37 . 1.369(4) yes C36 . H361 . 0.925 no C37 . C38 . 1.377(4) yes C37 . H371 . 0.925 no C38 . C39 . 1.383(3) yes C38 . H381 . 0.937 no C39 . H391 . 0.922 no C40 . C41 . 1.394(3) yes C40 . C45 . 1.384(3) yes C41 . C42 . 1.392(3) yes C41 . H411 . 0.969 no C42 . C43 . 1.384(4) yes C42 . H421 . 0.932 no C43 . C44 . 1.372(4) yes C43 . H431 . 0.957 no C44 . C45 . 1.395(4) yes C44 . H441 . 0.937 no C45 . H451 . 0.929 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 P1 . Cr1 . P2 . 94.764(19) yes P1 . Cr1 . P3 . 96.78(2) yes P2 . Cr1 . P3 . 95.214(19) yes P1 . Cr1 . N1 . 36.61(5) yes P2 . Cr1 . N1 . 124.28(6) yes P3 . Cr1 . N1 . 111.61(5) yes P1 . Cr1 . N2 . 109.25(6) yes P2 . Cr1 . N2 . 36.12(5) yes P3 . Cr1 . N2 . 124.13(6) yes N1 . Cr1 . N2 . 118.81(8) yes P1 . Cr1 . N3 . 126.16(6) yes P2 . Cr1 . N3 . 113.37(6) yes P3 . Cr1 . N3 . 38.84(5) yes N1 . Cr1 . N3 . 118.11(8) yes N2 . Cr1 . N3 . 120.68(8) yes Cr1 . P1 . C4 . 126.25(7) yes N1 . P1 . C4 . 106.68(9) yes Cr1 . P1 . C10 . 125.16(7) yes N1 . P1 . C10 . 105.95(9) yes C4 . P1 . C10 . 101.98(10) yes Cr1 . P2 . C19 . 124.24(7) yes N2 . P2 . C19 . 107.23(9) yes Cr1 . P2 . C25 . 126.28(7) yes N2 . P2 . C25 . 104.91(10) yes C19 . P2 . C25 . 102.40(10) yes Cr1 . P3 . C34 . 125.31(7) yes N3 . P3 . C34 . 107.24(9) yes Cr1 . P3 . C40 . 127.57(7) yes N3 . P3 . C40 . 107.27(10) yes C34 . P3 . C40 . 103.28(10) yes P1 . N1 . Cr1 . 101.91(9) yes P1 . N1 . C1 . 124.23(13) yes Cr1 . N1 . C1 . 133.78(14) yes P2 . N2 . Cr1 . 102.90(9) yes P2 . N2 . C16 . 122.83(14) yes Cr1 . N2 . C16 . 134.03(14) yes P3 . N3 . Cr1 . 96.54(8) yes P3 . N3 . C31 . 123.76(14) yes Cr1 . N3 . C31 . 139.18(15) yes N1 . C1 . C2 . 111.75(18) yes N1 . C1 . C3 . 110.60(17) yes C2 . C1 . C3 . 109.99(18) yes N1 . C1 . H11 . 107.5 no C2 . C1 . H11 . 107.8 no C3 . C1 . H11 . 109.1 no C1 . C2 . H21 . 110.6 no C1 . C2 . H22 . 108.6 no H21 . C2 . H22 . 111.7 no C1 . C2 . H23 . 110.6 no H21 . C2 . H23 . 109.1 no H22 . C2 . H23 . 106.1 no C1 . C3 . H31 . 108.0 no C1 . C3 . H32 . 112.7 no H31 . C3 . H32 . 110.5 no C1 . C3 . H33 . 108.7 no H31 . C3 . H33 . 108.9 no H32 . C3 . H33 . 108.0 no P1 . C4 . C5 . 125.20(17) yes P1 . C4 . C9 . 116.16(17) yes C5 . C4 . C9 . 118.6(2) yes C4 . C5 . C6 . 120.3(2) yes C4 . C5 . H51 . 119.9 no C6 . C5 . H51 . 119.8 no C5 . C6 . C7 . 120.6(2) yes C5 . C6 . H61 . 121.6 no C7 . C6 . H61 . 117.8 no C6 . C7 . C8 . 119.7(2) yes C6 . C7 . H71 . 120.3 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 120.1(2) yes C7 . C8 . H81 . 120.2 no C9 . C8 . H81 . 119.7 no C4 . C9 . C8 . 120.8(2) yes C4 . C9 . H91 . 115.6 no C8 . C9 . H91 . 123.6 no P1 . C10 . C11 . 121.00(16) yes P1 . C10 . C15 . 121.13(17) yes C11 . C10 . C15 . 117.4(2) yes C10 . C11 . C12 . 121.2(2) yes C10 . C11 . H111 . 117.3 no C12 . C11 . H111 . 121.4 no C11 . C12 . C13 . 120.2(2) yes C11 . C12 . H121 . 119.1 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 119.8(2) yes C12 . C13 . H131 . 123.1 no C14 . C13 . H131 . 117.1 no C13 . C14 . C15 . 120.2(2) yes C13 . C14 . H141 . 121.0 no C15 . C14 . H141 . 118.8 no C10 . C15 . C14 . 121.2(2) yes C10 . C15 . H151 . 118.2 no C14 . C15 . H151 . 120.5 no N2 . C16 . C17 . 111.58(18) yes N2 . C16 . C18 . 109.89(17) yes C17 . C16 . C18 . 110.37(19) yes N2 . C16 . H161 . 108.7 no C17 . C16 . H161 . 108.8 no C18 . C16 . H161 . 107.4 no C16 . C17 . H171 . 113.2 no C16 . C17 . H172 . 109.3 no H171 . C17 . H172 . 109.3 no C16 . C17 . H173 . 109.7 no H171 . C17 . H173 . 107.5 no H172 . C17 . H173 . 107.6 no C16 . C18 . H181 . 110.9 no C16 . C18 . H182 . 107.4 no H181 . C18 . H182 . 109.6 no C16 . C18 . H183 . 110.2 no H181 . C18 . H183 . 109.8 no H182 . C18 . H183 . 109.0 no P2 . C19 . C20 . 124.84(17) yes P2 . C19 . C24 . 116.85(17) yes C20 . C19 . C24 . 118.2(2) yes C19 . C20 . C21 . 120.4(2) yes C19 . C20 . H201 . 118.3 no C21 . C20 . H201 . 121.3 no C20 . C21 . C22 . 120.7(2) yes C20 . C21 . H211 . 118.7 no C22 . C21 . H211 . 120.5 no C21 . C22 . C23 . 119.6(2) yes C21 . C22 . H221 . 119.8 no C23 . C22 . H221 . 120.6 no C22 . C23 . C24 . 119.9(2) yes C22 . C23 . H231 . 121.8 no C24 . C23 . H231 . 118.3 no C19 . C24 . C23 . 121.1(2) yes C19 . C24 . H241 . 119.1 no C23 . C24 . H241 . 119.8 no P2 . C25 . C26 . 120.35(17) yes P2 . C25 . C30 . 121.02(17) yes C26 . C25 . C30 . 118.2(2) yes C25 . C26 . C27 . 121.1(2) yes C25 . C26 . H261 . 120.6 no C27 . C26 . H261 . 118.2 no C26 . C27 . C28 . 119.7(2) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 120.9 no C27 . C28 . C29 . 120.0(2) yes C27 . C28 . H281 . 118.2 no C29 . C28 . H281 . 121.8 no C28 . C29 . C30 . 120.0(2) yes C28 . C29 . H291 . 118.7 no C30 . C29 . H291 . 121.3 no C29 . C30 . C25 . 120.8(2) yes C29 . C30 . H301 . 118.6 no C25 . C30 . H301 . 120.4 no N3 . C31 . C32 . 111.45(18) yes N3 . C31 . C33 . 110.41(18) yes C32 . C31 . C33 . 110.2(2) yes N3 . C31 . H311 . 106.9 no C32 . C31 . H311 . 110.2 no C33 . C31 . H311 . 107.6 no C31 . C32 . H321 . 107.6 no C31 . C32 . H322 . 110.4 no H321 . C32 . H322 . 107.9 no C31 . C32 . H323 . 110.4 no H321 . C32 . H323 . 109.8 no H322 . C32 . H323 . 110.8 no C31 . C33 . H331 . 109.7 no C31 . C33 . H332 . 109.8 no H331 . C33 . H332 . 109.9 no C31 . C33 . H333 . 107.3 no H331 . C33 . H333 . 110.7 no H332 . C33 . H333 . 109.4 no P3 . C34 . C35 . 126.03(18) yes P3 . C34 . C39 . 115.39(16) yes C35 . C34 . C39 . 118.4(2) yes C34 . C35 . C36 . 119.5(2) yes C34 . C35 . H351 . 120.4 no C36 . C35 . H351 . 120.1 no C35 . C36 . C37 . 120.8(2) yes C35 . C36 . H361 . 118.5 no C37 . C36 . H361 . 120.7 no C36 . C37 . C38 . 120.5(2) yes C36 . C37 . H371 . 119.3 no C38 . C37 . H371 . 120.1 no C37 . C38 . C39 . 118.9(2) yes C37 . C38 . H381 . 120.6 no C39 . C38 . H381 . 120.4 no C34 . C39 . C38 . 122.0(2) yes C34 . C39 . H391 . 119.0 no C38 . C39 . H391 . 119.0 no P3 . C40 . C41 . 121.11(18) yes P3 . C40 . C45 . 119.53(18) yes C41 . C40 . C45 . 118.7(2) yes C40 . C41 . C42 . 120.3(2) yes C40 . C41 . H411 . 118.5 no C42 . C41 . H411 . 121.1 no C41 . C42 . C43 . 120.2(3) yes C41 . C42 . H421 . 118.1 no C43 . C42 . H421 . 121.7 no C42 . C43 . C44 . 119.8(2) yes C42 . C43 . H431 . 120.2 no C44 . C43 . H431 . 120.0 no C43 . C44 . C45 . 120.2(3) yes C43 . C44 . H441 . 122.3 no C45 . C44 . H441 . 117.4 no C44 . C45 . C40 . 120.7(3) yes C44 . C45 . H451 . 118.3 no C40 . C45 . H451 . 121.1 no _iucr_refine_instructions_details_constraints ; # # Punched on 28/11/12 at 10:29:59 # #LIST 12 BLOCK SCALE X'S, U'S REM CONT ENANTIO RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 28/11/12 at 10:29:59 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.056 0.250 0.000 521 65 ' ' 2 0.035 0.750 0.500 521 65 ' ' _platon_squeeze_details ;During the structure solution, electron density difference maps revealed that there were considerable disordered solvent molecules which could not be successfully modeled. From history, the remaining solvate was likely pentane in a volume of 1045.8 \%A3 per unit cell (21.4%). It appeared that the cavity area contained ca. four pentane molecules, located near the twofold screw axes at (0, 1/4, 0) and (0, 3/4, 1/2). Modeling with or without restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE technique, in order to produce a "solvate-free" structure factor set. PLATON reported a total electron density of 129 e- per unit cell, likely representing four pentane molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca. 1.75 % in R. ; _database_code_depnum_ccdc_archive 'CCDC 966655' ####################################################################### # # 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_2 _audit_creation_date 2012-11-30 _audit_creation_method CRYSTALS_ver_14.43 _oxford_structure_analysis_title 'sk_782_0m in Pa-3' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 20.6666(3) _cell_length_b 20.6666(3) _cell_length_c 20.6666(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8826.9(2) _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3 ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z y,z,x -y,-z,-x z,x,y -z,-x,-y x+1/2,y,-z+1/2 -x+1/2,-y,z+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 z+1/2,x,-y+1/2 -z+1/2,-x,y+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z+1/2,-x+1/2,-y -z+1/2,x+1/2,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C45 H51 Cr1.00 Fe1.00 I1.00 N3 P3 # Dc = 1.45 Fooo = 3920.00 Mu = 14.17 M = 320.53 # Found Formula = C45 H51 Cr1 Fe1 I1 N3 P3 # Dc = 1.45 FOOO = 3920.00 Mu = 14.17 M = 320.53 _chemical_formula_sum 'C45 H51 Cr1 Fe1 I1 N3 P3' _chemical_formula_moiety 'C45 H51 Cr1 Fe1 I1 N3 P3' _chemical_compound_source ? _chemical_formula_weight 961.59 _cell_measurement_reflns_used 2518 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3920.000 _exptl_absorpt_coefficient_mu 1.417 # Sheldrick geometric approximatio 0.77 0.80 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.80 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 19602 _reflns_number_total 3373 _diffrn_reflns_av_R_equivalents 0.074 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 3373 # Theoretical number of reflections is about 6744 _diffrn_reflns_theta_min 1.707 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.477 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 1 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 1.69 _oxford_diffrn_Wilson_scale 819.95 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.00 _refine_diff_density_max 1.22 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 3373 _refine_ls_number_restraints 0 _refine_ls_number_parameters 163 _oxford_refine_ls_R_factor_ref 0.0682 _refine_ls_wR_factor_ref 0.0798 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0022679 _refine_ls_shift/su_mean 0.0000569 # The values computed with all filters except I/sigma _oxford_reflns_number_all 3373 _refine_ls_R_factor_all 0.0682 _refine_ls_wR_factor_all 0.0798 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2281 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_gt 0.0702 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +14.48P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Fe1 Fe 0.827594(19) 0.327594(19) 0.172406(19) 0.0139 1.0000 Uani S T . . . . Cr1 Cr 0.89379(2) 0.39379(2) 0.10621(2) 0.0122 1.0000 Uani S T . . . . I1 I 0.755900(10) 0.255900(10) 0.244100(10) 0.0371 1.0000 Uani S T . . . . P1 P 0.83530(4) 0.28585(4) 0.07100(4) 0.0149 1.0000 Uani . . . . . . N1 N 0.87704(11) 0.34359(11) 0.03250(11) 0.0157 1.0000 Uani . . . . . . C1 C 0.76153(14) 0.26506(14) 0.02647(15) 0.0189 1.0000 Uani . . . . . . C2 C 0.76199(17) 0.24180(16) -0.03662(16) 0.0288 1.0000 Uani . . . . . . C3 C 0.70451(19) 0.22885(18) -0.06851(19) 0.0389 1.0000 Uani . . . . . . C4 C 0.64615(18) 0.23832(17) -0.0374(2) 0.0393 1.0000 Uani . . . . . . C5 C 0.64451(16) 0.25946(16) 0.0256(2) 0.0338 1.0000 Uani . . . . . . C6 C 0.70253(15) 0.27329(15) 0.05747(17) 0.0251 1.0000 Uani . . . . . . C7 C 0.88201(14) 0.21095(14) 0.06729(14) 0.0157 1.0000 Uani . . . . . . C8 C 0.94946(14) 0.21225(15) 0.06640(14) 0.0193 1.0000 Uani . . . . . . C9 C 0.98442(15) 0.15514(15) 0.07150(15) 0.0227 1.0000 Uani . . . . . . C10 C 0.95267(15) 0.09665(15) 0.07794(14) 0.0227 1.0000 Uani . . . . . . C11 C 0.88562(16) 0.09514(15) 0.08022(15) 0.0238 1.0000 Uani . . . . . . C12 C 0.85059(15) 0.15192(14) 0.07496(15) 0.0213 1.0000 Uani . . . . . . C13 C 0.90225(17) 0.42520(16) -0.04975(16) 0.0287 1.0000 Uani . . . . . . C14 C 0.88284(16) 0.35510(15) -0.03834(15) 0.0250 1.0000 Uani . . . . . . C15 C 0.93051(19) 0.30964(17) -0.06924(17) 0.0383 1.0000 Uani . . . . . . H21 H 0.8015 0.2341 -0.0572 0.0348 1.0000 Uiso R . . . . . H31 H 0.7060 0.2137 -0.1116 0.0471 1.0000 Uiso R . . . . . H41 H 0.6074 0.2303 -0.0591 0.0477 1.0000 Uiso R . . . . . H51 H 0.6049 0.2638 0.0479 0.0409 1.0000 Uiso R . . . . . H61 H 0.7022 0.2872 0.1002 0.0309 1.0000 Uiso R . . . . . H81 H 0.9706 0.2516 0.0623 0.0236 1.0000 Uiso R . . . . . H91 H 1.0295 0.1566 0.0721 0.0276 1.0000 Uiso R . . . . . H101 H 0.9760 0.0583 0.0805 0.0267 1.0000 Uiso R . . . . . H111 H 0.8649 0.0552 0.0851 0.0289 1.0000 Uiso R . . . . . H121 H 0.8053 0.1502 0.0766 0.0257 1.0000 Uiso R . . . . . H131 H 0.8718 0.4557 -0.0282 0.0424 1.0000 Uiso R . . . . . H132 H 0.9465 0.4320 -0.0302 0.0433 1.0000 Uiso R . . . . . H133 H 0.9034 0.4344 -0.0967 0.0436 1.0000 Uiso R . . . . . H141 H 0.8406 0.3484 -0.0610 0.0299 1.0000 Uiso R . . . . . H151 H 0.9181 0.2646 -0.0603 0.0578 1.0000 Uiso R . . . . . H152 H 0.9738 0.3205 -0.0504 0.0582 1.0000 Uiso R . . . . . H153 H 0.9293 0.3181 -0.1162 0.0583 1.0000 Uiso R . . . . . 