# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _audit_creation_date 13-05-31 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 076jtnp12 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 10.1814(2) _cell_length_b 20.4882(4) _cell_length_c 16.7346(3) _cell_angle_alpha 90 _cell_angle_beta 103.1581(11) _cell_angle_gamma 90 _cell_volume 3399.16(11) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-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' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C37 H50 Ga1 Mn1 N2 O2 # Dc = 1.33 Fooo = 1431.80 Mu = 11.98 M = 679.46 # Found Formula = C37 H49.95 Ga1.00 Mn1 N2 O2 # Dc = 1.33 FOOO = 1431.80 Mu = 11.98 M = 679.41 _chemical_formula_sum 'C37 H49.95 Ga Mn N2 O2' _chemical_formula_moiety 'C37 H49.95 Ga Mn N2 O2' _chemical_compound_source . _chemical_formula_weight 679.41 _cell_measurement_reflns_used 7771 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_max 0.460 _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1431.796 _exptl_absorpt_coefficient_mu 1.198 # Sheldrick geometric approximatio 0.70 0.79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.79 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 41038 _reflns_number_total 7688 _diffrn_reflns_av_R_equivalents 0.059 # Number of reflections without Friedels Law is 14617 # Number of reflections with Friedels Law is 7688 # Theoretical number of reflections is about 7772 _diffrn_reflns_theta_min 5.103 _diffrn_reflns_theta_max 27.453 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.904 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 1.98 _oxford_diffrn_Wilson_scale 70.55 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.07 _refine_diff_density_max 1.74 # 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>-3.0\s(I) _refine_ls_number_reflns 7688 _refine_ls_number_restraints 4 _refine_ls_number_parameters 392 _oxford_refine_ls_R_factor_ref 0.1473 _refine_ls_wR_factor_ref 0.2096 _refine_ls_goodness_of_fit_ref 1.0437 _refine_ls_shift/su_max 0.0089359 _refine_ls_shift/su_mean 0.0001445 # The values computed from all data _oxford_reflns_number_all 7688 _refine_ls_R_factor_all 0.1473 _refine_ls_wR_factor_all 0.2096 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4038 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_gt 0.1459 # 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 # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 5.65 6.68 1.85 ; # 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 Ga1 Ga 0.27054(7) 0.24889(4) 0.49067(5) 0.0241 0.975(3) Uani . . P 1 1 . Mn2 Mn 0.52772(11) 0.24849(7) 0.56783(7) 0.0379 1.0000 Uani . . . . . . C3 C 0.5539(11) 0.3334(5) 0.5782(7) 0.0607 1.0000 Uani . . . . . . O4 O 0.5786(9) 0.3879(4) 0.5877(7) 0.0989 1.0000 Uani . . . . . . C5 C 0.5355(8) 0.2535(6) 0.4640(6) 0.0563 1.0000 Uani . . . . . . O6 O 0.5493(7) 0.2558(5) 0.3967(4) 0.0805 1.0000 Uani . . . . . . C7 C 0.5383(10) 0.1559(5) 0.6292(7) 0.0647 1.0000 Uani . . . . . . C8 C 0.6294(11) 0.1573(5) 0.5780(7) 0.0611 1.0000 Uani . . . . . . C9 C 0.7204(10) 0.2069(5) 0.6037(6) 0.0569 1.0000 Uani . . . . . . C10 C 0.6919(8) 0.2382(5) 0.6728(5) 0.0472 1.0000 Uani . . . . . . C11 C 0.5796(10) 0.2065(6) 0.6887(6) 0.0621 1.0000 Uani . . . . . . C12 C 0.7708(12) 0.2907(7) 0.7216(7) 0.0793 1.0000 Uani . . . . . . N13 N 0.1462(6) 0.1803(3) 0.5104(3) 0.0234 1.0000 Uani . . . . . . C14 C 0.1945(7) 0.1171(3) 0.5421(4) 0.0271 1.0000 Uani . . . . . . C15 C 0.2011(8) 0.1036(3) 0.6266(4) 0.0308 1.0000 Uani . . . . . . C16 C 0.2546(8) 0.0446(4) 0.6571(5) 0.0390 1.0000 Uani . . . . . . C17 C 0.3029(8) -0.0001(4) 0.6090(6) 0.0427 1.0000 Uani . . . . . . C18 C 0.2927(8) 0.0129(4) 0.5271(6) 0.0399 1.0000 Uani . . . . . . C19 C 0.2386(7) 0.0716(3) 0.4916(5) 0.0283 1.0000 Uani . . . . . . C20 C 0.2274(8) 0.0828(4) 0.4011(5) 0.0375 1.0000 Uani . . . . . . C21 C 0.3665(9) 0.0875(5) 0.3819(5) 0.0476 1.0000 Uani . . . . . . C22 C 0.1448(9) 0.0291(4) 0.3491(6) 0.0482 1.0000 Uani . . . . . . C23 C 0.1540(9) 0.1530(4) 0.6824(4) 0.0389 1.0000 Uani . . . . . . C24 C 0.2638(11) 0.1722(6) 0.7545(7) 0.0719 1.0000 Uani . . . . . . C25 C 0.0336(10) 0.1262(5) 0.7144(6) 0.0547 1.0000 Uani . . . . . . C26 C 0.0127(7) 0.1903(3) 0.4843(4) 0.0258 1.0000 Uani . . . . . . C27 C -0.0811(8) 0.1318(3) 0.4753(5) 0.0323 1.0000 Uani . . . . . . C28 C -0.0450(6) 0.2517(3) 0.4664(4) 0.0246 1.0000 Uani . . . . . . C29 C 0.0177(7) 0.3131(3) 0.4867(4) 0.0260 1.0000 Uani . . . . . . N30 N 0.1499(5) 0.3208(3) 0.5086(3) 0.0214 1.0000 Uani . . . . . . C31 C 0.2058(7) 0.3848(3) 0.5319(4) 0.0256 1.0000 Uani . . . . . . C32 C 0.2238(8) 0.4290(3) 0.4717(5) 0.0315 1.0000 Uani . . . . . . C33 C 0.1793(9) 0.4148(4) 0.3802(5) 0.0387 1.0000 Uani . . . . . . C34 C 0.3014(10) 0.4056(5) 0.3424(6) 0.0524 1.0000 Uani . . . . . . C35 C 0.0866(10) 0.4683(5) 0.3346(6) 0.0541 1.0000 Uani . . . . . . C36 C 0.2853(8) 0.4889(4) 0.4961(5) 0.0387 1.0000 Uani . . . . . . C37 C 0.3290(9) 0.5032(4) 0.5776(6) 0.0446 1.0000 Uani . . . . . . C38 C 0.3145(8) 0.4589(4) 0.6367(5) 0.0389 1.0000 Uani . . . . . . C39 C 0.2552(8) 0.3987(3) 0.6164(4) 0.0310 1.0000 Uani . . . . . . C40 C 0.2414(8) 0.3496(4) 0.6819(4) 0.0364 1.0000 Uani . . . . . . C41 C 0.3610(10) 0.3511(5) 0.7563(5) 0.0536 1.0000 Uani . . . . . . C42 C 0.1100(10) 0.3604(6) 0.7090(6) 0.0604 1.0000 Uani . . . . . . C43 C -0.0753(8) 0.3707(4) 0.4843(5) 0.0339 1.0000 Uani . . . . . . Ga101 Ga 0.288(3) 0.2510(19) 0.5300(8) 0.0241 0.025(3) Uani . . P 1 2 . H11 H 0.2606 0.2514 0.3959 0.0224 0.975(3) Uiso R . P 1 1 . H12 H 0.3815 0.2548 0.5772 0.0172 0.975(3) Uiso R . P 1 1 . H71 H 0.4636 0.1249 0.6263 0.0780 1.0000 Uiso R . . . . . H81 H 0.6282 0.1283 0.5314 0.0729 1.0000 Uiso R . . . . . H91 H 0.7972 0.2173 0.5792 0.0682 1.0000 Uiso R . . . . . H111 H 0.5363 0.2173 0.7335 0.0741 1.0000 Uiso R . . . . . H121 H 0.7125 0.3145 0.7493 0.1191 1.0000 Uiso R . . . . . H122 H 0.8035 0.3197 0.6850 0.1191 1.0000 Uiso R . . . . . H123 H 0.8455 0.2722 0.7612 0.1191 1.0000 Uiso R . . . . . H161 H 0.2584 0.0348 0.7115 0.0460 1.0000 Uiso R . . . . . H171 H 0.3420 -0.0387 0.6315 0.0511 1.0000 Uiso R . . . . . H181 H 0.3226 -0.0179 0.4947 0.0480 1.0000 Uiso R . . . . . H201 H 0.1803 0.1242 0.3856 0.0449 1.0000 Uiso R . . . . . H211 H 0.4157 0.0482 0.3985 0.0710 1.0000 Uiso R . . . . . H212 H 0.4137 0.1243 0.4095 0.0709 1.0000 Uiso R . . . . . H213 H 0.3563 0.0932 0.3241 0.0710 1.0000 Uiso R . . . . . H221 H 0.0598 0.0239 0.3640 0.0719 1.0000 Uiso R . . . . . H222 H 0.1936 -0.0110 0.3578 0.0719 1.0000 Uiso R . . . . . H223 H 0.1290 0.0408 0.2927 0.0719 1.0000 Uiso R . . . . . H231 H 0.1228 0.1918 0.6505 0.0471 1.0000 Uiso R . . . . . H241 H 0.2281 0.2003 0.7901 0.1069 1.0000 Uiso R . . . . . H242 H 0.3340 0.1945 0.7362 0.1070 1.0000 Uiso R . . . . . H243 H 0.3011 0.1341 0.7844 0.1068 1.0000 Uiso R . . . . . H251 H 0.0026 0.1600 0.7455 0.0820 1.0000 Uiso R . . . . . H252 H -0.0373 0.1139 0.6687 0.0820 1.0000 Uiso R . . . . . H253 H 0.0632 0.0891 0.7486 0.0820 1.0000 Uiso R . . . . . H271 H -0.0766 0.1136 0.5280 0.0489 1.0000 Uiso R . . . . . H272 H -0.1715 0.1453 0.4512 0.0490 1.0000 Uiso R . . . . . H273 H -0.0529 0.1002 0.4409 0.0492 1.0000 Uiso R . . . . . H281 H -0.1348 0.2526 0.4385 0.0292 1.0000 Uiso R . . . . . H331 H 0.1279 0.3743 0.3731 0.0459 1.0000 Uiso R . . . . . H341 H 0.3531 0.4452 0.3487 0.0777 1.0000 Uiso R . . . . . H342 H 0.2720 0.3950 0.2854 0.0779 1.0000 Uiso R . . . . . H343 H 0.3569 0.3709 0.3701 0.0778 1.0000 Uiso R . . . . . H351 H 0.1361 0.5080 0.3365 0.0809 1.0000 Uiso R . . . . . H352 H 0.0533 0.4556 0.2789 0.0808 1.0000 Uiso R . . . . . H353 H 0.0122 0.4750 0.3601 0.0809 1.0000 Uiso R . . . . . H361 H 0.2966 0.5191 0.4570 0.0461 1.0000 Uiso R . . . . . H371 H 0.3694 0.5430 0.5929 0.0529 1.0000 Uiso R . . . . . H381 H 0.3466 0.4695 0.6916 0.0458 1.0000 Uiso R . . . . . H401 H 0.2377 0.3065 0.6573 0.0439 1.0000 Uiso R . . . . . H411 H 0.3546 0.3145 0.7909 0.0800 1.0000 Uiso R . . . . . H412 H 0.4432 0.3485 0.7378 0.0800 1.0000 Uiso R . . . . . H413 H 0.3597 0.3907 0.7860 0.0800 1.0000 Uiso R . . . . . H421 H 0.0999 0.3282 0.7486 0.0899 1.0000 Uiso R . . . . . H422 H 0.0349 0.3572 0.6627 0.0900 1.0000 Uiso R . . . . . H423 H 0.1094 0.4029 0.7328 0.0900 1.0000 Uiso R . . . . . H431 H -0.0819 0.3938 0.4342 0.0512 1.0000 Uiso R . . . . . H432 H -0.1623 0.3554 0.4872 0.0511 1.0000 Uiso R . . . . . H433 H -0.0398 0.3985 0.5294 0.0509 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 Ga1 0.0239(3) 0.0200(3) 0.0285(5) 0.0001(4) 0.0064(3) 0.0004(3) Mn2 0.0346(6) 0.0354(6) 0.0439(6) 0.0036(6) 0.0094(5) 0.0001(6) C3 0.059(6) 0.040(5) 0.087(8) 0.015(5) 0.023(6) 0.000(5) O4 0.070(5) 0.046(4) 0.183(10) 0.012(5) 0.033(6) -0.015(4) C5 0.039(4) 0.077(7) 0.054(5) 0.008(6) 0.014(4) 0.004(5) O6 0.060(4) 0.138(7) 0.052(4) 0.016(5) 0.031(3) 0.009(5) C7 0.046(6) 0.049(6) 0.091(8) 0.029(6) -0.003(5) 0.004(4) C8 0.059(6) 0.045(5) 0.075(7) -0.004(5) 0.007(5) 0.015(5) C9 0.051(6) 0.065(6) 0.053(6) -0.001(5) 0.009(5) 0.002(5) C10 0.031(4) 0.061(6) 0.049(5) 0.005(4) 0.009(3) 0.004(4) C11 0.054(6) 0.078(7) 0.055(6) 0.024(5) 0.014(5) 0.007(5) C12 0.074(8) 0.100(10) 0.061(7) 0.000(7) 0.009(6) -0.011(7) N13 0.025(3) 0.022(3) 0.024(3) -0.004(2) 0.008(2) 0.001(2) C14 0.026(4) 0.022(3) 0.033(4) 0.004(3) 0.008(3) -0.002(3) C15 0.038(4) 0.023(3) 0.030(4) 0.003(3) 0.003(3) -0.007(3) C16 0.039(4) 0.035(4) 0.042(4) 0.014(3) 0.006(3) -0.009(3) C17 0.031(4) 0.029(4) 0.065(6) 0.013(4) 0.002(4) 0.001(3) C18 0.040(4) 0.027(4) 0.056(5) -0.006(4) 0.015(4) 0.005(3) C19 0.028(4) 0.017(3) 0.042(4) 0.000(3) 0.012(3) 0.003(3) C20 0.047(5) 0.030(4) 0.035(4) -0.006(3) 0.010(4) 0.009(3) C21 0.050(5) 0.055(5) 0.043(5) -0.004(4) 0.021(4) 0.003(4) C22 0.055(5) 0.040(5) 0.048(5) -0.015(4) 0.008(4) 0.011(4) C23 0.065(6) 0.028(4) 0.026(4) 0.007(3) 0.014(4) 0.004(4) C24 0.060(6) 0.092(9) 0.063(6) -0.036(6) 0.014(5) -0.032(6) C25 0.050(6) 0.062(6) 0.053(5) -0.010(5) 0.013(4) 0.001(5) C26 0.024(3) 0.027(4) 0.027(4) -0.002(3) 0.008(3) -0.002(3) C27 0.036(4) 0.026(4) 0.035(4) 0.001(3) 0.006(3) -0.005(3) C28 0.030(3) 0.020(3) 0.026(3) 0.000(3) 0.012(2) 0.005(3) C29 0.034(4) 0.023(3) 0.023(3) 0.000(3) 0.011(3) 0.003(3) N30 0.024(3) 0.015(2) 0.026(3) -0.002(2) 0.008(2) -0.001(2) C31 0.026(3) 0.024(3) 0.027(3) 0.000(3) 0.005(3) 0.006(3) C32 0.032(4) 0.024(3) 0.040(4) 0.003(3) 0.009(3) 0.005(3) C33 0.054(5) 0.028(4) 0.035(4) 0.006(3) 0.012(4) -0.002(4) C34 0.069(6) 0.050(5) 0.044(5) 0.004(4) 0.024(5) -0.002(5) C35 0.073(7) 0.042(5) 0.044(5) 0.011(4) 0.005(5) 0.003(5) C36 0.040(4) 0.021(3) 0.055(5) 0.006(3) 0.011(4) -0.001(3) C37 0.047(5) 0.021(4) 0.064(6) -0.003(4) 0.008(4) -0.006(3) C38 0.044(5) 0.037(4) 0.033(4) -0.012(3) 0.002(3) 0.000(3) C39 0.039(4) 0.024(3) 0.030(4) -0.002(3) 0.008(3) 0.004(3) C40 0.048(5) 0.033(4) 0.029(4) -0.006(3) 0.011(3) -0.006(3) C41 0.066(6) 0.060(6) 0.033(4) 0.006(4) 0.008(4) -0.005(5) C42 0.053(6) 0.085(8) 0.047(5) 0.020(5) 0.020(5) -0.004(5) C43 0.029(4) 0.028(4) 0.044(4) -0.002(3) 0.007(3) 0.008(3) Ga101 0.0239(3) 0.0200(3) 0.0285(5) 0.0001(4) 0.0064(3) 0.0004(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12814(7) 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 Ga1 . Mn2 . 2.6427(13) yes Ga1 . N13 . 1.969(6) yes Ga1 . N30 . 1.984(5) yes Ga1 . H11 . 1.566 no Ga1 . H12 . 1.626 no Mn2 . C3 . 1.763(10) yes Mn2 . C5 . 1.760(9) yes Mn2 . C7 . 2.149(10) yes Mn2 . C8 . 2.123(10) yes Mn2 . C9 . 2.097(10) yes Mn2 . C10 . 2.142(8) yes Mn2 . C11 . 2.151(10) yes Mn2 . H12 . 1.538 no Mn2 . C3 . 1.763(10) yes Mn2 . C5 . 1.760(9) yes Mn2 . C7 . 2.149(10) yes Mn2 . C8 . 2.123(10) yes Mn2 . C9 . 2.097(10) yes Mn2 . C10 . 2.142(8) yes Mn2 . C11 . 2.151(10) yes Mn2 . Ga101 . 2.38(3) yes C3 . O4 . 1.147(12) yes C5 . O6 . 1.167(10) yes C7 . C8 . 1.398(15) yes C7 . C11 . 1.433(16) yes C7 . H71 . 0.983 no C8 . C9 . 1.376(14) yes C8 . H81 . 0.980 no C9 . C10 . 1.408(13) yes C9 . H91 . 0.985 no C10 . C11 . 1.393(13) yes C10 . C12 . 1.473(14) yes C11 . H111 . 0.978 no C12 . H121 . 0.965 no C12 . H122 . 0.965 no C12 . H123 . 0.966 no N13 . C14 . 1.441(8) yes N13 . C26 . 1.346(9) yes N13 . C14 . 1.441(8) yes N13 . C26 . 1.346(9) yes N13 . Ga101 . 2.02(4) yes C14 . C15 . 1.427(10) yes C14 . C19 . 1.400(10) yes C15 . C16 . 1.374(10) yes C15 . C23 . 1.527(10) yes C16 . C17 . 1.381(12) yes C16 . H161 . 0.925 no C17 . C18 . 1.377(12) yes C17 . H171 . 0.926 no C18 . C19 . 1.398(10) yes C18 . H181 . 0.927 no C19 . C20 . 1.510(10) yes C20 . C21 . 1.525(11) yes C20 . C22 . 1.530(11) yes C20 . H201 . 0.980 no C21 . H211 . 0.955 no C21 . H212 . 0.955 no C21 . H213 . 0.955 no C22 . H221 . 0.960 no C22 . H222 . 0.955 no C22 . H223 . 0.951 no C23 . C24 . 1.498(12) yes C23 . C25 . 1.546(12) yes C23 . H231 . 0.971 no C24 . H241 . 0.959 no C24 . H242 . 0.955 no C24 . H243 . 0.958 no C25 . H251 . 0.961 no C25 . H252 . 0.958 no C25 . H253 . 0.957 no C26 . C27 . 1.519(9) yes C26 . C28 . 1.391(10) yes C27 . H271 . 0.949 no C27 . H272 . 0.958 no C27 . H273 . 0.954 no C28 . C29 . 1.417(10) yes C28 . H281 . 0.926 no C29 . N30 . 1.321(9) yes C29 . C43 . 1.508(9) yes N30 . C31 . 1.447(8) yes N30 . C31 . 1.447(8) yes N30 . Ga101 . 1.98(4) yes C31 . C32 . 1.399(10) yes C31 . C39 . 1.418(10) yes C32 . C33 . 1.523(11) yes C32 . C36 . 1.395(10) yes C33 . C34 . 1.529(12) yes C33 . C35 . 1.531(11) yes C33 . H331 . 0.975 no C34 . H341 . 0.959 no C34 . H342 . 0.958 no C34 . H343 . 0.960 no C35 . H351 . 0.955 no C35 . H352 . 0.953 no C35 . H353 . 0.959 no C36 . C37 . 1.367(12) yes C36 . H361 . 0.927 no C37 . C38 . 1.375(12) yes C37 . H371 . 0.923 no C38 . C39 . 1.382(10) yes C38 . H381 . 0.927 no C39 . C40 . 1.518(10) yes C40 . C41 . 1.530(11) yes C40 . C42 . 1.523(12) yes C40 . H401 . 0.972 no C41 . H411 . 0.959 no C41 . H412 . 0.957 no C41 . H413 . 0.954 no C42 . H421 . 0.958 no C42 . H422 . 0.959 no C42 . H423 . 0.958 no C43 . H431 . 0.952 no C43 . H432 . 0.951 no C43 . H433 . 0.949 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 Mn2 . Ga1 . N13 . 121.28(16) yes Mn2 . Ga1 . N30 . 120.48(16) yes N13 . Ga1 . N30 . 93.50(19) yes Mn2 . Ga1 . H11 . 108.8 no N13 . Ga1 . H11 . 107.3 no N30 . Ga1 . H11 . 103.2 no Mn2 . Ga1 . H12 . 32.3 no N13 . Ga1 . H12 . 104.3 no N30 . Ga1 . H12 . 98.0 no H11 . Ga1 . H12 . 140.4 no Ga1 . Mn2 . C3 . 99.0(4) yes Ga1 . Mn2 . C5 . 77.3(3) yes C3 . Mn2 . C5 . 90.0(5) yes Ga1 . Mn2 . C7 . 99.9(3) yes C3 . Mn2 . C7 . 146.6(5) yes C5 . Mn2 . C7 . 120.9(5) yes Ga1 . Mn2 . C8 . 116.9(3) yes C3 . Mn2 . C8 . 143.2(5) yes C5 . Mn2 . C8 . 90.0(5) yes C7 . Mn2 . C8 . 38.2(4) yes Ga1 . Mn2 . C9 . 154.1(3) yes C3 . Mn2 . C9 . 105.2(5) yes C5 . Mn2 . C9 . 93.3(4) yes C7 . Mn2 . C9 . 64.1(4) yes C8 . Mn2 . C9 . 38.1(4) yes Ga1 . Mn2 . C10 . 154.5(2) yes C3 . Mn2 . C10 . 86.8(5) yes C5 . Mn2 . C10 . 127.8(4) yes C7 . Mn2 . C10 . 64.9(4) yes C8 . Mn2 . C10 . 64.7(4) yes Ga1 . Mn2 . C11 . 117.7(3) yes C3 . Mn2 . C11 . 107.7(5) yes C5 . Mn2 . C11 . 153.5(5) yes C7 . Mn2 . C11 . 38.9(4) yes C8 . Mn2 . C11 . 64.0(4) yes Ga1 . Mn2 . H12 . 34.4 no C3 . Mn2 . H12 . 92.0 no C5 . Mn2 . H12 . 111.0 no C7 . Mn2 . H12 . 88.2 no C8 . Mn2 . H12 . 122.1 no C9 . Mn2 . C10 . 38.8(3) yes C9 . Mn2 . C11 . 63.6(4) yes C10 . Mn2 . C11 . 37.9(3) yes C9 . Mn2 . H12 . 150.3 no C10 . Mn2 . H12 . 121.1 no C11 . Mn2 . H12 . 88.5 no C3 . Mn2 . C5 . 90.0(5) yes C3 . Mn2 . C7 . 146.6(5) yes C5 . Mn2 . C7 . 120.9(5) yes C3 . Mn2 . C8 . 143.2(5) yes C5 . Mn2 . C8 . 90.0(5) yes C7 . Mn2 . C8 . 38.2(4) yes C3 . Mn2 . C9 . 105.2(5) yes C5 . Mn2 . C9 . 93.3(4) yes C7 . Mn2 . C9 . 64.1(4) yes C8 . Mn2 . C9 . 38.1(4) yes C3 . Mn2 . C10 . 86.8(5) yes C5 . Mn2 . C10 . 127.8(4) yes C7 . Mn2 . C10 . 64.9(4) yes C8 . Mn2 . C10 . 64.7(4) yes C9 . Mn2 . C10 . 38.8(3) yes C3 . Mn2 . C11 . 107.7(5) yes C5 . Mn2 . C11 . 153.5(5) yes C7 . Mn2 . C11 . 38.9(4) yes C8 . Mn2 . C11 . 64.0(4) yes C9 . Mn2 . C11 . 63.6(4) yes C3 . Mn2 . Ga101 . 97.3(10) yes C5 . Mn2 . Ga101 . 90.6(4) yes C7 . Mn2 . Ga101 . 94.8(9) yes C8 . Mn2 . Ga101 . 119.5(10) yes C9 . Mn2 . Ga101 . 157.1(10) yes C10 . Mn2 . C11 . 37.9(3) yes C10 . Mn2 . Ga101 . 141.5(4) yes C11 . Mn2 . Ga101 . 106.1(5) yes Mn2 . C3 . O4 . 175.9(10) yes Mn2 . C5 . O6 . 175.7(8) yes Mn2 . C7 . C8 . 69.9(6) yes Mn2 . C7 . C11 . 70.6(6) yes C8 . C7 . C11 . 106.2(9) yes Mn2 . C7 . H71 . 126.3 no C8 . C7 . H71 . 126.7 no C11 . C7 . H71 . 127.0 no Mn2 . C8 . C7 . 71.9(6) yes Mn2 . C8 . C9 . 69.9(6) yes C7 . C8 . C9 . 108.5(10) yes Mn2 . C8 . H81 . 123.6 no C7 . C8 . H81 . 125.8 no C9 . C8 . H81 . 125.7 no Mn2 . C9 . C8 . 72.0(6) yes Mn2 . C9 . C10 . 72.3(5) yes C8 . C9 . C10 . 110.1(9) yes Mn2 . C9 . H91 . 124.9 no C8 . C9 . H91 . 124.8 no C10 . C9 . H91 . 125.1 no Mn2 . C10 . C9 . 68.9(5) yes Mn2 . C10 . C11 . 71.4(5) yes C9 . C10 . C11 . 106.0(9) yes Mn2 . C10 . C12 . 127.4(8) yes C9 . C10 . C12 . 126.8(9) yes C11 . C10 . C12 . 127.1(10) yes Mn2 . C11 . C7 . 70.5(6) yes Mn2 . C11 . C10 . 70.7(5) yes C7 . C11 . C10 . 109.2(10) yes Mn2 . C11 . H111 . 124.9 no C7 . C11 . H111 . 125.9 no C10 . C11 . H111 . 124.9 no C10 . C12 . H121 . 108.6 no C10 . C12 . H122 . 