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 Fe1 0.01392(16) 0.01392(16) 0.01392(16) 0.00105(17) 0.00105(17) -0.00105(17) Cr1 0.01225(18) 0.01225(18) 0.01225(18) -0.00022(19) -0.00022(19) 0.00022(19) I1 0.03714(13) 0.03714(13) 0.03714(13) 0.01236(10) 0.01236(10) -0.01236(10) P1 0.0155(4) 0.0135(4) 0.0156(4) -0.0010(3) -0.0001(3) -0.0015(3) N1 0.0175(13) 0.0152(12) 0.0144(12) -0.0010(10) 0.0013(10) -0.0001(11) C1 0.0211(16) 0.0120(14) 0.0235(16) 0.0016(12) -0.0040(13) -0.0037(13) C2 0.0303(18) 0.0313(19) 0.0250(17) -0.0021(15) -0.0017(15) -0.0114(16) C3 0.046(2) 0.039(2) 0.032(2) -0.0038(18) -0.0107(19) -0.0185(19) C4 0.036(2) 0.029(2) 0.053(3) 0.0020(19) -0.024(2) -0.0106(17) C5 0.0218(17) 0.0217(18) 0.058(3) 0.0005(18) -0.0069(17) -0.0042(15) C6 0.0209(17) 0.0195(16) 0.0349(19) -0.0039(15) -0.0048(15) -0.0007(14) C7 0.0188(15) 0.0142(14) 0.0141(14) -0.0025(12) 0.0014(13) -0.0001(12) C8 0.0215(16) 0.0182(15) 0.0182(15) -0.0011(13) 0.0027(13) -0.0009(13) C9 0.0183(16) 0.0273(17) 0.0226(16) -0.0046(14) 0.0033(14) 0.0047(14) C10 0.0271(17) 0.0218(17) 0.0193(16) -0.0014(14) 0.0016(14) 0.0068(14) C11 0.0303(18) 0.0142(15) 0.0269(17) 0.0016(14) 0.0046(15) -0.0012(14) C12 0.0212(16) 0.0193(16) 0.0234(16) 0.0000(14) 0.0017(14) -0.0002(14) C13 0.0322(19) 0.0279(18) 0.0260(18) 0.0057(15) 0.0025(16) -0.0012(16) C14 0.0296(18) 0.0243(17) 0.0213(17) -0.0010(14) 0.0005(15) -0.0069(15) C15 0.058(3) 0.0276(19) 0.0291(19) -0.0023(16) 0.0052(19) -0.0013(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.037717(4) 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 Fe1 . P1 17_645 2.2720(8) yes Fe1 . P1 13_556 2.2720(8) yes Fe1 . Cr1 . 2.3696(10) yes Fe1 . I1 . 2.5663(8) yes Fe1 . P1 . 2.2720(8) yes Cr1 . P1 17_645 2.6396(9) yes Cr1 . P1 13_556 2.6396(9) yes Cr1 . N1 13_556 1.875(2) yes Cr1 . N1 17_645 1.875(2) yes Cr1 . P1 . 2.6396(9) yes Cr1 . N1 . 1.875(2) yes P1 . N1 . 1.674(2) yes P1 . C1 . 1.832(3) yes P1 . C7 . 1.826(3) yes N1 . C14 . 1.488(4) yes C1 . C2 . 1.390(4) yes C1 . C6 . 1.388(4) yes C2 . C3 . 1.384(5) yes C2 . H21 . 0.933 no C3 . C4 . 1.380(5) yes C3 . H31 . 0.944 no C4 . C5 . 1.374(5) yes C4 . H41 . 0.933 no C5 . C6 . 1.398(4) yes C5 . H51 . 0.943 no C6 . H61 . 0.927 no C7 . C8 . 1.394(4) yes C7 . C12 . 1.391(4) yes C8 . C9 . 1.388(4) yes C8 . H81 . 0.927 no C9 . C10 . 1.382(4) yes C9 . H91 . 0.932 no C10 . C11 . 1.387(4) yes C10 . H101 . 0.929 no C11 . C12 . 1.383(4) yes C11 . H111 . 0.935 no C12 . H121 . 0.936 no C13 . C14 . 1.522(4) yes C13 . H131 . 0.997 no C13 . H132 . 1.009 no C13 . H133 . 0.989 no C14 . C15 . 1.504(5) yes C14 . H141 . 1.000 no C15 . H151 . 0.983 no C15 . H152 . 1.001 no C15 . H153 . 0.986 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 P1 17_645 Fe1 . P1 13_556 108.19(3) yes P1 17_645 Fe1 . Cr1 . 69.28(2) yes P1 13_556 Fe1 . Cr1 . 69.28(2) yes P1 17_645 Fe1 . I1 . 110.72(2) yes P1 13_556 Fe1 . I1 . 110.72(2) yes Cr1 . Fe1 . I1 . 179.996 yes P1 17_645 Fe1 . P1 . 108.19(3) yes P1 13_556 Fe1 . P1 . 108.19(3) yes Cr1 . Fe1 . P1 . 69.28(2) yes I1 . Fe1 . P1 . 110.72(2) yes P1 17_645 Cr1 . P1 13_556 88.41(3) yes P1 17_645 Cr1 . N1 13_556 111.62(8) yes P1 13_556 Cr1 . N1 13_556 39.10(7) yes P1 17_645 Cr1 . N1 17_645 39.10(7) yes P1 13_556 Cr1 . N1 17_645 118.95(8) yes N1 13_556 Cr1 . N1 17_645 119.817(11) yes P1 17_645 Cr1 . Fe1 . 53.62(2) yes P1 13_556 Cr1 . Fe1 . 53.62(2) yes N1 13_556 Cr1 . Fe1 . 92.46(8) yes N1 17_645 Cr1 . Fe1 . 92.46(8) yes P1 17_645 Cr1 . P1 . 88.41(3) yes P1 13_556 Cr1 . P1 . 88.41(3) yes N1 13_556 Cr1 . P1 . 118.95(8) yes N1 17_645 Cr1 . P1 . 111.62(8) yes Fe1 . Cr1 . P1 . 53.62(2) yes P1 17_645 Cr1 . N1 . 118.95(8) yes P1 13_556 Cr1 . N1 . 111.62(8) yes N1 13_556 Cr1 . N1 . 119.817(11) yes N1 17_645 Cr1 . N1 . 119.817(11) yes Fe1 . Cr1 . N1 . 92.46(8) yes P1 . Cr1 . N1 . 39.10(7) yes Cr1 . P1 . Fe1 . 57.10(3) yes Fe1 . P1 . N1 . 101.76(9) yes Cr1 . P1 . C1 . 135.88(10) yes Fe1 . P1 . C1 . 119.62(10) yes N1 . P1 . C1 . 110.94(13) yes Cr1 . P1 . C7 . 119.07(10) yes Fe1 . P1 . C7 . 113.43(10) yes N1 . P1 . C7 . 108.18(13) yes C1 . P1 . C7 . 102.71(13) yes P1 . N1 . Cr1 . 95.94(12) yes P1 . N1 . C14 . 128.5(2) yes Cr1 . N1 . C14 . 134.10(19) yes P1 . C1 . C2 . 123.1(3) yes P1 . C1 . C6 . 118.1(2) yes C2 . C1 . C6 . 118.8(3) yes C1 . C2 . C3 . 120.5(3) yes C1 . C2 . H21 . 119.5 no C3 . C2 . H21 . 120.0 no C2 . C3 . C4 . 120.1(3) yes C2 . C3 . H31 . 119.0 no C4 . C3 . H31 . 121.0 no C3 . C4 . C5 . 120.5(3) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 119.3 no C4 . C5 . C6 . 119.4(3) yes C4 . C5 . H51 . 121.0 no C6 . C5 . H51 . 119.6 no C5 . C6 . C1 . 120.7(3) yes C5 . C6 . H61 . 120.3 no C1 . C6 . H61 . 118.9 no P1 . C7 . C8 . 120.8(2) yes P1 . C7 . C12 . 119.5(2) yes C8 . C7 . C12 . 119.0(3) yes C7 . C8 . C9 . 120.2(3) yes C7 . C8 . H81 . 119.3 no C9 . C8 . H81 . 120.5 no C8 . C9 . C10 . 120.3(3) yes C8 . C9 . H91 . 119.6 no C10 . C9 . H91 . 120.1 no C9 . C10 . C11 . 119.8(3) yes C9 . C10 . H101 . 120.4 no C11 . C10 . H101 . 119.8 no C10 . C11 . C12 . 120.1(3) yes C10 . C11 . H111 . 118.8 no C12 . C11 . H111 . 121.1 no C7 . C12 . C11 . 120.6(3) yes C7 . C12 . H121 . 120.2 no C11 . C12 . H121 . 119.2 no C14 . C13 . H131 . 111.6 no C14 . C13 . H132 . 108.0 no H131 . C13 . H132 . 107.8 no C14 . C13 . H133 . 110.0 no H131 . C13 . H133 . 109.3 no H132 . C13 . H133 . 110.1 no C13 . C14 . N1 . 109.0(3) yes C13 . C14 . C15 . 110.9(3) yes N1 . C14 . C15 . 111.8(3) yes C13 . C14 . H141 . 106.8 no N1 . C14 . H141 . 111.6 no C15 . C14 . H141 . 106.7 no C14 . C15 . H151 . 110.0 no C14 . C15 . H152 . 106.3 no H151 . C15 . H152 . 111.8 no C14 . C15 . H153 . 106.9 no H151 . C15 . H153 . 110.2 no H152 . C15 . H153 . 111.6 no _iucr_refine_instructions_details_constraints ; # # Punched on 30/11/12 at 09:33:18 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 30/11/12 at 09:33:18 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 966656' ####################################################################### # # 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_3 _audit_creation_date 2013-06-25 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 'sk_947_0ma in Pa-3' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 20.6768(2) _cell_length_b 20.6768(2) _cell_length_c 20.6768(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8839.95(15) _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3 ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z y,z,x -y,-z,-x z,x,y -z,-x,-y x+1/2,y,-z+1/2 -x+1/2,-y,z+1/2 y+1/2,z,-x+1/2 -y+1/2,-z,x+1/2 z+1/2,x,-y+1/2 -z+1/2,-x,y+1/2 y+1/2,-z+1/2,-x -y+1/2,z+1/2,x z+1/2,-x+1/2,-y -z+1/2,x+1/2,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 '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' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C45 H51 Co1.00 Cr1.00 I1.00 N3 P3 # Dc = 1.45 Fooo = 3928.00 Mu = 14.62 M = 321.56 # Found Formula = C45 H51 Co1 Cr1 I1 N3 P3 # Dc = 1.45 FOOO = 3928.00 Mu = 14.62 M = 321.56 _chemical_formula_sum 'C45 H51 Co1 Cr1 I1 N3 P3' _chemical_formula_moiety 'C45 H51 Co1 Cr1 I1 N3 P3' _chemical_compound_source ? _chemical_formula_weight 964.67 _cell_measurement_reflns_used 8910 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_min 0.210 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_max 0.500 _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3928 _exptl_absorpt_coefficient_mu 1.462 # Sheldrick geometric approximatio 0.69 0.74 # No experimental values of Tmin/max available _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.74 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 41303 _reflns_number_total 4291 _diffrn_reflns_av_R_equivalents 0.047 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4291 # Theoretical number of reflections is about 8574 _diffrn_reflns_theta_min 2.955 _diffrn_reflns_theta_max 29.973 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.973 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 2 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.59 _refine_diff_density_max 1.09 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 4291 _refine_ls_number_restraints 0 _refine_ls_number_parameters 163 _oxford_refine_ls_R_factor_ref 0.0397 _refine_ls_wR_factor_ref 0.0749 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0012536 _refine_ls_shift/su_mean 0.0001120 # The values computed with all filters except I/sigma _oxford_reflns_number_all 4291 _refine_ls_R_factor_all 0.0397 _refine_ls_wR_factor_all 0.0749 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3587 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_gt 0.0639 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 6.55P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 0.318658(11) 0.318658(11) 0.318658(11) 0.0131 1.0000 Uani S T . . . . Cr1 Cr 0.393519(14) 0.393519(14) 0.393519(14) 0.0145 1.0000 Uani S T . . . . I1 I 0.247602(6) 0.247602(6) 0.247602(6) 0.0291 1.0000 Uani S T . . . . P1 P 0.41935(2) 0.33682(2) 0.27891(2) 0.0147 1.0000 Uani . . . . . . N1 N 0.46020(7) 0.38237(7) 0.33260(7) 0.0165 1.0000 Uani . . . . . . C1 C 0.46386(9) 0.26329(9) 0.25829(9) 0.0188 1.0000 Uani . . . . . . C2 C 0.52777(11) 0.26353(11) 0.23606(11) 0.0286 1.0000 Uani . . . . . . C3 C 0.55961(11) 0.20583(12) 0.22404(13) 0.0378 1.0000 Uani . . . . . . C4 C 0.52786(12) 0.14735(11) 0.23301(12) 0.0342 1.0000 Uani . . . . . . C5 C 0.46382(12) 0.14642(10) 0.25185(10) 0.0279 1.0000 Uani . . . . . . C6 C 0.43213(10) 0.20447(9) 0.26510(9) 0.0216 1.0000 Uani . . . . . . C7 C 0.42140(9) 0.38151(9) 0.20307(9) 0.0174 1.0000 Uani . . . . . . C8 C 0.42108(9) 0.44905(9) 0.20337(9) 0.0209 1.0000 Uani . . . . . . C9 C 0.41732(10) 0.48332(10) 0.14595(10) 0.0245 1.0000 Uani . . . . . . C10 C 0.41337(10) 0.45094(11) 0.08755(10) 0.0259 1.0000 Uani . . . . . . C11 C 0.41281(10) 0.38381(10) 0.08657(10) 0.0256 1.0000 Uani . . . . . . C12 C 0.41672(9) 0.34922(10) 0.14401(9) 0.0213 1.0000 Uani . . . . . . C14 C 0.52545(9) 0.40972(9) 0.32311(10) 0.0210 1.0000 Uani . . . . . . C13 C 0.57661(10) 0.36915(11) 0.35719(11) 0.0295 1.0000 Uani . . . . . . C15 C 0.52807(11) 0.47887(11) 0.34801(12) 0.0327 1.0000 Uani . . . . . . H21 H 0.5480 0.3029 0.2284 0.0340 1.0000 Uiso R . . . . . H31 H 0.6021 0.2073 0.2102 0.0449 1.0000 Uiso R . . . . . H41 H 0.5496 0.1082 0.2256 0.0407 1.0000 Uiso R . . . . . H51 H 0.4424 0.1069 0.2568 0.0330 1.0000 Uiso R . . . . . H61 H 0.3890 0.2039 0.2791 0.0260 1.0000 Uiso R . . . . . H81 H 0.4232 0.4715 0.2429 0.0245 1.0000 Uiso R . . . . . H91 H 0.4171 0.5283 0.1469 0.0284 1.0000 Uiso R . . . . . H101 H 0.4113 0.4743 0.0493 0.0310 1.0000 Uiso R . . . . . H111 H 0.4104 0.3623 0.0478 0.0302 1.0000 Uiso R . . . . . H121 H 0.4164 0.3037 0.1430 0.0261 1.0000 Uiso R . . . . . H141 H 0.5340 0.4090 0.2762 0.0238 1.0000 Uiso R . . . . . H131 H 0.6192 0.3855 0.3474 0.0441 1.0000 Uiso R . . . . . H132 H 0.5704 0.3714 0.4032 0.0433 1.0000 Uiso R . . . . . H133 H 0.5740 0.3239 0.3447 0.0430 1.0000 Uiso R . . . . . H151 H 0.5704 0.4954 0.3414 0.0487 1.0000 Uiso R . . . . . H152 H 0.4970 0.5048 0.3242 0.0488 1.0000 Uiso R . . . . . H153 H 0.5184 0.4795 0.3933 0.0483 1.0000 Uiso R . . . . . 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 0.01310(9) 0.01310(9) 0.01310(9) -0.00012(8) -0.00012(8) -0.00012(8) Cr1 0.01453(10) 0.01453(10) 0.01453(10) 0.00055(10) 0.00055(10) 0.00055(10) I1 0.02909(7) 0.02909(7) 0.02909(7) -0.00769(5) -0.00769(5) -0.00769(5) P1 0.0148(2) 0.0152(2) 0.0142(2) 0.00017(16) 0.00156(16) 0.00036(16) N1 0.0139(7) 0.0187(7) 0.0171(7) -0.0005(6) 0.0003(6) -0.0016(6) C1 0.0204(9) 0.0209(9) 0.0151(8) -0.0010(7) 0.0009(7) 0.0053(7) C2 0.0224(10) 0.0287(11) 0.0345(12) -0.0074(9) 0.0046(9) 0.0003(8) C3 0.0231(11) 0.0409(13) 0.0495(14) -0.0168(11) 0.0061(10) 0.0078(10) C4 0.0355(12) 0.0293(11) 0.0379(12) -0.0123(9) 0.0006(10) 0.0132(9) C5 0.0387(12) 0.0210(10) 0.0242(10) -0.0031(8) 0.0043(9) 0.0039(9) C6 0.0261(10) 0.0198(9) 0.0189(9) -0.0008(7) 0.0036(7) 0.0024(7) C7 0.0138(8) 0.0208(9) 0.0175(8) 0.0026(7) 0.0009(6) -0.0003(7) C8 0.0209(9) 0.0205(9) 0.0212(9) 0.0012(7) 0.0005(7) 0.0009(7) C9 0.0249(10) 0.0200(9) 0.0286(10) 0.0074(8) 0.0016(8) 0.0018(8) C10 0.0230(10) 0.0332(11) 0.0217(9) 0.0102(8) -0.0004(8) -0.0009(8) C11 0.0281(10) 0.0316(11) 0.0172(9) 0.0010(8) -0.0022(8) -0.0043(8) C12 0.0228(9) 0.0226(9) 0.0185(9) 0.0012(7) -0.0004(7) -0.0020(7) C14 0.0153(8) 0.0241(9) 0.0236(9) 0.0039(8) 0.0010(7) -0.0025(7) C13 0.0185(9) 0.0351(11) 0.0349(12) 0.0009(9) -0.0058(8) 0.0010(8) C15 0.0261(11) 0.0254(10) 0.0466(14) 0.0005(10) -0.0033(10) -0.0083(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.037617(3) 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 . P1 3_555 2.2697(5) yes Co1 . P1 5_555 2.2697(5) yes Co1 . Cr1 . 2.6810(6) yes Co1 . I1 . 2.5447(5) yes Co1 . P1 . 2.2697(5) yes Cr1 . P1 3_555 2.6973(5) yes Cr1 . P1 5_555 2.6973(5) yes Cr1 . N1 3_555 1.8818(15) yes Cr1 . N1 5_555 1.8818(15) yes Cr1 . P1 . 2.6973(5) yes Cr1 . N1 . 1.8818(15) yes P1 . N1 . 1.6831(15) yes P1 . C1 . 1.8276(19) yes P1 . C7 . 1.8207(18) yes N1 . C14 . 1.476(2) yes C1 . C2 . 1.399(3) yes C1 . C6 . 1.389(3) yes C2 . C3 . 1.385(3) yes C2 . H21 . 0.929 no C3 . C4 . 1.388(4) yes C3 . H31 . 0.924 no C4 . C5 . 1.380(3) yes C4 . H41 . 0.938 no C5 . C6 . 1.395(3) yes C5 . H51 . 0.934 no C6 . H61 . 0.939 no C7 . C8 . 1.396(3) yes C7 . C12 . 1.395(3) yes C8 . C9 . 1.385(3) yes C8 . H81 . 0.941 no C9 . C10 . 1.383(3) yes C9 . H91 . 0.930 no C10 . C11 . 1.388(3) yes C10 . H101 . 0.928 no C11 . C12 . 1.389(3) yes C11 . H111 . 0.919 no C12 . H121 . 0.941 no C14 . C13 . 1.523(3) yes C14 . C15 . 1.521(3) yes C14 . H141 . 0.986 no C13 . H131 . 0.965 no C13 . H132 . 0.962 no C13 . H133 . 0.972 no C15 . H151 . 0.950 no C15 . H152 . 0.971 no C15 . H153 . 0.957 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 P1 3_555 Co1 . P1 5_555 103.904(17) yes P1 3_555 Co1 . Cr1 . 65.412(14) yes P1 5_555 Co1 . Cr1 . 65.412(14) yes P1 3_555 Co1 . I1 . 114.588(14) yes P1 5_555 Co1 . I1 . 114.588(14) yes Cr1 . Co1 . I1 . 179.995 yes P1 3_555 Co1 . P1 . 103.904(17) yes P1 5_555 Co1 . P1 . 103.904(17) yes Cr1 . Co1 . P1 . 65.412(14) yes I1 . Co1 . P1 . 114.588(14) yes P1 3_555 Cr1 . P1 5_555 83.005(19) yes P1 3_555 Cr1 . Co1 . 49.922(12) yes P1 5_555 Cr1 . Co1 . 49.922(12) yes P1 3_555 Cr1 . N1 3_555 38.14(5) yes P1 5_555 Cr1 . N1 3_555 110.09(5) yes Co1 . Cr1 . N1 3_555 88.04(5) yes P1 3_555 Cr1 . N1 5_555 112.15(5) yes P1 5_555 Cr1 . N1 5_555 38.14(5) yes Co1 . Cr1 . N1 5_555 88.04(5) yes N1 3_555 Cr1 . N1 5_555 119.884(6) yes P1 3_555 Cr1 . P1 . 83.005(19) yes P1 5_555 Cr1 . P1 . 83.005(19) yes Co1 . Cr1 . P1 . 49.922(12) yes N1 3_555 Cr1 . P1 . 112.15(5) yes N1 5_555 Cr1 . P1 . 110.09(5) yes P1 3_555 Cr1 . N1 . 110.09(5) yes P1 5_555 Cr1 . N1 . 112.15(5) yes Co1 . Cr1 . N1 . 88.04(5) yes N1 3_555 Cr1 . N1 . 119.884(6) yes N1 5_555 Cr1 . N1 . 119.884(6) yes P1 . Cr1 . N1 . 38.14(5) yes Cr1 . P1 . Co1 . 64.666(16) yes Co1 . P1 . N1 . 108.31(6) yes Cr1 . P1 . C1 . 131.78(6) yes Co1 . P1 . C1 . 114.12(7) yes N1 . P1 . C1 . 111.52(8) yes Cr1 . P1 . C7 . 122.73(6) yes Co1 . P1 . C7 . 114.66(6) yes N1 . P1 . C7 . 105.80(8) yes C1 . P1 . C7 . 102.10(8) yes P1 . N1 . Cr1 . 98.18(7) yes P1 . N1 . C14 . 125.84(12) yes Cr1 . N1 . C14 . 135.38(12) yes P1 . C1 . C2 . 123.31(15) yes P1 . C1 . C6 . 117.84(15) yes C2 . C1 . C6 . 118.86(18) yes C1 . C2 . C3 . 120.3(2) yes C1 . C2 . H21 . 119.0 no C3 . C2 . H21 . 120.7 no C2 . C3 . C4 . 120.1(2) yes C2 . C3 . H31 . 118.6 no C4 . C3 . H31 . 121.3 no C3 . C4 . C5 . 120.2(2) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 119.6 no C4 . C5 . C6 . 119.6(2) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 120.5 no C5 . C6 . C1 . 120.77(19) yes C5 . C6 . H61 . 119.8 no C1 . C6 . H61 . 119.4 no P1 . C7 . C8 . 120.24(14) yes P1 . C7 . C12 . 120.62(14) yes C8 . C7 . C12 . 118.83(17) yes C7 . C8 . C9 . 120.54(18) yes C7 . C8 . H81 . 119.8 no C9 . C8 . H81 . 119.7 no C8 . C9 . C10 . 120.27(19) yes C8 . C9 . H91 . 119.5 no C10 . C9 . H91 . 120.2 no C9 . C10 . C11 . 119.82(18) yes C9 . C10 . H101 . 119.6 no C11 . C10 . H101 . 120.6 no C10 . C11 . C12 . 120.13(19) yes C10 . C11 . H111 . 119.8 no C12 . C11 . H111 . 120.0 no C7 . C12 . C11 . 120.41(18) yes C7 . C12 . H121 . 119.9 no C11 . C12 . H121 . 119.7 no N1 . C14 . C13 . 111.25(16) yes N1 . C14 . C15 . 110.36(16) yes C13 . C14 . C15 . 109.66(17) yes N1 . C14 . H141 . 106.8 no C13 . C14 . H141 . 108.8 no C15 . C14 . H141 . 109.9 no C14 . C13 . H131 . 110.1 no C14 . C13 . H132 . 109.7 no H131 . C13 . H132 . 108.2 no C14 . C13 . H133 . 111.6 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 107.6 no C14 . C15 . H151 . 108.7 no C14 . C15 . H152 . 108.9 no H151 . C15 . H152 . 109.8 no C14 . C15 . H153 . 109.7 no H151 . C15 . H153 . 109.2 no H152 . C15 . H153 . 110.5 no _iucr_refine_instructions_details_constraints ; # # Punched on 25/06/13 at 16:57:51 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 25/06/13 at 16:57:51 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 966657' ####################################################################### # # 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_sk_4 _audit_creation_date 2013-05-29 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 'sk_821rr_0m in P-3c1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.2739(3) _cell_length_b 16.2739(3) _cell_length_c 23.1328(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5305.69(18) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3 c 1 ' _symmetry_space_group_name_Hall '-P 3 2"c ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x-y,z y,-x+y,-z -x+y,-x,z x-y,x,-z -x+y,y,z+1/2 x-y,-y,-z+1/2 x,x-y,z+1/2 -x,-x+y,-z+1/2 -y,-x,z+1/2 y,x,-z+1/2 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C48 H60 Cr1.00 Fe1.00 N3 P4.00 # Dc = 1.14 Fooo = 1916.00 Mu = 6.30 M = 303.59 # Found Formula = C48 H60 Cr1 Fe1 N3 P4 # Dc = 1.14 FOOO = 1916.00 Mu = 6.30 M = 303.59 _chemical_formula_sum 'C48 H60 Cr1 Fe1 N3 P4' _chemical_formula_moiety 'C48 H60 Cr1 Fe1 N3 P4' _chemical_compound_source ? _chemical_formula_weight 910.76 _cell_measurement_reflns_used 6427 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_min 0.210 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_max 0.400 _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1916 _exptl_absorpt_coefficient_mu 0.630 # Sheldrick geometric approximatio 0.82 0.88 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.88 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 4891 _reflns_number_total 4891 _diffrn_reflns_av_R_equivalents 0.071 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4891 # Theoretical number of reflections is about 9773 _diffrn_reflns_theta_min 1.761 _diffrn_reflns_theta_max 29.409 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.409 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -19 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.42 _refine_diff_density_max 0.51 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 4891 _refine_ls_number_restraints 0 _refine_ls_number_parameters 172 _oxford_refine_ls_R_factor_ref 0.0514 _refine_ls_wR_factor_ref 0.0985 _refine_ls_goodness_of_fit_ref 0.9917 _refine_ls_shift/su_max 0.0029529 _refine_ls_shift/su_mean 0.0000808 # The values computed with all filters except I/sigma _oxford_reflns_number_all 4891 _refine_ls_R_factor_all 0.0514 _refine_ls_wR_factor_all 0.0985 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3444 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_gt 0.0852 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.21P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Fe1 Fe 0.6667 0.3333 0.588792(15) 0.0159 1.0000 Uani S T . . . . Cr1 Cr 0.6667 0.3333 0.691828(17) 0.0156 1.0000 Uani S T . . . . P1 P 0.56009(3) 0.37157(3) 0.621921(18) 0.0231 1.0000 Uani . . . . . . P2 P 0.6667 0.3333 0.49098(3) 0.0224 1.0000 Uani S T . . . . N1 N 0.56004(10) 0.35060(10) 0.69282(6) 0.0239 1.0000 Uani . . . . . . C1 C 0.50149(14) 0.35974(14) 0.73786(8) 0.0324 1.0000 Uani . . . . . . C2 C 0.55955(17) 0.39516(18) 0.79338(8) 0.0432 1.0000 Uani . . . . . . C3 C 0.41042(16) 0.26653(17) 0.74766(10) 0.0459 1.0000 Uani . . . . . . C4 C 0.59084(12) 0.49630(12) 0.61675(7) 0.0253 1.0000 Uani . . . . . . C5 C 0.63508(14) 0.55929(13) 0.66212(8) 0.0315 1.0000 Uani . . . . . . C6 C 0.66415(16) 0.65493(15) 0.65601(9) 0.0408 1.0000 Uani . . . . . . C7 C 0.65056(16) 0.68902(15) 0.60469(10) 0.0425 1.0000 Uani . . . . . . C8 C 0.60810(15) 0.62793(15) 0.55861(9) 0.0375 1.0000 Uani . . . . . . C9 C 0.57836(13) 0.53234(13) 0.56466(8) 0.0304 1.0000 Uani . . . . . . C10 C 0.43534(12) 0.31326(13) 0.59802(7) 0.0256 1.0000 Uani . . . . . . C11 C 0.37824(14) 0.35385(15) 0.60594(9) 0.0370 1.0000 Uani . . . . . . C12 C 0.28355(15) 0.30581(17) 0.58990(11) 0.0472 1.0000 Uani . . . . . . C13 C 0.24481(15) 0.21708(16) 0.56545(11) 0.0474 1.0000 Uani . . . . . . C14 C 0.30037(15) 0.17591(15) 0.55681(10) 0.0424 1.0000 Uani . . . . . . C15 C 0.39485(14) 0.22397(13) 0.57277(8) 0.0308 1.0000 Uani . . . . . . C16 C 0.70136(16) 0.44510(14) 0.45379(8) 0.0387 1.0000 Uani . . . . . . H11 H 0.4842 0.4079 0.7254 0.0381 1.0000 Uiso R . . . . . H21 H 0.5246 0.4002 0.8242 0.0642 1.0000 Uiso R . . . . . H22 H 0.5765 0.3490 0.8052 0.0633 1.0000 Uiso R . . . . . H23 H 0.6154 0.4558 0.7880 0.0643 1.0000 Uiso R . . . . . H31 H 0.3717 0.2737 0.7765 0.0682 1.0000 Uiso R . . . . . H32 H 0.4244 0.2191 0.7620 0.0681 1.0000 Uiso R . . . . . H33 H 0.3735 0.2406 0.7129 0.0678 1.0000 Uiso R . . . . . H51 H 0.6439 0.5360 0.6973 0.0374 1.0000 Uiso R . . . . . H61 H 0.6945 0.6965 0.6874 0.0492 1.0000 Uiso R . . . . . H71 H 0.6692 0.7524 0.6015 0.0509 1.0000 Uiso R . . . . . H81 H 0.6012 0.6518 0.5233 0.0448 1.0000 Uiso R . . . . . H91 H 0.5489 0.4898 0.5332 0.0360 1.0000 Uiso R . . . . . H111 H 0.4052 0.4162 0.6221 0.0436 1.0000 Uiso R . . . . . H121 H 0.2461 0.3332 0.5963 0.0572 1.0000 Uiso R . . . . . H131 H 0.1816 0.1858 0.5531 0.0566 1.0000 Uiso R . . . . . H141 H 0.2752 0.1143 0.5405 0.0503 1.0000 Uiso R . . . . . H151 H 0.4319 0.1967 0.5667 0.0366 1.0000 Uiso R . . . . . H161 H 0.7649 0.4937 0.4649 0.0576 1.0000 Uiso R . . . . . H162 H 0.6568 0.4661 0.4628 0.0581 1.0000 Uiso R . . . . . H163 H 0.6990 0.4360 0.4121 0.0578 1.0000 Uiso R . . . . . 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 Fe1 0.01704(12) 0.01704(12) 0.01362(17) 0.0000 0.0000 0.00852(6) Cr1 0.01660(13) 0.01660(13) 0.01359(19) 0.0000 0.0000 0.00830(7) P1 0.0262(2) 0.0265(2) 0.0209(2) -0.00299(17) -0.00481(17) 0.01639(19) P2 0.0233(2) 0.0233(2) 0.0206(3) 0.0000 0.0000 0.01165(11) N1 0.0289(7) 0.0320(8) 0.0176(6) -0.0014(6) 0.0014(5) 0.0204(7) C1 0.0375(10) 0.0461(11) 0.0244(9) -0.0006(8) 0.0066(7) 0.0291(9) C2 0.0540(13) 0.0656(15) 0.0231(9) -0.0068(9) 0.0037(9) 0.0397(12) C3 0.0409(12) 0.0623(15) 0.0379(11) 0.0055(10) 0.0146(9) 0.0283(11) C4 0.0266(9) 0.0273(9) 0.0272(8) -0.0022(7) -0.0034(7) 0.0174(8) C5 0.0372(10) 0.0312(9) 0.0290(9) -0.0034(7) -0.0043(8) 0.0193(8) C6 0.0495(13) 0.0324(10) 0.0414(11) -0.0093(9) -0.0077(9) 0.0213(10) C7 0.0503(13) 0.0269(10) 0.0556(13) -0.0003(9) -0.0057(10) 0.0233(10) C8 0.0422(11) 0.0360(10) 0.0427(11) 0.0048(9) -0.0057(9) 0.0259(9) C9 0.0328(10) 0.0340(10) 0.0307(9) -0.0031(7) -0.0082(7) 0.0215(8) C10 0.0266(8) 0.0289(9) 0.0235(8) -0.0017(7) -0.0024(6) 0.0156(7) C11 0.0311(10) 0.0391(11) 0.0460(12) -0.0099(9) -0.0046(8) 0.0215(9) C12 0.0311(11) 0.0535(14) 0.0646(15) -0.0042(11) -0.0040(10) 0.0268(11) C13 0.0261(10) 0.0433(12) 0.0648(15) 0.0024(11) -0.0105(10) 0.0114(9) C14 0.0387(11) 0.0281(10) 0.0522(13) -0.0023(9) -0.0128(10) 0.0105(9) C15 0.0338(10) 0.0281(9) 0.0329(9) -0.0013(7) -0.0049(8) 0.0173(8) C16 0.0560(13) 0.0343(10) 0.0243(9) 0.0072(8) 0.0025(9) 0.0215(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.081450(19) 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 Fe1 . P1 3_655 2.2500(4) yes Fe1 . P1 5_665 2.2500(4) yes Fe1 . Cr1 . 2.3835(5) yes Fe1 . P1 . 2.2500(4) yes Fe1 . P2 . 2.2627(8) yes Cr1 . P1 5_665 2.6627(5) yes Cr1 . P1 3_655 2.6627(5) yes Cr1 . N1 3_655 1.8915(14) yes Cr1 . N1 5_665 1.8915(14) yes Cr1 . P1 . 2.6627(5) yes Cr1 . N1 . 1.8915(14) yes P1 . N1 . 1.6751(14) yes P1 . C4 . 1.8355(17) yes P1 . C10 . 1.8442(18) yes P2 . C16 3_655 1.8276(19) yes P2 . C16 5_665 1.8276(19) yes P2 . C16 . 1.8276(19) yes N1 . C1 . 1.469(2) yes C1 . C2 . 1.526(3) yes C1 . C3 . 1.517(3) yes C1 . H11 . 0.998 no C2 . H21 . 0.941 no C2 . H22 . 0.961 no C2 . H23 . 0.958 no C3 . H31 . 0.963 no C3 . H32 . 0.966 no C3 . H33 . 0.966 no C4 . C5 . 1.390(2) yes C4 . C9 . 1.399(2) yes C5 . C6 . 1.389(3) yes C5 . H51 . 0.939 no C6 . C7 . 1.374(3) yes C6 . H61 . 0.946 no C7 . C8 . 1.384(3) yes C7 . H71 . 0.921 no C8 . C9 . 1.386(3) yes C8 . H81 . 0.936 no C9 . H91 . 0.953 no C10 . C11 . 1.395(2) yes C10 . C15 . 1.389(2) yes C11 . C12 . 1.385(3) yes C11 . H111 . 0.958 no C12 . C13 . 1.375(3) yes C12 . H121 . 0.929 no C13 . C14 . 1.383(3) yes C13 . H131 . 0.936 no C14 . C15 . 1.382(3) yes C14 . H141 . 0.951 no C15 . H151 . 0.920 no C16 . H161 . 0.970 no C16 . H162 . 0.967 no C16 . H163 . 0.974 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 P1 3_655 Fe1 . P1 5_665 109.024(14) yes P1 3_655 Fe1 . Cr1 . 70.085(14) yes P1 5_665 Fe1 . Cr1 . 70.086(14) yes P1 3_655 Fe1 . P1 . 109.024(14) yes P1 5_665 Fe1 . P1 . 109.024(14) yes Cr1 . Fe1 . P1 . 70.086(13) yes P1 3_655 Fe1 . P2 . 109.915(14) yes P1 5_665 Fe1 . P2 . 109.915(14) yes Cr1 . Fe1 . P2 . 179.995 yes P1 . Fe1 . P2 . 109.915(14) yes P1 5_665 Cr1 . P1 3_655 86.947(17) yes P1 5_665 Cr1 . N1 3_655 108.24(5) yes P1 3_655 Cr1 . N1 3_655 38.69(4) yes P1 5_665 Cr1 . N1 5_665 38.69(4) yes P1 3_655 Cr1 . N1 5_665 119.31(4) yes N1 3_655 Cr1 . N1 5_665 119.985 yes P1 5_665 Cr1 . Fe1 . 52.604(12) yes P1 3_655 Cr1 . Fe1 . 52.604(12) yes N1 3_655 Cr1 . Fe1 . 90.69(4) yes N1 5_665 Cr1 . Fe1 . 90.69(4) yes P1 5_665 Cr1 . P1 . 86.947(17) yes P1 3_655 Cr1 . P1 . 86.947(17) yes N1 3_655 Cr1 . P1 . 119.31(4) yes N1 5_665 Cr1 . P1 . 108.24(5) yes Fe1 . Cr1 . P1 . 52.604(11) yes P1 5_665 Cr1 . N1 . 119.31(4) yes P1 3_655 Cr1 . N1 . 108.24(5) yes N1 3_655 Cr1 . N1 . 119.985 yes N1 5_665 Cr1 . N1 . 119.985 yes Fe1 . Cr1 . N1 . 90.69(4) yes P1 . Cr1 . N1 . 38.69(4) yes Cr1 . P1 . Fe1 . 57.311(14) yes Fe1 . P1 . N1 . 101.48(5) yes Cr1 . P1 . C4 . 116.66(6) yes Fe1 . P1 . C4 . 117.51(6) yes N1 . P1 . C4 . 105.14(8) yes Cr1 . P1 . C10 . 137.73(6) yes Fe1 . P1 . C10 . 123.92(6) yes N1 . P1 . C10 . 107.49(8) yes C4 . P1 . C10 . 99.84(8) yes C16 3_655 P2 . C16 5_665 99.65(8) yes C16 3_655 P2 . Fe1 . 118.08(7) yes C16 5_665 P2 . Fe1 . 118.08(7) yes C16 3_655 P2 . C16 . 99.65(8) yes C16 5_665 P2 . C16 . 99.65(8) yes Fe1 . P2 . C16 . 118.08(7) yes P1 . N1 . Cr1 . 96.40(7) yes P1 . N1 . C1 . 127.45(12) yes Cr1 . N1 . C1 . 135.51(12) yes N1 . C1 . C2 . 108.95(15) yes N1 . C1 . C3 . 111.33(16) yes C2 . C1 . C3 . 111.26(17) yes N1 . C1 . H11 . 109.0 no C2 . C1 . H11 . 108.1 no C3 . C1 . H11 . 