108.8 no H121 . C12 . H122 . 109.4 no C10 . C12 . H123 . 109.8 no H121 . C12 . H123 . 109.9 no H122 . C12 . H123 . 110.2 no Ga1 . N13 . C14 . 121.6(4) yes Ga1 . N13 . C26 . 118.5(5) yes C14 . N13 . C26 . 119.5(6) yes C14 . N13 . C26 . 119.5(6) yes C14 . N13 . Ga101 . 114.4(10) yes C26 . N13 . Ga101 . 125.1(11) yes N13 . C14 . C15 . 118.4(6) yes N13 . C14 . C19 . 120.3(6) yes C15 . C14 . C19 . 121.3(6) yes C14 . C15 . C16 . 117.7(7) yes C14 . C15 . C23 . 121.7(6) yes C16 . C15 . C23 . 120.5(7) yes C15 . C16 . C17 . 122.0(8) yes C15 . C16 . H161 . 118.8 no C17 . C16 . H161 . 119.2 no C16 . C17 . C18 . 119.7(7) yes C16 . C17 . H171 . 120.5 no C18 . C17 . H171 . 119.8 no C17 . C18 . C19 . 121.5(7) yes C17 . C18 . H181 . 119.4 no C19 . C18 . H181 . 119.1 no C14 . C19 . C18 . 117.8(7) yes C14 . C19 . C20 . 122.9(6) yes C18 . C19 . C20 . 119.3(7) yes C19 . C20 . C21 . 111.0(7) yes C19 . C20 . C22 . 111.6(7) yes C21 . C20 . C22 . 110.0(7) yes C19 . C20 . H201 . 108.5 no C21 . C20 . H201 . 108.1 no C22 . C20 . H201 . 107.4 no C20 . C21 . H211 . 109.7 no C20 . C21 . H212 . 109.7 no H211 . C21 . H212 . 110.6 no C20 . C21 . H213 . 109.2 no H211 . C21 . H213 . 109.0 no H212 . C21 . H213 . 108.7 no C20 . C22 . H221 . 110.1 no C20 . C22 . H222 . 109.4 no H221 . C22 . H222 . 109.5 no C20 . C22 . H223 . 109.2 no H221 . C22 . H223 . 109.1 no H222 . C22 . H223 . 109.5 no C15 . C23 . C24 . 112.7(8) yes C15 . C23 . C25 . 111.2(7) yes C24 . C23 . C25 . 108.6(7) yes C15 . C23 . H231 . 108.4 no C24 . C23 . H231 . 108.6 no C25 . C23 . H231 . 107.2 no C23 . C24 . H241 . 109.8 no C23 . C24 . H242 . 110.1 no H241 . C24 . H242 . 109.2 no C23 . C24 . H243 . 110.0 no H241 . C24 . H243 . 109.0 no H242 . C24 . H243 . 108.7 no C23 . C25 . H251 . 108.4 no C23 . C25 . H252 . 109.2 no H251 . C25 . H252 . 109.9 no C23 . C25 . H253 . 108.7 no H251 . C25 . H253 . 110.2 no H252 . C25 . H253 . 110.3 no N13 . C26 . C27 . 118.5(6) yes N13 . C26 . C28 . 123.7(6) yes C27 . C26 . C28 . 117.8(6) yes C26 . C27 . H271 . 108.8 no C26 . C27 . H272 . 109.6 no H271 . C27 . H272 . 110.0 no C26 . C27 . H273 . 109.2 no H271 . C27 . H273 . 109.7 no H272 . C27 . H273 . 109.5 no C26 . C28 . C29 . 127.3(6) yes C26 . C28 . H281 . 116.5 no C29 . C28 . H281 . 116.3 no C28 . C29 . N30 . 123.2(6) yes C28 . C29 . C43 . 116.2(6) yes N30 . C29 . C43 . 120.5(6) yes Ga1 . N30 . C29 . 119.8(4) yes Ga1 . N30 . C31 . 119.6(4) yes C29 . N30 . C31 . 119.7(6) yes C29 . N30 . C31 . 119.7(6) yes C29 . N30 . Ga101 . 126.9(11) yes C31 . N30 . Ga101 . 112.7(11) yes N30 . C31 . C32 . 120.1(6) yes N30 . C31 . C39 . 118.7(6) yes C32 . C31 . C39 . 120.8(7) yes C31 . C32 . C33 . 122.9(7) yes C31 . C32 . C36 . 118.9(7) yes C33 . C32 . C36 . 118.2(7) yes C32 . C33 . C34 . 110.8(7) yes C32 . C33 . C35 . 111.9(7) yes C34 . C33 . C35 . 110.5(7) yes C32 . C33 . H331 . 108.2 no C34 . C33 . H331 . 108.1 no C35 . C33 . H331 . 107.2 no C33 . C34 . H341 . 109.2 no C33 . C34 . H342 . 110.0 no H341 . C34 . H342 . 109.9 no C33 . C34 . H343 . 109.7 no H341 . C34 . H343 . 109.0 no H342 . C34 . H343 . 109.1 no C33 . C35 . H351 . 109.4 no C33 . C35 . H352 . 109.5 no H351 . C35 . H352 . 109.5 no C33 . C35 . H353 . 109.9 no H351 . C35 . H353 . 109.1 no H352 . C35 . H353 . 109.5 no C32 . C36 . C37 . 120.2(8) yes C32 . C36 . H361 . 120.0 no C37 . C36 . H361 . 119.8 no C36 . C37 . C38 . 120.9(7) yes C36 . C37 . H371 . 119.3 no C38 . C37 . H371 . 119.8 no C37 . C38 . C39 . 121.6(7) yes C37 . C38 . H381 . 119.2 no C39 . C38 . H381 . 119.2 no C31 . C39 . C38 . 117.5(7) yes C31 . C39 . C40 . 121.1(6) yes C38 . C39 . C40 . 121.4(7) yes C39 . C40 . C41 . 112.8(7) yes C39 . C40 . C42 . 110.5(7) yes C41 . C40 . C42 . 110.2(7) yes C39 . C40 . H401 . 107.3 no C41 . C40 . H401 . 108.0 no C42 . C40 . H401 . 107.8 no C40 . C41 . H411 . 109.0 no C40 . C41 . H412 . 109.2 no H411 . C41 . H412 . 109.7 no C40 . C41 . H413 . 109.7 no H411 . C41 . H413 . 109.8 no H412 . C41 . H413 . 109.4 no C40 . C42 . H421 . 110.2 no C40 . C42 . H422 . 110.1 no H421 . C42 . H422 . 108.7 no C40 . C42 . H423 . 110.2 no H421 . C42 . H423 . 109.0 no H422 . C42 . H423 . 108.6 no C29 . C43 . H431 . 109.3 no C29 . C43 . H432 . 109.2 no H431 . C43 . H432 . 109.2 no C29 . C43 . H433 . 109.0 no H431 . C43 . H433 . 109.9 no H432 . C43 . H433 . 110.3 no N13 . Ga101 . N30 . 92.1(13) yes N13 . Ga101 . Mn2 . 132.8(18) yes N30 . Ga101 . Mn2 . 135.1(18) yes Ga1 . H12 . Mn2 . 113.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C36 . H361 . O4 2_666 151.0(3) 0.927 2.498 3.339(13) yes _iucr_refine_instruction_details_constraints ; # # Punched on 31/05/13 at 15:51:00 # #LIST 12 BLOCK SCALE X'S U'S REM GA(1,U'S) UNTIL C(43) GA(101,U[ISO]) RIDE GA(1,U'S) GA(101,U'S) EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) RIDE GA ( 1,X'S) H ( 11,X'S) H ( 12,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) H ( 123,X'S) H ( 122,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 213,X'S) H ( 212,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 223,X'S) H ( 222,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 243,X'S) H ( 242,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 253,X'S) H ( 252,X'S) RIDE C ( 27,X'S) H ( 272,X'S) H ( 271,X'S) H ( 273,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 342,X'S) H ( 341,X'S) H ( 343,X'S) RIDE C ( 35,X'S) H ( 352,X'S) H ( 351,X'S) H ( 353,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 ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 413,X'S) H ( 412,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 423,X'S) H ( 422,X'S) RIDE C ( 43,X'S) H ( 433,X'S) H ( 432,X'S) H ( 431,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 31/05/13 at 15:51:00 # #LIST 16 PLANAR N(13) N(30) GA(101) MN(2) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 944059' ####################################################################### # # 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_051jtrt13 _vrf_PLAT_094_051jtrt13 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.12 RESPONSE: the residual density is localised around Mo(2) and correspond to a minor disorder component, possibly a kappa-1 Ga-H-Mo complex. ; _audit_creation_date 13-06-11 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '051jtrt13 in P 43 21 2 ' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 9.08300(10) _cell_length_b 9.08300(10) _cell_length_c 41.8928(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3456.19(7) _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2 ' _symmetry_space_group_name_Hall 'P 4nw 2abw' loop_ _symmetry_equiv_pos_as_xyz x,y,z -y+1/2,x+1/2,z+3/4 -x,-y,z+1/2 x+1/2,-y+1/2,-z+1/4 -y,-x,-z+1/2 y+1/2,-x+1/2,z+1/4 y,x,-z -x+1/2,y+1/2,-z+3/4 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' 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' 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' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 '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' Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C30 H32.50 Co0.50 Ga1 Mo0.25 N2 O3 # Dc = 1.14 Fooo = 1488.00 Mu = 11.41 M = 296.14 # Found Formula = C34 H41 Ga1 Mo1 N2 O5 # Dc = 1.39 FOOO = 1488.00 Mu = 11.83 M = 361.68 _chemical_formula_sum 'C34 H41 Ga1 Mo1 N2 O5' _chemical_formula_moiety 'C34 H41 Ga1 Mo1 N2 O5' _chemical_compound_source . _chemical_formula_weight 723.37 _cell_measurement_reflns_used 3991 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.120 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_max 0.210 _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1488.000 _exptl_absorpt_coefficient_mu 1.183 # Sheldrick geometric approximatio 0.80 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.87 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 63662 _reflns_number_total 3933 _diffrn_reflns_av_R_equivalents 0.052 # Number of reflections without Friedels Law is 3933 # Number of reflections with Friedels Law is 2385 # Theoretical number of reflections is about 1980 _diffrn_reflns_theta_min 5.106 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.477 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 51 _reflns_limit_h_min -7 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 54 _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 -1.45 _refine_diff_density_max 3.07 # 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>0.0\s(I) _refine_ls_number_reflns 3933 _refine_ls_number_restraints 382 _refine_ls_number_parameters 271 _oxford_refine_ls_R_factor_ref 0.0659 _refine_ls_wR_factor_ref 0.1298 _refine_ls_goodness_of_fit_ref 0.8947 _refine_ls_shift/su_max 0.0074406 _refine_ls_shift/su_mean 0.0007610 # The values computed with all filters except I/sigma _oxford_reflns_number_all 3933 _refine_ls_R_factor_all 0.0659 _refine_ls_wR_factor_all 0.1298 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3331 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_gt 0.1170 # 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 unk _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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 14.0 19.5 8.66 2.13 ; # 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 C35 C 0.3923(14) 0.7749(13) 0.5684(2) 0.0499 0.3782 Uani D . . 1 1 . C36 C 0.2275(16) 0.7445(19) 0.5613(5) 0.0549 0.3782 Uani D . . 1 1 . C37 C 0.408(2) 0.9130(15) 0.5898(4) 0.0548 0.3782 Uani D . . 1 1 . C38 C 0.3481(8) 0.7499(7) 0.56036(15) 0.0484 0.6218 Uani D . . 1 2 . C39 C 0.1841(8) 0.7204(11) 0.5678(3) 0.0592 0.6218 Uani D . . 1 2 . C40 C 0.3883(11) 0.9102(8) 0.5689(3) 0.0557 0.6218 Uani D . . 1 2 . C25 C 0.4632(16) 0.6394(16) 0.5850(3) 0.0383 0.2450 Uani D . . 1 1 . C26 C 0.447(2) 0.592(2) 0.6165(3) 0.0339 0.2450 Uani D . . 1 1 . C27 C 0.524(4) 0.472(3) 0.6278(4) 0.0306 0.2450 Uani D . . 1 1 . C28 C 0.625(3) 0.401(3) 0.6089(4) 0.0289 0.2450 Uani D . . 1 1 . C29 C 0.653(3) 0.448(3) 0.5776(4) 0.0274 0.2450 Uani D . . 1 1 . C30 C 0.4470(7) 0.6414(8) 0.57920(13) 0.0375 0.7550 Uani D . . 1 2 . C31 C 0.4075(10) 0.6062(12) 0.61057(14) 0.0418 0.7550 Uani D . . 1 2 . C32 C 0.4863(12) 0.5050(12) 0.62782(13) 0.0412 0.7550 Uani D . . 1 2 . C33 C 0.6033(10) 0.4310(10) 0.61455(15) 0.0393 0.7550 Uani D . . 1 2 . C34 C 0.6511(10) 0.4629(11) 0.58349(15) 0.0326 0.7550 Uani D . . 1 2 . Ga1 Ga 0.50514(6) 0.50514(6) 0.5000 0.0285 1.0000 Uani S T . . . . Mo2 Mo 0.30147(4) 0.30147(4) 0.5000 0.0289 1.0000 Uani S T . . . . C3 C 0.2957(6) 0.3088(7) 0.45107(12) 0.0362 1.0000 Uani . . . . . . C5 C 0.1374(6) 0.4556(7) 0.5023(2) 0.0477 1.0000 Uani . . . . . . C7 C 0.1467(6) 0.1467(6) 0.5000 0.0541 1.0000 Uani S T . . . . C10 C 0.7156(5) 0.7129(5) 0.52987(9) 0.0222 1.0000 Uani . . . . . . C11 C 0.7884(7) 0.7811(7) 0.55834(10) 0.0360 1.0000 Uani . . . . . . C12 C 0.7623(5) 0.7623(5) 0.500000(7) 0.0262 1.0000 Uani S T . . . . C13 C 0.5721(5) 0.5700(5) 0.56624(7) 0.0271 1.0000 Uani D . . . . . C20 C 0.7766(9) 0.3781(10) 0.56619(19) 0.0593 1.0000 Uani . . . . . . C21 C 0.7355(11) 0.2183(12) 0.5599(3) 0.0841 1.0000 Uani . . . . . . C22 C 0.9203(10) 0.3836(11) 0.5858(3) 0.0945 1.0000 Uani . . . . . . O4 O 0.2882(5) 0.3061(6) 0.42400(9) 0.0513 1.0000 Uani . . . . . . O6 O 0.0405(6) 0.5281(8) 0.5034(2) 0.0927 1.0000 Uani . . . . . . O8 O 0.0565(5) 0.0565(5) 0.5000 0.0944 1.0000 Uani S T . . . . N9 N 0.6123(5) 0.6097(4) 0.53412(8) 0.0213 1.0000 Uani . . . . . . H351 H 0.4221 0.7881 0.5462 0.0562 0.3782 Uiso R . . 1 1 . H361 H 0.2112 0.6394 0.5614 0.0761 0.3782 Uiso R . . 1 1 . H363 H 0.1870 0.7870 0.5803 0.0760 0.3782 Uiso R . . 1 1 . H362 H 0.1805 0.7876 0.5429 0.0760 0.3782 Uiso R . . 1 1 . H371 H 0.5102 0.9376 0.5876 0.0769 0.3782 Uiso R . . 1 1 . H373 H 0.3859 0.8988 0.6121 0.0770 0.3782 Uiso R . . 1 1 . H372 H 0.3482 0.9918 0.5816 0.0772 0.3782 Uiso R . . 1 1 . H381 H 0.3762 0.7394 0.5379 0.0559 0.6218 Uiso R . . 1 2 . H391 H 0.1639 0.6240 0.5590 0.0881 0.6218 Uiso R . . 1 2 . H393 H 0.1552 0.7224 0.5900 0.0880 0.6218 Uiso R . . 1 2 . H392 H 0.1289 0.7937 0.5562 0.0879 0.6218 Uiso R . . 1 2 . H401 H 0.4920 0.9283 0.5666 0.0800 0.6218 Uiso R . . 1 2 . H403 H 0.3588 0.9185 0.5909 0.0802 0.6218 Uiso R . . 1 2 . H402 H 0.3326 0.9772 0.5558 0.0800 0.6218 Uiso R . . 1 2 . H261 H 0.3841 0.6421 0.6303 0.0391 0.2450 Uiso R . . 1 1 . H271 H 0.5064 0.4374 0.6483 0.0361 0.2450 Uiso R . . 1 1 . H281 H 0.6751 0.3191 0.6169 0.0340 0.2450 Uiso R . . 1 1 . H311 H 0.3272 0.6533 0.6201 0.0492 0.7550 Uiso R . . 1 2 . H321 H 0.4596 0.4849 0.6490 0.0481 0.7550 Uiso R . . 1 2 . H331 H 0.6517 0.3584 0.6262 0.0461 0.7550 Uiso R . . 1 2 . H112 H 0.8322 0.7080 0.5718 0.0561 1.0000 Uiso R . . . . . H111 H 0.7180 0.8348 0.5707 0.0561 1.0000 Uiso R . . . . . H113 H 0.8643 0.8482 0.5514 0.0562 1.0000 Uiso R . . . . . H121 H 0.8351 0.8351 0.5000 0.0324 1.0000 Uiso RS . . . . . H212 H 0.8183 0.1662 0.5510 0.1201 1.0000 Uiso R . . . . . H211 H 0.7049 0.1729 0.5797 0.1201 1.0000 Uiso R . . . . . H213 H 0.6546 0.2162 0.5450 0.1199 1.0000 Uiso R . . . . . H222 H 0.9985 0.3377 0.5741 0.1320 1.0000 Uiso R . . . . . H221 H 0.9028 0.3298 0.6054 0.1321 1.0000 Uiso R . . . . . H223 H 0.9459 0.4844 0.5907 0.1318 1.0000 Uiso R . . . . . H201 H 0.7988 0.4249 0.5457 0.0740 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 C35 0.056(6) 0.041(5) 0.052(5) 0.002(4) 0.015(5) 0.015(5) C36 0.059(7) 0.045(6) 0.061(6) 0.010(6) 0.016(6) 0.012(6) C37 0.062(7) 0.043(6) 0.058(6) -0.002(5) 0.021(6) 0.016(6) C38 0.048(4) 0.042(4) 0.055(4) 0.002(3) 0.013(3) 0.007(3) C39 0.050(5) 0.051(5) 0.076(5) 0.005(5) 0.019(5) 0.005(4) C40 0.057(5) 0.042(4) 0.067(5) 0.009(4) 0.007(5) 0.005(4) C25 0.046(5) 0.036(5) 0.033(5) -0.002(4) 0.007(4) 0.007(4) C26 0.039(6) 0.036(6) 0.026(5) -0.004(5) 0.004(6) 0.005(6) C27 0.036(7) 0.035(7) 0.020(6) -0.001(6) 0.001(6) 0.002(6) C28 0.036(7) 0.034(6) 0.017(6) -0.002(6) 0.002(6) 0.002(6) C29 0.036(6) 0.031(5) 0.015(5) 0.001(5) 0.000(5) -0.003(5) C30 0.049(3) 0.038(3) 0.026(3) -0.002(3) 0.012(3) 0.001(3) C31 0.057(4) 0.043(4) 0.026(3) -0.002(3) 0.016(3) -0.001(3) C32 0.057(5) 0.044(4) 0.023(3) -0.001(3) 0.012(3) -0.008(3) C33 0.052(4) 0.046(4) 0.020(3) 0.006(3) 0.002(3) -0.007(3) C34 0.041(3) 0.039(4) 0.017(3) 0.008(3) -0.003(3) -0.006(3) Ga1 0.0314(2) 0.0314(2) 0.0226(3) -0.0001(2) 0.0001(2) -0.0039(3) Mo2 0.02648(17) 0.02648(17) 0.0337(3) 0.0009(2) -0.0009(2) -0.0007(2) C3 0.031(3) 0.034(3) 0.044(3) -0.004(3) -0.008(3) -0.001(2) C5 0.031(3) 0.053(3) 0.059(4) 0.006(4) 0.002(4) 0.000(2) C7 0.049(3) 0.049(3) 0.065(6) 0.005(5) -0.005(5) -0.016(4) C10 0.022(2) 0.025(2) 0.0203(17) -0.0012(19) -0.0046(18) 0.0006(15) C11 0.044(3) 0.043(4) 0.0209(19) -0.003(2) -0.006(2) -0.010(2) C12 0.0282(18) 0.0282(18) 0.022(3) 0.000(2) 0.000(2) -0.005(2) C13 0.036(2) 0.028(2) 0.0178(17) 0.0011(17) 0.0020(18) -0.0040(16) C20 0.051(5) 0.068(5) 0.059(4) 0.035(4) 0.004(3) 0.025(4) C21 0.076(7) 0.080(7) 0.096(7) -0.009(6) -0.007(5) 0.038(6) C22 0.047(5) 0.076(6) 0.160(11) 0.057(7) -0.023(6) -0.007(5) O4 0.054(3) 0.062(3) 0.0369(19) -0.003(2) -0.014(2) -0.008(2) O6 0.047(3) 0.134(6) 0.097(5) 0.030(5) 0.014(4) 0.060(3) O8 0.090(4) 0.090(4) 0.103(6) 0.013(6) -0.013(6) -0.061(5) N9 0.025(2) 0.022(2) 0.0168(15) 0.0011(16) -0.0002(16) 0.0030(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.20572(17) 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 C35 . C36 . 1.551(5) yes C35 . C37 . 1.548(5) yes C35 . C25 . 1.553(5) yes C35 . H351 . 0.978 no C36 . H361 . 0.966 no C36 . H363 . 0.961 no C36 . H362 . 0.964 no C37 . H371 . 0.960 no C37 . H373 . 0.961 no C37 . H372 . 0.961 no C38 . C39 . 1.546(5) yes C38 . C40 . 1.543(5) yes C38 . C30 . 1.550(5) yes C38 . H381 . 0.980 no C39 . H391 . 0.966 no C39 . H393 . 0.968 no C39 . H392 . 0.966 no C40 . H401 . 0.961 no C40 . H403 . 0.964 no C40 . H402 . 0.963 no C25 . C26 . 1.400(6) yes C25 . C13 . 1.411(6) yes C26 . C27 . 1.375(6) yes C26 . H261 . 0.931 no C27 . C28 . 1.373(6) yes C27 . H271 . 0.932 no C28 . C29 . 1.402(6) yes C28 . H281 . 0.930 no C29 . C13 . 1.415(6) yes C29 . C20 . 1.373(13) yes C30 . C31 . 1.399(4) yes C30 . C13 . 1.417(5) yes C31 . C32 . 1.371(5) yes C31 . H311 . 0.935 no C32 . C33 . 1.374(5) yes C32 . H321 . 0.936 no C33 . C34 . 1.402(4) yes C33 . H331 . 0.932 no C34 . C13 . 1.408(5) yes C34 . C20 . 1.555(9) yes Ga1 . N9 7_556 1.973(3) yes Ga1 . Mo2 . 2.6162(10) yes Ga1 . N9 . 1.973(3) yes Mo2 . C3 7_556 2.051(5) yes Mo2 . C5 7_556 2.047(6) yes Mo2 . C3 . 2.051(5) yes Mo2 . C5 . 2.047(6) yes Mo2 . C7 . 1.988(8) yes C3 . O4 . 1.136(6) yes C5 . O6 . 1.100(7) yes C7 . O8 . 1.159(10) yes C10 . C11 . 1.498(5) yes C10 . C12 . 1.395(5) yes C10 . N9 . 1.338(5) yes C11 . H112 . 0.958 no C11 . H111 . 0.957 no C11 . H113 . 0.965 no C12 . H121 . 0.936 no C13 . N9 . 1.440(4) yes C13 . N9 . 1.440(4) yes C20 . C21 . 1.521(13) yes C20 . C22 . 1.544(11) yes C20 . H201 . 0.979 no C20 . C21 . 1.521(13) yes C20 . C22 . 1.544(11) yes C20 . H201 . 0.979 no C21 . H212 . 0.965 no C21 . H211 . 0.965 no C21 . H213 . 0.965 no C22 . H222 . 0.960 no C22 . H221 . 0.967 no C22 . H223 . 0.966 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 C36 . C35 . C37 . 110.20(6) yes C36 . C35 . C25 . 110.21(6) yes C37 . C35 . C25 . 110.20(6) yes C36 . C35 . H351 . 96.0 no C37 . C35 . H351 . 115.3 no C25 . C35 . H351 . 114.0 no C35 . C36 . H361 . 108.9 no C35 . C36 . H363 . 97.9 no H361 . C36 . H363 . 109.4 no C35 . C36 . H362 . 120.7 no H361 . C36 . H362 . 109.8 no H363 . C36 . H362 . 109.4 no C35 . C37 . H371 . 102.7 no C35 . C37 . H373 . 115.7 no H371 . C37 . H373 . 109.1 no C35 . C37 . H372 . 110.1 no H371 . C37 . H372 . 109.7 no H373 . C37 . H372 . 109.2 no C39 . C38 . C40 . 110.19(6) yes C39 . C38 . C30 . 110.21(6) yes C40 . C38 . C30 . 110.20(6) yes C39 . C38 . H381 . 115.3 no C40 . C38 . H381 . 104.6 no C30 . C38 . H381 . 106.1 no C38 . C39 . H391 . 105.3 no C38 . C39 . H393 . 116.9 no H391 . C39 . H393 . 109.4 no C38 . C39 . H392 . 106.2 no H391 . C39 . H392 . 109.5 no H393 . C39 . H392 . 109.4 no C38 . C40 . H401 . 111.7 no C38 . C40 . H403 . 103.2 no H401 . C40 . H403 . 110.8 no C38 . C40 . H402 . 109.9 no H401 . C40 . H402 . 110.5 no H403 . C40 . H402 . 110.5 no C35 . C25 . C26 . 128.6(7) yes C35 . C25 . C13 . 113.4(7) yes C26 . C25 . C13 . 117.41(7) yes C25 . C26 . C27 . 120.92(7) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 119.3 no C26 . C27 . C28 . 121.19(7) yes C26 . C27 . H271 . 119.6 no C28 . C27 . H271 . 119.2 no C27 . C28 . C29 . 120.92(7) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 119.4 no C28 . C29 . C13 . 117.43(7) yes C28 . C29 . C20 . 109.5(10) yes C13 . C29 . C20 . 132.0(10) yes C38 . C30 . C31 . 118.4(4) yes C38 . C30 . C13 . 124.1(4) yes C31 . C30 . C13 . 117.46(6) yes C30 . C31 . C32 . 120.95(6) yes C30 . C31 . H311 . 119.7 no C32 . C31 . H311 . 119.3 no C31 . C32 . C33 . 121.21(6) yes C31 . C32 . H321 . 119.6 no C33 . C32 . H321 . 119.2 no C32 . C33 . C34 . 120.94(6) yes C32 . C33 . H331 . 119.9 no C34 . C33 . H331 . 119.2 no C33 . C34 . C13 . 117.45(6) yes C33 . C34 . C20 . 123.9(4) yes C13 . C34 . C20 . 118.5(4) yes N9 7_556 Ga1 . Mo2 . 133.57(10) yes N9 7_556 Ga1 . N9 . 92.86(19) yes Mo2 . Ga1 . N9 . 133.57(10) yes Ga1 . Mo2 . C3 7_556 89.73(14) yes Ga1 . Mo2 . C5 7_556 91.79(18) yes C3 7_556 Mo2 . C5 7_556 90.4(3) yes Ga1 . Mo2 . C3 . 89.73(14) yes C3 7_556 Mo2 . C3 . 179.5(3) yes C5 7_556 Mo2 . C3 . 89.7(3) yes Ga1 . Mo2 . C5 . 91.79(18) yes C3 7_556 Mo2 . C5 . 89.7(3) yes C5 7_556 Mo2 . C5 . 176.4(4) yes C3 . Mo2 . C5 . 90.4(3) yes Ga1 . Mo2 . C7 . 179.994 yes C3 7_556 Mo2 . C7 . 90.27(14) yes C5 7_556 Mo2 . C7 . 88.21(18) yes C3 . Mo2 . C7 . 90.27(14) yes C5 . Mo2 . C7 . 88.21(18) yes Mo2 . C3 . O4 . 176.3(5) yes Mo2 . C5 . O6 . 173.6(7) yes Mo2 . C7 . O8 . 179.990 yes C11 . C10 . C12 . 116.6(4) yes C11 . C10 . N9 . 119.6(4) yes C12 . C10 . N9 . 123.9(4) yes C10 . C11 . H112 . 111.5 no C10 . C11 . H111 . 110.3 no H112 . C11 . H111 . 108.1 no C10 . C11 . H113 . 109.6 no H112 . C11 . H113 . 108.6 no H111 . C11 . H113 . 108.6 no C10 . C12 . C10 7_556 127.5(5) yes C10 . C12 . H121 . 116.2 no C10 7_556 C12 . H121 . 116.2 no C29 . C13 . C25 . 121.86(7) yes C29 . C13 . N9 . 112.3(5) yes C25 . C13 . N9 . 125.8(6) yes C30 . C13 . C34 . 121.88(6) yes C30 . C13 . N9 . 116.5(4) yes C34 . C13 . N9 . 121.6(4) yes C29 . C20 . C21 . 107.5(18) yes C29 . C20 . C22 . 119.2(17) yes C21 . C20 . C22 . 109.3(6) yes C29 . C20 . H201 . 105.9 no C21 . C20 . H201 . 108.3 no C22 . C20 . H201 . 106.2 no C34 . C20 . C21 . 111.9(8) yes C34 . C20 . C22 . 110.8(8) yes C21 . C20 . C22 . 109.3(6) yes C34 . C20 . H201 . 110.1 no C21 . C20 . H201 . 108.3 no C22 . C20 . H201 . 106.2 no C20 . C21 . H212 . 110.1 no C20 . C21 . H211 . 109.3 no H212 . C21 . H211 . 110.3 no C20 . C21 . H213 . 108.5 no H212 . C21 . H213 . 109.4 no H211 . C21 . H213 . 109.2 no C20 . C22 . H222 . 109.8 no C20 . C22 . H221 . 107.2 no H222 . C22 . H221 . 109.6 no C20 . C22 . H223 . 110.3 no H222 . C22 . H223 . 110.0 no H221 . C22 . H223 . 109.9 no C13 . N9 . Ga1 . 115.5(3) yes C13 . N9 . C10 . 118.5(3) yes Ga1 . N9 . C10 . 125.9(3) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C39 . H363 . C37 . 120.5(16) 0.801 2.345 2.837(15) yes _iucr_refine_instruction_details_constraints ; # # Punched on 11/06/13 at 16:46:34 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 363,X'S) H ( 362,X'S) RIDE C ( 37,X'S) H ( 371,X'S) H ( 373,X'S) H ( 372,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 393,X'S) H ( 392,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 403,X'S) H ( 402,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 ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 111,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) H ( 213,X'S) RIDE C ( 22,X'S) H ( 222,X'S) H ( 221,X'S) H ( 223,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 11/06/13 at 16:46:35 # #LIST 16 SAME C(13) C(25) C(26) C(27) C(28) C(29) AND CONT C(13) C(30) C(31) C(32) C(33) C(34) AND CONT C(13) C(29) C(28) C(27) C(26) C(25) AND CONT C(13) C(34) C(33) C(32) C(31) C(30) SIMU 0.01 C(13) C(25) C(26) C(27) C(28) C(29) AND CONT C(13) C(30) C(31) C(32) C(33) C(34) AND CONT C(13) C(29) C(28) C(27) C(26) C(25) AND CONT C(13) C(34) C(33) C(32) C(31) C(30) DELU 0.01 C(13) C(25) C(26) C(27) C(28) C(29) AND CONT C(13) C(30) C(31) C(32) C(33) C(34) AND CONT C(13) C(29) C(28) C(27) C(26) C(25) AND CONT C(13) C(34) C(33) C(32) C(31) C(30) SAME C(38) C(40) C(39) C(30) AND CONT C(38) C(39) C(30) C(40) AND CONT C(38) C(30) C(40) C(39) AND CONT C(35) C(37) C(36) C(25) AND CONT C(35) C(36) C(25) C(37) AND CONT C(35) C(25) C(37) C(36) SIMU 0.01 C(38) C(40) C(39) C(30) AND CONT C(38) C(39) C(30) C(40) AND CONT C(38) C(30) C(40) C(39) AND CONT C(35) C(37) C(36) C(25) AND CONT C(35) C(36) C(25) C(37) AND CONT C(35) C(25) C(37) C(36) DELU 0.01 C(38) C(40) C(39) C(30) AND CONT C(38) C(39) C(30) C(40) AND CONT C(38) C(30) C(40) C(39) AND CONT C(35) C(37) C(36) C(25) AND CONT C(35) C(36) C(25) C(37) AND CONT C(35) C(25) C(37) C(36) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 944060' ####################################################################### # # 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 _cell_length_a 9.15777(10) _cell_length_b 35.5896(6) _cell_length_c 21.1050(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6878.57(17) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b n m ' _symmetry_space_group_name_Hall '-P 2c 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 -x,-y,z+1/2 x,y,-z+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 0.0181 0.0091 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 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 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' Ga -1.2846 0.7763 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' W -5.4734 5.5774 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C77.50 H77.50 Ga2.50 N5 O5 W1.25 # Dc = 3.02 Fooo = 3232.00 Mu = 106.42 M = 1563.11 # Found Formula = C34 H41 Ga1 N2 O5 W1 # Dc = 1.57 FOOO = 3232.00 Mu = 73.78 M = 811.28 _chemical_formula_sum 'C34 H41 Ga1 N2 O5 W1' _chemical_formula_moiety 'C34 H41 Ga1 N2 O5 W1' _chemical_compound_source . _chemical_formula_weight 811.28 _cell_measurement_reflns_used 14158 _cell_measurement_theta_min 3 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 7.378 # Sheldrick geometric approximatio 0.48 0.74 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.74 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _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 150 _diffrn_reflns_number 37303 _reflns_number_total 7351 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections without Friedels Law is 11360 # Number of reflections with Friedels Law is 7351 # Theoretical number of reflections is about 7189 _diffrn_reflns_theta_min 3.249 _diffrn_reflns_theta_max 76.084 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 74.563 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 44 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 2.08 _oxford_diffrn_Wilson_scale 1.08 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.15 _refine_diff_density_max 3.62 # 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>-3.0\s(I) _refine_ls_number_reflns 7319 _refine_ls_number_restraints 220 _refine_ls_number_parameters 417 _oxford_refine_ls_R_factor_ref 0.0620 _refine_ls_wR_factor_ref 0.1196 _refine_ls_goodness_of_fit_ref 0.8871 _refine_ls_shift/su_max 0.0233517 _refine_ls_shift/su_mean 0.0010188 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7319 _refine_ls_R_factor_all 0.0620 _refine_ls_wR_factor_all 0.1196 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6867 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_gt 0.1190 # 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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.208E+04 0.327E+04 0.209E+04 898. 194. ; # 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 W1 W 0.70826(4) 0.484430(10) 0.7500 0.0246 1.0000 Uani S T . . . . Ga2 Ga 0.50034(10) 0.43501(3) 0.7500 0.0204 1.0000 Uani S T . . . . N3 N 0.3943(5) 0.40913(12) 0.6826(2) 0.0222 1.0000 Uani . . . . . . C4 C 0.4276(7) 0.42050(17) 0.6189(3) 0.0277 1.0000 Uani . . . . . . C5 C 0.5455(8) 0.40299(17) 0.5875(4) 0.0520 1.0000 Uani D . . . . . C6 C 0.5723(10) 0.4145(2) 0.5246(3) 0.0518 1.0000 Uani . . . . . . C7 C 0.4916(10) 0.4425(2) 0.4969(3) 0.0544 1.0000 Uani . . . . . . C8 C 0.3842(8) 0.4594(2) 0.5288(3) 0.0474 1.0000 Uani . . . . . . C9 C 0.3464(6) 0.44906(17) 0.5902(3) 0.0391 1.0000 Uani D . . . . . C10 C 0.2222(5) 0.46873(15) 0.6249(3) 0.0540 1.0000 Uani D . . . . . C11 C 0.2636(8) 0.5081(2) 0.6446(5) 0.0690 1.0000 Uani D . . . . . C12 C 0.0833(7) 0.4700(2) 0.5852(5) 0.0766 1.0000 Uani D . . . . . C13 C 0.6372(8) 0.37212(16) 0.6179(3) 0.0767 1.0000 Uani D . . . . . C14 C 0.7992(9) 0.3807(2) 0.6144(6) 0.0886 1.0000 Uani D . . . . . C15 C 0.6081(11) 0.33426(19) 0.5884(6) 0.0978 1.0000 Uani D . . . . . C16 C 0.2887(6) 0.38303(15) 0.6911(3) 0.0242 1.0000 Uani . . . . . . C17 C 0.2450(8) 0.3705(2) 0.750000(7) 0.0211 1.0000 Uani S T . . . . C18 C 0.2168(8) 0.36599(19) 0.6337(3) 0.0394 1.0000 Uani . . . . . . C19 C 0.8748(12) 0.5216(3) 0.7500 0.0437 1.0000 Uani S T . . . . O20 O 0.9617(10) 0.5436(3) 0.7500 0.0722 1.0000 Uani S T . . . . C21 C 0.7028(7) 0.48530(17) 0.6534(3) 0.0307 1.0000 Uani . . . . . . O22 O 0.7018(6) 0.48783(15) 0.5998(2) 0.0496 1.0000 Uani . . . . . . C23 C 0.8577(13) 0.4420(3) 0.7500 0.0506 1.0000 Uani S T . . . . O24 O 0.9563(11) 0.4227(3) 0.7500 0.0876 1.0000 Uani S T . . . . C25 C 0.5736(12) 0.5291(3) 0.7500 0.0427 1.0000 Uani S T . . . . O26 O 0.5056(10) 0.5555(2) 0.7500 0.0799 1.0000 Uani S T . . . . W27 W 0.72347(4) 0.236480(11) 0.7500 0.0300 1.0000 Uani S T . . . . Ga28 Ga 0.52013(10) 0.18583(3) 0.7500 0.0209 1.0000 Uani S T . . . . N29 N 0.4159(5) 0.15946(12) 0.6826(2) 0.0222 1.0000 Uani . . . . . . C30 C 0.4536(7) 0.16951(16) 0.6187(3) 0.0275 1.0000 Uani . . . . . . C31 C 0.3749(6) 0.19735(16) 0.5868(3) 0.0383 1.0000 Uani D . . . . . C32 C 0.4151(9) 0.2059(2) 0.5249(3) 0.0455 1.0000 Uani . . . . . . C33 C 0.5272(10) 0.1871(2) 0.4960(3) 0.0542 1.0000 Uani . . . . . . C34 C 0.6035(11) 0.1601(2) 0.5274(4) 0.0616 1.0000 Uani . . . . . . C35 C 0.5714(8) 0.15076(18) 0.5896(3) 0.0553 1.0000 Uani D . . . . . C36 C 0.6586(7) 0.12068(16) 0.6240(3) 0.0764 1.0000 Uani D . . . . . C37 C 0.8210(9) 0.1280(2) 0.6206(5) 0.0840 1.0000 Uani D . . . . . C38 C 0.6262(10) 0.08171(19) 0.5986(5) 0.0927 1.0000 Uani D . . . . . C39 C 0.2511(5) 0.21872(15) 0.6184(2) 0.0541 1.0000 Uani D . . . . . C40 C 0.1110(7) 0.2170(2) 0.5796(5) 0.0700 1.0000 Uani D . . . . . C41 C 0.2912(8) 0.25940(19) 0.6306(5) 0.0660 1.0000 Uani D . . . . . C42 C 0.3131(6) 0.13311(14) 0.6907(3) 0.0226 1.0000 Uani . . . . . . C43 C 0.2664(9) 0.1205(2) 0.750000(7) 0.0303 1.0000 Uani S T . . . . C44 C 0.2390(8) 0.1158(2) 0.6342(3) 0.0392 1.0000 Uani . . . . . . C45 C 0.8887(14) 0.1962(3) 0.7500 0.0529 1.0000 Uani S T . . . . O46 O 0.9779(9) 0.1769(3) 0.7500 0.0766 1.0000 Uani S T . . . . C47 C 0.5751(13) 0.2798(3) 0.7500 0.0508 1.0000 Uani S T . . . . O48 O 0.5030(11) 0.3051(2) 0.7500 0.0706 1.0000 Uani S T . . . . C49 C 0.7220(7) 0.23677(17) 0.6533(4) 0.0353 1.0000 Uani . . . . . . O50 O 0.7262(6) 0.23852(15) 0.5994(3) 0.0518 1.0000 Uani . . . . . . C51 C 0.8778(16) 0.2756(4) 0.7500 0.0665 1.0000 Uani S T . . . . O52 O 0.9706(13) 0.2972(3) 0.7500 0.1017 1.0000 Uani S T . . . . H61 H 0.6463 0.4029 0.5015 0.0641 1.0000 Uiso R . . . . . H71 H 0.5117 0.4497 0.4558 0.0661 1.0000 Uiso R . . . . . H81 H 0.3328 0.4789 0.5091 0.0580 1.0000 Uiso R . . . . . H101 H 0.2006 0.4541 0.6631 0.0672 1.0000 Uiso R . . . . . H111 H 0.1867 0.5185 0.6699 0.1030 1.0000 Uiso R . . . . . H112 H 0.3526 0.5070 0.6689 0.1032 1.0000 Uiso R . . . . . H113 H 0.2766 0.5231 0.6073 0.1028 1.0000 Uiso R . . . . . H122 H 0.0088 0.4831 0.6086 0.1151 1.0000 Uiso R . . . . . H123 H 0.1040 0.4833 0.5464 0.1149 1.0000 Uiso R . . . . . H121 H 0.0515 0.4447 0.5756 0.1151 1.0000 Uiso R . . . . . H131 H 0.6089 0.3704 0.6625 0.0923 1.0000 Uiso R . . . . . H143 H 0.8527 0.3613 0.6362 0.1311 1.0000 Uiso R . . . . . H141 H 0.8194 0.4047 0.6341 0.1311 1.0000 Uiso R . . . . . H142 H 0.8304 0.3814 0.5707 0.1310 1.0000 Uiso R . . . . . H151 H 0.6836 0.3170 0.6017 0.1441 1.0000 Uiso R . . . . . H152 H 0.5135 0.3257 0.6027 0.1443 1.0000 Uiso R . . . . . H153 H 0.6086 0.3371 0.5429 0.1437 1.0000 Uiso R . . . . . H171 H 0.1768 0.3511 0.7500 0.0280 1.0000 Uiso RS . . . . . H182 H 0.1501 0.3468 0.6466 0.0623 1.0000 Uiso R . . . . . H181 H 0.1653 0.3851 0.6114 0.0621 1.0000 Uiso R . . . . . H183 H 0.2887 0.3553 0.6068 0.0618 1.0000 Uiso R . . . . . H321 H 0.3650 0.2246 0.5030 0.0562 1.0000 Uiso R . . . . . H331 H 0.5513 0.1931 0.4543 0.0651 1.0000 Uiso R . . . . . H341 H 0.6793 0.1475 0.5065 0.0731 1.0000 Uiso R . . . . . H361 H 0.6301 0.1210 0.6688 0.0913 1.0000 Uiso R . . . . . H371 H 0.8715 0.1080 0.6419 0.1231 1.0000 Uiso R . . . . . H372 H 0.8425 0.1516 0.6406 0.1231 1.0000 Uiso R . . . . . H373 H 0.8505 0.1288 0.5768 0.1230 1.0000 Uiso R . . . . . H382 H 0.6988 0.0644 0.6144 0.1352 1.0000 Uiso R . . . . . H383 H 0.5311 0.0742 0.6132 0.1352 1.0000 Uiso R . . . . . H381 H 0.6277 0.0823 0.5528 0.1348 1.0000 Uiso R . . . . . H391 H 0.2314 0.2068 0.6593 0.0661 1.0000 Uiso R . . . . . H403 H 0.0307 0.2254 0.6053 0.1051 1.0000 Uiso R . . . . . H401 H 0.1200 0.2330 0.5429 0.1051 1.0000 Uiso R . . . . . H402 H 0.0930 0.1916 0.5659 0.1051 1.0000 Uiso R . . . . . H411 H 0.2129 0.2716 0.6528 0.1000 1.0000 Uiso R . . . . . H412 H 0.3786 0.2602 0.6559 0.1000 1.0000 Uiso R . . . . . H413 H 0.3079 0.2716 0.5908 0.0998 1.0000 Uiso R . . . . . H431 H 0.1959 0.1017 0.7500 0.0363 1.0000 Uiso RS . . . . . H442 H 0.1731 0.0963 0.6471 0.0621 1.0000 Uiso R . . . . . H441 H 0.1853 0.1346 0.6117 0.0622 1.0000 Uiso R . . . . . H443 H 0.3108 0.1052 0.6066 0.0620 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 W1 0.02193(18) 0.0281(2) 0.02379(19) 0.0000 0.0000 -0.00210(14) Ga2 0.0209(4) 0.0254(4) 0.0150(4) 0.0000 0.0000 -0.0011(4) N3 0.023(2) 0.025(2) 0.019(2) 0.0006(18) -0.0006(18) -0.0030(18) C4 0.033(3) 0.033(3) 0.017(3) -0.003(2) -0.001(2) -0.009(2) C5 0.080(5) 0.038(3) 0.037(4) -0.001(3) 0.022(4) 0.007(3) C6 0.081(6) 0.051(4) 0.023(3) -0.009(3) 0.021(4) -0.010(4) C7 0.082(6) 0.061(5) 0.021(3) 0.009(3) -0.002(4) -0.034(4) C8 0.049(4) 0.060(5) 0.033(4) 0.020(3) -0.011(3) -0.022(4) C9 0.031(3) 0.049(3) 0.037(3) 0.016(3) -0.004(3) -0.010(3) C10 0.036(3) 0.065(3) 0.061(4) 0.024(3) 0.001(3) 0.004(3) C11 0.052(4) 0.081(5) 0.075(5) -0.005(4) 0.004(4) 0.008(4) C12 0.047(4) 0.083(5) 0.099(6) 0.012(5) -0.013(4) 0.000(4) C13 0.097(5) 0.056(4) 0.077(4) 0.008(3) 0.032(4) 0.028(4) C14 0.102(6) 0.069(5) 0.094(6) -0.003(5) 0.010(5) 0.028(5) C15 0.103(6) 0.059(4) 0.131(7) 0.012(5) 0.029(6) 0.011(5) C16 0.028(3) 0.026(3) 0.019(3) -0.002(2) -0.003(2) -0.002(2) C17 0.021(3) 0.030(4) 0.012(4) 0.0000 0.0000 -0.001(3) C18 0.046(4) 0.040(4) 0.032(4) -0.001(3) -0.011(3) -0.016(3) C19 0.046(6) 0.059(6) 0.026(5) 0.0000 0.0000 -0.012(5) O20 0.062(6) 0.077(6) 0.077(6) 0.0000 0.0000 -0.043(5) C21 0.032(3) 0.036(3) 0.024(3) 0.006(2) -0.002(2) -0.008(3) O22 0.062(3) 0.058(3) 0.028(3) 0.014(2) -0.004(2) -0.019(3) C23 0.053(6) 0.050(6) 0.049(6) 0.0000 0.0000 0.019(5) O24 0.070(6) 0.112(8) 0.080(7) 0.0000 0.0000 0.072(6) C25 0.047(6) 0.036(5) 0.044(6) 0.0000 0.0000 -0.001(5) O26 0.060(5) 0.041(4) 0.140(10) 0.0000 0.0000 0.021(4) W27 0.0238(2) 0.0266(2) 0.0395(2) 0.0000 0.0000 -0.00464(15) Ga28 0.0195(4) 0.0235(4) 0.0198(5) 0.0000 0.0000 -0.0007(4) N29 0.026(2) 0.022(2) 0.019(2) 0.0000(18) -0.0001(18) -0.0010(18) C30 0.038(3) 0.027(3) 0.017(3) -0.001(2) 0.003(2) -0.003(2) C31 0.035(3) 0.044(3) 0.036(3) 0.014(3) -0.007(3) -0.005(3) C32 0.058(4) 0.048(4) 0.030(4) 0.015(3) -0.009(3) -0.015(3) C33 0.085(6) 0.056(5) 0.022(3) 0.003(3) 0.010(4) -0.018(4) C34 0.096(7) 0.057(5) 0.032(4) -0.001(4) 0.037(4) 0.012(5) C35 0.087(5) 0.043(3) 0.036(4) 0.005(3) 0.031(4) 0.023(4) C36 0.104(5) 0.059(3) 0.066(4) 0.011(3) 0.040(4) 0.042(4) C37 0.109(6) 0.069(5) 0.074(5) 0.002(4) 0.018(5) 0.043(5) C38 0.109(6) 0.059(4) 0.109(6) 0.020(4) 0.043(6) 0.029(5) C39 0.042(3) 0.060(3) 0.060(4) 0.024(3) -0.005(3) 0.011(3) C40 0.045(4) 0.068(4) 0.098(6) 0.026(4) -0.013(4) 0.003(4) C41 0.052(4) 0.072(4) 0.073(5) -0.007(4) -0.014(4) 0.018(4) C42 0.025(3) 0.023(3) 0.021(3) -0.001(2) -0.003(2) 0.002(2) C43 0.016(4) 0.021(4) 0.053(6) 0.0000 0.0000 -0.001(3) C44 0.055(4) 0.042(4) 0.020(3) 0.003(3) -0.010(3) -0.014(3) C45 0.056(7) 0.059(7) 0.044(6) 0.0000 0.0000 -0.002(6) O46 0.039(4) 0.095(7) 0.096(8) 0.0000 0.0000 0.039(5) C47 0.053(6) 0.032(5) 0.068(8) 0.0000 0.0000 0.000(5) O48 0.086(7) 0.049(5) 0.077(7) 0.0000 0.0000 0.024(5) C49 0.030(3) 0.030(3) 0.046(4) 0.008(3) 0.007(3) -0.003(2) O50 0.055(3) 0.057(3) 0.044(3) 0.013(2) 0.016(2) -0.002(3) C51 0.071(9) 0.051(7) 0.077(9) 0.0000 0.0000 -0.034(6) O52 0.093(8) 0.075(7) 0.137(11) 0.0000 0.0000 -0.056(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.929(2) 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 W1 . C21 6_556 2.039(6) yes W1 . Ga2 . 