108.1 no C1 . C2 . H21 . 112.6 no C1 . C2 . H22 . 108.1 no H21 . C2 . H22 . 105.9 no C1 . C2 . H23 . 111.6 no H21 . C2 . H23 . 108.2 no H22 . C2 . H23 . 110.3 no C1 . C3 . H31 . 110.7 no C1 . C3 . H32 . 110.3 no H31 . C3 . H32 . 106.7 no C1 . C3 . H33 . 113.3 no H31 . C3 . H33 . 109.2 no H32 . C3 . H33 . 106.4 no P1 . C4 . C5 . 121.37(13) yes P1 . C4 . C9 . 120.22(13) yes C5 . C4 . C9 . 118.13(16) yes C4 . C5 . C6 . 120.67(18) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 120.3 no C5 . C6 . C7 . 120.45(19) yes C5 . C6 . H61 . 119.2 no C7 . C6 . H61 . 120.4 no C6 . C7 . C8 . 119.91(19) yes C6 . C7 . H71 . 119.5 no C8 . C7 . H71 . 120.6 no C7 . C8 . C9 . 119.82(18) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 120.5 no C4 . C9 . C8 . 121.01(17) yes C4 . C9 . H91 . 118.6 no C8 . C9 . H91 . 120.4 no P1 . C10 . C11 . 122.64(14) yes P1 . C10 . C15 . 119.25(13) yes C11 . C10 . C15 . 118.08(17) yes C10 . C11 . C12 . 120.92(19) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 120.0(2) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 120.2 no C12 . C13 . C14 . 120.03(19) yes C12 . C13 . H131 . 119.9 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 119.95(19) yes C13 . C14 . H141 . 121.8 no C15 . C14 . H141 . 118.3 no C10 . C15 . C14 . 121.06(18) yes C10 . C15 . H151 . 119.1 no C14 . C15 . H151 . 119.9 no P2 . C16 . H161 . 111.1 no P2 . C16 . H162 . 109.7 no H161 . C16 . H162 . 109.7 no P2 . C16 . H163 . 110.2 no H161 . C16 . H163 . 109.3 no H162 . C16 . H163 . 106.7 no _iucr_refine_instructions_details_constraints ; # # Punched on 29/05/13 at 15:17:44 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 29/05/13 at 15:17:44 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.001 936 66 ' ' _platon_squeeze_details ; During the structure solution, electron density difference maps revealed that there were considerable disordered solvent molecules which could not be successfully modeled. From history, the remaining solvate was likely ether in a volume of 936.5 \%A3 per unit cell (17.7%). It appeared that the cavity area contained ca two ether molecules, located near the -3 position at (0, 0, 0). Modeling with or without restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE, technique, in order to produce a "solvate-free" structure factor set. PLATON reported a total electron density of 65 e- per unit cell, likely representing two ether molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca. 1.5 % in R. ; _database_code_depnum_ccdc_archive 'CCDC 966658' ####################################################################### # # 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_5 _audit_creation_date 2013-04-05 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 'sk_870_0m in P-3c1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.2999(6) _cell_length_b 16.2999(6) _cell_length_c 22.8438(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5256.2(3) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3 c 1 ' _symmetry_space_group_name_Hall '-P 3 2"c ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x-y,z y,-x+y,-z -x+y,-x,z x-y,x,-z -x+y,y,z+1/2 x-y,-y,-z+1/2 x,x-y,z+1/2 -x,-x+y,-z+1/2 -y,-x,z+1/2 y,x,-z+1/2 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 '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' _cell_formula_units_Z 4 # Given Formula = C48 H60 Co1.00 Cr1.00 N3 P4.00 # Dc = 1.15 Fooo = 1920.00 Mu = 6.76 M = 304.62 # Found Formula = C48 H60 Co1 Cr1 N3 P4 # Dc = 1.15 FOOO = 1920.00 Mu = 6.76 M = 304.62 _chemical_formula_sum 'C48 H60 Co1 Cr1 N3 P4' _chemical_formula_moiety 'C48 H60 Co1 Cr1 N3 P4' _chemical_compound_source ? _chemical_formula_weight 913.85 _cell_measurement_reflns_used 9735 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_min 0.220 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_max 0.370 _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.676 # Sheldrick geometric approximatio 0.86 0.86 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.86 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 5119 _reflns_number_total 5119 _diffrn_reflns_av_R_equivalents 0.052 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5119 # Theoretical number of reflections is about 10242 _diffrn_reflns_theta_min 1.783 _diffrn_reflns_theta_max 30.023 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.023 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -19 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 1.32 _oxford_diffrn_Wilson_scale 162.43 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.71 _refine_diff_density_max 0.59 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5119 _refine_ls_number_restraints 0 _refine_ls_number_parameters 172 _oxford_refine_ls_R_factor_ref 0.0431 _refine_ls_wR_factor_ref 0.0968 _refine_ls_goodness_of_fit_ref 1.0465 _refine_ls_shift/su_max 0.0018760 _refine_ls_shift/su_mean 0.0000844 # The values computed with all filters except I/sigma _oxford_reflns_number_all 5119 _refine_ls_R_factor_all 0.0431 _refine_ls_wR_factor_all 0.0968 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4031 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_gt 0.0819 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.59P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Cr1 Cr 0.6667 0.3333 0.306622(17) 0.0150 1.0000 Uani S T . . . . Co2 Co 0.6667 0.3333 0.408691(13) 0.0125 1.0000 Uani S T . . . . P1 P 0.62760(3) 0.43604(3) 0.379086(15) 0.0161 1.0000 Uani . . . . . . P2 P 0.6667 0.3333 0.50446(3) 0.0171 1.0000 Uani S T . . . . N1 N 0.64731(9) 0.43689(9) 0.30641(5) 0.0192 1.0000 Uani . . . . . . C1 C 0.63769(13) 0.49516(12) 0.26101(7) 0.0261 1.0000 Uani . . . . . . C2 C 0.60349(16) 0.43772(14) 0.20467(7) 0.0352 1.0000 Uani . . . . . . C3 C 0.73099(15) 0.58714(14) 0.25134(8) 0.0379 1.0000 Uani . . . . . . C4 C 0.68542(11) 0.56150(11) 0.40192(6) 0.0199 1.0000 Uani . . . . . . C5 C 0.64383(13) 0.61763(12) 0.39332(8) 0.0294 1.0000 Uani . . . . . . C6 C 0.69109(15) 0.71263(13) 0.40858(9) 0.0373 1.0000 Uani . . . . . . C7 C 0.78074(15) 0.75331(13) 0.43285(9) 0.0386 1.0000 Uani . . . . . . C8 C 0.82292(13) 0.69885(13) 0.44183(9) 0.0338 1.0000 Uani . . . . . . C9 C 0.77525(12) 0.60342(12) 0.42667(7) 0.0245 1.0000 Uani . . . . . . C10 C 0.50328(11) 0.40684(11) 0.38325(6) 0.0199 1.0000 Uani . . . . . . C11 C 0.44051(12) 0.36326(12) 0.33718(7) 0.0256 1.0000 Uani . . . . . . C12 C 0.34503(13) 0.33492(15) 0.34316(8) 0.0341 1.0000 Uani . . . . . . C13 C 0.31072(13) 0.34873(15) 0.39492(9) 0.0355 1.0000 Uani . . . . . . C14 C 0.37171(13) 0.39073(13) 0.44165(8) 0.0301 1.0000 Uani . . . . . . C15 C 0.46702(12) 0.41969(12) 0.43573(7) 0.0242 1.0000 Uani . . . . . . C16 C 0.73980(14) 0.44563(13) 0.54275(7) 0.0342 1.0000 Uani . . . . . . H11 H 0.5875 0.5115 0.2744 0.0305 1.0000 Uiso R . . . . . H21 H 0.5946 0.4731 0.1742 0.0523 1.0000 Uiso R . . . . . H22 H 0.6489 0.4223 0.1915 0.0517 1.0000 Uiso R . . . . . H23 H 0.5424 0.3806 0.2101 0.0522 1.0000 Uiso R . . . . . H31 H 0.7541 0.6222 0.2873 0.0560 1.0000 Uiso R . . . . . H32 H 0.7781 0.5732 0.2359 0.0565 1.0000 Uiso R . . . . . H33 H 0.7199 0.6259 0.2235 0.0565 1.0000 Uiso R . . . . . H51 H 0.5815 0.5891 0.3772 0.0345 1.0000 Uiso R . . . . . H61 H 0.6621 0.7479 0.4025 0.0452 1.0000 Uiso R . . . . . H71 H 0.8131 0.8185 0.4439 0.0462 1.0000 Uiso R . . . . . H81 H 0.8840 0.7258 0.4588 0.0409 1.0000 Uiso R . . . . . H91 H 0.8045 0.5678 0.4322 0.0292 1.0000 Uiso R . . . . . H111 H 0.4635 0.3525 0.3025 0.0314 1.0000 Uiso R . . . . . H121 H 0.3048 0.3062 0.3112 0.0413 1.0000 Uiso R . . . . . H131 H 0.2469 0.3302 0.3986 0.0440 1.0000 Uiso R . . . . . H141 H 0.3493 0.3995 0.4773 0.0360 1.0000 Uiso R . . . . . H151 H 0.5087 0.4495 0.4679 0.0283 1.0000 Uiso R . . . . . H161 H 0.7210 0.4909 0.5314 0.0521 1.0000 Uiso R . . . . . H162 H 0.8064 0.4700 0.5336 0.0516 1.0000 Uiso R . . . . . H163 H 0.7332 0.4360 0.5843 0.0504 1.0000 Uiso R . . . . . 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 Cr1 0.01598(12) 0.01598(12) 0.01315(17) 0.0000 0.0000 0.00799(6) Co2 0.01330(11) 0.01330(11) 0.01089(14) 0.0000 0.0000 0.00665(5) P1 0.01896(18) 0.01685(18) 0.01461(16) -0.00116(13) -0.00207(13) 0.01049(15) P2 0.01957(19) 0.01957(19) 0.0122(3) 0.0000 0.0000 0.00979(10) N1 0.0255(6) 0.0213(6) 0.0144(5) 0.0023(4) -0.0007(5) 0.0142(5) C1 0.0387(9) 0.0294(8) 0.0176(7) 0.0054(6) -0.0014(6) 0.0227(7) C2 0.0556(12) 0.0436(11) 0.0163(7) 0.0033(7) -0.0060(7) 0.0322(10) C3 0.0513(12) 0.0313(10) 0.0304(9) 0.0126(7) 0.0043(8) 0.0202(9) C4 0.0239(7) 0.0175(7) 0.0189(7) -0.0007(5) -0.0016(5) 0.0108(6) C5 0.0335(9) 0.0242(8) 0.0348(9) -0.0028(7) -0.0099(7) 0.0176(7) C6 0.0434(11) 0.0216(8) 0.0518(12) -0.0021(8) -0.0047(9) 0.0200(8) C7 0.0388(11) 0.0200(8) 0.0509(12) -0.0082(8) 0.0002(9) 0.0103(8) C8 0.0249(8) 0.0275(9) 0.0431(10) -0.0096(7) -0.0028(7) 0.0086(7) C9 0.0229(8) 0.0245(8) 0.0270(8) -0.0030(6) -0.0007(6) 0.0126(7) C10 0.0214(7) 0.0197(7) 0.0217(7) -0.0013(5) -0.0032(5) 0.0125(6) C11 0.0244(8) 0.0311(8) 0.0231(7) -0.0048(6) -0.0047(6) 0.0153(7) C12 0.0257(9) 0.0449(11) 0.0330(9) -0.0063(8) -0.0103(7) 0.0186(8) C13 0.0222(8) 0.0443(11) 0.0453(10) -0.0039(8) -0.0012(7) 0.0207(8) C14 0.0282(9) 0.0346(9) 0.0337(9) -0.0049(7) 0.0028(7) 0.0206(8) C15 0.0256(8) 0.0262(8) 0.0251(7) -0.0060(6) -0.0023(6) 0.0162(7) C16 0.0431(10) 0.0291(9) 0.0188(7) -0.0056(6) -0.0048(7) 0.0094(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.078657(18) 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 Cr1 . P1 5_665 2.6485(4) yes Cr1 . P1 3_655 2.6485(4) yes Cr1 . N1 3_655 1.8658(12) yes Cr1 . N1 5_665 1.8658(12) yes Cr1 . Co2 . 2.3316(5) yes Cr1 . P1 . 2.6485(4) yes Cr1 . N1 . 1.8658(12) yes Co2 . P1 3_655 2.1753(4) yes Co2 . P1 5_665 2.1753(4) yes Co2 . P1 . 2.1753(4) yes Co2 . P2 . 2.1878(7) yes P1 . N1 . 1.6898(13) yes P1 . C4 . 1.8480(15) yes P1 . C10 . 1.8378(15) yes P2 . C16 3_655 1.8315(17) yes P2 . C16 5_665 1.8315(17) yes P2 . C16 . 1.8315(17) yes N1 . C1 . 1.4667(19) yes C1 . C2 . 1.524(2) yes C1 . C3 . 1.526(3) yes C1 . H11 . 1.025 no C2 . H21 . 0.959 no C2 . H22 . 0.942 no C2 . H23 . 0.972 no C3 . H31 . 0.964 no C3 . H32 . 0.969 no C3 . H33 . 0.975 no C4 . C5 . 1.398(2) yes C4 . C9 . 1.389(2) yes C5 . C6 . 1.385(2) yes C5 . H51 . 0.955 no C6 . C7 . 1.383(3) yes C6 . H61 . 0.919 no C7 . C8 . 1.383(3) yes C7 . H71 . 0.955 no C8 . C9 . 1.391(2) yes C8 . H81 . 0.948 no C9 . H91 . 0.926 no C10 . C11 . 1.390(2) yes C10 . C15 . 1.398(2) yes C11 . C12 . 1.391(2) yes C11 . H111 . 0.930 no C12 . C13 . 1.374(3) yes C12 . H121 . 0.935 no C13 . C14 . 1.384(3) yes C13 . H131 . 0.931 no C14 . C15 . 1.386(2) yes C14 . H141 . 0.933 no C15 . H151 . 0.952 no C16 . H161 . 0.966 no C16 . H162 . 0.974 no C16 . H163 . 0.960 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 P1 5_665 Cr1 . P1 3_655 85.069(15) yes P1 5_665 Cr1 . N1 3_655 118.16(4) yes P1 3_655 Cr1 . N1 3_655 39.37(4) yes P1 5_665 Cr1 . N1 5_665 39.37(4) yes P1 3_655 Cr1 . N1 5_665 107.82(4) yes N1 3_655 Cr1 . N1 5_665 119.999(3) yes P1 5_665 Cr1 . Co2 . 51.317(10) yes P1 3_655 Cr1 . Co2 . 51.317(10) yes N1 3_655 Cr1 . Co2 . 90.15(4) yes N1 5_665 Cr1 . Co2 . 90.15(4) yes P1 5_665 Cr1 . P1 . 85.069(15) yes P1 3_655 Cr1 . P1 . 85.069(15) yes N1 3_655 Cr1 . P1 . 107.82(4) yes N1 5_665 Cr1 . P1 . 118.16(4) yes Co2 . Cr1 . P1 . 51.317(10) yes P1 5_665 Cr1 . N1 . 107.82(4) yes P1 3_655 Cr1 . N1 . 118.16(4) yes N1 3_655 Cr1 . N1 . 119.999(3) yes N1 5_665 Cr1 . N1 . 119.999 yes Co2 . Cr1 . N1 . 90.15(4) yes P1 . Cr1 . N1 . 39.37(4) yes P1 3_655 Co2 . P1 5_665 110.794(12) yes P1 3_655 Co2 . Cr1 . 71.887(12) yes P1 5_665 Co2 . Cr1 . 71.887(12) yes P1 3_655 Co2 . P1 . 110.794(12) yes P1 5_665 Co2 . P1 . 110.794(11) yes Cr1 . Co2 . P1 . 71.887(12) yes P1 3_655 Co2 . P2 . 108.113(12) yes P1 5_665 Co2 . P2 . 108.113(12) yes Cr1 . Co2 . P2 . 179.995 yes P1 . Co2 . P2 . 108.113(12) yes Cr1 . P1 . Co2 . 56.796(13) yes Co2 . P1 . N1 . 100.61(5) yes Cr1 . P1 . C4 . 136.48(5) yes Co2 . P1 . C4 . 125.48(5) yes N1 . P1 . C4 . 106.17(7) yes Cr1 . P1 . C10 . 116.81(5) yes Co2 . P1 . C10 . 119.59(5) yes N1 . P1 . C10 . 103.50(7) yes C4 . P1 . C10 . 99.10(7) yes C16 3_655 P2 . C16 5_665 99.09(7) yes C16 3_655 P2 . Co2 . 118.52(6) yes C16 5_665 P2 . Co2 . 118.52(6) yes C16 3_655 P2 . C16 . 99.09(7) yes C16 5_665 P2 . C16 . 99.09(7) yes Co2 . P2 . C16 . 118.52(6) yes P1 . N1 . Cr1 . 96.17(6) yes P1 . N1 . C1 . 128.21(11) yes Cr1 . N1 . C1 . 135.15(10) yes N1 . C1 . C2 . 108.91(14) yes N1 . C1 . C3 . 111.21(14) yes C2 . C1 . C3 . 111.10(15) yes N1 . C1 . H11 . 108.4 no C2 . C1 . H11 . 108.4 no C3 . C1 . H11 . 108.7 no C1 . C2 . H21 . 111.2 no C1 . C2 . H22 . 109.8 no H21 . C2 . H22 . 107.6 no C1 . C2 . H23 . 111.5 no H21 . C2 . H23 . 106.1 no H22 . C2 . H23 . 110.4 no C1 . C3 . H31 . 111.2 no C1 . C3 . H32 . 109.9 no H31 . C3 . H32 . 109.1 no C1 . C3 . H33 . 108.4 no H31 . C3 . H33 . 108.5 no H32 . C3 . H33 . 109.9 no P1 . C4 . C5 . 122.59(12) yes P1 . C4 . C9 . 119.21(12) yes C5 . C4 . C9 . 118.16(14) yes C4 . C5 . C6 . 121.02(16) yes C4 . C5 . H51 . 118.8 no C6 . C5 . H51 . 120.2 no C5 . C6 . C7 . 120.02(17) yes C5 . C6 . H61 . 119.2 no C7 . C6 . H61 . 