2.5921(10) yes W1 . C19 . 2.019(11) yes W1 . C21 . 2.039(6) yes W1 . C23 . 2.038(11) yes W1 . C25 . 2.012(11) yes Ga2 . N3 6_556 1.953(5) yes Ga2 . N3 . 1.953(5) yes N3 . C4 . 1.438(7) yes N3 . C16 . 1.353(7) yes C4 . C5 . 1.412(9) yes C4 . C9 . 1.397(8) yes C5 . C6 . 1.410(10) yes C5 . C13 . 1.525(6) yes C6 . C7 . 1.370(12) yes C6 . H61 . 0.931 no C7 . C8 . 1.335(12) yes C7 . H71 . 0.924 no C8 . C9 . 1.392(9) yes C8 . H81 . 0.936 no C9 . C10 . 1.523(6) yes C10 . C11 . 1.511(6) yes C10 . C12 . 1.524(6) yes C10 . H101 . 0.978 no C11 . H111 . 0.958 no C11 . H112 . 0.964 no C11 . H113 . 0.960 no C12 . H122 . 0.962 no C12 . H123 . 0.965 no C12 . H121 . 0.968 no C13 . C14 . 1.517(6) yes C13 . C15 . 1.509(6) yes C13 . H131 . 0.977 no C14 . H143 . 0.964 no C14 . H141 . 0.968 no C14 . H142 . 0.964 no C15 . H151 . 0.966 no C15 . H152 . 0.966 no C15 . H153 . 0.965 no C16 . C17 . 1.380(7) yes C16 . C18 . 1.506(8) yes C17 . H171 . 0.930 no C18 . H182 . 0.957 no C18 . H181 . 0.953 no C18 . H183 . 0.949 no C19 . O20 . 1.118(13) yes C21 . O22 . 1.135(8) yes C23 . O24 . 1.134(13) yes C25 . O26 . 1.127(13) yes W27 . C49 6_556 2.040(8) yes W27 . Ga28 . 2.5917(10) yes W27 . C45 . 2.084(13) yes W27 . C47 . 2.056(11) yes W27 . C49 . 2.040(8) yes W27 . C51 . 1.985(11) yes Ga28 . N29 6_556 1.953(5) yes Ga28 . N29 . 1.953(5) yes N29 . C30 . 1.437(7) yes N29 . C42 . 1.340(7) yes C30 . C31 . 1.399(8) yes C30 . C35 . 1.409(9) yes C31 . C32 . 1.391(9) yes C31 . C39 . 1.520(6) yes C32 . C33 . 1.368(12) yes C32 . H321 . 0.932 no C33 . C34 . 1.361(12) yes C33 . H331 . 0.931 no C34 . C35 . 1.386(10) yes C34 . H341 . 0.937 no C35 . C36 . 1.520(6) yes C36 . C37 . 1.512(6) yes C36 . C38 . 1.517(6) yes C36 . H361 . 0.980 no C37 . H371 . 0.961 no C37 . H372 . 0.962 no C37 . H373 . 0.962 no C38 . H382 . 0.966 no C38 . H383 . 0.962 no C38 . H381 . 0.967 no C39 . C40 . 1.524(6) yes C39 . C41 . 1.515(6) yes C39 . H391 . 0.980 no C40 . H403 . 0.962 no C40 . H401 . 0.964 no C40 . H402 . 0.964 no C41 . H411 . 0.961 no C41 . H412 . 0.963 no C41 . H413 . 0.958 no C42 . C43 . 1.397(7) yes C42 . C44 . 1.504(8) yes C43 . H431 . 0.931 no C44 . H442 . 0.957 no C44 . H441 . 0.958 no C44 . H443 . 0.956 no C45 . O46 . 1.068(14) yes C47 . O48 . 1.115(13) yes C49 . O50 . 1.142(9) yes C51 . O52 . 1.146(14) yes 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 C21 6_556 W1 . Ga2 . 89.56(16) yes C21 6_556 W1 . C19 . 90.49(16) yes Ga2 . W1 . C19 . 178.2(3) yes C21 6_556 W1 . C21 . 176.7(4) yes Ga2 . W1 . C21 . 89.56(16) yes C19 . W1 . C21 . 90.49(16) yes C21 6_556 W1 . C23 . 91.58(18) yes Ga2 . W1 . C23 . 89.5(4) yes C19 . W1 . C23 . 88.7(5) yes C21 . W1 . C23 . 91.58(18) yes C21 6_556 W1 . C25 . 88.46(18) yes Ga2 . W1 . C25 . 94.9(3) yes C19 . W1 . C25 . 86.9(5) yes C21 . W1 . C25 . 88.46(18) yes C23 . W1 . C25 . 175.6(5) yes N3 6_556 Ga2 . W1 . 133.27(13) yes N3 6_556 Ga2 . N3 . 93.5(3) yes W1 . Ga2 . N3 . 133.27(13) yes Ga2 . N3 . C4 . 116.3(3) yes Ga2 . N3 . C16 . 125.7(4) yes C4 . N3 . C16 . 117.9(5) yes N3 . C4 . C5 . 118.5(5) yes N3 . C4 . C9 . 119.8(5) yes C5 . C4 . C9 . 121.7(6) yes C4 . C5 . C6 . 116.5(6) yes C4 . C5 . C13 . 122.8(6) yes C6 . C5 . C13 . 120.7(6) yes C5 . C6 . C7 . 121.3(7) yes C5 . C6 . H61 . 119.4 no C7 . C6 . H61 . 119.3 no C6 . C7 . C8 . 120.6(7) yes C6 . C7 . H71 . 119.7 no C8 . C7 . H71 . 119.6 no C7 . C8 . C9 . 122.3(7) yes C7 . C8 . H81 . 118.8 no C9 . C8 . H81 . 118.9 no C4 . C9 . C8 . 117.5(6) yes C4 . C9 . C10 . 121.6(5) yes C8 . C9 . C10 . 120.8(6) yes C9 . C10 . C11 . 111.84(7) yes C9 . C10 . C12 . 111.86(7) yes C11 . C10 . C12 . 109.44(7) yes C9 . C10 . H101 . 107.6 no C11 . C10 . H101 . 108.5 no C12 . C10 . H101 . 107.4 no C10 . C11 . H111 . 109.1 no C10 . C11 . H112 . 108.7 no H111 . C11 . H112 . 109.9 no C10 . C11 . H113 . 108.7 no H111 . C11 . H113 . 109.6 no H112 . C11 . H113 . 110.8 no C10 . C12 . H122 . 109.0 no C10 . C12 . H123 . 108.5 no H122 . C12 . H123 . 109.6 no C10 . C12 . H121 . 109.8 no H122 . C12 . H121 . 110.2 no H123 . C12 . H121 . 109.6 no C5 . C13 . C14 . 111.85(7) yes C5 . C13 . C15 . 111.83(7) yes C14 . C13 . C15 . 109.43(7) yes C5 . C13 . H131 . 107.8 no C14 . C13 . H131 . 108.7 no C15 . C13 . H131 . 107.1 no C13 . C14 . H143 . 109.2 no C13 . C14 . H141 . 110.1 no H143 . C14 . H141 . 109.3 no C13 . C14 . H142 . 110.0 no H143 . C14 . H142 . 108.9 no H141 . C14 . H142 . 109.3 no C13 . C15 . H151 . 108.6 no C13 . C15 . H152 . 108.1 no H151 . C15 . H152 . 110.6 no C13 . C15 . H153 . 108.5 no H151 . C15 . H153 . 110.6 no H152 . C15 . H153 . 110.3 no N3 . C16 . C17 . 123.3(5) yes N3 . C16 . C18 . 118.8(5) yes C17 . C16 . C18 . 117.9(5) yes C16 . C17 . C16 6_556 128.5(7) yes C16 . C17 . H171 . 115.8 no C16 6_556 C17 . H171 . 115.8 no C16 . C18 . H182 . 109.7 no C16 . C18 . H181 . 109.1 no H182 . C18 . H181 . 109.7 no C16 . C18 . H183 . 109.8 no H182 . C18 . H183 . 109.1 no H181 . C18 . H183 . 109.5 no W1 . C19 . O20 . 176.3(11) yes W1 . C21 . O22 . 176.2(6) yes W1 . C23 . O24 . 169.4(12) yes W1 . C25 . O26 . 175.7(10) yes C49 6_556 W27 . Ga28 . 89.94(17) yes C49 6_556 W27 . C45 . 90.47(17) yes Ga28 . W27 . C45 . 92.5(3) yes C49 6_556 W27 . C47 . 89.54(17) yes Ga28 . W27 . C47 . 92.7(3) yes C45 . W27 . C47 . 174.8(5) yes C49 6_556 W27 . C49 . 179.1(3) yes Ga28 . W27 . C49 . 89.94(17) yes C45 . W27 . C49 . 90.47(17) yes C47 . W27 . C49 . 89.54(17) yes C49 6_556 W27 . C51 . 90.06(17) yes Ga28 . W27 . C51 . 179.5(5) yes C45 . W27 . C51 . 88.0(6) yes C47 . W27 . C51 . 86.8(6) yes C49 . W27 . C51 . 90.06(17) yes N29 6_556 Ga28 . W27 . 133.27(13) yes N29 6_556 Ga28 . N29 . 93.5(3) yes W27 . Ga28 . N29 . 133.27(13) yes Ga28 . N29 . C30 . 116.5(3) yes Ga28 . N29 . C42 . 126.0(4) yes C30 . N29 . C42 . 117.5(5) yes N29 . C30 . C31 . 120.3(5) yes N29 . C30 . C35 . 118.4(5) yes C31 . C30 . C35 . 121.3(6) yes C30 . C31 . C32 . 118.1(6) yes C30 . C31 . C39 . 121.8(5) yes C32 . C31 . C39 . 120.1(5) yes C31 . C32 . C33 . 120.7(7) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 119.8 no C32 . C33 . C34 . 120.8(7) yes C32 . C33 . H331 . 119.1 no C34 . C33 . H331 . 120.1 no C33 . C34 . C35 . 121.5(7) yes C33 . C34 . H341 . 119.2 no C35 . C34 . H341 . 119.2 no C30 . C35 . C34 . 117.5(6) yes C30 . C35 . C36 . 121.8(5) yes C34 . C35 . C36 . 120.7(6) yes C35 . C36 . C37 . 111.84(7) yes C35 . C36 . C38 . 111.84(7) yes C37 . C36 . C38 . 109.45(7) yes C35 . C36 . H361 . 108.2 no C37 . C36 . H361 . 107.9 no C38 . C36 . H361 . 107.4 no C36 . C37 . H371 . 108.8 no C36 . C37 . H372 . 109.3 no H371 . C37 . H372 . 110.1 no C36 . C37 . H373 . 109.2 no H371 . C37 . H373 . 109.6 no H372 . C37 . H373 . 109.8 no C36 . C38 . H382 . 109.0 no C36 . C38 . H383 . 108.5 no H382 . C38 . H383 . 109.5 no C36 . C38 . H381 . 109.3 no H382 . C38 . H381 . 110.5 no H383 . C38 . H381 . 109.9 no C31 . C39 . C40 . 111.85(7) yes C31 . C39 . C41 . 111.83(7) yes C40 . C39 . C41 . 109.45(7) yes C31 . C39 . H391 . 108.0 no C40 . C39 . H391 . 107.6 no C41 . C39 . H391 . 108.0 no C39 . C40 . H403 . 109.1 no C39 . C40 . H401 . 109.6 no H403 . C40 . H401 . 109.6 no C39 . C40 . H402 . 110.0 no H403 . C40 . H402 . 109.4 no H401 . C40 . H402 . 109.2 no C39 . C41 . H411 . 109.5 no C39 . C41 . H412 . 108.9 no H411 . C41 . H412 . 109.5 no C39 . C41 . H413 . 108.9 no H411 . C41 . H413 . 110.1 no H412 . C41 . H413 . 109.9 no N29 . C42 . C43 . 123.7(5) yes N29 . C42 . C44 . 120.3(5) yes C43 . C42 . C44 . 116.1(5) yes C42 . C43 . C42 6_556 127.3(7) yes C42 . C43 . H431 . 116.4 no C42 6_556 C43 . H431 . 116.4 no C42 . C44 . H442 . 110.9 no C42 . C44 . H441 . 109.7 no H442 . C44 . H441 . 108.9 no C42 . C44 . H443 . 109.5 no H442 . C44 . H443 . 108.7 no H441 . C44 . H443 . 109.0 no W27 . C45 . O46 . 176.7(12) yes W27 . C47 . O48 . 174.9(11) yes W27 . C49 . O50 . 176.4(6) yes W27 . C51 . O52 . 177.6(14) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C43 . H431 . O26 4_546 175.6(3) 0.931 2.471 3.400(10) yes _iucr_refine_instructions_details_constraints ; # # Punched on 12/03/13 at 18:02:06 # #LIST 12 BLOCK SCALE X'S, U'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 ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 122,X'S) H ( 123,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 143,X'S) H ( 141,X'S) H ( 142,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 182,X'S) H ( 181,X'S) H ( 183,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S) H ( 373,X'S) RIDE C ( 38,X'S) H ( 382,X'S) H ( 383,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 403,X'S) H ( 401,X'S) H ( 402,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 442,X'S) H ( 441,X'S) H ( 443,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 12/03/13 at 18:02:06 # #LIST 16 SAME C(5) C(13) C(14) C(15) AND CONT C(5) C(13) C(15) C(14) AND CONT C(9) C(10) C(11) C(12) AND CONT C(9) C(10) C(12) C(11) AND CONT C(31) C(39) C(40) C(41) AND CONT C(31) C(39) C(41) C(40) AND CONT C(35) C(36) C(37) C(38) AND CONT C(35) C(36) C(38) C(37) SIMU 0.01 C(5) C(13) C(14) C(15) AND CONT C(5) C(13) C(15) C(14) AND CONT C(9) C(10) C(11) C(12) AND CONT C(9) C(10) C(12) C(11) AND CONT C(31) C(39) C(40) C(41) AND CONT C(31) C(39) C(41) C(40) AND CONT C(35) C(36) C(37) C(38) AND CONT C(35) C(36) C(38) C(37) DELU 0.01 C(5) C(13) C(14) C(15) AND CONT C(5) C(13) C(15) C(14) AND CONT C(9) C(10) C(11) C(12) AND CONT C(9) C(10) C(12) C(11) AND CONT C(31) C(39) C(40) C(41) AND CONT C(31) C(39) C(41) C(40) AND CONT C(35) C(36) C(37) C(38) AND CONT C(35) C(36) C(38) C(37) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # start Validation Reply Form _vrf_PLAT220_1 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.7 Ratio RESPONSE: This arises from a carbon atom in the aromatic ring of the Dipp ligand. The metrics of these atoms are not discussed in the paper. ; _vrf_PLAT234_1 ; PROBLEM: Large Hirshfeld Difference W27 -- C45 .. 0.17 Ang RESPONSE: The Hirshfeld test assumes that the components of the anisotropic displacement parameters along chemical bonds are equal in magnitude. While the original test was defined in absolute terms (see H. L. Hirshfeld, Acta. Cryst. (1976). A32. 239-244), the current implementation is with reference to the associated standard uncertainty. Thus, where the standard uncertainty is small (eg. for the heavy atoms) small deviations from the Hirshfeld condition occasionally give rise to CHECKCIF alerts. The atoms have been checked to confirm ther agree with all other data available regarding type assignmetn. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 944061' ####################################################################### # # 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 _cell_length_a 8.8239(2) _cell_length_b 19.5134(4) _cell_length_c 21.4040(4) _cell_angle_alpha 90.0148(16) _cell_angle_beta 89.9906(18) _cell_angle_gamma 90.0029(19) _cell_volume 3685.43(14) _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 0.0181 0.0091 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 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co -2.3653 3.6143 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' Ga -1.2846 0.7763 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C41.25 H41.25 Co1.25 Ga1.25 N2.50 O3.75 # Dc = 1.43 Fooo = 1648.00 Mu = 58.12 M = 1585.72 # Found Formula = C36 H41 Co2 Ga1 N2 O7 # Dc = 1.44 FOOO = 1648.00 Mu = 82.19 M = 1602.63 _chemical_formula_sum 'C36 H41 Co2 Ga1 N2 O7' _chemical_formula_moiety 'C36 H41 Co2 Ga1 N2 O7' _chemical_compound_source . _chemical_formula_weight 801.32 _cell_measurement_reflns_used 23826 _cell_measurement_theta_min 3 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 8.219 # Sheldrick geometric approximatio 0.44 0.44 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.44 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _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 150 _diffrn_reflns_number 39477 _reflns_number_total 15179 _diffrn_reflns_av_R_equivalents 0.024 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 15179 # Theoretical number of reflections is about 30819 _diffrn_reflns_theta_min 3.065 _diffrn_reflns_theta_max 76.098 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 73.815 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -24 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 1.41 _oxford_diffrn_Wilson_scale 0.12 _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 0.38 # 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>-3.0\s(I) _refine_ls_number_reflns 15117 _refine_ls_number_restraints 0 _refine_ls_number_parameters 865 _oxford_refine_ls_R_factor_ref 0.0339 _refine_ls_wR_factor_ref 0.0744 _refine_ls_goodness_of_fit_ref 0.9226 _refine_ls_shift/su_max 0.0013116 _refine_ls_shift/su_mean 0.0001126 # The values computed with all filters except I/sigma _oxford_reflns_number_all 15120 _refine_ls_R_factor_all 0.0340 _refine_ls_wR_factor_all 0.0745 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 13685 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_gt 0.0648 # 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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.127E+04 0.197E+04 0.107E+04 295. ; # 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 Ga1 Ga 0.19144(3) 0.749991(13) 0.120632(12) 0.0115 1.0000 Uani . . . . . . Co2 Co 0.38164(4) 0.749995(19) 0.191340(17) 0.0152 1.0000 Uani . . . . . . Co3 Co 0.60226(4) 0.75001(2) 0.277991(18) 0.0212 1.0000 Uani . . . . . . C4 C 0.5129(3) 0.82973(17) 0.29558(15) 0.0385 1.0000 Uani . . . . . . O5 O 0.4626(3) 0.88176(15) 0.30817(16) 0.0718 1.0000 Uani . . . . . . C6 C 0.7257(3) 0.74986(12) 0.21179(11) 0.0208 1.0000 Uani . . . . . . O7 O 0.8106(2) 0.74992(10) 0.17135(9) 0.0323 1.0000 Uani . . . . . . C8 C 0.7373(4) 0.7505(2) 0.33910(15) 0.0530 1.0000 Uani . . . . . . O9 O 0.8231(3) 0.7498(2) 0.37911(13) 0.0988 1.0000 Uani . . . . . . C10 C 0.5121(3) 0.67038(18) 0.29570(15) 0.0388 1.0000 Uani . . . . . . O11 O 0.4619(3) 0.61805(15) 0.30817(16) 0.0728 1.0000 Uani . . . . . . C12 C 0.4536(3) 0.82882(14) 0.16090(13) 0.0283 1.0000 Uani . . . . . . O13 O 0.5067(2) 0.87833(12) 0.14244(13) 0.0537 1.0000 Uani . . . . . . C14 C 0.4542(3) 0.67129(14) 0.16086(13) 0.0279 1.0000 Uani . . . . . . O15 O 0.5062(2) 0.62160(12) 0.14264(13) 0.0531 1.0000 Uani . . . . . . C16 C 0.2408(3) 0.75006(14) 0.25084(12) 0.0244 1.0000 Uani . . . . . . O17 O 0.1521(2) 0.75009(12) 0.28979(10) 0.0390 1.0000 Uani . . . . . . N18 N 0.08405(19) 0.67629(9) 0.08083(8) 0.0123 1.0000 Uani . . . . . . C20 C 0.1467(2) 0.60804(11) 0.08923(10) 0.0132 1.0000 Uani . . . . . . C21 C 0.1209(2) 0.57311(11) 0.14557(10) 0.0153 1.0000 Uani . . . . . . C22 C 0.0177(3) 0.60167(12) 0.19632(10) 0.0179 1.0000 Uani . . . . . . C23 C 0.0710(3) 0.58386(16) 0.26233(12) 0.0322 1.0000 Uani . . . . . . C24 C -0.1454(3) 0.57670(15) 0.18670(13) 0.0287 1.0000 Uani . . . . . . C25 C 0.1893(3) 0.50950(12) 0.15339(12) 0.0225 1.0000 Uani . . . . . . C26 C 0.2796(3) 0.48113(12) 0.10711(12) 0.0242 1.0000 Uani . . . . . . C27 C 0.3027(3) 0.51644(12) 0.05189(11) 0.0215 1.0000 Uani . . . . . . C28 C 0.2383(2) 0.58056(12) 0.04187(10) 0.0160 1.0000 Uani . . . . . . C29 C 0.2722(3) 0.61883(14) -0.01855(11) 0.0246 1.0000 Uani . . . . . . C30 C 0.4308(4) 0.65177(17) -0.01497(15) 0.0399 1.0000 Uani . . . . . . C31 C 0.2623(4) 0.57220(18) -0.07595(13) 0.0425 1.0000 Uani . . . . . . C32 C -0.0356(2) 0.68572(11) 0.04346(10) 0.0139 1.0000 Uani . . . . . . C33 C -0.1137(3) 0.62423(12) 0.01471(12) 0.0225 1.0000 Uani . . . . . . C34 C -0.0929(2) 0.74998(12) 0.02793(10) 0.0168 1.0000 Uani . . . . . . C35 C -0.0361(2) 0.81421(11) 0.04354(10) 0.0148 1.0000 Uani . . . . . . N36 N 0.08402(19) 0.82386(9) 0.08080(8) 0.0122 1.0000 Uani . . . . . . C37 C 0.1469(2) 0.89203(11) 0.08913(10) 0.0132 1.0000 Uani . . . . . . C38 C 0.2378(2) 0.91933(11) 0.04181(10) 0.0165 1.0000 Uani . . . . . . C39 C 0.2725(3) 0.88127(14) -0.01854(11) 0.0246 1.0000 Uani . . . . . . C40 C 0.4296(3) 0.84842(16) -0.01505(15) 0.0379 1.0000 Uani . . . . . . C41 C 0.2624(4) 0.92781(18) -0.07602(13) 0.0417 1.0000 Uani . . . . . . C42 C 0.3032(3) 0.98364(12) 0.05196(12) 0.0214 1.0000 Uani . . . . . . C43 C 0.2795(3) 1.01878(13) 0.10719(13) 0.0256 1.0000 Uani . . . . . . C44 C 0.1896(3) 0.99072(12) 0.15325(11) 0.0219 1.0000 Uani . . . . . . C45 C 0.1210(2) 0.92666(11) 0.14558(10) 0.0158 1.0000 Uani . . . . . . C46 C 0.0175(3) 0.89835(12) 0.19628(10) 0.0179 1.0000 Uani . . . . . . C47 C 0.0707(3) 0.91622(16) 0.26243(12) 0.0310 1.0000 Uani . . . . . . C48 C -0.1454(3) 0.92316(15) 0.18664(13) 0.0290 1.0000 Uani . . . . . . C49 C -0.1130(3) 0.87562(12) 0.01491(12) 0.0229 1.0000 Uani . . . . . . Ga50 Ga 0.69143(3) 0.250017(13) 0.379391(12) 0.0116 1.0000 Uani . . . . . . Co51 Co 0.88158(4) 0.250023(19) 0.308678(17) 0.0153 1.0000 Uani . . . . . . Co52 Co 1.10228(4) 0.25003(2) 0.222036(18) 0.0214 1.0000 Uani . . . . . . C53 C 1.2259(3) 0.24981(12) 0.28812(11) 0.0207 1.0000 Uani . . . . . . O54 O 1.3105(2) 0.25002(10) 0.32859(9) 0.0326 1.0000 Uani . . . . . . C55 C 1.2386(4) 0.2498(3) 0.16110(15) 0.0542 1.0000 Uani . . . . . . O56 O 1.3230(3) 0.2499(2) 0.12093(13) 0.0979 1.0000 Uani . . . . . . C57 C 1.0130(3) 0.32990(18) 0.20452(16) 0.0404 1.0000 Uani . . . . . . O58 O 0.9622(3) 0.38216(15) 0.19243(16) 0.0711 1.0000 Uani . . . . . . C59 C 1.0123(3) 0.17018(18) 0.20457(16) 0.0419 1.0000 Uani . . . . . . O60 O 0.9621(3) 0.11798(15) 0.19214(16) 0.0720 1.0000 Uani . . . . . . C61 C 0.7411(3) 0.24974(14) 0.24908(12) 0.0243 1.0000 Uani . . . . . . O62 O 0.6515(2) 0.25017(12) 0.21016(10) 0.0387 1.0000 Uani . . . . . . C63 C 0.9537(3) 0.32864(15) 0.33914(13) 0.0295 1.0000 Uani . . . . . . O64 O 1.0065(2) 0.37847(12) 0.35742(13) 0.0527 1.0000 Uani . . . . . . C65 C 0.9538(3) 0.17125(14) 0.33904(13) 0.0290 1.0000 Uani . . . . . . O66 O 1.0065(2) 0.12158(12) 0.35739(13) 0.0549 1.0000 Uani . . . . . . N67 N 0.58379(19) 0.17615(9) 0.41895(8) 0.0122 1.0000 Uani . . . . . . C68 C 0.6465(2) 0.10814(11) 0.41067(10) 0.0126 1.0000 Uani . . . . . . C69 C 0.6208(2) 0.07310(11) 0.35421(10) 0.0159 1.0000 Uani . . . . . . C70 C 0.5176(3) 0.10161(12) 0.30382(11) 0.0182 1.0000 Uani . . . . . . C71 C 0.5709(3) 0.08391(16) 0.23780(12) 0.0317 1.0000 Uani . . . . . . C72 C 0.3552(3) 0.07692(15) 0.31319(13) 0.0294 1.0000 Uani . . . . . . C73 C 0.6895(3) 0.00942(12) 0.34653(11) 0.0221 1.0000 Uani . . . . . . C74 C 0.7795(3) -0.01892(13) 0.39298(12) 0.0251 1.0000 Uani . . . . . . C75 C 0.8027(3) 0.01639(12) 0.44800(12) 0.0215 1.0000 Uani . . . . . . C76 C 0.7378(2) 0.08067(12) 0.45809(10) 0.0166 1.0000 Uani . . . . . . C77 C 0.7728(3) 0.11881(13) 0.51847(11) 0.0241 1.0000 Uani . . . . . . C78 C 0.9301(4) 0.15182(16) 0.51512(15) 0.0391 1.0000 Uani . . . . . . C79 C 0.7623(4) 0.07225(18) 0.57602(13) 0.0412 1.0000 Uani . . . . . . C80 C 0.4642(2) 0.18553(11) 0.45644(10) 0.0145 1.0000 Uani . . . . . . C81 C 0.3867(3) 0.12436(12) 0.48524(12) 0.0224 1.0000 Uani . . . . . . C82 C 0.4071(2) 0.24986(12) 0.47205(10) 0.0158 1.0000 Uani . . . . . . C83 C 0.4639(2) 0.31422(11) 0.45643(10) 0.0139 1.0000 Uani . . . . . . N84 N 0.58407(19) 0.32356(9) 0.41891(8) 0.0113 1.0000 Uani . . . . . . C85 C 0.6465(2) 0.39187(11) 0.41078(10) 0.0129 1.0000 Uani . . . . . . C86 C 0.6203(2) 0.42672(11) 0.35421(10) 0.0159 1.0000 Uani . . . . . . C87 C 0.5175(3) 0.39861(12) 0.30403(10) 0.0180 1.0000 Uani . . . . . . C88 C 0.5709(3) 0.41617(16) 0.23771(12) 0.0310 1.0000 Uani . . . . . . C89 C 0.3544(3) 0.42325(15) 0.31332(13) 0.0292 1.0000 Uani . . . . . . C90 C 0.6893(3) 0.49073(12) 0.34671(11) 0.0224 1.0000 Uani . . . . . . C91 C 0.7795(3) 0.51887(13) 0.39299(12) 0.0252 1.0000 Uani . . . . . . C92 C 0.8031(3) 0.48354(12) 0.44794(12) 0.0208 1.0000 Uani . . . . . . C93 C 0.7380(2) 0.41934(12) 0.45813(10) 0.0162 1.0000 Uani . . . . . . C94 C 0.7728(3) 0.38128(14) 0.51840(11) 0.0253 1.0000 Uani . . . . . . C95 C 0.9302(4) 0.34864(16) 0.51492(15) 0.0388 1.0000 Uani . . . . . . C96 C 0.7630(4) 0.42760(18) 0.57601(13) 0.0409 1.0000 Uani . . . . . . C97 C 0.3864(3) 0.37553(12) 0.48522(12) 0.0227 1.0000 Uani . . . . . . H221 H 0.0176 0.6532 0.1929 0.0218 1.0000 Uiso R . . . . . H233 H 0.0133 0.6109 0.2922 0.0480 1.0000 Uiso R . . . . . H231 H 0.1780 0.5945 0.2659 0.0481 1.0000 Uiso R . . . . . H232 H 0.0545 0.5353 0.2698 0.0479 1.0000 Uiso R . . . . . H241 H -0.2096 0.5953 0.2194 0.0451 1.0000 Uiso R . . . . . H242 H -0.1837 0.5924 0.1465 0.0449 1.0000 Uiso R . . . . . H243 H -0.1458 0.5273 0.1883 0.0448 1.0000 Uiso R . . . . . H251 H 0.1738 0.4854 0.1908 0.0273 1.0000 Uiso R . . . . . H261 H 0.3242 0.4381 0.1126 0.0290 1.0000 Uiso R . . . . . H271 H 0.3651 0.4967 0.0205 0.0266 1.0000 Uiso R . . . . . H291 H 0.1972 0.6563 -0.0229 0.0305 1.0000 Uiso R . . . . . H303 H 0.4492 0.6774 -0.0532 0.0610 1.0000 Uiso R . . . . . H301 H 0.4366 0.6836 0.0202 0.0607 1.0000 Uiso R . . . . . H302 H 0.5082 0.6171 -0.0096 0.0609 1.0000 Uiso R . . . . . H311 H 0.2768 0.5998 -0.1122 0.0649 1.0000 Uiso R . . . . . H312 H 0.1624 0.5511 -0.0774 0.0652 1.0000 Uiso R . . . . . H313 H 0.3407 0.5376 -0.0745 0.0649 1.0000 Uiso R . . . . . H332 H -0.2195 0.6338 0.0082 0.0369 1.0000 Uiso R . . . . . H333 H -0.1030 0.5842 0.0400 0.0368 1.0000 Uiso R . . . . . H331 H -0.0687 0.6140 -0.0256 0.0378 1.0000 Uiso R . . . . . H341 H -0.1792 0.7502 0.0033 0.0216 1.0000 Uiso R . . . . . H391 H 0.1975 0.8438 -0.0225 0.0298 1.0000 Uiso R . . . . . H402 H 0.4487 0.8223 -0.0531 0.0581 1.0000 Uiso R . . . . . H403 H 0.5078 0.8827 -0.0094 0.0583 1.0000 Uiso R . . . . . H401 H 0.4352 0.8168 0.0199 0.0578 1.0000 Uiso R . . . . . H411 H 0.2746 0.8999 -0.1123 0.0649 1.0000 Uiso R . . . . . H413 H 0.3428 0.9617 -0.0750 0.0649 1.0000 Uiso R . . . . . H412 H 0.1642 0.9502 -0.0771 0.0650 1.0000 Uiso R . . . . . H421 H 0.3655 1.0034 0.0206 0.0267 1.0000 Uiso R . . . . . H431 H 0.3237 1.0619 0.1131 0.0303 1.0000 Uiso R . . . . . H441 H 0.1735 1.0150 0.1907 0.0270 1.0000 Uiso R . . . . . H461 H 0.0197 0.8470 0.1923 0.0217 1.0000 Uiso R . . . . . H472 H 0.0091 0.8904 0.2919 0.0480 1.0000 Uiso R . . . . . H473 H 0.0581 0.9653 0.2696 0.0479 1.0000 Uiso R . . . . . H471 H 0.1756 0.9028 0.2660 0.0480 1.0000 Uiso R . . . . . H481 H -0.2110 0.9049 0.2191 0.0462 1.0000 Uiso R . . . . . H483 H -0.1472 0.9729 0.1886 0.0457 1.0000 Uiso R . . . . . H482 H -0.1832 0.9080 0.1463 0.0458 1.0000 Uiso R . . . . . H492 H -0.1043 0.9159 0.0400 0.0378 1.0000 Uiso R . . . . . H491 H -0.2191 0.8660 0.0079 0.0374 1.0000 Uiso R . . . . . H493 H -0.0680 0.8853 -0.0251 0.0387 1.0000 Uiso R . . . . . H701 H 0.5186 0.1532 0.3076 0.0221 1.0000 Uiso R . . . . . H713 H 0.5107 0.1102 0.2083 0.0489 1.0000 Uiso R . . . . . H711 H 0.6771 0.0967 0.2338 0.0490 1.0000 Uiso R . . . . . H712 H 0.5575 0.0350 0.2299 0.0489 1.0000 Uiso R . . . . . H721 H 0.2909 0.0952 0.2803 0.0460 1.0000 Uiso R . . . . . H722 H 0.3161 0.0926 0.3533 0.0457 1.0000 Uiso R . . . . . H723 H 0.3540 0.0271 0.3112 0.0457 1.0000 Uiso R . . . . . H731 H 0.6742 -0.0149 0.3091 0.0269 1.0000 Uiso R . . . . . H741 H 0.8240 -0.0620 0.3873 0.0301 1.0000 Uiso R . . . . . H751 H 0.8651 -0.0035 0.4794 0.0258 1.0000 Uiso R . . . . . H771 H 0.6983 0.1564 0.5224 0.0300 1.0000 Uiso R . . . . . H783 H 0.9489 0.1774 0.5532 0.0601 1.0000 Uiso R . . . . . H781 H 1.0076 0.1175 0.5096 0.0601 1.0000 Uiso R . . . . . H782 H 0.9350 0.1835 0.4802 0.0597 1.0000 Uiso R . . . . . H791 H 0.7750 0.1002 0.6124 0.0640 1.0000 Uiso R . . . . . H792 H 0.8416 0.0378 0.5745 0.0638 1.0000 Uiso R . . . . . H793 H 0.6621 0.0508 0.5766 0.0642 1.0000 Uiso R . . . . . H812 H 0.2796 0.1337 0.4912 0.0367 1.0000 Uiso R . . . . . H813 H 0.4302 0.1158 0.5263 0.0379 1.0000 Uiso R . . . . . H811 H 0.3984 0.0834 0.4610 0.0368 1.0000 Uiso R . . . . . H821 H 0.3210 0.2499 0.4965 0.0204 1.0000 Uiso R . . . . . H871 H 0.5196 0.3471 0.3073 0.0222 1.0000 Uiso R . . . . . H882 H 0.5136 0.3891 0.2077 0.0481 1.0000 Uiso R . . . . . H883 H 0.5531 0.4650 0.2303 0.0481 1.0000 Uiso R . . . . . H881 H 0.6780 0.4055 0.2342 0.0482 1.0000 Uiso R . . . . . H891 H 0.2902 0.4045 0.2809 0.0449 1.0000 Uiso R . . . . . H893 H 0.3528 0.4727 0.3112 0.0448 1.0000 Uiso R . . . . . H892 H 0.3172 0.4089 0.3537 0.0451 1.0000 Uiso R . . . . . H901 H 0.6737 0.5148 0.3093 0.0274 1.0000 Uiso R . . . . . H911 H 0.8247 0.5620 0.3875 0.0302 1.0000 Uiso R . . . . . H921 H 0.8664 0.5033 0.4793 0.0256 1.0000 Uiso R . . . . . H941 H 0.6981 0.3437 0.5225 0.0309 1.0000 Uiso R . . . . . H952 H 0.9487 0.3224 0.5527 0.0592 1.0000 Uiso R . . . . . H953 H 1.0086 0.3828 0.5101 0.0591 1.0000 Uiso R . . . . . H951 H 0.9355 0.3170 0.4797 0.0587 1.0000 Uiso R . . . . . H961 H 0.7731 0.3992 0.6122 0.0630 1.0000 Uiso R . . . . . H963 H 0.8441 0.4607 0.5751 0.0630 1.0000 Uiso R . . . . . H962 H 0.6653 0.4503 0.5764 0.0631 1.0000 Uiso R . . . . . H972 H 0.3961 0.4166 0.4610 0.0377 1.0000 Uiso R . . . . . H971 H 0.4286 0.3844 0.5262 0.0387 1.0000 Uiso R . . . . . H973 H 0.2804 0.3661 0.4912 0.0375 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 Ga1 0.00987(12) 0.01234(12) 0.01229(12) 0.00093(9) -0.00417(9) -0.00035(9) Co2 0.01145(17) 0.01764(18) 0.01654(18) 0.00090(14) -0.00667(13) -0.00063(13) Co3 0.01222(17) 0.0382(2) 0.01321(18) 0.00054(16) -0.00367(13) -0.00059(16) C4 0.0191(13) 0.0525(19) 0.0438(17) -0.0250(15) -0.0040(11) -0.0064(12) O5 0.0341(13) 0.0654(18) 0.116(3) -0.0623(18) -0.0031(14) 0.0026(12) C6 0.0193(11) 0.0201(11) 0.0232(12) 0.0018(9) -0.0052(9) -0.0003(9) O7 0.0322(10) 0.0359(11) 0.0286(10) 0.0010(8) 0.0114(8) -0.0007(8) C8 0.0278(16) 0.109(3) 0.0222(15) -0.0009(17) -0.0040(12) -0.0013(17) O9 0.0457(16) 0.216(5) 0.0346(15) 0.004(2) -0.0289(13) -0.003(2) C10 0.0190(13) 0.055(2) 0.0426(17) 0.0267(15) -0.0027(11) 0.0003(12) O11 0.0369(13) 0.0654(18) 0.116(3) 0.0642(18) -0.0019(14) -0.0052(12) C12 0.0166(12) 0.0318(14) 0.0364(15) 0.0094(11) -0.0166(10) -0.0046(10) O13 0.0328(12) 0.0437(13) 0.0846(19) 0.0352(13) -0.0291(12) -0.0180(10) C14 0.0131(11) 0.0309(14) 0.0396(15) -0.0073(11) -0.0148(10) 0.0007(10) O15 0.0310(11) 0.0424(13) 0.0858(19) -0.0326(13) -0.0290(11) 0.0168(10) C16 0.0180(12) 0.0282(13) 0.0270(13) 0.0024(10) -0.0068(10) 0.0004(9) O17 0.0284(11) 0.0559(14) 0.0326(11) 0.0011(9) 0.0070(8) -0.0009(9) N18 0.0099(8) 0.0145(9) 0.0127(8) 0.0021(7) -0.0014(6) -0.0002(7) C20 0.0104(10) 0.0127(10) 0.0165(10) 0.0006(8) -0.0040(8) -0.0021(8) C21 0.0155(10) 0.0170(10) 0.0135(10) 0.0000(8) -0.0024(8) -0.0030(8) C22 0.0194(11) 0.0187(11) 0.0156(11) 0.0029(8) 0.0007(8) -0.0011(9) C23 0.0342(15) 0.0452(17) 0.0171(12) 0.0066(11) 0.0012(10) 0.0009(12) C24 0.0183(12) 0.0357(15) 0.0321(14) -0.0018(11) 0.0040(10) -0.0011(10) C25 0.0244(12) 0.0198(12) 0.0233(12) 0.0074(9) -0.0040(9) -0.0010(9) C26 0.0249(12) 0.0153(11) 0.0324(14) -0.0007(9) -0.0047(10) 0.0050(9) C27 0.0204(11) 0.0201(12) 0.0240(12) -0.0065(9) -0.0019(9) 0.0038(9) C28 0.0132(10) 0.0186(11) 0.0162(11) -0.0029(8) -0.0025(8) -0.0011(8) C29 0.0260(13) 0.0284(13) 0.0194(12) 0.0019(10) 0.0063(9) 0.0036(10) C30 0.0409(17) 0.0379(17) 0.0408(17) 0.0028(13) 0.0159(13) -0.0084(13) C31 0.056(2) 0.053(2) 0.0190(13) -0.0044(13) 0.0030(12) 0.0034(15) C32 0.0125(10) 0.0176(10) 0.0115(10) -0.0023(8) -0.0013(7) -0.0029(8) C33 0.0225(12) 0.0186(11) 0.0263(12) -0.0017(9) -0.0121(9) -0.0038(9) C34 0.0105(10) 0.0215(11) 0.0185(11) 0.0023(8) -0.0076(8) -0.0008(8) C35 0.0139(10) 0.0187(11) 0.0117(10) 0.0011(8) -0.0003(8) 0.0030(8) N36 0.0105(8) 0.0124(8) 0.0138(8) 0.0018(7) -0.0014(6) 0.0006(6) C37 0.0095(9) 0.0128(10) 0.0174(10) 0.0029(8) -0.0036(8) 0.0012(7) C38 0.0151(10) 0.0172(11) 0.0171(11) 0.0038(8) -0.0018(8) 0.0009(8) C39 0.0273(13) 0.0296(13) 0.0167(11) 0.0005(10) 0.0063(9) -0.0063(10) C40 0.0376(16) 0.0351(16) 0.0411(17) 0.0012(13) 0.0150(13) 0.0061(13) C41 0.055(2) 0.053(2) 0.0172(13) 0.0058(12) 0.0039(12) -0.0063(15) C42 0.0169(11) 0.0210(12) 0.0263(12) 0.0071(9) -0.0015(9) -0.0049(9) C43 0.0257(13) 0.0163(11) 0.0347(14) 0.0026(10) -0.0068(10) -0.0059(9) C44 0.0273(13) 0.0154(11) 0.0229(12) -0.0053(9) -0.0043(9) -0.0013(9) C45 0.0149(10) 0.0154(10) 0.0171(11) 0.0016(8) -0.0028(8) 0.0020(8) C46 0.0196(11) 0.0185(11) 0.0157(11) -0.0035(8) 0.0023(8) 0.0013(9) C47 0.0328(14) 0.0428(16) 0.0172(12) -0.0026(11) 0.0019(10) -0.0020(12) C48 0.0167(12) 0.0376(15) 0.0328(14) 0.0027(11) 0.0035(10) 0.0002(10) C49 0.0229(12) 0.0199(12) 0.0259(12) 0.0045(9) -0.0120(9) 0.0025(9) Ga50 0.00999(12) 0.01241(12) 0.01246(13) 0.00073(9) 0.00439(9) -0.00042(9) Co51 0.01168(17) 0.01789(18) 0.01620(18) 0.00080(14) 0.00692(13) -0.00040(13) Co52 0.01237(18) 0.0385(2) 0.01320(18) 0.00104(16) 0.00375(13) -0.00069(16) C53 0.0195(11) 0.0208(11) 0.0217(12) 0.0004(9) 0.0057(9) 0.0004(9) O54 0.0339(10) 0.0353(11) 0.0284(10) 0.0013(8) -0.0111(8) -0.0001(8) C55 0.0261(15) 0.113(3) 0.0232(15) -0.0022(17) 0.0058(12) 0.0017(17) O56 0.0473(16) 0.214(5) 0.0325(14) 0.000(2) 0.0290(12) -0.001(2) C57 0.0168(13) 0.055(2) 0.0495(18) 0.0307(15) 0.0032(12) -0.0039(12) O58 0.0342(13) 0.0658(18) 0.113(2) 0.0632(18) 0.0043(14) 0.0049(12) C59 0.0191(13) 0.058(2) 0.0482(18) -0.0295(16) 0.0042(12) 0.0020(13) O60 0.0379(14) 0.0660(18) 0.112(2) -0.0624(18) 0.0034(14) -0.0047(12) C61 0.0188(12) 0.0296(13) 0.0245(13) -0.0005(10) 0.0069(10) -0.0004(10) O62 0.0281(10) 0.0560(14) 0.0320(11) 0.0012(9) -0.0065(8) -0.0005(9) C63 0.0182(12) 0.0336(15) 0.0367(15) -0.0078(11) 0.0163(10) -0.0034(10) O64 0.0319(11) 0.0422(13) 0.0841(18) -0.0341(12) 0.0282(11) -0.0166(10) C65 0.0146(11) 0.0332(14) 0.0391(15) 0.0103(12) 0.0149(10) 0.0032(10) O66 0.0317(12) 0.0453(14) 0.0877(19) 0.0388(13) 0.0302(12) 0.0183(10) N67 0.0115(8) 0.0121(8) 0.0131(8) 0.0004(6) 0.0011(6) -0.0005(6) C68 0.0098(9) 0.0118(10) 0.0163(10) 0.0034(8) 0.0040(7) -0.0005(7) C69 0.0163(10) 0.0152(10) 0.0161(11) -0.0005(8) 0.0026(8) -0.0036(8) C70 0.0178(11) 0.0194(11) 0.0175(11) 0.0008(9) -0.0008(8) -0.0014(9) C71 0.0342(15) 0.0441(16) 0.0168(12) -0.0054(11) -0.0011(10) 0.0005(12) C72 0.0179(12) 0.0362(15) 0.0342(15) 0.0055(11) -0.0038(10) -0.0012(10) C73 0.0251(12) 0.0190(11) 0.0224(12) -0.0040(9) 0.0033(9) -0.0005(9) C74 0.0258(13) 0.0160(11) 0.0335(14) 0.0013(10) 0.0064(10) 0.0065(9) C75 0.0197(11) 0.0190(11) 0.0258(12) 0.0076(9) 0.0014(9) 0.0024(9) C76 0.0128(10) 0.0204(11) 0.0168(11) 0.0034(8) 0.0031(8) -0.0010(8) C77 0.0267(13) 0.0254(12) 0.0201(12) 0.0015(10) -0.0061(9) 0.0042(10) C78 0.0393(17) 0.0361(16) 0.0417(17) -0.0022(13) -0.0159(13) -0.0095(13) C79 0.0534(19) 0.0521(19) 0.0179(13) 0.0067(12) -0.0035(12) 0.0041(15) C80 0.0127(10) 0.0175(10) 0.0132(10) 0.0018(8) 0.0008(8) -0.0040(8) C81 0.0204(12) 0.0199(12) 0.0269(12) 0.0028(9) 0.0122(9) -0.0032(9) C82 0.0121(10) 0.0206(11) 0.0146(10) 0.0000(8) 0.0077(8) -0.0013(8) C83 0.0121(10) 0.0176(10) 0.0119(10) -0.0005(8) 0.0011(7) 0.0017(8) N84 0.0099(8) 0.0117(8) 0.0122(8) 0.0013(6) 0.0009(6) -0.0016(6) C85 0.0100(9) 0.0131(10) 0.0157(10) -0.0001(8) 0.0044(7) 0.0000(8) C86 0.0157(10) 0.0155(10) 0.0165(11) 0.0021(8) 0.0038(8) 0.0018(8) C87 0.0185(11) 0.0197(11) 0.0159(11) 0.0036(8) -0.0004(8) 0.0006(9) C88 0.0336(15) 0.0429(16) 0.0164(12) 0.0054(11) -0.0004(10) -0.0005(12) C89 0.0175(12) 0.0354(15) 0.0345(15) -0.0028(11) -0.0033(10) -0.0002(10) C90 0.0275(13) 0.0180(11) 0.0216(12) 0.0050(9) 0.0036(9) 0.0006(9) C91 0.0277(13) 0.0157(11) 0.0323(14) -0.0008(10) 0.0070(10) -0.0054(9) C92 0.0167(11) 0.0189(11) 0.0269(12) -0.0054(9) 0.0017(9) -0.0039(9) C93 0.0143(10) 0.0182(11) 0.0160(11) -0.0026(8) 0.0017(8) -0.0006(8) C94 0.0272(13) 0.0295(13) 0.0191(12) 0.0034(10) -0.0065(9) -0.0049(10) C95 0.0394(17) 0.0345(16) 0.0424(17) 0.0058(13) -0.0163(13) 0.0056(13) C96 0.0505(19) 0.054(2) 0.0182(13) -0.0037(12) -0.0031(12) -0.0070(15) C97 0.0218(12) 0.0199(11) 0.0263(12) -0.0022(9) 0.0121(9) 0.0030(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.921(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 Ga1 . Co2 . 2.2601(4) yes Ga1 . N18 . 1.9214(18) yes Ga1 . N36 . 1.9246(17) yes Co2 . Co3 . 2.6890(5) yes Co2 . C12 . 1.787(3) yes Co2 . C14 . 1.787(3) yes Co2 . C16 . 1.779(3) yes Co3 . C4 . 1.784(3) yes Co3 . C6 . 1.787(3) yes Co3 . C8 . 1.770(3) yes Co3 . C10 . 1.786(3) yes C4 . O5 . 1.140(4) yes C6 . O7 . 1.145(3) yes C8 . O9 . 1.143(4) yes C10 . O11 . 1.144(4) yes C12 . O13 . 1.144(3) yes C14 . O15 . 1.141(3) yes C16 . O17 . 1.143(3) yes N18 . C20 . 1.453(3) yes N18 . C32 . 1.337(3) yes C20 . C21 . 1.404(3) yes C20 . C28 . 1.403(3) yes C21 . C22 . 1.523(3) yes C21 . C25 . 1.391(3) yes C22 . C23 . 1.529(3) yes C22 . C24 . 1.534(3) yes C22 . H221 . 1.007 no C23 . H233 . 0.972 no C23 . H231 . 0.970 no C23 . H232 . 0.973 no C24 . H241 . 0.970 no C24 . H242 . 0.973 no C24 . H243 . 0.966 no C25 . C26 . 1.386(4) yes C25 . H251 . 0.940 no C26 . C27 . 1.383(4) yes C26 . H261 . 0.936 no C27 . C28 . 1.391(3) yes C27 . H271 . 0.949 no C28 . C29 . 1.523(3) yes C29 . C30 . 1.542(4) yes C29 . C31 . 1.531(4) yes C29 . H291 . 0.991 no C30 . H303 . 0.973 no C30 . H301 . 0.977 no C30 . H302 . 0.968 no C31 . H311 . 0.954 no C31 . H312 . 0.973 no C31 . H313 . 0.967 no C32 . C33 . 1.514(3) yes C32 . C34 . 1.392(3) yes C33 . H332 . 0.962 no C33 . H333 . 0.955 no C33 . H331 . 0.971 no C34 . C35 . 1.391(3) yes C34 . H341 . 0.926 no C35 . N36 . 1.340(3) yes C35 . C49 . 1.508(3) yes N36 . C37 . 1.452(3) yes C37 . C38 . 1.398(3) yes C37 . C45 . 