120.7 no C6 . C7 . C8 . 119.79(17) yes C6 . C7 . H71 . 120.2 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 120.11(17) yes C7 . C8 . H81 . 120.5 no C9 . C8 . H81 . 119.3 no C8 . C9 . C4 . 120.90(16) yes C8 . C9 . H91 . 119.5 no C4 . C9 . H91 . 119.6 no P1 . C10 . C11 . 121.85(12) yes P1 . C10 . C15 . 119.97(11) yes C11 . C10 . C15 . 117.88(14) yes C10 . C11 . C12 . 120.71(15) yes C10 . C11 . H111 . 118.6 no C12 . C11 . H111 . 120.7 no C11 . C12 . C13 . 120.64(16) yes C11 . C12 . H121 . 118.5 no C13 . C12 . H121 . 120.8 no C12 . C13 . C14 . 119.62(17) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 119.92(16) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 119.5 no C10 . C15 . C14 . 121.22(15) yes C10 . C15 . H151 . 119.4 no C14 . C15 . H151 . 119.4 no P2 . C16 . H161 . 109.8 no P2 . C16 . H162 . 109.9 no H161 . C16 . H162 . 110.2 no P2 . C16 . H163 . 110.2 no H161 . C16 . H163 . 109.8 no H162 . C16 . H163 . 106.9 no _iucr_refine_instructions_details_constraints ; # # Punched on 05/04/13 at 09:09:37 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 05/04/13 at 09:09:37 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.001 924 98 ' ' _platon_squeeze_details ; During the structure solution, electron density difference maps revealed that there were considerable disordered solvent molecules which could not be successfully modeled. From history, the remaining solvate was likely diethyl ether in a volume of 923.6 \%A3 per unit cell (17.6%). It appeared that the cavity area contained ca. three ether molecules, located near the position at (0, 0, 0). Modeling with or without restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE technique, in order to produce a "solvate-free" structure factor set. PLATON reported a total electron density of 97 e- per unit cell, likely representing three diethyl ether molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca. 1.9 % in R. ; _database_code_depnum_ccdc_archive 'CCDC 966659' ####################################################################### # # 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_6*0.75THF _audit_creation_date 2013-05-15 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 'sk_835_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.7036(3) _cell_length_b 22.2854(6) _cell_length_c 22.5333(6) _cell_angle_alpha 61.7630(10) _cell_angle_beta 81.3270(10) _cell_angle_gamma 87.5150(10) _cell_volume 4678.8(2) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' _cell_formula_units_Z 4 # Given Formula = C48 H57 Cr1 Cu1 I1 N3 O0.75 P3 # Dc = 1.45 Fooo = 2092.00 Mu = 14.87 M = 2046.74 # Found Formula = C48 H57 Cr1 Cu1 I1 N3 O0.75 P3 # Dc = 1.45 FOOO = 2092.00 Mu = 14.87 M = 2046.73 _chemical_formula_sum 'C48 H57 Cr1 Cu1 I1 N3 O0.75 P3' _chemical_formula_moiety 'C48 H57 Cr1 Cu1 I1 N3 O0.75 P3' _chemical_compound_source ? _chemical_formula_weight 1023.37 _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _cell_measurement_temperature 120 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 1.487 # Sheldrick geometric approximatio 0.79 0.94 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 81740 _reflns_number_total 22585 _diffrn_reflns_av_R_equivalents 0.054 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 22585 # Theoretical number of reflections is about 45407 _diffrn_reflns_theta_min 1.830 _diffrn_reflns_theta_max 28.049 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.049 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -25 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.17 _refine_diff_density_max 1.66 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 22585 _refine_ls_number_restraints 2 _refine_ls_number_parameters 1044 _oxford_refine_ls_R_factor_ref 0.0729 _refine_ls_wR_factor_ref 0.1193 _refine_ls_goodness_of_fit_ref 1.0135 _refine_ls_shift/su_max 0.0091843 _refine_ls_shift/su_mean 0.0001369 # The values computed with all filters except I/sigma _oxford_reflns_number_all 22585 _refine_ls_R_factor_all 0.0729 _refine_ls_wR_factor_all 0.1193 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 17671 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_gt 0.1142 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +26.47P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Cu1 Cu 0.58620(5) 0.70800(2) 0.02428(2) 0.0115 1.0000 Uani . . . . . . Cu101 Cu 0.92086(5) 0.75441(3) 0.45259(3) 0.0184 1.0000 Uani D U . . . . Cr1 Cr 0.80107(6) 0.77372(3) -0.04750(3) 0.0122 1.0000 Uani . . . . . . Cr101 Cr 1.11438(7) 0.81305(4) 0.46544(4) 0.0185 1.0000 Uani . . . . . . I1 I 0.37961(3) 0.644403(15) 0.097296(14) 0.0188 1.0000 Uani . . . . . . I101 I 0.73756(5) 0.69386(3) 0.44188(2) 0.0285 0.904(3) Uani . . P . . . I102 I 0.6996(10) 0.7182(7) 0.4413(5) 0.103(3) 0.096(3) Uiso D U P . . . P1 P 0.63055(10) 0.70860(5) -0.07976(5) 0.0119 1.0000 Uani . . . . . . P2 P 0.75929(10) 0.66080(5) 0.07899(5) 0.0142 1.0000 Uani . . . . . . P3 P 0.59024(10) 0.82200(5) 0.00024(5) 0.0133 1.0000 Uani . . . . . . P101 P 0.95774(11) 0.86538(6) 0.36615(6) 0.0195 1.0000 Uani . . . . . . P102 P 1.10661(12) 0.69670(6) 0.45281(6) 0.0223 1.0000 Uani . . . . . . P103 P 0.89287(11) 0.76117(6) 0.55337(6) 0.0181 1.0000 Uani . . . . . . O1 O 0.4951(10) 0.5312(6) 0.4221(6) 0.067(3) 0.5000 Uiso . . . 1 1 . O2 O 0.5719(4) 0.3480(2) 0.3491(2) 0.0430 1.0000 Uani . . . . . . N1 N 0.7597(3) 0.76093(18) -0.11911(17) 0.0146 1.0000 Uani . . . . . . N2 N 0.8829(3) 0.70750(18) 0.02194(18) 0.0158 1.0000 Uani . . . . . . N3 N 0.7392(3) 0.84963(17) -0.03969(17) 0.0148 1.0000 Uani . . . . . . N101 N 1.0783(4) 0.8929(2) 0.38839(19) 0.0233 1.0000 Uani . . . . . . N102 N 1.2161(4) 0.7494(2) 0.4521(2) 0.0236 1.0000 Uani . . . . . . N103 N 1.0339(3) 0.79324(19) 0.55329(19) 0.0193 1.0000 Uani . . . . . . C1 C 0.8177(4) 0.7807(2) -0.1900(2) 0.0195 1.0000 Uani . . . . . . C2 C 0.9619(5) 0.7891(3) -0.1973(3) 0.0320 1.0000 Uani . . . . . . C3 C 0.7631(5) 0.8461(2) -0.2402(2) 0.0263 1.0000 Uani . . . . . . C4 C 0.6770(4) 0.6288(2) -0.0792(2) 0.0141 1.0000 Uani . . . . . . C5 C 0.8030(4) 0.6096(2) -0.0755(2) 0.0188 1.0000 Uani . . . . . . C6 C 0.8380(5) 0.5468(2) -0.0701(2) 0.0255 1.0000 Uani . . . . . . C7 C 0.7495(5) 0.5030(2) -0.0689(2) 0.0253 1.0000 Uani . . . . . . C8 C 0.6232(5) 0.5211(2) -0.0721(2) 0.0227 1.0000 Uani . . . . . . C9 C 0.5882(4) 0.5837(2) -0.0765(2) 0.0188 1.0000 Uani . . . . . . C10 C 0.5078(4) 0.7358(2) -0.1348(2) 0.0131 1.0000 Uani . . . . . . C11 C 0.5193(4) 0.7305(2) -0.1947(2) 0.0198 1.0000 Uani . . . . . . C12 C 0.4244(5) 0.7535(2) -0.2353(2) 0.0230 1.0000 Uani . . . . . . C13 C 0.3176(4) 0.7810(2) -0.2165(2) 0.0235 1.0000 Uani . . . . . . C14 C 0.3048(4) 0.7858(2) -0.1573(2) 0.0232 1.0000 Uani . . . . . . C15 C 0.3997(4) 0.7631(2) -0.1160(2) 0.0168 1.0000 Uani . . . . . . C16 C 1.0181(4) 0.6951(2) 0.0293(2) 0.0215 1.0000 Uani . . . . . . C17 C 1.0896(4) 0.7621(2) 0.0033(3) 0.0273 1.0000 Uani . . . . . . C18 C 1.0746(4) 0.6566(2) -0.0081(3) 0.0270 1.0000 Uani . . . . . . C19 C 0.7594(4) 0.6691(2) 0.1554(2) 0.0172 1.0000 Uani . . . . . . C20 C 0.8292(5) 0.7192(3) 0.1569(3) 0.0284 1.0000 Uani . . . . . . C21 C 0.8173(6) 0.7256(3) 0.2156(3) 0.0389 1.0000 Uani . . . . . . C22 C 0.7363(6) 0.6840(3) 0.2723(3) 0.0380 1.0000 Uani . . . . . . C23 C 0.6638(5) 0.6349(3) 0.2711(3) 0.0324 1.0000 Uani . . . . . . C24 C 0.6746(5) 0.6274(2) 0.2134(2) 0.0239 1.0000 Uani . . . . . . C25 C 0.7897(4) 0.5699(2) 0.1110(2) 0.0166 1.0000 Uani . . . . . . C26 C 0.8761(4) 0.5369(2) 0.1560(2) 0.0214 1.0000 Uani . . . . . . C27 C 0.8972(5) 0.4683(2) 0.1793(2) 0.0259 1.0000 Uani . . . . . . C28 C 0.8320(5) 0.4313(3) 0.1580(3) 0.0301 1.0000 Uani . . . . . . C29 C 0.7457(5) 0.4634(3) 0.1138(3) 0.0312 1.0000 Uani . . . . . . C30 C 0.7236(5) 0.5324(2) 0.0909(2) 0.0234 1.0000 Uani . . . . . . C31 C 0.7967(4) 0.9178(2) -0.0641(2) 0.0195 1.0000 Uani . . . . . . C32 C 0.8910(5) 0.9360(3) -0.1286(3) 0.0299 1.0000 Uani . . . . . . C33 C 0.8641(5) 0.9193(3) -0.0092(3) 0.0280 1.0000 Uani . . . . . . C34 C 0.4849(4) 0.8780(2) -0.0577(2) 0.0174 1.0000 Uani . . . . . . C35 C 0.5238(5) 0.9122(2) -0.1282(2) 0.0221 1.0000 Uani . . . . . . C36 C 0.4399(5) 0.9509(2) -0.1725(2) 0.0272 1.0000 Uani . . . . . . C37 C 0.3162(5) 0.9555(3) -0.1468(3) 0.0325 1.0000 Uani . . . . . . C38 C 0.2755(5) 0.9216(3) -0.0772(3) 0.0323 1.0000 Uani . . . . . . C39 C 0.3597(4) 0.8829(2) -0.0329(3) 0.0248 1.0000 Uani . . . . . . C40 C 0.5546(4) 0.8425(2) 0.0701(2) 0.0162 1.0000 Uani . . . . . . C41 C 0.5525(4) 0.9099(2) 0.0586(2) 0.0219 1.0000 Uani . . . . . . C42 C 0.5332(5) 0.9236(3) 0.1129(3) 0.0290 1.0000 Uani . . . . . . C43 C 0.5133(5) 0.8706(3) 0.1792(3) 0.0343 1.0000 Uani . . . . . . C44 C 0.5097(5) 0.8041(3) 0.1910(3) 0.0336 1.0000 Uani . . . . . . C45 C 0.5303(5) 0.7900(3) 0.1365(2) 0.0256 1.0000 Uani . . . . . . C46 C 0.5419(6) 0.3792(3) 0.2820(3) 0.0406 1.0000 Uani . . . . . . C47 C 0.5418(6) 0.4550(3) 0.2598(3) 0.0396 1.0000 Uani . . . . . . C48 C 0.5015(5) 0.4580(3) 0.3253(3) 0.0342 1.0000 Uani . . . . . . C49 C 0.5023(6) 0.3847(3) 0.3800(3) 0.0413 1.0000 Uani . . . . . . C51 C 0.5842(11) 0.5266(5) 0.4599(4) 0.0942 1.0000 Uani . . . . . . C101 C 1.1271(5) 0.9639(3) 0.3564(2) 0.0285 1.0000 Uani . . . . . . C102 C 1.2683(5) 0.9644(3) 0.3557(3) 0.0395 1.0000 Uani . . . . . . C103 C 1.0603(5) 1.0001(3) 0.3937(3) 0.0324 1.0000 Uani . . . . . . C104 C 1.0067(5) 0.8796(2) 0.2791(2) 0.0227 1.0000 Uani . . . . . . C105 C 1.1325(5) 0.8773(3) 0.2541(3) 0.0346 1.0000 Uani . . . . . . C106 C 1.1654(6) 0.8815(3) 0.1901(3) 0.0404 1.0000 Uani . . . . . . C107 C 1.0755(6) 0.8878(3) 0.1506(3) 0.0421 1.0000 Uani . . . . . . C108 C 0.9500(6) 0.8903(3) 0.1743(3) 0.0383 1.0000 Uani . . . . . . C109 C 0.9146(5) 0.8857(3) 0.2387(3) 0.0292 1.0000 Uani . . . . . . C110 C 0.8290(4) 0.9249(2) 0.3529(2) 0.0208 1.0000 Uani . . . . . . C111 C 0.8415(5) 0.9931(3) 0.3031(3) 0.0294 1.0000 Uani . . . . . . C112 C 0.7447(6) 1.0362(3) 0.2977(3) 0.0392 1.0000 Uani . . . . . . C113 C 0.6303(6) 1.0132(3) 0.3405(3) 0.0420 1.0000 Uani . . . . . . C114 C 0.6148(5) 0.9462(3) 0.3888(3) 0.0431 1.0000 Uani . . . . . . C115 C 0.7142(5) 0.9014(3) 0.3960(3) 0.0323 1.0000 Uani . . . . . . C116 C 1.3555(5) 0.7429(3) 0.4438(2) 0.0303 1.0000 Uani . . . . . . C117 C 1.4106(5) 0.7714(3) 0.4839(3) 0.0341 1.0000 Uani . . . . . . C118 C 1.4111(5) 0.7810(3) 0.3690(3) 0.0408 1.0000 Uani . . . . . . C119 C 1.1178(5) 0.6150(3) 0.5276(2) 0.0270 1.0000 Uani . . . . . . C120 C 1.1725(5) 0.6097(3) 0.5820(3) 0.0294 1.0000 Uani . . . . . . C121 C 1.1685(5) 0.5480(3) 0.6413(3) 0.0367 1.0000 Uani . . . . . . C122 C 1.1095(6) 0.4915(3) 0.6479(3) 0.0393 1.0000 Uani . . . . . . C123 C 1.0523(6) 0.4953(3) 0.5952(3) 0.0427 1.0000 Uani . . . . . . C124 C 1.0570(6) 0.5568(3) 0.5352(3) 0.0382 1.0000 Uani . . . . . . C125 C 1.1547(5) 0.6765(3) 0.3831(3) 0.0285 1.0000 Uani . . . . . . C126 C 1.2562(6) 0.6362(4) 0.3833(3) 0.0476 1.0000 Uani . . . . . . C127 C 1.2938(6) 0.6241(4) 0.3285(3) 0.0538 1.0000 Uani . . . . . . C128 C 1.2299(6) 0.6506(4) 0.2740(3) 0.0487 1.0000 Uani . . . . . . C129 C 1.1260(7) 0.6901(3) 0.2734(3) 0.0474 1.0000 Uani . . . . . . C130 C 1.0874(5) 0.7030(3) 0.3279(3) 0.0324 1.0000 Uani . . . . . . C131 C 1.0686(4) 0.7988(2) 0.6111(2) 0.0233 1.0000 Uani . . . . . . C132 C 1.1578(4) 0.8620(2) 0.5862(2) 0.0218 1.0000 Uani . . . . . . C133 C 1.1350(5) 0.7353(3) 0.6569(2) 0.0268 1.0000 Uani . . . . . . C134 C 0.7714(4) 0.8175(2) 0.5627(2) 0.0195 1.0000 Uani . . . . . . C135 C 0.8001(5) 0.8848(3) 0.5456(3) 0.0274 1.0000 Uani . . . . . . C136 C 0.7032(6) 0.9280(3) 0.5465(3) 0.0374 1.0000 Uani . . . . . . C137 C 0.5791(5) 0.9051(3) 0.5633(3) 0.0380 1.0000 Uani . . . . . . C138 C 0.5495(5) 0.8392(3) 0.5804(3) 0.0315 1.0000 Uani . . . . . . C139 C 0.6446(5) 0.7948(3) 0.5804(2) 0.0270 1.0000 Uani . . . . . . C140 C 0.8510(4) 0.6821(2) 0.6319(2) 0.0208 1.0000 Uani . . . . . . C141 C 0.8208(5) 0.6805(2) 0.6949(2) 0.0235 1.0000 Uani . . . . . . C142 C 0.7900(5) 0.6190(3) 0.7541(2) 0.0274 1.0000 Uani . . . . . . C143 C 0.7928(5) 0.5589(3) 0.7505(3) 0.0297 1.0000 Uani . . . . . . C144 C 0.8232(5) 0.5597(2) 0.6880(3) 0.0286 1.0000 Uani . . . . . . C145 C 0.8520(5) 0.6208(2) 0.6290(2) 0.0257 1.0000 Uani . . . . . . C500 C 0.4044(16) 0.4828(9) 0.4705(8) 0.060(4) 0.5000 Uiso . . . . . . C501 C 0.532(2) 0.5232(11) 0.5182(11) 0.087(6) 0.5000 Uiso . . . . . . H11 H 0.8014 0.7440 -0.2005 0.0237 1.0000 Uiso R . . . . . H21 H 0.9950 0.7461 -0.1694 0.0481 1.0000 Uiso R . . . . . H22 H 0.9830 0.8211 -0.1828 0.0477 1.0000 Uiso R . . . . . H23 H 0.9991 0.8052 -0.2439 0.0480 1.0000 Uiso R . . . . . H31 H 0.6735 0.8427 -0.2332 0.0397 1.0000 Uiso R . . . . . H32 H 0.7894 0.8832 -0.2340 0.0395 1.0000 Uiso R . . . . . H33 H 0.7939 0.8555 -0.2858 0.0395 1.0000 Uiso R . . . . . H51 H 0.8632 0.6389 -0.0766 0.0230 1.0000 Uiso R . . . . . H61 H 0.9211 0.5345 -0.0677 0.0310 1.0000 Uiso R . . . . . H71 H 0.7734 0.4609 -0.0660 0.0312 1.0000 Uiso R . . . . . H81 H 0.5634 0.4923 -0.0726 0.0268 1.0000 Uiso R . . . . . H91 H 0.5055 0.5956 -0.0773 0.0233 1.0000 Uiso R . . . . . H111 H 0.5904 0.7113 -0.2072 0.0238 1.0000 Uiso R . . . . . H121 H 0.4321 0.7491 -0.2747 0.0278 1.0000 Uiso R . . . . . H131 H 0.2558 0.7965 -0.2438 0.0287 1.0000 Uiso R . . . . . H141 H 0.2332 0.8046 -0.1444 0.0277 1.0000 Uiso R . . . . . H151 H 0.3914 0.7658 -0.0758 0.0207 1.0000 Uiso R . . . . . H161 H 1.0231 0.6681 0.0777 0.0258 1.0000 Uiso R . . . . . H171 H 1.0535 0.7837 0.0295 0.0417 1.0000 Uiso R . . . . . H172 H 1.1771 0.7548 0.0067 0.0414 1.0000 Uiso R . . . . . H173 H 1.0786 0.7905 -0.0433 0.0418 1.0000 Uiso R . . . . . H181 H 1.0700 0.6826 -0.0559 0.0408 1.0000 Uiso R . . . . . H182 H 1.1626 0.6485 -0.0030 0.0408 1.0000 Uiso R . . . . . H183 H 1.0301 0.6140 0.0091 0.0405 1.0000 Uiso R . . . . . H201 H 0.8840 0.7483 0.1187 0.0336 1.0000 Uiso R . . . . . H211 H 0.8652 0.7581 0.2172 0.0469 1.0000 Uiso R . . . . . H221 H 0.7287 0.6892 0.3111 0.0460 1.0000 Uiso R . . . . . H231 H 0.6082 0.6074 0.3089 0.0392 1.0000 Uiso R . . . . . H241 H 0.6250 0.5947 0.2127 0.0293 1.0000 Uiso R . . . . . H261 H 0.9211 0.5606 0.1710 0.0261 1.0000 Uiso R . . . . . H271 H 0.9549 0.4470 0.2091 0.0310 1.0000 Uiso R . . . . . H281 H 0.8442 0.3851 0.1741 0.0371 1.0000 Uiso R . . . . . H291 H 0.7014 0.4388 0.0991 0.0383 1.0000 Uiso R . . . . . H301 H 0.6639 0.5534 0.0624 0.0280 1.0000 Uiso R . . . . . H311 H 0.7291 0.9502 -0.0739 0.0240 1.0000 Uiso R . . . . . H321 H 0.9569 0.9033 -0.1200 0.0450 1.0000 Uiso R . . . . . H322 H 0.9274 0.9807 -0.1461 0.0448 1.0000 Uiso R . . . . . H323 H 0.8471 0.9351 -0.1619 0.0449 1.0000 Uiso R . . . . . H331 H 0.8049 0.9078 0.0311 0.0427 1.0000 Uiso R . . . . . H332 H 0.9291 0.8870 0.0009 0.0428 1.0000 Uiso R . . . . . H333 H 0.8990 0.9640 -0.0258 0.0430 1.0000 Uiso R . . . . . H351 H 0.6059 0.9084 -0.1458 0.0265 1.0000 Uiso R . . . . . H361 H 0.4674 0.9734 -0.2187 0.0325 1.0000 Uiso R . . . . . H371 H 0.2618 0.9814 -0.1764 0.0392 1.0000 Uiso R . . . . . H381 H 0.1933 0.9250 -0.0597 0.0388 1.0000 Uiso R . . . . . H391 H 0.3330 0.8598 0.0137 0.0297 1.0000 Uiso R . . . . . H411 H 0.5639 0.9456 0.0141 0.0270 1.0000 Uiso R . . . . . H421 H 0.5337 0.9689 0.1048 0.0349 1.0000 Uiso R . . . . . H431 H 0.5012 0.8804 0.2157 0.0410 1.0000 Uiso R . . . . . H441 H 0.4952 0.7690 0.2351 0.0405 1.0000 Uiso R . . . . . H451 H 0.5270 0.7456 0.1441 0.0311 1.0000 Uiso R . . . . . H461 H 0.6043 0.3692 0.2513 0.0491 1.0000 Uiso R . . . . . H462 H 0.4554 0.3632 0.2826 0.0490 1.0000 Uiso R . . . . . H471 H 0.6262 0.4755 0.2396 0.0481 1.0000 Uiso R . . . . . H472 H 0.4824 0.4783 0.2278 0.0481 1.0000 Uiso R . . . . . H481 H 0.5596 0.4860 0.3311 0.0422 1.0000 Uiso R . . . . . H482 H 0.4172 0.4762 0.3254 0.0421 1.0000 Uiso R . . . . . H491 H 0.5463 0.3822 0.4167 0.0504 1.0000 Uiso R . . . . . H492 H 0.4150 0.3654 0.3983 0.0505 1.0000 Uiso R . . . . . H1011 H 1.1102 0.9875 0.3094 0.0349 1.0000 Uiso R . . . . . H1021 H 1.2854 0.9372 0.4015 0.0601 1.0000 Uiso R . . . . . H1022 H 1.3002 1.0106 0.3380 0.0596 1.0000 Uiso R . . . . . H1023 H 1.3070 0.9447 0.3275 0.0595 1.0000 Uiso R . . . . . H1031 H 1.0711 0.9745 0.4407 0.0491 1.0000 Uiso R . . . . . H1032 H 1.0960 1.0457 0.3739 0.0488 1.0000 Uiso R . . . . . H1033 H 0.9724 1.0016 0.3882 0.0480 1.0000 Uiso R . . . . . H1051 H 1.1951 0.8733 0.2803 0.0421 1.0000 Uiso R . . . . . H1061 H 1.2501 0.8795 0.1741 0.0489 1.0000 Uiso R . . . . . H1071 H 1.0997 0.8903 0.1077 0.0507 1.0000 Uiso R . . . . . H1081 H 0.8883 0.8950 0.1474 0.0460 1.0000 Uiso R . . . . . H1091 H 0.8281 0.8850 0.2561 0.0347 1.0000 Uiso R . . . . . H1111 H 0.9170 1.0091 0.2738 0.0361 1.0000 Uiso R . . . . . H1121 H 0.7553 1.0822 0.2640 0.0468 1.0000 Uiso R . . . . . H1131 H 0.5644 1.0431 0.3363 0.0513 1.0000 Uiso R . . . . . H1141 H 0.5371 0.9299 0.4174 0.0523 1.0000 Uiso R . . . . . H1151 H 0.7034 0.8561 0.4294 0.0392 1.0000 Uiso R . . . . . H1161 H 1.3762 0.6946 0.4624 0.0366 1.0000 Uiso R . . . . . H1171 H 1.3823 0.8175 0.4697 0.0510 1.0000 Uiso R . . . . . H1172 H 1.5023 0.7721 0.4755 0.0510 1.0000 Uiso R . . . . . H1173 H 1.3795 0.7438 0.5318 0.0504 1.0000 Uiso R . . . . . H1181 H 1.4041 0.8296 0.3536 0.0607 1.0000 Uiso R . . . . . H1182 H 1.4977 0.7710 0.3644 0.0611 1.0000 Uiso R . . . . . H1183 H 1.3682 0.7678 0.3425 0.0610 1.0000 Uiso R . . . . . H1201 H 1.2120 0.6481 0.5791 0.0348 1.0000 Uiso R . . . . . H1211 H 1.2065 0.5451 0.6772 0.0442 1.0000 Uiso R . . . . . H1221 H 1.1069 0.4502 0.6884 0.0480 1.0000 Uiso R . . . . . H1231 H 1.0101 0.4570 0.6004 0.0522 1.0000 Uiso R . . . . . H1241 H 1.0182 0.5596 0.4997 0.0471 1.0000 Uiso R . . . . . H1261 H 1.2990 0.6167 0.4211 0.0572 1.0000 Uiso R . . . . . H1271 H 1.3617 0.5973 0.3288 0.0651 1.0000 Uiso R . . . . . H1281 H 1.2574 0.6427 0.2369 0.0589 1.0000 Uiso R . . . . . H1291 H 1.0839 0.7093 0.2355 0.0568 1.0000 Uiso R . . . . . H1301 H 1.0170 0.7297 0.3278 0.0391 1.0000 Uiso R . . . . . H1311 H 0.9912 0.8015 0.6375 0.0289 1.0000 Uiso R . . . . . H1321 H 1.2319 0.8583 0.5610 0.0324 1.0000 Uiso R . . . . . H1322 H 1.1178 0.9008 0.5593 0.0328 1.0000 Uiso R . . . . . H1323 H 1.1778 0.8650 0.6219 0.0324 1.0000 Uiso R . . . . . H1331 H 1.0811 0.6958 0.6713 0.0409 1.0000 Uiso R . . . . . H1332 H 1.2156 0.7321 0.6316 0.0416 1.0000 Uiso R . . . . . H1333 H 1.1509 0.7385 0.6964 0.0409 1.0000 Uiso R . . . . . H1351 H 0.8834 0.9011 0.5334 0.0333 1.0000 Uiso R . . . . . H1361 H 0.7220 0.9728 0.5355 0.0451 1.0000 Uiso R . . . . . H1371 H 0.5146 0.9347 0.5628 0.0461 1.0000 Uiso R . . . . . H1381 H 0.4664 0.8240 0.5916 0.0381 1.0000 Uiso R . . . . . H1391 H 0.6236 0.7498 0.5918 0.0326 1.0000 Uiso R . . . . . H1411 H 0.8200 0.7205 0.6976 0.0290 1.0000 Uiso R . . . . . H1421 H 0.7689 0.6188 0.7963 0.0330 1.0000 Uiso R . . . . . H1431 H 0.7742 0.5175 0.7895 0.0365 1.0000 Uiso R . . . . . H1441 H 0.8224 0.5192 0.6859 0.0350 1.0000 Uiso R . . . . . H1451 H 0.8711 0.6207 0.5872 0.0308 1.0000 Uiso R . . . . . H5001 H 0.3220 0.4967 0.4597 0.0733 0.5000 Uiso R . . . . . H5002 H 0.4206 0.4407 0.4701 0.0733 0.5000 Uiso R . . . . . H5011 H 0.5054 0.5669 0.5118 0.1072 0.5000 Uiso R . . . . . H5012 H 0.5881 0.5059 0.5511 0.1072 0.5000 Uiso R . . . . . H511 H 0.6408 0.5651 0.4358 0.1076 0.5000 Uiso R . . 1 1 . H512 H 0.6293 0.4863 0.4689 0.1076 0.5000 Uiso R . . 1 1 . H513 H 0.6572 0.5121 0.4412 0.1076 0.5000 Uiso R . . 1 2 . H514 H 0.5677 0.5722 0.4289 0.1076 0.5000 Uiso R . . 1 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 Cu1 0.0128(2) 0.0121(2) 0.0103(2) -0.00574(19) -0.00197(18) -0.00027(18) Cu101 0.0209(3) 0.0200(3) 0.0156(3) -0.0091(2) -0.0041(2) 0.0012(2) Cr1 0.0137(3) 0.0119(3) 0.0109(3) -0.0051(3) -0.0025(2) 0.0000(2) Cr101 0.0187(3) 0.0222(4) 0.0143(3) -0.0083(3) -0.0027(3) 0.0019(3) I1 0.01597(13) 0.02197(15) 0.01868(14) -0.01056(12) 0.00212(10) -0.00520(11) I101 0.0254(3) 0.0396(3) 0.0294(2) -0.02318(19) -0.00328(15) -0.00745(17) P1 0.0130(5) 0.0134(5) 0.0109(5) -0.0069(4) -0.0023(4) 0.0008(4) P2 0.0137(5) 0.0144(5) 0.0125(5) -0.0041(4) -0.0039(4) -0.0012(4) P3 0.0174(5) 0.0112(5) 0.0130(5) -0.0070(4) -0.0027(4) 0.0002(4) P101 0.0204(6) 0.0204(6) 0.0156(5) -0.0062(5) -0.0049(4) 0.0009(4) P102 0.0263(6) 0.0275(6) 0.0195(6) -0.0153(5) -0.0084(5) 0.0080(5) P103 0.0202(6) 0.0205(6) 0.0155(5) -0.0100(5) -0.0029(4) 0.0003(4) O2 0.042(2) 0.036(2) 0.044(2) -0.0151(19) -0.0012(19) 0.0045(18) N1 0.0154(17) 0.0169(17) 0.0115(16) -0.0070(14) -0.0007(13) 0.0010(14) N2 0.0105(16) 0.0172(18) 0.0168(18) -0.0053(15) -0.0030(13) -0.0002(13) N3 0.0177(17) 0.0125(17) 0.0141(17) -0.0059(14) -0.0027(14) -0.0027(14) N101 0.024(2) 0.022(2) 0.0199(19) -0.0055(16) -0.0062(16) -0.0032(16) N102 0.021(2) 0.031(2) 0.021(2) -0.0140(17) -0.0059(16) 0.0049(16) N103 0.0190(18) 0.023(2) 0.0180(18) -0.0115(16) -0.0020(15) -0.0001(15) C1 0.022(2) 0.024(2) 0.013(2) -0.0101(18) 0.0010(17) -0.0012(18) C2 0.022(2) 0.050(3) 0.023(3) -0.019(2) 0.006(2) -0.003(2) C3 0.035(3) 0.023(2) 0.012(2) -0.0023(18) -0.0004(19) -0.007(2) C4 0.020(2) 0.0138(19) 0.0097(18) -0.0066(16) -0.0018(15) 0.0010(16) C5 0.018(2) 0.020(2) 0.023(2) -0.0136(19) -0.0070(17) 0.0040(17) C6 0.026(2) 0.028(3) 0.025(2) -0.013(2) -0.0062(19) 0.009(2) C7 0.043(3) 0.014(2) 0.019(2) -0.0084(18) -0.002(2) 0.006(2) C8 0.029(2) 0.017(2) 0.021(2) -0.0080(18) -0.0024(19) -0.0019(18) C9 0.017(2) 0.018(2) 0.021(2) -0.0098(18) -0.0005(17) 0.0009(17) C10 0.0145(19) 0.0095(18) 0.0154(19) -0.0058(16) -0.0021(15) -0.0013(15) C11 0.021(2) 0.025(2) 0.018(2) -0.0136(19) -0.0043(17) 0.0068(18) C12 0.034(3) 0.026(2) 0.013(2) -0.0117(19) -0.0064(18) 0.001(2) C13 0.023(2) 0.025(2) 0.023(2) -0.009(2) -0.0129(19) 0.0046(19) C14 0.019(2) 0.025(2) 0.031(3) -0.017(2) -0.0100(19) 0.0080(18) C15 0.017(2) 0.019(2) 0.017(2) -0.0093(17) -0.0038(16) 0.0006(16) C16 0.013(2) 0.021(2) 0.024(2) -0.0030(19) -0.0084(17) 0.0001(17) C17 0.017(2) 0.024(2) 0.039(3) -0.013(2) -0.004(2) -0.0014(18) C18 0.015(2) 0.024(2) 0.036(3) -0.009(2) -0.0052(19) 0.0026(18) C19 0.018(2) 0.019(2) 0.014(2) -0.0066(17) -0.0073(16) 0.0020(17) C20 0.028(3) 0.030(3) 0.032(3) -0.017(2) -0.007(2) -0.003(2) C21 0.044(3) 0.044(3) 0.043(3) -0.030(3) -0.015(3) -0.003(3) C22 0.050(3) 0.047(3) 0.029(3) -0.024(3) -0.018(3) 0.012(3) C23 0.041(3) 0.038(3) 0.017(2) -0.011(2) -0.004(2) 0.004(2) C24 0.031(3) 0.021(2) 0.016(2) -0.0062(19) -0.0042(19) -0.0011(19) C25 0.017(2) 0.013(2) 0.0131(19) -0.0011(16) -0.0008(16) -0.0012(16) C26 0.019(2) 0.024(2) 0.019(2) -0.0076(19) -0.0048(17) 0.0004(18) C27 0.023(2) 0.022(2) 0.023(2) -0.0036(19) -0.0034(19) 0.0046(19) C28 0.040(3) 0.019(2) 0.027(3) -0.008(2) -0.007(2) 0.005(2) C29 0.047(3) 0.021(2) 0.028(3) -0.012(2) -0.008(2) -0.004(2) C30 0.029(2) 0.023(2) 0.018(2) -0.0079(19) -0.0080(19) 0.0005(19) C31 0.027(2) 0.013(2) 0.019(2) -0.0083(17) -0.0023(18) -0.0039(17) C32 0.037(3) 0.024(2) 0.027(3) -0.012(2) 0.006(2) -0.013(2) C33 0.031(3) 0.026(3) 0.033(3) -0.017(2) -0.008(2) -0.006(2) C34 0.023(2) 0.014(2) 0.021(2) -0.0108(17) -0.0095(17) 0.0000(17) C35 0.031(3) 0.021(2) 0.021(2) -0.0150(19) -0.0086(19) 0.0061(19) C36 0.044(3) 0.022(2) 0.020(2) -0.011(2) -0.015(2) 0.003(2) C37 0.039(3) 0.026(3) 0.041(3) -0.018(2) -0.027(2) 0.010(2) C38 0.021(2) 0.032(3) 0.048(3) -0.021(3) -0.011(2) 0.001(2) C39 0.021(2) 0.024(2) 0.028(3) -0.011(2) -0.0053(19) -0.0016(19) C40 0.018(2) 0.019(2) 0.014(2) -0.0095(17) -0.0035(16) 0.0033(16) C41 0.027(2) 0.020(2) 0.021(2) -0.0119(19) -0.0008(18) 0.0000(18) C42 0.036(3) 0.028(3) 0.034(3) -0.024(2) -0.004(2) 0.002(2) C43 0.046(3) 0.042(3) 0.027(3) -0.026(2) -0.007(2) 0.006(3) C44 0.052(3) 0.033(3) 0.017(2) -0.013(2) -0.006(2) 0.013(2) C45 0.039(3) 0.023(2) 0.015(2) -0.0104(19) -0.0003(19) 0.004(2) C46 0.042(3) 0.036(3) 0.044(3) -0.021(3) 0.001(3) -0.009(3) C47 0.041(3) 0.031(3) 0.042(3) -0.013(3) -0.005(3) -0.001(2) C48 0.030(3) 0.029(3) 0.043(3) -0.018(3) -0.003(2) 0.000(2) C49 0.042(3) 0.045(3) 0.036(3) -0.019(3) -0.003(3) 0.006(3) C51 0.143(10) 0.086(7) 0.048(5) -0.027(5) -0.004(5) -0.039(6) C101 0.031(3) 0.026(3) 0.021(2) -0.004(2) -0.004(2) -0.011(2) C102 0.030(3) 0.034(3) 0.043(3) -0.007(3) -0.008(2) -0.004(2) C103 0.043(3) 0.027(3) 0.026(3) -0.009(2) -0.009(2) -0.002(2) C104 0.028(2) 0.018(2) 0.018(2) -0.0060(18) -0.0005(18) -0.0002(18) C105 0.032(3) 0.043(3) 0.026(3) -0.014(2) -0.005(2) 0.009(2) C106 0.042(3) 0.042(3) 0.030(3) -0.015(3) 0.004(2) 0.006(3) C107 0.069(4) 0.031(3) 0.024(3) -0.015(2) 0.008(3) 0.001(3) C108 0.060(4) 0.030(3) 0.030(3) -0.017(2) -0.011(3) -0.003(3) C109 0.036(3) 0.028(3) 0.025(3) -0.013(2) -0.007(2) -0.002(2) C110 0.022(2) 0.023(2) 0.021(2) -0.0120(19) -0.0093(18) 0.0082(18) C111 0.030(3) 0.028(3) 0.026(3) -0.007(2) -0.009(2) 0.001(2) C112 0.052(4) 0.029(3) 0.043(3) -0.020(3) -0.018(3) 0.012(3) C113 0.048(4) 0.057(4) 0.036(3) -0.031(3) -0.024(3) 0.030(3) C114 0.028(3) 0.066(4) 0.035(3) -0.024(3) -0.009(2) 0.016(3) C115 0.033(3) 0.038(3) 0.022(2) -0.011(2) -0.007(2) 0.007(2) C116 0.026(3) 0.045(3) 0.022(2) -0.016(2) -0.008(2) 0.011(2) C117 0.024(3) 0.051(3) 0.030(3) -0.021(3) -0.006(2) 0.005(2) C118 0.028(3) 0.066(4) 0.021(3) -0.016(3) 0.000(2) 0.006(3) C119 0.037(3) 0.027(3) 0.022(2) -0.014(2) -0.012(2) 0.012(2) C120 0.030(3) 0.032(3) 0.026(3) -0.014(2) -0.005(2) 0.004(2) C121 0.032(3) 0.050(4) 0.028(3) -0.017(3) -0.013(2) 0.011(3) C122 0.044(3) 0.030(3) 0.038(3) -0.010(2) -0.013(3) 0.014(3) C123 0.067(4) 0.026(3) 0.036(3) -0.015(2) -0.010(3) 0.002(3) C124 0.060(4) 0.032(3) 0.034(3) -0.022(3) -0.017(3) 0.011(3) C125 0.034(3) 0.034(3) 0.024(2) -0.019(2) -0.007(2) 0.008(2) C126 0.046(4) 0.070(4) 0.052(4) -0.047(4) -0.023(3) 0.032(3) C127 0.049(4) 0.081(5) 0.056(4) -0.053(4) -0.012(3) 0.027(4) C128 0.060(4) 0.066(4) 0.036(3) -0.040(3) 0.002(3) 0.004(3) C129 0.069(4) 0.056(4) 0.030(3) -0.029(3) -0.016(3) 0.021(3) C130 0.042(3) 0.036(3) 0.024(3) -0.017(2) -0.010(2) 0.008(2) C131 0.024(2) 0.032(3) 0.023(2) -0.020(2) -0.0057(19) 0.004(2) C132 0.022(2) 0.020(2) 0.024(2) -0.0110(19) -0.0008(18) -0.0027(18) C133 0.029(3) 0.034(3) 0.021(2) -0.015(2) -0.010(2) 0.004(2) C134 0.019(2) 0.026(2) 0.017(2) -0.0127(19) -0.0030(17) 0.0033(18) C135 0.025(2) 0.029(3) 0.033(3) -0.017(2) -0.008(2) 0.002(2) C136 0.045(3) 0.030(3) 0.048(3) -0.026(3) -0.017(3) 0.013(2) C137 0.033(3) 0.054(4) 0.034(3) -0.027(3) -0.005(2) 0.017(3) C138 0.022(2) 0.043(3) 0.027(3) -0.014(2) -0.005(2) 0.008(2) C139 0.025(2) 0.036(3) 0.021(2) -0.014(2) -0.0036(19) 0.003(2) C140 0.022(2) 0.022(2) 0.018(2) -0.0090(19) -0.0042(17) 0.0005(18) C141 0.038(3) 0.019(2) 0.015(2) -0.0106(18) 0.0007(19) -0.001(2) C142 0.031(3) 0.032(3) 0.015(2) -0.007(2) -0.0034(19) 0.003(2) C143 0.032(3) 0.027(3) 0.021(2) -0.005(2) -0.002(2) -0.001(2) C144 0.034(3) 0.019(2) 0.031(3) -0.010(2) -0.007(2) 0.004(2) C145 0.031(3) 0.027(3) 0.022(2) -0.014(2) -0.004(2) 0.002(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.077299(10) 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 Cu1 . Cr1 . 