1.403(3) yes C38 . C39 . 1.521(3) yes C38 . C42 . 1.398(3) yes C39 . C40 . 1.529(4) yes C39 . C41 . 1.532(4) yes C39 . H391 . 0.991 no C40 . H402 . 0.976 no C40 . H403 . 0.968 no C40 . H401 . 0.971 no C41 . H411 . 0.954 no C41 . H413 . 0.970 no C41 . H412 . 0.971 no C42 . C43 . 1.383(4) yes C42 . H421 . 0.949 no C43 . C44 . 1.378(4) yes C43 . H431 . 0.936 no C44 . C45 . 1.399(3) yes C44 . H441 . 0.941 no C45 . C46 . 1.522(3) yes C46 . C47 . 1.532(3) yes C46 . C48 . 1.531(3) yes C46 . H461 . 1.006 no C47 . H472 . 0.973 no C47 . H473 . 0.977 no C47 . H471 . 0.965 no C48 . H481 . 0.971 no C48 . H483 . 0.972 no C48 . H482 . 0.972 no C49 . H492 . 0.955 no C49 . H491 . 0.966 no C49 . H493 . 0.963 no Ga50 . Co51 . 2.2594(4) yes Ga50 . N67 . 1.9228(17) yes Ga50 . N84 . 1.9161(18) yes Co51 . Co52 . 2.6890(5) yes Co51 . C61 . 1.779(3) yes Co51 . C63 . 1.784(3) yes Co51 . C65 . 1.787(3) yes Co52 . C53 . 1.787(3) yes Co52 . C55 . 1.774(3) yes Co52 . C57 . 1.786(3) yes Co52 . C59 . 1.788(3) yes C53 . O54 . 1.144(3) yes C55 . O56 . 1.138(4) yes C57 . O58 . 1.144(4) yes C59 . O60 . 1.142(4) yes C61 . O62 . 1.149(3) yes C63 . O64 . 1.147(3) yes C65 . O66 . 1.145(3) yes N67 . C68 . 1.448(3) yes N67 . C80 . 1.338(3) yes C68 . C69 . 1.407(3) yes C68 . C76 . 1.403(3) yes C69 . C70 . 1.517(3) yes C69 . C73 . 1.392(3) yes C70 . C71 . 1.528(3) yes C70 . C72 . 1.525(3) yes C70 . H701 . 1.010 no C71 . H713 . 0.973 no C71 . H711 . 0.973 no C71 . H712 . 0.977 no C72 . H721 . 0.972 no C72 . H722 . 0.974 no C72 . H723 . 0.972 no C73 . C74 . 1.387(4) yes C73 . H731 . 0.941 no C74 . C75 . 1.380(4) yes C74 . H741 . 0.936 no C75 . C76 . 1.396(3) yes C75 . H751 . 0.952 no C76 . C77 . 1.523(3) yes C77 . C78 . 1.531(4) yes C77 . C79 . 1.534(4) yes C77 . H771 . 0.988 no C78 . H783 . 0.971 no C78 . H781 . 0.966 no C78 . H782 . 0.971 no C79 . H791 . 0.956 no C79 . H792 . 0.971 no C79 . H793 . 0.977 no C80 . C81 . 1.508(3) yes C80 . C82 . 1.393(3) yes C81 . H812 . 0.971 no C81 . H813 . 0.974 no C81 . H811 . 0.958 no C82 . C83 . 1.393(3) yes C82 . H821 . 0.923 no C83 . N84 . 1.343(3) yes C83 . C97 . 1.509(3) yes N84 . C85 . 1.453(3) yes C85 . C86 . 1.408(3) yes C85 . C93 . 1.402(3) yes C86 . C87 . 1.509(3) yes C86 . C90 . 1.399(3) yes C87 . C88 . 1.535(3) yes C87 . C89 . 1.529(3) yes C87 . H871 . 1.007 no C88 . H882 . 0.973 no C88 . H883 . 0.978 no C88 . H881 . 0.971 no C89 . H891 . 0.968 no C89 . H893 . 0.966 no C89 . H892 . 0.967 no C90 . C91 . 1.384(4) yes C90 . H901 . 0.939 no C91 . C92 . 1.379(4) yes C91 . H911 . 0.939 no C92 . C93 . 1.395(3) yes C92 . H921 . 0.955 no C93 . C94 . 1.520(3) yes C94 . C95 . 1.529(4) yes C94 . C96 . 1.531(4) yes C94 . H941 . 0.990 no C95 . H952 . 0.971 no C95 . H953 . 0.966 no C95 . H951 . 0.974 no C96 . H961 . 0.957 no C96 . H963 . 0.965 no C96 . H962 . 0.969 no C97 . H972 . 0.959 no C97 . H971 . 0.969 no C97 . H973 . 0.961 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 Co2 . Ga1 . N18 . 131.54(5) yes Co2 . Ga1 . N36 . 131.50(5) yes N18 . Ga1 . N36 . 96.96(7) yes Ga1 . Co2 . Co3 . 178.43(2) yes Ga1 . Co2 . C12 . 91.12(8) yes Co3 . Co2 . C12 . 89.68(8) yes Ga1 . Co2 . C14 . 91.25(8) yes Co3 . Co2 . C14 . 89.56(8) yes C12 . Co2 . C14 . 118.64(14) yes Ga1 . Co2 . C16 . 87.75(8) yes Co3 . Co2 . C16 . 90.68(8) yes C12 . Co2 . C16 . 120.57(13) yes C14 . Co2 . C16 . 120.80(13) yes Co2 . Co3 . C4 . 79.95(9) yes Co2 . Co3 . C6 . 83.94(8) yes C4 . Co3 . C6 . 115.96(14) yes Co2 . Co3 . C8 . 175.93(11) yes C4 . Co3 . C8 . 97.85(17) yes C6 . Co3 . C8 . 100.12(13) yes Co2 . Co3 . C10 . 79.86(9) yes C4 . Co3 . C10 . 121.12(14) yes C6 . Co3 . C10 . 116.01(14) yes C8 . Co3 . C10 . 98.52(17) yes Co3 . C4 . O5 . 176.5(3) yes Co3 . C6 . O7 . 176.7(2) yes Co3 . C8 . O9 . 178.6(4) yes Co3 . C10 . O11 . 176.2(3) yes Co2 . C12 . O13 . 176.6(2) yes Co2 . C14 . O15 . 177.1(2) yes Co2 . C16 . O17 . 178.9(2) yes Ga1 . N18 . C20 . 116.31(13) yes Ga1 . N18 . C32 . 123.47(15) yes C20 . N18 . C32 . 120.05(18) yes N18 . C20 . C21 . 119.32(19) yes N18 . C20 . C28 . 118.69(19) yes C21 . C20 . C28 . 121.9(2) yes C20 . C21 . C22 . 122.1(2) yes C20 . C21 . C25 . 117.8(2) yes C22 . C21 . C25 . 120.0(2) yes C21 . C22 . C23 . 113.1(2) yes C21 . C22 . C24 . 110.44(19) yes C23 . C22 . C24 . 109.9(2) yes C21 . C22 . H221 . 108.3 no C23 . C22 . H221 . 107.1 no C24 . C22 . H221 . 107.8 no C22 . C23 . H233 . 108.8 no C22 . C23 . H231 . 108.9 no H233 . C23 . H231 . 109.9 no C22 . C23 . H232 . 109.1 no H233 . C23 . H232 . 110.0 no H231 . C23 . H232 . 110.0 no C22 . C24 . H241 . 109.4 no C22 . C24 . H242 . 110.1 no H241 . C24 . H242 . 108.5 no C22 . C24 . H243 . 108.4 no H241 . C24 . H243 . 110.3 no H242 . C24 . H243 . 110.1 no C21 . C25 . C26 . 121.3(2) yes C21 . C25 . H251 . 119.1 no C26 . C25 . H251 . 119.5 no C25 . C26 . C27 . 119.8(2) yes C25 . C26 . H261 . 120.7 no C27 . C26 . H261 . 119.5 no C26 . C27 . C28 . 121.3(2) yes C26 . C27 . H271 . 119.2 no C28 . C27 . H271 . 119.5 no C20 . C28 . C27 . 117.9(2) yes C20 . C28 . C29 . 122.6(2) yes C27 . C28 . C29 . 119.4(2) yes C28 . C29 . C30 . 109.9(2) yes C28 . C29 . C31 . 112.2(2) yes C30 . C29 . C31 . 109.8(2) yes C28 . C29 . H291 . 108.0 no C30 . C29 . H291 . 107.7 no C31 . C29 . H291 . 109.0 no C29 . C30 . H303 . 108.9 no C29 . C30 . H301 . 110.5 no H303 . C30 . H301 . 108.2 no C29 . C30 . H302 . 110.8 no H303 . C30 . H302 . 110.1 no H301 . C30 . H302 . 108.3 no C29 . C31 . H311 . 108.0 no C29 . C31 . H312 . 109.2 no H311 . C31 . H312 . 109.5 no C29 . C31 . H313 . 110.4 no H311 . C31 . H313 . 109.0 no H312 . C31 . H313 . 110.7 no N18 . C32 . C33 . 119.5(2) yes N18 . C32 . C34 . 123.61(19) yes C33 . C32 . C34 . 116.83(19) yes C32 . C33 . H332 . 110.3 no C32 . C33 . H333 . 111.9 no H332 . C33 . H333 . 109.6 no C32 . C33 . H331 . 109.8 no H332 . C33 . H331 . 107.9 no H333 . C33 . H331 . 107.2 no C32 . C34 . C35 . 128.6(2) yes C32 . C34 . H341 . 116.0 no C35 . C34 . H341 . 115.4 no C34 . C35 . N36 . 123.7(2) yes C34 . C35 . C49 . 117.14(19) yes N36 . C35 . C49 . 119.1(2) yes Ga1 . N36 . C35 . 123.25(15) yes Ga1 . N36 . C37 . 116.33(13) yes C35 . N36 . C37 . 120.26(17) yes N36 . C37 . C38 . 118.66(19) yes N36 . C37 . C45 . 118.98(19) yes C38 . C37 . C45 . 122.3(2) yes C37 . C38 . C39 . 123.0(2) yes C37 . C38 . C42 . 117.8(2) yes C39 . C38 . C42 . 119.1(2) yes C38 . C39 . C40 . 110.2(2) yes C38 . C39 . C41 . 112.4(2) yes C40 . C39 . C41 . 109.9(2) yes C38 . C39 . H391 . 107.4 no C40 . C39 . H391 . 107.5 no C41 . C39 . H391 . 109.3 no C39 . C40 . H402 . 109.6 no C39 . C40 . H403 . 111.3 no H402 . C40 . H403 . 109.9 no C39 . C40 . H401 . 110.5 no H402 . C40 . H401 . 107.6 no H403 . C40 . H401 . 107.9 no C39 . C41 . H411 . 108.0 no C39 . C41 . H413 . 110.1 no H411 . C41 . H413 . 109.0 no C39 . C41 . H412 . 109.8 no H411 . C41 . H412 . 109.7 no H413 . C41 . H412 . 110.2 no C38 . C42 . C43 . 121.0(2) yes C38 . C42 . H421 . 119.6 no C43 . C42 . H421 . 119.4 no C42 . C43 . C44 . 120.1(2) yes C42 . C43 . H431 . 119.9 no C44 . C43 . H431 . 120.0 no C43 . C44 . C45 . 121.4(2) yes C43 . C44 . H441 . 119.7 no C45 . C44 . H441 . 119.0 no C37 . C45 . C44 . 117.4(2) yes C37 . C45 . C46 . 122.5(2) yes C44 . C45 . C46 . 120.0(2) yes C45 . C46 . C47 . 113.1(2) yes C45 . C46 . C48 . 110.64(19) yes C47 . C46 . C48 . 109.9(2) yes C45 . C46 . H461 . 106.9 no C47 . C46 . H461 . 107.3 no C48 . C46 . H461 . 108.8 no C46 . C47 . H472 . 108.1 no C46 . C47 . H473 . 109.5 no H472 . C47 . H473 . 110.0 no C46 . C47 . H471 . 107.8 no H472 . C47 . H471 . 110.2 no H473 . C47 . H471 . 111.3 no C46 . C48 . H481 . 110.3 no C46 . C48 . H483 . 109.0 no H481 . C48 . H483 . 109.1 no C46 . C48 . H482 . 110.2 no H481 . C48 . H482 . 108.6 no H483 . C48 . H482 . 109.6 no C35 . C49 . H492 . 113.0 no C35 . C49 . H491 . 110.2 no H492 . C49 . H491 . 108.9 no C35 . C49 . H493 . 109.4 no H492 . C49 . H493 . 107.7 no H491 . C49 . H493 . 107.4 no Co51 . Ga50 . N67 . 131.44(5) yes Co51 . Ga50 . N84 . 131.50(5) yes N67 . Ga50 . N84 . 97.06(7) yes Ga50 . Co51 . Co52 . 178.45(2) yes Ga50 . Co51 . C61 . 87.88(8) yes Co52 . Co51 . C61 . 90.57(8) yes Ga50 . Co51 . C63 . 91.15(8) yes Co52 . Co51 . C63 . 89.64(8) yes C61 . Co51 . C63 . 120.87(13) yes Ga50 . Co51 . C65 . 91.21(8) yes Co52 . Co51 . C65 . 89.58(8) yes C61 . Co51 . C65 . 120.46(13) yes C63 . Co51 . C65 . 118.67(14) yes Co51 . Co52 . C53 . 84.05(7) yes Co51 . Co52 . C55 . 176.27(11) yes C53 . Co52 . C55 . 99.68(13) yes Co51 . Co52 . C57 . 79.95(9) yes C53 . Co52 . C57 . 115.97(14) yes C55 . Co52 . C57 . 98.43(18) yes Co51 . Co52 . C59 . 79.77(9) yes C53 . Co52 . C59 . 115.75(14) yes C55 . Co52 . C59 . 98.35(18) yes C57 . Co52 . C59 . 121.37(15) yes Co52 . C53 . O54 . 176.9(2) yes Co52 . C55 . O56 . 178.2(3) yes Co52 . C57 . O58 . 176.9(3) yes Co52 . C59 . O60 . 176.3(3) yes Co51 . C61 . O62 . 179.1(2) yes Co51 . C63 . O64 . 176.8(2) yes Co51 . C65 . O66 . 176.8(2) yes Ga50 . N67 . C68 . 116.39(13) yes Ga50 . N67 . C80 . 123.43(15) yes C68 . N67 . C80 . 119.97(17) yes N67 . C68 . C69 . 119.25(19) yes N67 . C68 . C76 . 118.77(19) yes C69 . C68 . C76 . 121.9(2) yes C68 . C69 . C70 . 121.9(2) yes C68 . C69 . C73 . 117.7(2) yes C70 . C69 . C73 . 120.3(2) yes C69 . C70 . C71 . 112.9(2) yes C69 . C70 . C72 . 110.76(19) yes C71 . C70 . C72 . 109.8(2) yes C69 . C70 . H701 . 107.7 no C71 . C70 . H701 . 107.3 no C72 . C70 . H701 . 108.2 no C70 . C71 . H713 . 108.3 no C70 . C71 . H711 . 108.6 no H713 . C71 . H711 . 109.5 no C70 . C71 . H712 . 110.0 no H713 . C71 . H712 . 109.8 no H711 . C71 . H712 . 110.6 no C70 . C72 . H721 . 109.7 no C70 . C72 . H722 . 110.5 no H721 . C72 . H722 . 108.4 no C70 . C72 . H723 . 108.7 no H721 . C72 . H723 . 109.2 no H722 . C72 . H723 . 110.4 no C69 . C73 . C74 . 121.4(2) yes C69 . C73 . H731 . 119.2 no C74 . C73 . H731 . 119.4 no C73 . C74 . C75 . 119.9(2) yes C73 . C74 . H741 . 120.4 no C75 . C74 . H741 . 119.7 no C74 . C75 . C76 . 121.3(2) yes C74 . C75 . H751 . 119.0 no C76 . C75 . H751 . 119.7 no C68 . C76 . C75 . 117.9(2) yes C68 . C76 . C77 . 123.0(2) yes C75 . C76 . C77 . 119.1(2) yes C76 . C77 . C78 . 110.5(2) yes C76 . C77 . C79 . 112.3(2) yes C78 . C77 . C79 . 110.0(2) yes C76 . C77 . H771 . 107.5 no C78 . C77 . H771 . 107.1 no C79 . C77 . H771 . 109.3 no C77 . C78 . H783 . 109.4 no C77 . C78 . H781 . 110.8 no H783 . C78 . H781 . 109.8 no C77 . C78 . H782 . 110.2 no H783 . C78 . H782 . 108.1 no H781 . C78 . H782 . 108.5 no C77 . C79 . H791 . 108.0 no C77 . C79 . H792 . 109.9 no H791 . C79 . H792 . 109.7 no C77 . C79 . H793 . 108.6 no H791 . C79 . H793 . 109.8 no H792 . C79 . H793 . 110.9 no N67 . C80 . C81 . 119.6(2) yes N67 . C80 . C82 . 123.52(19) yes C81 . C80 . C82 . 116.81(19) yes C80 . C81 . H812 . 110.3 no C80 . C81 . H813 . 109.1 no H812 . C81 . H813 . 107.3 no C80 . C81 . H811 . 113.0 no H812 . C81 . H811 . 109.4 no H813 . C81 . H811 . 107.6 no C80 . C82 . C83 . 128.67(19) yes C80 . C82 . H821 . 115.7 no C83 . C82 . H821 . 115.6 no C82 . C83 . N84 . 123.36(19) yes C82 . C83 . C97 . 116.99(19) yes N84 . C83 . C97 . 119.63(19) yes Ga50 . N84 . C83 . 123.56(15) yes Ga50 . N84 . C85 . 116.54(13) yes C83 . N84 . C85 . 119.71(17) yes N84 . C85 . C86 . 118.95(19) yes N84 . C85 . C93 . 118.84(19) yes C86 . C85 . C93 . 122.1(2) yes C85 . C86 . C87 . 122.4(2) yes C85 . C86 . C90 . 117.3(2) yes C87 . C86 . C90 . 120.3(2) yes C86 . C87 . C88 . 113.1(2) yes C86 . C87 . C89 . 111.0(2) yes C88 . C87 . C89 . 109.8(2) yes C86 . C87 . H871 . 107.5 no C88 . C87 . H871 . 106.3 no C89 . C87 . H871 . 108.8 no C87 . C88 . H882 . 109.3 no C87 . C88 . H883 . 108.6 no H882 . C88 . H883 . 109.7 no C87 . C88 . H881 . 108.8 no H882 . C88 . H881 . 109.8 no H883 . C88 . H881 . 110.7 no C87 . C89 . H891 . 109.8 no C87 . C89 . H893 . 108.8 no H891 . C89 . H893 . 109.6 no C87 . C89 . H892 . 110.1 no H891 . C89 . H892 . 109.4 no H893 . C89 . H892 . 109.1 no C86 . C90 . C91 . 121.5(2) yes C86 . C90 . H901 . 118.7 no C91 . C90 . H901 . 119.8 no C90 . C91 . C92 . 119.9(2) yes C90 . C91 . H911 . 120.7 no C92 . C91 . H911 . 119.4 no C91 . C92 . C93 . 121.4(2) yes C91 . C92 . H921 . 119.1 no C93 . C92 . H921 . 119.5 no C85 . C93 . C92 . 117.8(2) yes C85 . C93 . C94 . 122.9(2) yes C92 . C93 . C94 . 119.3(2) yes C93 . C94 . C95 . 110.2(2) yes C93 . C94 . C96 . 112.5(2) yes C95 . C94 . C96 . 109.7(2) yes C93 . C94 . H941 . 107.6 no C95 . C94 . H941 . 107.5 no C96 . C94 . H941 . 109.2 no C94 . C95 . H952 . 109.4 no C94 . C95 . H953 . 111.6 no H952 . C95 . H953 . 109.4 no C94 . C95 . H951 . 110.2 no H952 . C95 . H951 . 107.6 no H953 . C95 . H951 . 108.6 no C94 . C96 . H961 . 107.7 no C94 . C96 . H963 . 109.7 no H961 . C96 . H963 . 109.6 no C94 . C96 . H962 . 109.1 no H961 . C96 . H962 . 110.0 no H963 . C96 . H962 . 110.7 no C83 . C97 . H972 . 113.6 no C83 . C97 . H971 . 109.7 no H972 . C97 . H971 . 107.9 no C83 . C97 . H973 . 110.1 no H972 . C97 . H973 . 108.6 no H971 . C97 . H973 . 106.7 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C29 . H291 . C32 . 130.52 0.991 2.562 3.293(4) yes C39 . H391 . C35 . 130.97 0.991 2.565 3.300(4) yes C77 . H771 . C80 . 130.74 0.988 2.567 3.298(4) yes C94 . H941 . C83 . 130.82 0.990 2.569 3.302(4) yes _iucr_refine_instructions_details_constraints ; # # Punched on 10/03/13 at 14:39:47 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 233,X'S) H ( 231,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 303,X'S) H ( 301,X'S) H ( 302,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) H ( 313,X'S) RIDE C ( 33,X'S) H ( 332,X'S) H ( 333,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 402,X'S) H ( 403,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 413,X'S) H ( 412,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 ( 46,X'S) H ( 461,X'S) RIDE C ( 47,X'S) H ( 472,X'S) H ( 473,X'S) H ( 471,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 483,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 492,X'S) H ( 491,X'S) H ( 493,X'S) RIDE C ( 70,X'S) H ( 701,X'S) RIDE C ( 71,X'S) H ( 713,X'S) H ( 711,X'S) H ( 712,X'S) RIDE C ( 72,X'S) H ( 721,X'S) H ( 722,X'S) H ( 723,X'S) RIDE C ( 73,X'S) H ( 731,X'S) RIDE C ( 74,X'S) H ( 741,X'S) RIDE C ( 75,X'S) H ( 751,X'S) RIDE C ( 77,X'S) H ( 771,X'S) RIDE C ( 78,X'S) H ( 783,X'S) H ( 781,X'S) H ( 782,X'S) RIDE C ( 79,X'S) H ( 791,X'S) H ( 792,X'S) H ( 793,X'S) RIDE C ( 81,X'S) H ( 812,X'S) H ( 813,X'S) H ( 811,X'S) RIDE C ( 82,X'S) H ( 821,X'S) RIDE C ( 87,X'S) H ( 871,X'S) RIDE C ( 88,X'S) H ( 882,X'S) H ( 883,X'S) H ( 881,X'S) RIDE C ( 89,X'S) H ( 891,X'S) H ( 893,X'S) H ( 892,X'S) RIDE C ( 90,X'S) H ( 901,X'S) RIDE C ( 91,X'S) H ( 911,X'S) RIDE C ( 92,X'S) H ( 921,X'S) RIDE C ( 94,X'S) H ( 941,X'S) RIDE C ( 95,X'S) H ( 952,X'S) H ( 953,X'S) H ( 951,X'S) RIDE C ( 96,X'S) H ( 961,X'S) H ( 963,X'S) H ( 962,X'S) RIDE C ( 97,X'S) H ( 972,X'S) H ( 971,X'S) H ( 973,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 10/03/13 at 14:39:47 # #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 944062' ####################################################################### # # 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_037jtrt13 _audit_creation_date 13-06-05 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '037jtrt13 in P 21/m' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 8.86000(10) _cell_length_b 21.5544(2) _cell_length_c 9.08180(10) _cell_angle_alpha 90 _cell_angle_beta 108.6007(4) _cell_angle_gamma 90 _cell_volume 1643.77(3) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m ' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y+1/2,z -x,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' 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' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 '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' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C17.50 H22.50 Ga0.50 Mn0.50 N1 O2 # Dc = 0.69 Fooo = 684.00 Mu = 6.22 M = 170.60 # Found Formula = C33 H42 Ga1 Mn1 N2 O4 # Dc = 1.32 FOOO = 684.00 Mu = 12.40 M = 327.68 _chemical_formula_sum 'C33 H42 Ga1 Mn1 N2 O4' _chemical_formula_moiety 'C33 H42 Ga1 Mn1 N2 O4' _chemical_compound_source ? _chemical_formula_weight 655.36 _cell_measurement_reflns_used 3815 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.180 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.240 # Sheldrick geometric approximatio 0.75 0.80 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.80 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 46587 _reflns_number_total 3844 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections without Friedels Law is 7447 # Number of reflections with Friedels Law is 3844 # Theoretical number of reflections is about 3775 _diffrn_reflns_theta_min 5.101 _diffrn_reflns_theta_max 27.497 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.947 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _oxford_diffrn_Wilson_B_factor 1.65 _oxford_diffrn_Wilson_scale 3.61 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.61 _refine_diff_density_max 0.62 # 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>-3.0\s(I) _refine_ls_number_reflns 3844 _refine_ls_number_restraints 42 _refine_ls_number_parameters 223 _oxford_refine_ls_R_factor_ref 0.0435 _refine_ls_wR_factor_ref 0.0787 _refine_ls_goodness_of_fit_ref 0.9152 _refine_ls_shift/su_max 0.0005783 _refine_ls_shift/su_mean 0.0000179 # The values computed with all filters except I/sigma _oxford_reflns_number_all 3844 _refine_ls_R_factor_all 0.0435 _refine_ls_wR_factor_all 0.0787 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3082 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_gt 0.0653 # 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 mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 19.1 29.5 16.9 6.76 1.51 ; # 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 O27 O 0.2744(17) 0.2500 0.292(3) 0.0398 0.50(8) Uani DS T P 2 1 . O28 O 0.303(3) 0.2500 0.338(4) 0.0487 0.50(8) Uani DS T P 2 2 . O29 O 0.785(3) 0.2500 0.5459(10) 0.0410 0.50(8) Uani DS T P 2 1 . O30 O 0.822(3) 0.2500 0.530(2) 0.0570 0.50(8) Uani DS T P 2 2 . C25 C 1.1756(8) 0.4311(6) 0.3271(10) 0.0521 0.70(3) Uani D . P 1 1 . C26 C 1.1898(11) 0.4068(11) 0.297(2) 0.0432 0.30(3) Uani D . P 1 2 . Ga1 Ga 0.77283(4) 0.2500 0.09426(4) 0.0189 1.0000 Uani S T . . . . Mn2 Mn 0.57712(5) 0.2500 0.21873(5) 0.0211 1.0000 Uani S T . . . . C3 C 0.7169(4) 0.2500 0.4136(4) 0.0365 1.0000 Uani DS T . . . . C5 C 0.5531(3) 0.16608(11) 0.1930(3) 0.0288 1.0000 Uani . . . . . . C7 C 0.3995(4) 0.2500 0.2751(4) 0.0370 1.0000 Uani DS T . . . . C10 C 0.8207(2) 0.37863(9) 0.0251(2) 0.0196 1.0000 Uani . . . . . . C11 C 0.6968(2) 0.40274(10) -0.1008(2) 0.0243 1.0000 Uani . . . . . . C12 C 0.6462(3) 0.46303(10) -0.0881(3) 0.0284 1.0000 Uani . . . . . . C13 C 0.7144(3) 0.49767(10) 0.0442(3) 0.0300 1.0000 Uani . . . . . . C14 C 0.8352(3) 0.47332(11) 0.1665(3) 0.0297 1.0000 Uani . . . . . . C15 C 0.8913(2) 0.41321(10) 0.1599(2) 0.0235 1.0000 Uani . . . . . . C16 C 1.0270(3) 0.38802(12) 0.2955(3) 0.0328 1.0000 Uani D . . . . . C17 C 0.9866(3) 0.38806(17) 0.4455(3) 0.0513 1.0000 Uani . . . . . . C19 C 0.6190(3) 0.36558(12) -0.2475(3) 0.0333 1.0000 Uani . . . . . . C20 C 0.4469(3) 0.34842(14) -0.2605(3) 0.0437 1.0000 Uani . . . . . . C21 C 0.6213(3) 0.40035(16) -0.3937(3) 0.0491 1.0000 Uani . . . . . . C22 C 0.9888(2) 0.30793(10) -0.0521(2) 0.0231 1.0000 Uani . . . . . . C23 C 1.0448(3) 0.250000(7) -0.0781(4) 0.0245 1.0000 Uani S T . . . . C24 C 1.0595(3) 0.36346(11) -0.1061(3) 0.0380 1.0000 Uani . . . . . . O6 O 0.5229(2) 0.11445(8) 0.1753(2) 0.0431 1.0000 Uani . . . . . . N9 N 0.87508(19) 0.31597(8) 0.01418(19) 0.0194 1.0000 Uani . . . . . . H251 H 1.2633 0.4128 0.4060 0.0797 0.70(3) Uiso R . P 1 1 . H253 H 1.1542 0.4711 0.3619 0.0799 0.70(3) Uiso R . P 1 1 . H252 H 1.2035 0.4362 0.2332 0.0801 0.70(3) Uiso R . P 1 1 . H261 H 1.2679 0.3889 0.3863 0.0619 0.30(3) Uiso R . P 1 2 . H263 H 1.1986 0.4514 0.3003 0.0619 0.30(3) Uiso R . P 1 2 . H262 H 1.2055 0.3914 0.2039 0.0619 0.30(3) Uiso R . P 1 2 . H121 H 0.5647 0.4803 -0.1712 0.0340 1.0000 Uiso R . . . . . H131 H 0.6766 0.5378 0.0514 0.0363 1.0000 Uiso R . . . . . H141 H 0.8817 0.4976 0.2553 0.0366 1.0000 Uiso R . . . . . H171 H 0.8869 0.3658 0.4323 0.0768 1.0000 Uiso R . . . . . H173 H 0.9742 0.4299 0.4776 0.0774 1.0000 Uiso R . . . . . H172 H 1.0714 0.3679 0.5270 0.0765 1.0000 Uiso R . . . . . H191 H 0.6775 0.3269 -0.2419 0.0402 1.0000 Uiso R . . . . . H201 H 0.4026 0.3233 -0.3528 0.0656 1.0000 Uiso R . . . . . H203 H 0.3847 0.3863 -0.2693 0.0657 1.0000 Uiso R . . . . . H202 H 0.4445 0.3248 -0.1703 0.0659 1.0000 Uiso R . . . . . H211 H 0.5791 0.3737 -0.4829 0.0733 1.0000 Uiso R . . . . . H213 H 0.7291 0.4113 -0.3846 0.0737 1.0000 Uiso R . . . . . H212 H 0.5581 0.4380 -0.4061 0.0737 1.0000 Uiso R . . . . . H231 H 1.1267 0.2500 -0.1222 0.0289 1.0000 Uiso RS . . . . . H242 H 1.0815 0.3959 -0.0308 0.0577 1.0000 Uiso R . . . . . H241 H 1.1541 0.3525 -0.1286 0.0572 1.0000 Uiso R . . . . . H243 H 0.9853 0.3794 -0.1991 0.0591 1.0000 Uiso R . . . . . H161 H 1.0409 0.3444 0.2728 0.0398 1.0000 Uiso R . . . . . H3 H 0.493(6) 0.2500 0.043(6) 0.064(14) 1.0000 Uiso S . . . . . 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 O27 0.028(3) 0.056(4) 0.042(6) 0.0000 0.020(4) 0.0000 O28 0.042(5) 0.065(5) 0.051(7) 0.0000 0.031(5) 0.0000 O29 0.048(6) 0.051(4) 0.023(3) 0.0000 0.009(3) 0.0000 O30 0.056(6) 0.075(6) 0.036(4) 0.0000 0.008(4) 0.0000 C25 0.026(2) 0.082(5) 0.048(3) 0.013(3) 0.0113(19) -0.002(2) C26 0.021(4) 0.068(7) 0.039(5) 0.008(5) 0.008(3) 0.018(4) Ga1 0.01883(15) 0.01805(15) 0.02188(16) 0.0000 0.00954(12) 0.0000 Mn2 0.0221(2) 0.0220(2) 0.0219(2) 0.0000 0.01078(18) 0.0000 C3 0.0445(19) 0.0328(17) 0.0313(16) 0.0000 0.0106(14) 0.0000 C5 0.0296(11) 0.0307(12) 0.0329(11) -0.0009(9) 0.0194(9) -0.0031(9) C7 0.0374(18) 0.0338(17) 0.046(2) 0.0000 0.0227(16) 0.0000 C10 0.0198(9) 0.0164(9) 0.0248(9) 0.0007(7) 0.0100(8) -0.0005(7) C11 0.0221(10) 0.0247(10) 0.0264(10) 0.0011(8) 0.0081(8) 0.0009(8) C12 0.0262(10) 0.0261(11) 0.0334(11) 0.0060(9) 0.0100(9) 0.0062(8) C13 0.0300(11) 0.0186(10) 0.0451(13) -0.0001(9) 0.0170(10) 0.0027(8) C14 0.0305(11) 0.0256(11) 0.0343(11) -0.0084(9) 0.0123(9) -0.0045(9) C15 0.0227(9) 0.0239(10) 0.0242(10) -0.0002(8) 0.0080(8) -0.0010(8) C16 0.0321(11) 0.0374(12) 0.0245(10) -0.0020(9) 0.0028(9) 0.0026(10) C17 0.0438(15) 0.079(2) 0.0285(12) 0.0038(13) 0.0073(11) -0.0064(15) C19 0.0312(11) 0.0349(12) 0.0282(11) -0.0024(9) 0.0019(9) 0.0063(10) C20 0.0418(14) 0.0499(16) 0.0325(13) 0.0017(11) 0.0019(11) -0.0128(12) C21 0.0429(14) 0.076(2) 0.0306(12) -0.0064(13) 0.0145(11) -0.0061(14) C22 0.0206(9) 0.0232(10) 0.0281(10) 0.0021(8) 0.0113(8) -0.0012(8) C23 0.0201(13) 0.0262(15) 0.0318(15) 0.0000 0.0150(12) 0.0000 C24 0.0423(13) 0.0260(11) 0.0584(16) 0.0044(11) 0.0338(13) -0.0032(10) O6 0.0498(11) 0.0297(9) 0.0623(12) -0.0099(8) 0.0355(10) -0.0117(8) N9 0.0181(8) 0.0178(8) 0.0235(8) 0.0002(6) 0.0081(6) -0.0005(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3829(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 O27 . C7 . 1.166(8) yes O28 . C7 . 1.167(8) yes O29 . C3 . 1.161(8) yes O30 . C3 . 1.168(8) yes C25 . C16 . 1.560(6) yes C25 . H251 . 0.957 no C25 . H253 . 0.958 no C25 . H252 . 0.968 no C26 . C16 . 1.493(8) yes C26 . H261 . 0.962 no C26 . H263 . 0.964 no C26 . H262 . 0.960 no Ga1 . N9 3_555 1.9473(16) yes Ga1 . Mn2 . 2.3528(5) yes Ga1 . N9 . 1.9473(16) yes Mn2 . C5 3_555 1.828(2) yes Mn2 . C3 . 1.807(3) yes Mn2 . C5 . 1.828(2) yes Mn2 . C7 . 1.803(3) yes Mn2 . H3 . 1.53(5) no C5 . O6 . 1.144(3) yes C10 . C11 . 1.408(3) yes C10 . C15 . 1.398(3) yes C10 . N9 . 1.448(2) yes C11 . C12 . 1.392(3) yes C11 . C19 . 1.518(3) yes C12 . C13 . 1.380(3) yes C12 . H121 . 0.939 no C13 . C14 . 1.377(3) yes C13 . H131 . 0.937 no C14 . C15 . 1.396(3) yes C14 . H141 . 0.939 no C15 . C16 . 1.521(3) yes C16 . C17 . 1.515(3) yes C16 . H161 . 0.978 no C16 . C17 . 1.515(3) yes C16 . H161 . 0.978 no C17 . H171 . 0.979 no C17 . H173 . 0.966 no C17 . H172 . 0.973 no C19 . C20 . 1.537(4) yes C19 . C21 . 1.530(4) yes C19 . H191 . 0.974 no C20 . H201 . 0.970 no C20 . H203 . 0.973 no C20 . H202 . 0.970 no C21 . H211 . 0.965 no C21 . H213 . 0.962 no C21 . H212 . 0.972 no C22 . C23 . 1.391(2) yes C22 . C24 . 1.504(3) yes C22 . N9 . 1.339(3) yes C23 . H231 . 0.934 no C24 . H242 . 0.954 no C24 . H241 . 0.953 no C24 . H243 . 0.954 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 C16 . C25 . H251 . 109.3 no C16 . C25 . H253 . 110.6 no H251 . C25 . H253 . 108.7 no C16 . C25 . H252 . 110.2 no H251 . C25 . H252 . 109.4 no H253 . C25 . H252 . 108.7 no C16 . C26 . H261 . 109.5 no C16 . C26 . H263 . 109.8 no H261 . C26 . H263 . 110.1 no C16 . C26 . H262 . 108.0 no H261 . C26 . H262 . 109.7 no H263 . C26 . H262 . 109.7 no N9 3_555 Ga1 . Mn2 . 132.95(5) yes N9 3_555 Ga1 . N9 . 93.82(10) yes Mn2 . Ga1 . N9 . 132.95(5) yes C5 3_555 Mn2 . Ga1 . 90.69(6) yes C5 3_555 Mn2 . C3 . 98.07(7) yes Ga1 . Mn2 . C3 . 95.19(12) yes C5 3_555 Mn2 . C5 . 163.60(15) yes Ga1 . Mn2 . C5 . 90.69(6) yes C3 . Mn2 . C5 . 98.07(7) yes C5 3_555 Mn2 . C7 . 87.70(7) yes Ga1 . Mn2 . C7 . 168.52(13) yes C3 . Mn2 . C7 . 96.29(17) yes C5 . Mn2 . C7 . 87.70(7) yes C5 3_555 Mn2 . H3 . 82.46(13) no Ga1 . Mn2 . H3 . 71.8(18) no C3 . Mn2 . H3 . 167.0(18) no C5 . Mn2 . H3 . 82.46(13) no C7 . Mn2 . H3 . 96.7(18) no O29 . C3 . Mn2 . 169.2(14) yes O30 . C3 . Mn2 . 171.4(19) yes Mn2 . C5 . O6 . 173.4(2) yes O27 . C7 . Mn2 . 171.6(15) yes O28 . C7 . Mn2 . 168.0(19) yes C11 . C10 . C15 . 121.96(18) yes C11 . C10 . N9 . 118.61(17) yes C15 . C10 . N9 . 119.43(17) yes C10 . C11 . C12 . 117.77(19) yes C10 . C11 . C19 . 122.43(19) yes C12 . C11 . C19 . 119.79(19) yes C11 . C12 . C13 . 120.9(2) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 119.7 no C12 . C13 . C14 . 120.5(2) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 119.9 no C13 . C14 . C15 . 121.0(2) yes C13 . C14 . H141 . 119.7 no C15 . C14 . H141 . 119.3 no C10 . C15 . C14 . 117.80(19) yes C10 . C15 . C16 . 122.39(19) yes C14 . C15 . C16 . 119.80(19) yes C15 . C16 . C25 . 109.8(3) yes C15 . C16 . C17 . 112.0(2) yes C25 . C16 . C17 . 105.2(5) yes C15 . C16 . H161 . 107.0 no C25 . C16 . H161 . 117.0 no C17 . C16 . H161 . 105.8 no C15 . C16 . C26 . 115.0(6) yes C15 . C16 . C17 . 112.0(2) yes C26 . C16 . C17 . 119.7(8) yes C15 . C16 . H161 . 107.0 no C26 . C16 . H161 . 94.4 no C17 . C16 . H161 . 105.8 no C16 . C17 . H171 . 110.6 no C16 . C17 . H173 . 110.7 no H171 . C17 . H173 . 108.1 no C16 . C17 . H172 . 109.7 no H171 . C17 . H172 . 108.8 no H173 . C17 . H172 . 108.8 no C11 . C19 . C20 . 110.8(2) yes C11 . C19 . C21 . 112.0(2) yes C20 . C19 . C21 . 109.8(2) yes C11 . C19 . H191 . 108.7 no C20 . C19 . H191 . 107.2 no C21 . C19 . H191 . 108.1 no C19 . C20 . H201 . 108.6 no C19 . C20 . H203 . 109.0 no H201 . C20 . H203 . 109.6 no C19 . C20 . H202 . 110.5 no H201 . C20 . H202 . 109.0 no H203 . C20 . H202 . 110.2 no C19 . C21 . H211 . 109.2 no C19 . C21 . H213 . 109.5 no H211 . C21 . H213 . 109.0 no C19 . C21 . H212 . 110.1 no H211 . C21 . H212 . 110.1 no H213 . C21 . H212 . 109.0 no C23 . C22 . C24 . 116.78(19) yes C23 . C22 . N9 . 123.53(19) yes C24 . C22 . N9 . 119.67(19) yes C22 . C23 . C22 3_555 127.7(3) yes C22 . C23 . H231 . 116.1 no C22 3_555 C23 . H231 . 116.1 no C22 . C24 . H242 . 111.1 no C22 . C24 . H241 . 111.0 no H242 . C24 . H241 . 110.1 no C22 . C24 . H243 . 109.5 no H242 . C24 . H243 . 107.2 no H241 . C24 . H243 . 107.7 no C10 . N9 . Ga1 . 116.79(12) yes C10 . N9 . C22 . 117.78(16) yes Ga1 . N9 . C22 . 125.41(14) yes _iucr_refine_instruction_details_constraints ; # # Punched on 05/06/13 at 12:03:07 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) EQUIV PART(2001,OCC) PART(2002,OCC) WEIGHT -1 PART(2002,OCC) CONT H(3,X'S,U[ISO]) RIDE C ( 25,X'S) H ( 251,X'S) H ( 253,X'S) H ( 252,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 263,X'S) H ( 262,X'S) REM RIDE MN ( 2,X'S) H ( 3,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 ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 173,X'S) H ( 172,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 203,X'S) H ( 202,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 213,X'S) H ( 212,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 242,X'S) H ( 241,X'S) H ( 243,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/06/13 at 12:03:07 # #LIST 16 SAME C(16) C(25) C(16) AND CONT C(16) C(26) C(16) SIMU 0.01 C(16) C(25) C(16) AND CONT C(16) C(26) C(16) DELU 0.01 C(16) C(25) C(16) AND CONT C(16) C(26) C(16) SAME C(7) O(28) C(7) AND CONT C(7) O(27) C(7) AND CONT C(3) O(29) C(3) AND CONT C(3) O(30) C(3) SIMU 0.01 C(7) O(28) C(7) AND CONT C(7) O(27) C(7) AND CONT C(3) O(29) C(3) AND CONT C(3) O(30) C(3) DELU 0.01 C(7) O(28) C(7) AND CONT C(7) O(27) C(7) AND CONT C(3) O(29) C(3) AND CONT C(3) O(30) C(3) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 944063' ####################################################################### # # 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_056jtrt13 _audit_creation_date 13-05-07 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '056jtrt13 in C 2/c' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 21.42720(10) _cell_length_b 16.89020(10) _cell_length_c 21.5723(2) _cell_angle_alpha 90 _cell_angle_beta 108.7295(4) _cell_angle_gamma 90 _cell_volume 7393.79(9) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-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' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C36 H42 Cl1 Co2 Ga1 N2 O7 # Dc = 1.51 Fooo = 2880.00 Mu = 17.32 M = 837.78 # Found Formula = C33 H41 Cl1 Co1 Ga1 N2 O4 # Dc = 1.25 FOOO = 2880.00 Mu = 12.83 M = 693.80 _chemical_formula_sum 'C33 H41 Cl1 Co1 Ga1 N2 O4' _chemical_formula_moiety 'C33 H41 Cl1 Co1 Ga1 N2 O4' _chemical_compound_source . _chemical_formula_weight 693.80 _cell_measurement_reflns_used 8664 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.190 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_max 0.290 _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.283 # Sheldrick geometric approximatio 0.70 0.78 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.78 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 121009 _reflns_number_total 8414 _diffrn_reflns_av_R_equivalents 0.024 # Number of reflections without Friedels Law is 8414 # Number of reflections with Friedels Law is 8414 # Theoretical number of reflections is about 8481 _diffrn_reflns_theta_min 5.099 _diffrn_reflns_theta_max 27.486 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.937 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -27 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 1.96 _oxford_diffrn_Wilson_scale 100.54 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.61 _refine_diff_density_max 0.56 # 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>0.0\s(I) _refine_ls_number_reflns 8414 _refine_ls_number_restraints 0 _refine_ls_number_parameters 379 _oxford_refine_ls_R_factor_ref 0.0480 _refine_ls_wR_factor_ref 0.0992 _refine_ls_goodness_of_fit_ref 0.9727 _refine_ls_shift/su_max 0.0020093 _refine_ls_shift/su_mean 0.0000365 # The values computed with all filters except I/sigma _oxford_reflns_number_all 8414 _refine_ls_R_factor_all 0.0480 _refine_ls_wR_factor_all 0.0992 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6609 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_gt 0.0816 # 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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 14.3 21.4 10.8 2.93 ; # 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 Ga1 Ga 0.205453(11) 0.606109(14) 0.233125(11) 0.0217 1.0000 Uani . . . . . . Cl2 Cl 0.28973(3) 0.52353(3) 0.25202(3) 0.0334 1.0000 Uani . . . . . . N3 N 0.20336(9) 0.68434(11) 0.16571(9) 0.0232 1.0000 Uani . . . . . . C4 C 0.19408(11) 0.76110(13) 0.17569(11) 0.0252 1.0000 Uani . . . . . . C5 C 0.19140(12) 0.79201(14) 0.23500(11) 0.0290 1.0000 Uani . . . . . . C6 C 0.20862(11) 0.75652(14) 0.29652(11) 0.0265 1.0000 Uani . . . . . . N7 N 0.22196(9) 0.67916(11) 0.30685(9) 0.0237 1.0000 Uani . . . . . . C8 C 0.25436(11) 0.65025(14) 0.37280(10) 0.0261 1.0000 Uani . . . . . . C9 C 0.21756(12) 0.62891(14) 0.41386(11) 0.0290 1.0000 Uani . . . . . . C10 C 0.14444(13) 0.64563(16) 0.39798(12) 0.0336 1.0000 Uani . . . . . . C11 C 0.13295(17) 0.70365(19) 0.44818(17) 0.0495 1.0000 Uani . . . . . . C12 C 0.10388(14) 0.57085(18) 0.39715(15) 0.0418 1.0000 Uani . . . . . . C13 C 0.25161(14) 0.59544(17) 0.47460(12) 0.0376 1.0000 Uani . . . . . . C14 C 0.31912(15) 0.58461(19) 0.49404(13) 0.0450 1.0000 Uani . . . . . . C15 C 0.35452(14) 0.60903(18) 0.45441(14) 0.0425 1.0000 Uani . . . . . . C16 C 0.32333(12) 0.64292(16) 0.39317(12) 0.0326 1.0000 Uani . . . . . . C17 C 0.36389(13) 0.67614(19) 0.35262(13) 0.0390 1.0000 Uani . . . . . . C18 C 0.38009(16) 0.7638(2) 0.36864(17) 0.0509 1.0000 Uani . . . . . . C19 C 0.42734(15) 0.6299(3) 0.36022(18) 0.0595 1.0000 Uani . . . . . . C20 C 0.21168(15) 0.81056(15) 0.35311(13) 0.0365 1.0000 Uani . . . . . . C21 C 0.18639(14) 0.82027(15) 0.12180(12) 0.0345 1.0000 Uani . . . . . . C22 C 0.21065(11) 0.65911(13) 0.10416(10) 0.0245 1.0000 Uani . . . . . . C23 C 0.15470(12) 0.64893(14) 0.04790(11) 0.0284 1.0000 Uani . . . . . . C24 C 0.16520(14) 0.62081(16) -0.00878(12) 0.0347 1.0000 Uani . . . . . . C25 C 0.22718(15) 0.60392(17) -0.01071(13) 0.0388 1.0000 Uani . . . . . . C26 C 0.28149(14) 0.61612(16) 0.04404(13) 0.0364 1.0000 Uani . . . . . . C27 C 0.27489(12) 0.64406(15) 0.10248(12) 0.0292 1.0000 Uani . . . . . . C28 C 0.33618(12) 0.66180(16) 0.16025(12) 0.0328 1.0000 Uani . . . . . . C29 C 0.39177(15) 0.6024(2) 0.16639(17) 0.0537 1.0000 Uani . . . . . . C30 C 0.35996(16) 0.7463(2) 0.15655(18) 0.0554 1.0000 Uani . . . . . . C31 C 0.08464(12) 0.67115(16) 0.04390(12) 0.0328 1.0000 Uani . . . . . . C32 C 0.03644(13) 0.60110(19) 0.02316(14) 0.0413 1.0000 Uani . . . . . . C33 C 0.05828(15) 0.73869(19) -0.00548(15) 0.0459 1.0000 Uani . . . . . . O34 O 0.16160(11) 0.46184(12) 0.10274(10) 0.0445 1.0000 Uani . . . . . . C35 C 0.14257(13) 0.48715(14) 0.14226(12) 0.0320 1.0000 Uani . . . . . . O36 O 0.04724(11) 0.67182(12) 