2.6419(8) yes Cu1 . I1 . 2.5638(6) yes Cu1 . P1 . 2.3145(11) yes Cu1 . P2 . 2.3134(11) yes Cu1 . P3 . 2.3345(11) yes Cu101 . Cr101 . 2.6183(9) yes Cu101 . I101 . 2.5316(6) yes Cu101 . I102 . 2.621(7) yes Cu101 . P101 . 2.3153(13) yes Cu101 . P102 . 2.3198(13) yes Cu101 . P103 . 2.3203(12) yes Cr1 . P1 . 2.7557(12) yes Cr1 . P2 . 2.7536(12) yes Cr1 . P3 . 2.7496(12) yes Cr1 . N1 . 1.882(3) yes Cr1 . N2 . 1.873(3) yes Cr1 . N3 . 1.866(4) yes Cr101 . P101 . 2.7693(13) yes Cr101 . P102 . 2.7449(14) yes Cr101 . P103 . 2.7454(13) yes Cr101 . N101 . 1.884(4) yes Cr101 . N102 . 1.860(4) yes Cr101 . N103 . 1.883(4) yes P1 . N1 . 1.688(4) yes P1 . C4 . 1.820(4) yes P1 . C10 . 1.828(4) yes P2 . N2 . 1.681(4) yes P2 . C19 . 1.818(4) yes P2 . C25 . 1.832(4) yes P3 . N3 . 1.690(4) yes P3 . C34 . 1.820(4) yes P3 . C40 . 1.820(4) yes P101 . N101 . 1.687(4) yes P101 . C104 . 1.828(5) yes P101 . C110 . 1.827(5) yes P102 . N102 . 1.687(4) yes P102 . C119 . 1.819(5) yes P102 . C125 . 1.828(5) yes P103 . N103 . 1.698(4) yes P103 . C134 . 1.827(5) yes P103 . C140 . 1.821(5) yes O1 . H5012 2_666 1.128 no O1 . C501 2_666 1.32(2) yes O1 . C51 . 1.342(13) yes O1 . C500 . 1.398(19) yes O2 . C46 . 1.416(7) yes O2 . C49 . 1.427(7) yes N1 . C1 . 1.480(5) yes N2 . C16 . 1.481(5) yes N3 . C31 . 1.476(5) yes N101 . C101 . 1.474(6) yes N102 . C116 . 1.485(6) yes N103 . C131 . 1.467(5) yes C1 . C2 . 1.538(6) yes C1 . C3 . 1.519(6) yes C1 . H11 . 0.981 no C2 . H21 . 0.953 no C2 . H22 . 0.960 no C2 . H23 . 0.959 no C3 . H31 . 0.949 no C3 . H32 . 0.963 no C3 . H33 . 0.953 no C4 . C5 . 1.399(6) yes C4 . C9 . 1.388(6) yes C5 . C6 . 1.387(6) yes C5 . H51 . 0.926 no C6 . C7 . 1.377(7) yes C6 . H61 . 0.920 no C7 . C8 . 1.396(7) yes C7 . H71 . 0.937 no C8 . C9 . 1.391(6) yes C8 . H81 . 0.930 no C9 . H91 . 0.913 no C10 . C11 . 1.397(6) yes C10 . C15 . 1.387(6) yes C11 . C12 . 1.386(6) yes C11 . H111 . 0.928 no C12 . C13 . 1.378(7) yes C12 . H121 . 0.931 no C13 . C14 . 1.374(6) yes C13 . H131 . 0.914 no C14 . C15 . 1.395(6) yes C14 . H141 . 0.932 no C15 . H151 . 0.927 no C16 . C17 . 1.515(6) yes C16 . C18 . 1.517(7) yes C16 . H161 . 0.973 no C17 . H171 . 0.957 no C17 . H172 . 0.951 no C17 . H173 . 0.958 no C18 . H181 . 0.961 no C18 . H182 . 0.965 no C18 . H183 . 0.955 no C19 . C20 . 1.385(6) yes C19 . C24 . 1.400(6) yes C20 . C21 . 1.384(7) yes C20 . H201 . 0.926 no C21 . C22 . 1.363(8) yes C21 . H211 . 0.923 no C22 . C23 . 1.381(8) yes C22 . H221 . 0.928 no C23 . C24 . 1.375(7) yes C23 . H231 . 0.917 no C24 . H241 . 0.927 no C25 . C26 . 1.393(6) yes C25 . C30 . 1.383(6) yes C26 . C27 . 1.382(6) yes C26 . H261 . 0.930 no C27 . C28 . 1.387(7) yes C27 . H271 . 0.925 no C28 . C29 . 1.380(7) yes C28 . H281 . 0.925 no C29 . C30 . 1.394(7) yes C29 . H291 . 0.935 no C30 . H301 . 0.923 no C31 . C32 . 1.527(6) yes C31 . C33 . 1.535(6) yes C31 . H311 . 0.972 no C32 . H321 . 0.964 no C32 . H322 . 0.957 no C32 . H323 . 0.952 no C33 . H331 . 0.955 no C33 . H332 . 0.951 no C33 . H333 . 0.953 no C34 . C35 . 1.401(6) yes C34 . C39 . 1.392(6) yes C35 . C36 . 1.390(6) yes C35 . H351 . 0.926 no C36 . C37 . 1.382(8) yes C36 . H361 . 0.922 no C37 . C38 . 1.387(8) yes C37 . H371 . 0.917 no C38 . C39 . 1.394(7) yes C38 . H381 . 0.925 no C39 . H391 . 0.927 no C40 . C41 . 1.399(6) yes C40 . C45 . 1.388(6) yes C41 . C42 . 1.381(6) yes C41 . H411 . 0.933 no C42 . C43 . 1.387(7) yes C42 . H421 . 0.936 no C43 . C44 . 1.378(7) yes C43 . H431 . 0.936 no C44 . C45 . 1.392(6) yes C44 . H441 . 0.923 no C45 . H451 . 0.921 no C46 . C47 . 1.517(8) yes C46 . H461 . 0.984 no C46 . H462 . 1.002 no C47 . C48 . 1.507(8) yes C47 . H471 . 0.973 no C47 . H472 . 0.974 no C48 . C49 . 1.512(8) yes C48 . H481 . 0.963 no C48 . H482 . 0.973 no C49 . H491 . 0.990 no C49 . H492 . 0.989 no C51 . C501 2_666 1.56(2) yes C51 . C500 2_666 1.504(18) yes C51 . C501 . 1.32(2) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C51 . C501 2_666 1.56(2) yes C51 . C500 2_666 1.504(18) yes C51 . C501 . 1.32(2) yes C51 . H513 . 0.950 no C51 . H514 . 0.950 no C101 . C102 . 1.510(7) yes C101 . C103 . 1.512(7) yes C101 . H1011 . 0.976 no C102 . H1021 . 0.960 no C102 . H1022 . 0.969 no C102 . H1023 . 0.966 no C103 . H1031 . 0.959 no C103 . H1032 . 0.964 no C103 . H1033 . 0.965 no C104 . C105 . 1.387(7) yes C104 . C109 . 1.400(7) yes C105 . C106 . 1.392(7) yes C105 . H1051 . 0.932 no C106 . C107 . 1.367(9) yes C106 . H1061 . 0.931 no C107 . C108 . 1.377(9) yes C107 . H1071 . 0.938 no C108 . C109 . 1.399(7) yes C108 . H1081 . 0.932 no C109 . H1091 . 0.947 no C110 . C111 . 1.394(7) yes C110 . C115 . 1.394(7) yes C111 . C112 . 1.361(7) yes C111 . H1111 . 0.926 no C112 . C113 . 1.387(9) yes C112 . H1121 . 0.943 no C113 . C114 . 1.367(9) yes C113 . H1131 . 0.932 no C114 . C115 . 1.401(8) yes C114 . H1141 . 0.939 no C115 . H1151 . 0.929 no C116 . C117 . 1.517(7) yes C116 . C118 . 1.519(7) yes C116 . H1161 . 0.982 no C117 . H1171 . 0.970 no C117 . H1172 . 0.971 no C117 . H1173 . 0.967 no C118 . H1181 . 0.972 no C118 . H1182 . 0.945 no C118 . H1183 . 0.955 no C119 . C120 . 1.390(7) yes C119 . C124 . 1.401(7) yes C120 . C121 . 1.388(7) yes C120 . H1201 . 0.942 no C121 . C122 . 1.367(8) yes C121 . H1211 . 0.934 no C122 . C123 . 1.384(8) yes C122 . H1221 . 0.938 no C123 . C124 . 1.393(8) yes C123 . H1231 . 0.931 no C124 . H1241 . 0.933 no C125 . C126 . 1.379(7) yes C125 . C130 . 1.397(7) yes C126 . C127 . 1.384(8) yes C126 . H1261 . 0.935 no C127 . C128 . 1.363(9) yes C127 . H1271 . 0.919 no C128 . C129 . 1.386(9) yes C128 . H1281 . 0.936 no C129 . C130 . 1.391(7) yes C129 . H1291 . 0.932 no C130 . H1301 . 0.940 no C131 . C132 . 1.554(6) yes C131 . C133 . 1.524(7) yes C131 . H1311 . 0.961 no C132 . H1321 . 0.929 no C132 . H1322 . 0.921 no C132 . H1323 . 0.895 no C133 . H1331 . 0.964 no C133 . H1332 . 0.979 no C133 . H1333 . 0.967 no C134 . C135 . 1.396(7) yes C134 . C139 . 1.401(6) yes C135 . C136 . 1.389(7) yes C135 . H1351 . 0.929 no C136 . C137 . 1.375(8) yes C136 . H1361 . 0.932 no C137 . C138 . 1.369(8) yes C137 . H1371 . 0.931 no C138 . C139 . 1.389(7) yes C138 . H1381 . 0.920 no C139 . H1391 . 0.939 no C140 . C141 . 1.391(6) yes C140 . C145 . 1.396(6) yes C141 . C142 . 1.393(6) yes C141 . H1411 . 0.923 no C142 . C143 . 1.379(7) yes C142 . H1421 . 0.941 no C143 . C144 . 1.387(7) yes C143 . H1431 . 0.928 no C144 . C145 . 1.385(7) yes C144 . H1441 . 0.927 no C145 . H1451 . 0.936 no C500 . H5001 . 0.950 no C500 . H5002 . 0.950 no C501 . H5002 2_666 1.117 no C501 . C501 2_666 1.80(4) yes C501 . H5011 . 0.950 no C501 . H5012 . 0.950 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 Cr1 . Cu1 . I1 . 178.14(3) yes Cr1 . Cu1 . P1 . 67.18(3) yes I1 . Cu1 . P1 . 114.64(3) yes Cr1 . Cu1 . P2 . 67.14(3) yes I1 . Cu1 . P2 . 111.64(3) yes P1 . Cu1 . P2 . 105.57(4) yes Cr1 . Cu1 . P3 . 66.75(3) yes I1 . Cu1 . P3 . 112.62(3) yes P1 . Cu1 . P3 . 106.10(4) yes P2 . Cu1 . P3 . 105.57(4) yes Cr101 . Cu101 . I101 . 178.03(3) yes Cr101 . Cu101 . I102 . 167.2(4) yes I101 . Cu101 . I102 . 14.6(3) yes Cr101 . Cu101 . P101 . 67.97(4) yes I101 . Cu101 . P101 . 113.65(4) yes I102 . Cu101 . P101 . 105.1(3) yes Cr101 . Cu101 . P102 . 67.23(4) yes I101 . Cu101 . P102 . 110.99(4) yes I102 . Cu101 . P102 . 125.5(4) yes P101 . Cu101 . P102 . 107.41(5) yes Cr101 . Cu101 . P103 . 67.23(3) yes I101 . Cu101 . P103 . 112.91(4) yes I102 . Cu101 . P103 . 106.0(3) yes P101 . Cu101 . P103 . 105.74(5) yes P102 . Cu101 . P103 . 105.62(5) yes Cu1 . Cr1 . P1 . 50.73(3) yes Cu1 . Cr1 . P2 . 50.73(3) yes P1 . Cr1 . P2 . 83.97(4) yes Cu1 . Cr1 . P3 . 51.27(3) yes P1 . Cr1 . P3 . 84.89(3) yes P2 . Cr1 . P3 . 84.54(4) yes Cu1 . Cr1 . N1 . 87.30(11) yes P1 . Cr1 . N1 . 36.97(11) yes P2 . Cr1 . N1 . 114.81(11) yes P3 . Cr1 . N1 . 107.14(11) yes Cu1 . Cr1 . N2 . 87.36(11) yes P1 . Cr1 . N2 . 108.35(11) yes P2 . Cr1 . N2 . 36.75(11) yes P3 . Cr1 . N2 . 113.34(11) yes N1 . Cr1 . N2 . 122.15(16) yes Cu1 . Cr1 . N3 . 88.20(11) yes P1 . Cr1 . N3 . 114.64(11) yes P2 . Cr1 . N3 . 108.67(11) yes P3 . Cr1 . N3 . 37.10(11) yes N1 . Cr1 . N3 . 118.25(15) yes N2 . Cr1 . N3 . 119.08(16) yes Cu101 . Cr101 . P101 . 50.81(3) yes Cu101 . Cr101 . P102 . 51.19(3) yes P101 . Cr101 . P102 . 85.29(4) yes Cu101 . Cr101 . P103 . 51.20(3) yes P101 . Cr101 . P103 . 84.16(4) yes P102 . Cr101 . P103 . 84.64(4) yes Cu101 . Cr101 . N101 . 87.35(12) yes P101 . Cr101 . N101 . 36.64(12) yes P102 . Cr101 . N101 . 114.23(13) yes P103 . Cr101 . N101 . 108.27(13) yes Cu101 . Cr101 . N102 . 87.88(12) yes P101 . Cr101 . N102 . 108.14(12) yes P102 . Cr101 . N102 . 37.06(13) yes P103 . Cr101 . N102 . 115.23(13) yes N101 . Cr101 . N102 . 118.49(18) yes Cu101 . Cr101 . N103 . 88.47(11) yes P101 . Cr101 . N103 . 114.49(12) yes P102 . Cr101 . N103 . 108.09(12) yes P103 . Cr101 . N103 . 37.52(11) yes N101 . Cr101 . N103 . 120.65(17) yes N102 . Cr101 . N103 . 120.46(17) yes Cr1 . P1 . Cu1 . 62.09(3) yes Cu1 . P1 . N1 . 103.68(12) yes Cr1 . P1 . C4 . 117.52(14) yes Cu1 . P1 . C4 . 117.49(13) yes N1 . P1 . C4 . 104.89(18) yes Cr1 . P1 . C10 . 135.32(13) yes Cu1 . P1 . C10 . 118.18(14) yes N1 . P1 . C10 . 110.11(18) yes C4 . P1 . C10 . 101.82(18) yes Cr1 . P2 . Cu1 . 62.13(3) yes Cu1 . P2 . N2 . 103.80(13) yes Cr1 . P2 . C19 . 120.27(15) yes Cu1 . P2 . C19 . 113.52(14) yes N2 . P2 . C19 . 107.74(19) yes Cr1 . P2 . C25 . 134.12(14) yes Cu1 . P2 . C25 . 120.77(14) yes N2 . P2 . C25 . 109.69(19) yes C19 . P2 . C25 . 100.9(2) yes Cr1 . P3 . Cu1 . 61.98(3) yes Cu1 . P3 . N3 . 103.51(13) yes Cr1 . P3 . C34 . 120.50(15) yes Cu1 . P3 . C34 . 116.57(13) yes N3 . P3 . C34 . 106.44(19) yes Cr1 . P3 . C40 . 133.08(14) yes Cu1 . P3 . C40 . 119.08(14) yes N3 . P3 . C40 . 109.51(18) yes C34 . P3 . C40 . 101.19(19) yes Cr101 . P101 . Cu101 . 61.22(3) yes Cu101 . P101 . N101 . 102.88(14) yes Cr101 . P101 . C104 . 123.37(16) yes Cu101 . P101 . C104 . 118.43(15) yes N101 . P101 . C104 . 107.3(2) yes Cr101 . P101 . C110 . 131.17(15) yes Cu101 . P101 . C110 . 118.35(16) yes N101 . P101 . C110 . 109.1(2) yes C104 . P101 . C110 . 100.3(2) yes Cr101 . P102 . Cu101 . 61.58(3) yes Cu101 . P102 . N102 . 102.77(14) yes Cr101 . P102 . C119 . 118.41(16) yes Cu101 . P102 . C119 . 116.77(17) yes N102 . P102 . C119 . 106.3(2) yes Cr101 . P102 . C125 . 134.26(18) yes Cu101 . P102 . C125 . 118.32(17) yes N102 . P102 . C125 . 109.8(2) yes C119 . P102 . C125 . 102.4(2) yes Cr101 . P103 . Cu101 . 61.57(3) yes Cu101 . P103 . N103 . 103.76(13) yes Cr101 . P103 . C134 . 121.00(15) yes Cu101 . P103 . C134 . 117.27(15) yes N103 . P103 . C134 . 107.0(2) yes Cr101 . P103 . C140 . 133.20(15) yes Cu101 . P103 . C140 . 116.81(15) yes N103 . P103 . C140 . 110.2(2) yes C134 . P103 . C140 . 101.6(2) yes H5012 2_666 O1 . C51 . 116.2 no C501 2_666 O1 . C51 . 71.9(11) yes C51 . O1 . C500 . 101.7(11) yes C46 . O2 . C49 . 104.2(4) yes P1 . N1 . Cr1 . 100.91(17) yes P1 . N1 . C1 . 123.1(3) yes Cr1 . N1 . C1 . 135.8(3) yes P2 . N2 . Cr1 . 101.44(17) yes P2 . N2 . C16 . 126.0(3) yes Cr1 . N2 . C16 . 132.5(3) yes P3 . N3 . Cr1 . 101.16(17) yes P3 . N3 . C31 . 127.3(3) yes Cr1 . N3 . C31 . 131.5(3) yes P101 . N101 . Cr101 . 101.6(2) yes P101 . N101 . C101 . 125.6(3) yes Cr101 . N101 . C101 . 132.6(3) yes P102 . N102 . Cr101 . 101.3(2) yes P102 . N102 . C116 . 127.1(3) yes Cr101 . N102 . C116 . 131.6(3) yes P103 . N103 . Cr101 . 99.98(18) yes P103 . N103 . C131 . 124.3(3) yes Cr101 . N103 . C131 . 135.7(3) yes N1 . C1 . C2 . 109.9(4) yes N1 . C1 . C3 . 111.1(4) yes C2 . C1 . C3 . 110.3(4) yes N1 . C1 . H11 . 109.0 no C2 . C1 . H11 . 107.3 no C3 . C1 . H11 . 109.1 no C1 . C2 . H21 . 108.7 no C1 . C2 . H22 . 110.7 no H21 . C2 . H22 . 108.8 no C1 . C2 . H23 . 110.0 no H21 . C2 . H23 . 109.8 no H22 . C2 . H23 . 108.8 no C1 . C3 . H31 . 110.9 no C1 . C3 . H32 . 108.9 no H31 . C3 . H32 . 109.3 no C1 . C3 . H33 . 110.4 no H31 . C3 . H33 . 109.1 no H32 . C3 . H33 . 108.3 no P1 . C4 . C5 . 119.6(3) yes P1 . C4 . C9 . 121.3(3) yes C5 . C4 . C9 . 118.9(4) yes C4 . C5 . C6 . 120.2(4) yes C4 . C5 . H51 . 120.0 no C6 . C5 . H51 . 119.8 no C5 . C6 . C7 . 120.3(4) yes C5 . C6 . H61 . 119.7 no C7 . C6 . H61 . 120.0 no C6 . C7 . C8 . 120.3(4) yes C6 . C7 . H71 . 120.4 no C8 . C7 . H71 . 119.3 no C7 . C8 . C9 . 119.1(4) yes C7 . C8 . H81 . 120.7 no C9 . C8 . H81 . 120.1 no C8 . C9 . C4 . 121.1(4) yes C8 . C9 . H91 . 120.0 no C4 . C9 . H91 . 118.9 no P1 . C10 . C11 . 122.6(3) yes P1 . C10 . C15 . 118.2(3) yes C11 . C10 . C15 . 119.1(4) yes C10 . C11 . C12 . 120.1(4) yes C10 . C11 . H111 . 119.8 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.4(4) yes C11 . C12 . H121 . 119.5 no C13 . C12 . H121 . 120.1 no C12 . C13 . C14 . 120.0(4) yes C12 . C13 . H131 . 119.9 no C14 . C13 . H131 . 120.1 no C13 . C14 . C15 . 120.4(4) yes C13 . C14 . H141 . 120.5 no C15 . C14 . H141 . 119.1 no C14 . C15 . C10 . 120.0(4) yes C14 . C15 . H151 . 120.8 no C10 . C15 . H151 . 119.1 no N2 . C16 . C17 . 110.0(4) yes N2 . C16 . C18 . 110.5(4) yes C17 . C16 . C18 . 111.0(4) yes N2 . C16 . H161 . 107.6 no C17 . C16 . H161 . 108.0 no C18 . C16 . H161 . 109.7 no C16 . C17 . H171 . 108.3 no C16 . C17 . H172 . 110.7 no H171 . C17 . H172 . 110.8 no C16 . C17 . H173 . 108.3 no H171 . C17 . H173 . 108.6 no H172 . C17 . H173 . 110.0 no C16 . C18 . H181 . 110.6 no C16 . C18 . H182 . 110.1 no H181 . C18 . H182 . 107.6 no C16 . C18 . H183 . 110.6 no H181 . C18 . H183 . 108.4 no H182 . C18 . H183 . 109.4 no P2 . C19 . C20 . 123.1(4) yes P2 . C19 . C24 . 117.9(3) yes C20 . C19 . C24 . 118.7(4) yes C19 . C20 . C21 . 119.9(5) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.0 no C20 . C21 . C22 . 121.2(5) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 118.6 no C21 . C22 . C23 . 119.6(5) yes C21 . C22 . H221 . 120.2 no C23 . C22 . H221 . 120.2 no C22 . C23 . C24 . 120.2(5) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 120.0 no C19 . C24 . C23 . 120.4(5) yes C19 . C24 . H241 . 119.8 no C23 . C24 . H241 . 119.8 no P2 . C25 . C26 . 122.2(3) yes P2 . C25 . C30 . 119.1(3) yes C26 . C25 . C30 . 118.7(4) yes C25 . C26 . C27 . 120.9(4) yes C25 . C26 . H261 . 120.7 no C27 . C26 . H261 . 118.4 no C26 . C27 . C28 . 120.1(4) yes C26 . C27 . H271 . 120.1 no C28 . C27 . H271 . 119.7 no C27 . C28 . C29 . 119.4(5) yes C27 . C28 . H281 . 120.8 no C29 . C28 . H281 . 119.8 no C28 . C29 . C30 . 120.4(5) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 119.6 no C29 . C30 . C25 . 120.5(4) yes C29 . C30 . H301 . 120.1 no C25 . C30 . H301 . 119.5 no N3 . C31 . C32 . 109.3(4) yes N3 . C31 . C33 . 110.7(4) yes C32 . C31 . C33 . 109.9(4) yes N3 . C31 . H311 . 107.7 no C32 . C31 . H311 . 110.0 no C33 . C31 . H311 . 109.2 no C31 . C32 . H321 . 111.0 no C31 . C32 . H322 . 110.7 no H321 . C32 . H322 . 109.8 no C31 . C32 . H323 . 108.4 no H321 . C32 . H323 . 108.1 no H322 . C32 . H323 . 108.8 no C31 . C33 . H331 . 109.7 no C31 . C33 . H332 . 109.0 no H331 . C33 . H332 . 109.3 no C31 . C33 . H333 . 109.1 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 110.3 no P3 . C34 . C35 . 121.2(3) yes P3 . C34 . C39 . 120.1(3) yes C35 . C34 . C39 . 118.5(4) yes C34 . C35 . C36 . 120.8(5) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 119.5 no C35 . C36 . C37 . 119.9(5) yes C35 . C36 . H361 . 119.6 no C37 . C36 . H361 . 120.5 no C36 . C37 . C38 . 120.2(5) yes C36 . C37 . H371 . 119.2 no C38 . C37 . H371 . 120.6 no C37 . C38 . C39 . 119.9(5) yes C37 . C38 . H381 . 120.7 no C39 . C38 . H381 . 119.4 no C38 . C39 . C34 . 120.7(5) yes C38 . C39 . H391 . 120.4 no C34 . C39 . H391 . 118.9 no P3 . C40 . C41 . 121.6(3) yes P3 . C40 . C45 . 119.3(3) yes C41 . C40 . C45 . 119.1(4) yes C40 . C41 . C42 . 120.1(4) yes C40 . C41 . H411 . 119.8 no C42 . C41 . H411 . 120.1 no C41 . C42 . C43 . 120.2(5) yes C41 . C42 . H421 . 119.6 no C43 . C42 . H421 . 120.2 no C42 . C43 . C44 . 120.2(5) yes C42 . C43 . H431 . 119.6 no C44 . C43 . H431 . 120.2 no C43 . C44 . C45 . 119.8(5) yes C43 . C44 . H441 . 119.9 no C45 . C44 . H441 . 120.2 no C44 . C45 . C40 . 120.5(5) yes C44 . C45 . H451 . 120.2 no C40 . C45 . H451 . 119.3 no O2 . C46 . C47 . 105.1(5) yes O2 . C46 . H461 . 111.5 no C47 . C46 . H461 . 111.0 no O2 . C46 . H462 . 109.6 no C47 . C46 . H462 . 109.7 no H461 . C46 . H462 . 109.9 no C46 . C47 . C48 . 103.7(5) yes C46 . C47 . H471 . 110.9 no C48 . C47 . H471 . 110.0 no C46 . C47 . H472 . 111.4 no C48 . C47 . H472 . 110.8 no H471 . C47 . H472 . 109.9 no C47 . C48 . C49 . 104.0(4) yes C47 . C48 . H481 . 111.2 no C49 . C48 . H481 . 110.9 no C47 . C48 . H482 . 109.5 no C49 . C48 . H482 . 111.4 no H481 . C48 . H482 . 109.7 no C48 . C49 . O2 . 107.0(5) yes C48 . C49 . H491 . 109.3 no O2 . C49 . H491 . 108.8 no C48 . C49 . H492 . 110.6 no O2 . C49 . H492 . 110.2 no H491 . C49 . H492 . 110.8 no C501 2_666 C51 . C500 2_666 97.3(13) yes C501 2_666 C51 . O1 . 53.3(9) yes C500 2_666 C51 . O1 . 140.1(12) yes C501 2_666 C51 . C501 . 77.1(15) yes O1 . C51 . C501 . 110.5(15) yes C501 2_666 C51 . H511 . 162.7 no C500 2_666 C51 . H511 . 95.4 no O1 . C51 . H511 . 109.8 no C501 . C51 . H511 . 109.7 no C501 2_666 C51 . H512 . 82.1 no C500 2_666 C51 . H512 . 90.5 no O1 . C51 . H512 . 108.5 no C501 . C51 . H512 . 108.9 no H511 . C51 . H512 . 109.5 no C501 2_666 C51 . C500 2_666 97.3(13) yes C501 2_666 C51 . C501 . 77.1(15) yes C501 2_666 C51 . H513 . 112.1 no C500 2_666 C51 . H513 . 111.7 no C501 . C51 . H513 . 140.1 no C501 2_666 C51 . H514 . 113.0 no C500 2_666 C51 . H514 . 112.9 no C501 . C51 . H514 . 101.1 no H513 . C51 . H514 . 109.5 no N101 . C101 . C102 . 109.5(4) yes N101 . C101 . C103 . 110.1(4) yes C102 . C101 . C103 . 111.6(4) yes N101 . C101 . H1011 . 109.0 no C102 . C101 . H1011 . 108.5 no C103 . C101 . H1011 . 108.2 no C101 . C102 . H1021 . 108.5 no C101 . C102 . H1022 . 110.0 no H1021 . C102 . H1022 . 109.7 no C101 . C102 . H1023 . 108.2 no H1021 . C102 . H1023 . 109.8 no H1022 . C102 . H1023 . 110.6 no C101 . C103 . H1031 . 108.0 no C101 . C103 . H1032 . 109.4 no H1031 . C103 . H1032 . 110.9 no C101 . C103 . H1033 . 106.8 no H1031 . C103 . H1033 . 111.4 no H1032 . C103 . H1033 . 110.2 no P101 . C104 . C105 . 121.6(4) yes P101 . C104 . C109 . 119.4(4) yes C105 . C104 . C109 . 118.6(5) yes C104 . C105 . C106 . 120.2(5) yes C104 . C105 . H1051 . 119.7 no C106 . C105 . H1051 . 120.1 no C105 . C106 . C107 . 121.1(5) yes C105 . C106 . H1061 . 119.5 no C107 . C106 . H1061 . 119.4 no C106 . C107 . C108 . 119.6(5) yes C106 . C107 . H1071 . 119.7 no C108 . C107 . H1071 . 120.6 no C107 . C108 . C109 . 120.2(5) yes C107 . C108 . H1081 . 120.0 no C109 . C108 . H1081 . 119.8 no C104 . C109 . C108 . 120.2(5) yes C104 . C109 . H1091 . 119.4 no C108 . C109 . H1091 . 120.4 no P101 . C110 . C111 . 123.1(4) yes P101 . C110 . C115 . 118.2(4) yes C111 . C110 . C115 . 118.6(4) yes C110 . C111 . C112 . 120.7(5) yes C110 . C111 . H1111 . 119.3 no C112 . C111 . H1111 . 120.0 no C111 . C112 . C113 . 121.0(5) yes C111 . C112 . H1121 . 119.5 no C113 . C112 . H1121 . 119.5 no C112 . C113 . C114 . 119.4(5) yes C112 . C113 . H1131 . 120.3 no C114 . C113 . H1131 . 120.3 no C113 . C114 . C115 . 120.5(6) yes C113 . C114 . H1141 . 120.1 no C115 . C114 . H1141 . 119.4 no C114 . C115 . C110 . 119.8(5) yes C114 . C115 . H1151 . 120.1 no C110 . C115 . H1151 . 120.2 no N102 . C116 . C117 . 108.8(4) yes N102 . C116 . C118 . 110.1(4) yes C117 . C116 . C118 . 110.6(5) yes N102 . C116 . H1161 . 109.7 no C117 . C116 . H1161 . 108.1 no C118 . C116 . H1161 . 109.5 no C116 . C117 . H1171 . 108.8 no C116 . C117 . H1172 . 110.4 no H1171 . C117 . H1172 . 109.2 no C116 . C117 . H1173 . 109.0 no H1171 . C117 . H1173 . 108.5 no H1172 . C117 . H1173 . 110.9 no C116 . C118 . H1181 . 108.5 no C116 . C118 . H1182 . 108.5 no H1181 . C118 . H1182 . 108.6 no C116 . C118 . H1183 . 110.9 no H1181 . C118 . H1183 . 110.4 no H1182 . C118 . H1183 . 109.8 no P102 . C119 . C120 . 121.6(4) yes P102 . C119 . C124 . 120.0(4) yes C120 . C119 . C124 . 118.0(5) yes C119 . C120 . C121 . 120.4(5) yes C119 . C120 . H1201 . 120.2 no C121 . C120 . H1201 . 119.4 no C120 . C121 . C122 . 121.0(5) yes C120 . C121 . H1211 . 119.5 no C122 . C121 . H1211 . 119.5 no C121 . C122 . C123 . 120.1(5) yes C121 . C122 . H1221 . 120.1 no C123 . C122 . H1221 . 119.8 no C122 . C123 . C124 . 119.3(6) yes C122 . C123 . H1231 . 119.8 no C124 . C123 . H1231 . 121.0 no C119 . C124 . C123 . 121.2(5) yes C119 . C124 . H1241 . 119.3 no C123 . C124 . H1241 . 119.5 no P102 . C125 . C126 . 121.8(4) yes P102 . C125 . C130 . 119.2(4) yes C126 . C125 . C130 . 119.1(5) yes C125 . C126 . C127 . 120.5(6) yes C125 . C126 . H1261 . 119.2 no C127 . C126 . H1261 . 120.3 no C126 . C127 . C128 . 120.8(6) yes C126 . C127 . H1271 . 120.1 no C128 . C127 . H1271 . 119.1 no C127 . C128 . C129 . 119.7(5) yes C127 . C128 . H1281 . 119.7 no C129 . C128 . H1281 . 120.6 no C128 . C129 . C130 . 120.2(6) yes C128 . C129 . H1291 . 119.5 no C130 . C129 . H1291 . 120.2 no C125 . C130 . C129 . 119.7(5) yes C125 . C130 . H1301 . 119.7 no C129 . C130 . H1301 . 120.5 no N103 . C131 . C132 . 111.1(4) yes N103 . C131 . C133 . 110.9(4) yes C132 . C131 . C133 . 108.6(4) yes N103 . C131 . H1311 . 107.0 no C132 . C131 . H1311 . 111.7 no C133 . C131 . H1311 . 107.4 no C131 . C132 . H1321 . 110.2 no C131 . C132 . H1322 . 109.3 no H1321 . C132 . H1322 . 109.1 no C131 . C132 . H1323 . 110.2 no H1321 . C132 . H1323 . 108.4 no H1322 . C132 . H1323 . 109.7 no C131 . C133 . H1331 . 109.0 no C131 . C133 . H1332 . 109.2 no H1331 . C133 . H1332 . 110.6 no C131 . C133 . H1333 . 109.5 no H1331 . C133 . H1333 . 109.3 no H1332 . C133 . H1333 . 109.2 no P103 . C134 . C135 . 121.7(3) yes P103 . C134 . C139 . 118.8(4) yes C135 . C134 . C139 . 119.1(4) yes C134 . C135 . C136 . 119.8(5) yes C134 . C135 . H1351 . 120.7 no C136 . C135 . H1351 . 119.6 no C135 . C136 . C137 . 120.4(5) yes C135 . C136 . H1361 . 120.0 no C137 . C136 . H1361 . 119.6 no C136 . C137 . C138 . 120.5(5) yes C136 . C137 . H1371 . 119.9 no C138 . C137 . H1371 . 119.7 no C137 . C138 . C139 . 120.3(5) yes C137 . C138 . H1381 . 120.4 no C139 . C138 . H1381 . 119.3 no C134 . C139 . C138 . 119.9(5) yes C134 . C139 . H1391 . 120.2 no C138 . C139 . H1391 . 119.9 no P103 . C140 . C141 . 122.1(4) yes P103 . C140 . C145 . 119.0(3) yes C141 . C140 . C145 . 118.9(4) yes C140 . C141 . C142 . 120.7(4) yes C140 . C141 . H1411 . 119.9 no C142 . C141 . H1411 . 119.4 no C141 . C142 . C143 . 119.7(4) yes C141 . C142 . H1421 . 119.8 no C143 . C142 . H1421 . 120.5 no C142 . C143 . C144 . 120.2(5) yes C142 . C143 . H1431 . 120.8 no C144 . C143 . H1431 . 119.0 no C143 . C144 . C145 . 120.2(5) yes C143 . C144 . H1441 . 119.6 no C145 . C144 . H1441 . 120.2 no C140 . C145 . C144 . 120.3(4) yes C140 . C145 . H1451 . 120.4 no C144 . C145 . H1451 . 119.3 no C51 2_666 C500 . O1 . 109.5(12) yes C51 2_666 C500 . H5001 . 110.7 no O1 . C500 . H5001 . 110.3 no C51 2_666 C500 . H5002 . 108.6 no O1 . C500 . H5002 . 108.2 no H5001 . C500 . H5002 . 109.5 no C51 2_666 C501 . H5002 2_666 144.8 no C51 2_666 C501 . O1 2_666 54.8(10) yes H5002 2_666 C501 . O1 2_666 103.9 no C51 2_666 C501 . C51 . 102.9(15) yes H5002 2_666 C501 . C51 . 111.9 no O1 2_666 C501 . C51 . 128.5(19) yes C51 2_666 C501 . C501 2_666 45.4(10) yes H5002 2_666 C501 . C501 2_666 168.4 no O1 2_666 C501 . C501 2_666 87.4(17) yes C51 . C501 . C501 2_666 57.6(13) yes C51 2_666 C501 . H5011 . 110.9 no H5002 2_666 C501 . H5011 . 52.0 no O1 2_666 C501 . H5011 . 120.7 no C51 . C501 . H5011 . 110.5 no C501 2_666 C501 . H5011 . 124.4 no C51 2_666 C501 . H5012 . 111.2 no H5002 2_666 C501 . H5012 . 60.9 no O1 2_666 C501 . H5012 . 56.9 no C51 . C501 . H5012 . 111.7 no C501 2_666 C501 . H5012 . 125.7 no H5011 . C501 . H5012 . 109.5 no O1 2_666 H5012 . C501 . 78.2 no _iucr_refine_instructions_details_constraints ; # # Punched on 15/05/13 at 15:46:18 # #LIST 12 BLOCK CONT SCALE CONT CU ( 1 ,X'S,U'S) UNTIL I ( 101 ) CONT I ( 102 ,X'S,U[ISO]) CONT P ( 1 ,X'S,U'S) UNTIL P ( 103 ) CONT O ( 1 ,X'S,U[ISO]) CONT O ( 2 ,X'S,U'S) UNTIL C ( 145 ) CONT C ( 500 ,X'S,U[ISO]) UNTIL C ( 501 ) SUMFIX I(101,OCC) AND I(102,OCC) RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) H ( 513,X'S) H ( 514,X'S) RIDE C ( 101,X'S) H (1011,X'S) RIDE C ( 102,X'S) H (1021,X'S) H (1022,X'S) H (1023,X'S) RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) H (1033,X'S) RIDE C ( 105,X'S) H (1051,X'S) RIDE C ( 106,X'S) H (1061,X'S) RIDE C ( 107,X'S) H (1071,X'S) RIDE C ( 108,X'S) H (1081,X'S) RIDE C ( 109,X'S) H (1091,X'S) RIDE C ( 111,X'S) H (1111,X'S) RIDE C ( 112,X'S) H (1121,X'S) RIDE C ( 113,X'S) H (1131,X'S) RIDE C ( 114,X'S) H (1141,X'S) RIDE C ( 115,X'S) H (1151,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 117,X'S) H (1171,X'S) H (1172,X'S) H (1173,X'S) RIDE C ( 118,X'S) H (1181,X'S) H (1182,X'S) H (1183,X'S) RIDE C ( 120,X'S) H (1201,X'S) RIDE C ( 121,X'S) H (1211,X'S) RIDE C ( 122,X'S) H (1221,X'S) RIDE C ( 123,X'S) H (1231,X'S) RIDE C ( 124,X'S) H (1241,X'S) RIDE C ( 126,X'S) H (1261,X'S) RIDE C ( 127,X'S) H (1271,X'S) RIDE C ( 128,X'S) H (1281,X'S) RIDE C ( 129,X'S) H (1291,X'S) RIDE C ( 130,X'S) H (1301,X'S) RIDE C ( 131,X'S) H (1311,X'S) RIDE C ( 132,X'S) H (1321,X'S) H (1322,X'S) H (1323,X'S) RIDE C ( 133,X'S) H (1331,X'S) H (1332,X'S) H (1333,X'S) RIDE C ( 135,X'S) H (1351,X'S) RIDE C ( 136,X'S) H (1361,X'S) RIDE C ( 137,X'S) H (1371,X'S) RIDE C ( 138,X'S) H (1381,X'S) RIDE C ( 139,X'S) H (1391,X'S) RIDE C ( 141,X'S) H (1411,X'S) RIDE C ( 142,X'S) H (1421,X'S) RIDE C ( 143,X'S) H (1431,X'S) RIDE C ( 144,X'S) H (1441,X'S) RIDE C ( 145,X'S) H (1451,X'S) RIDE C ( 500,X'S) H (5001,X'S) H (5002,X'S) RIDE C ( 501,X'S) H (5011,X'S) H (5012,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 15/05/13 at 15:46:18 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) A-VIBRATION 0.0, 0.005000 = CU(101) TO I(102) A-DISTANCE 2.530000 , 0.010000 = CU(101) TO I(102) END ; _database_code_depnum_ccdc_archive 'CCDC 966660'