0.20591(12) 0.0481 1.0000 Uani . . . . . . C37 C 0.07266(12) 0.61214(15) 0.20589(12) 0.0314 1.0000 Uani . . . . . . O38 O 0.18261(11) 0.43797(14) 0.32725(10) 0.0514 1.0000 Uani . . . . . . C39 C 0.15564(13) 0.47167(15) 0.28076(13) 0.0344 1.0000 Uani . . . . . . O40 O -0.00578(10) 0.41531(13) 0.16988(13) 0.0531 1.0000 Uani . . . . . . C41 C 0.03853(13) 0.45632(16) 0.18375(14) 0.0364 1.0000 Uani . . . . . . Co42 Co 0.110603(15) 0.518797(18) 0.205610(15) 0.0249 1.0000 Uani . . . . . . H51 H 0.1778 0.8450 0.2337 0.0335 1.0000 Uiso R . . . . . H101 H 0.1280 0.6706 0.3545 0.0384 1.0000 Uiso R . . . . . H112 H 0.0875 0.7189 0.4342 0.0728 1.0000 Uiso R . . . . . H113 H 0.1600 0.7507 0.4521 0.0726 1.0000 Uiso R . . . . . H111 H 0.1435 0.6785 0.4910 0.0728 1.0000 Uiso R . . . . . H121 H 0.0577 0.5838 0.3876 0.0613 1.0000 Uiso R . . . . . H123 H 0.1200 0.5450 0.4399 0.0617 1.0000 Uiso R . . . . . H122 H 0.1093 0.5347 0.3646 0.0623 1.0000 Uiso R . . . . . H131 H 0.2277 0.5794 0.5026 0.0441 1.0000 Uiso R . . . . . H141 H 0.3409 0.5604 0.5346 0.0532 1.0000 Uiso R . . . . . H151 H 0.4009 0.6028 0.4685 0.0500 1.0000 Uiso R . . . . . H171 H 0.3361 0.6731 0.3064 0.0454 1.0000 Uiso R . . . . . H182 H 0.4064 0.7831 0.3439 0.0752 1.0000 Uiso R . . . . . H183 H 0.4037 0.7685 0.4142 0.0748 1.0000 Uiso R . . . . . H181 H 0.3392 0.7938 0.3578 0.0744 1.0000 Uiso R . . . . . H191 H 0.4490 0.6474 0.3294 0.0879 1.0000 Uiso R . . . . . H193 H 0.4586 0.6359 0.4045 0.0874 1.0000 Uiso R . . . . . H192 H 0.4184 0.5743 0.3535 0.0873 1.0000 Uiso R . . . . . H202 H 0.2435 0.7925 0.3931 0.0530 1.0000 Uiso R . . . . . H201 H 0.2209 0.8634 0.3427 0.0535 1.0000 Uiso R . . . . . H203 H 0.1681 0.8108 0.3582 0.0530 1.0000 Uiso R . . . . . H213 H 0.2014 0.8705 0.1399 0.0500 1.0000 Uiso R . . . . . H211 H 0.2093 0.8034 0.0928 0.0504 1.0000 Uiso R . . . . . H212 H 0.1415 0.8253 0.0978 0.0502 1.0000 Uiso R . . . . . H241 H 0.1283 0.6131 -0.0473 0.0397 1.0000 Uiso R . . . . . H251 H 0.2331 0.5837 -0.0492 0.0462 1.0000 Uiso R . . . . . H261 H 0.3239 0.6051 0.0421 0.0421 1.0000 Uiso R . . . . . H281 H 0.3231 0.6573 0.2003 0.0381 1.0000 Uiso R . . . . . H292 H 0.4278 0.6098 0.2082 0.0794 1.0000 Uiso R . . . . . H291 H 0.4106 0.6081 0.1315 0.0800 1.0000 Uiso R . . . . . H293 H 0.3761 0.5484 0.1659 0.0799 1.0000 Uiso R . . . . . H303 H 0.3991 0.7568 0.1926 0.0820 1.0000 Uiso R . . . . . H301 H 0.3260 0.7830 0.1580 0.0818 1.0000 Uiso R . . . . . H302 H 0.3691 0.7540 0.1158 0.0820 1.0000 Uiso R . . . . . H311 H 0.0839 0.6896 0.0869 0.0385 1.0000 Uiso R . . . . . H321 H -0.0072 0.6203 0.0179 0.0607 1.0000 Uiso R . . . . . H323 H 0.0374 0.5800 -0.0185 0.0608 1.0000 Uiso R . . . . . H322 H 0.0479 0.5589 0.0560 0.0608 1.0000 Uiso R . . . . . H332 H 0.0175 0.7583 -0.0006 0.0674 1.0000 Uiso R . . . . . H331 H 0.0897 0.7814 0.0014 0.0676 1.0000 Uiso R . . . . . H333 H 0.0486 0.7191 -0.0495 0.0679 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 Ga1 0.02446(12) 0.02033(12) 0.01948(12) -0.00066(9) 0.00591(9) -0.00034(9) Cl2 0.0294(3) 0.0271(3) 0.0417(3) 0.0004(2) 0.0087(2) 0.0048(2) N3 0.0248(9) 0.0223(9) 0.0230(9) -0.0001(7) 0.0085(7) -0.0018(7) C4 0.0249(10) 0.0234(11) 0.0259(10) 0.0015(8) 0.0062(8) -0.0014(8) C5 0.0341(12) 0.0226(10) 0.0305(12) -0.0021(9) 0.0107(10) 0.0015(9) C6 0.0277(11) 0.0253(11) 0.0276(11) -0.0060(9) 0.0105(9) -0.0031(8) N7 0.0258(9) 0.0257(9) 0.0187(8) -0.0012(7) 0.0058(7) -0.0027(7) C8 0.0298(11) 0.0270(11) 0.0192(10) -0.0048(8) 0.0046(8) -0.0020(9) C9 0.0348(12) 0.0282(11) 0.0228(11) -0.0029(9) 0.0078(9) -0.0038(9) C10 0.0361(13) 0.0387(13) 0.0285(12) -0.0008(10) 0.0139(10) 0.0002(10) C11 0.0612(19) 0.0449(16) 0.0551(18) -0.0109(14) 0.0363(16) -0.0037(14) C12 0.0347(13) 0.0455(16) 0.0492(16) -0.0081(13) 0.0189(12) -0.0062(12) C13 0.0471(15) 0.0395(14) 0.0237(11) 0.0015(10) 0.0078(10) -0.0078(11) C14 0.0489(16) 0.0477(16) 0.0273(12) 0.0046(11) -0.0034(11) 0.0001(13) C15 0.0355(14) 0.0479(16) 0.0344(14) -0.0015(12) -0.0023(11) 0.0023(12) C16 0.0293(12) 0.0377(13) 0.0263(11) -0.0065(10) 0.0026(9) -0.0019(10) C17 0.0265(12) 0.0558(17) 0.0327(13) -0.0117(12) 0.0067(10) -0.0090(11) C18 0.0407(15) 0.0566(19) 0.0567(18) -0.0094(15) 0.0176(14) -0.0175(14) C19 0.0341(15) 0.085(3) 0.059(2) -0.0261(19) 0.0134(14) -0.0018(15) C20 0.0510(15) 0.0286(12) 0.0311(12) -0.0092(10) 0.0149(11) -0.0045(11) C21 0.0426(14) 0.0273(12) 0.0310(12) 0.0048(10) 0.0082(10) -0.0030(10) C22 0.0285(11) 0.0250(11) 0.0199(10) 0.0014(8) 0.0078(8) -0.0009(8) C23 0.0347(12) 0.0283(11) 0.0218(10) 0.0020(9) 0.0085(9) -0.0027(9) C24 0.0439(14) 0.0369(13) 0.0230(11) 0.0004(10) 0.0103(10) -0.0071(11) C25 0.0521(16) 0.0421(14) 0.0269(12) -0.0041(11) 0.0193(11) -0.0042(12) C26 0.0405(14) 0.0414(14) 0.0335(13) 0.0012(11) 0.0207(11) 0.0024(11) C27 0.0306(12) 0.0307(12) 0.0286(11) 0.0021(9) 0.0126(9) -0.0004(9) C28 0.0272(11) 0.0411(14) 0.0326(12) 0.0000(10) 0.0133(10) 0.0000(10) C29 0.0376(15) 0.075(2) 0.0492(17) 0.0010(16) 0.0154(13) 0.0167(15) C30 0.0447(17) 0.0556(19) 0.059(2) 0.0042(15) 0.0069(14) -0.0195(14) C31 0.0285(11) 0.0426(14) 0.0246(11) 0.0018(10) 0.0046(9) -0.0027(10) C32 0.0338(13) 0.0531(17) 0.0329(13) 0.0027(12) 0.0053(10) -0.0096(12) C33 0.0389(14) 0.0492(17) 0.0410(15) 0.0080(13) 0.0011(12) 0.0027(12) O34 0.0602(13) 0.0398(11) 0.0390(10) -0.0064(9) 0.0235(10) 0.0026(9) C35 0.0363(13) 0.0256(11) 0.0315(12) -0.0007(9) 0.0074(10) -0.0025(9) O36 0.0458(11) 0.0346(10) 0.0665(14) -0.0008(10) 0.0216(10) 0.0079(9) C37 0.0302(11) 0.0306(12) 0.0336(12) -0.0020(10) 0.0105(10) -0.0045(9) O38 0.0594(13) 0.0509(13) 0.0415(11) 0.0203(10) 0.0128(10) 0.0148(10) C39 0.0362(13) 0.0299(12) 0.0370(13) 0.0019(10) 0.0117(10) -0.0010(10) O40 0.0376(11) 0.0455(12) 0.0735(15) -0.0077(11) 0.0140(10) -0.0160(9) C41 0.0372(14) 0.0320(13) 0.0395(14) -0.0006(11) 0.0116(11) 0.0014(10) Co42 0.02747(16) 0.02246(15) 0.02371(15) 0.00031(11) 0.00670(12) -0.00187(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.11455(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 Ga1 . Cl2 . 2.2135(6) yes Ga1 . N3 . 1.9547(18) yes Ga1 . N7 . 1.9534(18) yes Ga1 . Co42 . 2.4255(4) yes N3 . C4 . 1.339(3) yes N3 . C22 . 1.450(3) yes C4 . C5 . 1.400(3) yes C4 . C21 . 1.502(3) yes C5 . C6 . 1.394(3) yes C5 . H51 . 0.938 no C6 . N7 . 1.341(3) yes C6 . C20 . 1.509(3) yes N7 . C8 . 1.453(3) yes C8 . C9 . 1.409(3) yes C8 . C16 . 1.405(3) yes C9 . C10 . 1.519(4) yes C9 . C13 . 1.398(3) yes C10 . C11 . 1.538(4) yes C10 . C12 . 1.530(4) yes C10 . H101 . 0.986 no C11 . H112 . 0.958 no C11 . H113 . 0.970 no C11 . H111 . 0.974 no C12 . H121 . 0.968 no C12 . H123 . 0.978 no C12 . H122 . 0.966 no C13 . C14 . 1.383(4) yes C13 . H131 . 0.947 no C14 . C15 . 1.376(4) yes C14 . H141 . 0.942 no C15 . C16 . 1.397(4) yes C15 . H151 . 0.948 no C16 . C17 . 1.524(4) yes C17 . C18 . 1.534(4) yes C17 . C19 . 1.530(4) yes C17 . H171 . 0.985 no C18 . H182 . 0.950 no C18 . H183 . 0.954 no C18 . H181 . 0.973 no C19 . H191 . 0.970 no C19 . H193 . 0.979 no C19 . H192 . 0.960 no C20 . H202 . 0.962 no C20 . H201 . 0.957 no C20 . H203 . 0.975 no C21 . H213 . 0.946 no C21 . H211 . 0.955 no C21 . H212 . 0.938 no C22 . C23 . 1.416(3) yes C22 . C27 . 1.412(3) yes C23 . C24 . 1.396(3) yes C23 . C31 . 1.523(3) yes C24 . C25 . 1.372(4) yes C24 . H241 . 0.954 no C25 . C26 . 1.382(4) yes C25 . H251 . 0.943 no C26 . C27 . 1.395(3) yes C26 . H261 . 0.942 no C27 . C28 . 1.522(3) yes C28 . C29 . 1.531(4) yes C28 . C30 . 1.526(4) yes C28 . H281 . 0.992 no C29 . H292 . 0.989 no C29 . H291 . 0.967 no C29 . H293 . 0.970 no C30 . H303 . 0.959 no C30 . H301 . 0.964 no C30 . H302 . 0.968 no C31 . C32 . 1.539(4) yes C31 . C33 . 1.539(4) yes C31 . H311 . 0.983 no C32 . H321 . 0.962 no C32 . H323 . 0.973 no C32 . H322 . 0.979 no C33 . H332 . 0.972 no C33 . H331 . 0.965 no C33 . H333 . 0.963 no O34 . C35 . 1.140(3) yes C35 . Co42 . 1.795(3) yes O36 . C37 . 1.146(3) yes C37 . Co42 . 1.775(3) yes O38 . C39 . 1.137(3) yes C39 . Co42 . 1.786(3) yes O40 . C41 . 1.135(3) yes C41 . Co42 . 1.804(3) yes 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 Cl2 . Ga1 . N3 . 112.67(6) yes Cl2 . Ga1 . N7 . 108.92(6) yes N3 . Ga1 . N7 . 97.68(8) yes Cl2 . Ga1 . Co42 . 103.41(2) yes N3 . Ga1 . Co42 . 114.31(6) yes N7 . Ga1 . Co42 . 120.12(6) yes Ga1 . N3 . C4 . 120.25(15) yes Ga1 . N3 . C22 . 119.94(14) yes C4 . N3 . C22 . 119.80(19) yes N3 . C4 . C5 . 124.0(2) yes N3 . C4 . C21 . 120.3(2) yes C5 . C4 . C21 . 115.7(2) yes C4 . C5 . C6 . 129.3(2) yes C4 . C5 . H51 . 115.6 no C6 . C5 . H51 . 115.0 no C5 . C6 . N7 . 123.7(2) yes C5 . C6 . C20 . 116.1(2) yes N7 . C6 . C20 . 120.2(2) yes Ga1 . N7 . C6 . 120.47(15) yes Ga1 . N7 . C8 . 119.32(14) yes C6 . N7 . C8 . 119.98(19) yes N7 . C8 . C9 . 120.9(2) yes N7 . C8 . C16 . 117.4(2) yes C9 . C8 . C16 . 121.7(2) yes C8 . C9 . C10 . 123.8(2) yes C8 . C9 . C13 . 117.6(2) yes C10 . C9 . C13 . 118.5(2) yes C9 . C10 . C11 . 110.3(2) yes C9 . C10 . C12 . 113.0(2) yes C11 . C10 . C12 . 108.4(2) yes C9 . C10 . H101 . 108.8 no C11 . C10 . H101 . 108.0 no C12 . C10 . H101 . 108.3 no C10 . C11 . H112 . 109.0 no C10 . C11 . H113 . 110.9 no H112 . C11 . H113 . 109.0 no C10 . C11 . H111 . 110.4 no H112 . C11 . H111 . 108.6 no H113 . C11 . H111 . 108.9 no C10 . C12 . H121 . 110.7 no C10 . C12 . H123 . 109.3 no H121 . C12 . H123 . 109.2 no C10 . C12 . H122 . 109.3 no H121 . C12 . H122 . 110.0 no H123 . C12 . H122 . 108.3 no C9 . C13 . C14 . 121.2(3) yes C9 . C13 . H131 . 119.1 no C14 . C13 . H131 . 119.7 no C13 . C14 . C15 . 120.2(3) yes C13 . C14 . H141 . 119.8 no C15 . C14 . H141 . 120.0 no C14 . C15 . C16 . 121.2(3) yes C14 . C15 . H151 . 119.8 no C16 . C15 . H151 . 118.9 no C8 . C16 . C15 . 117.9(2) yes C8 . C16 . C17 . 121.6(2) yes C15 . C16 . C17 . 120.4(2) yes C16 . C17 . C18 . 110.8(2) yes C16 . C17 . C19 . 113.7(3) yes C18 . C17 . C19 . 109.8(2) yes C16 . C17 . H171 . 106.9 no C18 . C17 . H171 . 107.4 no C19 . C17 . H171 . 108.0 no C17 . C18 . H182 . 109.7 no C17 . C18 . H183 . 108.7 no H182 . C18 . H183 . 109.6 no C17 . C18 . H181 . 109.1 no H182 . C18 . H181 . 109.7 no H183 . C18 . H181 . 110.0 no C17 . C19 . H191 . 112.0 no C17 . C19 . H193 . 111.0 no H191 . C19 . H193 . 107.9 no C17 . C19 . H192 . 110.9 no H191 . C19 . H192 . 108.0 no H193 . C19 . H192 . 106.8 no C6 . C20 . H202 . 111.6 no C6 . C20 . H201 . 109.4 no H202 . C20 . H201 . 111.5 no C6 . C20 . H203 . 107.5 no H202 . C20 . H203 . 109.2 no H201 . C20 . H203 . 107.5 no C4 . C21 . H213 . 109.8 no C4 . C21 . H211 . 110.9 no H213 . C21 . H211 . 111.1 no C4 . C21 . H212 . 109.0 no H213 . C21 . H212 . 107.4 no H211 . C21 . H212 . 108.5 no N3 . C22 . C23 . 120.7(2) yes N3 . C22 . C27 . 117.97(19) yes C23 . C22 . C27 . 121.4(2) yes C22 . C23 . C24 . 117.5(2) yes C22 . C23 . C31 . 124.5(2) yes C24 . C23 . C31 . 117.9(2) yes C23 . C24 . C25 . 121.8(2) yes C23 . C24 . H241 . 119.3 no C25 . C24 . H241 . 118.9 no C24 . C25 . C26 . 120.1(2) yes C24 . C25 . H251 . 120.5 no C26 . C25 . H251 . 119.5 no C25 . C26 . C27 . 121.4(2) yes C25 . C26 . H261 . 119.5 no C27 . C26 . H261 . 119.1 no C22 . C27 . C26 . 117.8(2) yes C22 . C27 . C28 . 122.4(2) yes C26 . C27 . C28 . 119.7(2) yes C27 . C28 . C29 . 112.6(2) yes C27 . C28 . C30 . 110.9(2) yes C29 . C28 . C30 . 110.7(3) yes C27 . C28 . H281 . 106.7 no C29 . C28 . H281 . 107.7 no C30 . C28 . H281 . 108.0 no C28 . C29 . H292 . 110.8 no C28 . C29 . H291 . 112.1 no H292 . C29 . H291 . 107.3 no C28 . C29 . H293 . 111.0 no H292 . C29 . H293 . 107.2 no H291 . C29 . H293 . 108.3 no C28 . C30 . H303 . 110.5 no C28 . C30 . H301 . 109.3 no H303 . C30 . H301 . 109.1 no C28 . C30 . H302 . 110.0 no H303 . C30 . H302 . 109.4 no H301 . C30 . H302 . 108.5 no C23 . C31 . C32 . 112.6(2) yes C23 . C31 . C33 . 111.0(2) yes C32 . C31 . C33 . 107.8(2) yes C23 . C31 . H311 . 109.8 no C32 . C31 . H311 . 107.7 no C33 . C31 . H311 . 107.7 no C31 . C32 . H321 . 108.1 no C31 . C32 . H323 . 109.8 no H321 . C32 . H323 . 108.9 no C31 . C32 . H322 . 111.1 no H321 . C32 . H322 . 109.8 no H323 . C32 . H322 . 109.1 no C31 . C33 . H332 . 108.6 no C31 . C33 . H331 . 111.4 no H332 . C33 . H331 . 109.7 no C31 . C33 . H333 . 110.0 no H332 . C33 . H333 . 108.0 no H331 . C33 . H333 . 109.1 no O34 . C35 . Co42 . 175.2(2) yes O36 . C37 . Co42 . 178.9(2) yes O38 . C39 . Co42 . 176.3(2) yes O40 . C41 . Co42 . 178.1(3) yes Ga1 . Co42 . C41 . 178.24(9) yes Ga1 . Co42 . C35 . 82.69(8) yes C41 . Co42 . C35 . 97.51(12) yes Ga1 . Co42 . C39 . 83.27(8) yes C41 . Co42 . C39 . 98.30(12) yes C35 . Co42 . C39 . 109.34(12) yes Ga1 . Co42 . C37 . 78.92(8) yes C41 . Co42 . C37 . 99.55(11) yes C35 . Co42 . C37 . 123.66(11) yes C39 . Co42 . C37 . 120.50(12) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C25 . H251 . O38 5_564 146.83(8) 0.943 2.560 3.389(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 07/05/13 at 12:54:58 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 113,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 123,X'S) H ( 122,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 ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 182,X'S) H ( 183,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 202,X'S) H ( 201,X'S) H ( 203,X'S) RIDE C ( 21,X'S) H ( 213,X'S) H ( 211,X'S) H ( 212,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 292,X'S) H ( 291,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 303,X'S) H ( 301,X'S) H ( 302,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 323,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 332,X'S) H ( 331,X'S) H ( 333,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 07/05/13 at 12:54:58 # #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 0.009 518 34 ' ' 2 0.500 0.500 0.203 518 34 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 944065' ####################################################################### # # 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_077jart13 _audit_creation_date 13-07-01 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '077jart13 in P -1' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 8.83270(10) _cell_length_b 18.3781(2) _cell_length_c 20.6752(2) _cell_angle_alpha 90.0077(7) _cell_angle_beta 90.0065(7) _cell_angle_gamma 85.7423(5) _cell_volume 3346.91(6) _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' 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' 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' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C37 H44 Ga1 Mn1 N2 O2 # Dc = 1.34 Fooo = 1424.00 Mu = 12.16 M = 1346.83 # Found Formula = C37 H48 Ga1 Mn1 N2 O2 # Dc = 1.34 FOOO = 1424.00 Mu = 12.17 M = 1354.90 _chemical_formula_sum 'C37 H48 Ga1 Mn1 N2 O2' _chemical_formula_moiety 'C37 H48 Ga1 Mn1 N2 O2' _chemical_compound_source . _chemical_formula_weight 677.45 _cell_measurement_reflns_used 13419 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.120 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_max 0.210 _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.217 # Sheldrick geometric approximatio 0.80 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.86 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 89054 _reflns_number_total 15175 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 25602 # Number of reflections with Friedels Law is 15175 # Theoretical number of reflections is about 15383 _diffrn_reflns_theta_min 5.137 _diffrn_reflns_theta_max 27.503 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.028 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -23 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 1.88 _oxford_diffrn_Wilson_scale 9.67 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.74 _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>0.0\s(I) _refine_ls_number_reflns 15175 _refine_ls_number_restraints 26 _refine_ls_number_parameters 795 _oxford_refine_ls_R_factor_ref 0.0560 _refine_ls_wR_factor_ref 0.0919 _refine_ls_goodness_of_fit_ref 0.9366 _refine_ls_shift/su_max 0.0009050 _refine_ls_shift/su_mean 0.0000419 # The values computed with all filters except I/sigma _oxford_reflns_number_all 15175 _refine_ls_R_factor_all 0.0560 _refine_ls_wR_factor_all 0.0919 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11421 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_gt 0.0749 # 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, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 19.9 28.6 13.9 3.51 ; # 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 Ga1 Ga 0.8317(3) 0.63698(8) 0.25115(3) 0.0185 0.914(14) Uani . . P 2 1 . Mn2 Mn 0.66391(4) 0.73897(2) 0.240990(16) 0.0248 1.0000 Uani D . . . . . C3 C 0.8149(3) 0.79579(15) 0.24817(13) 0.0340 1.0000 Uani . . . . . . O4 O 0.9088(3) 0.83767(12) 0.25144(12) 0.0511 1.0000 Uani . . . . . . C5 C 0.5040(3) 0.68509(16) 0.18194(13) 0.0350 1.0000 Uani . . . . . . C10 C 0.6066(3) 0.71990(15) 0.14183(12) 0.0341 1.0000 Uani . . . . . . C12 C 0.5894(4) 0.79555(15) 0.15559(12) 0.0362 1.0000 Uani . . . . . . C13 C 0.4773(3) 0.80700(15) 0.20434(13) 0.0358 1.0000 Uani . . . . . . C9 C 0.4227(3) 0.73883(17) 0.22031(13) 0.0369 1.0000 Uani . . . . . . C4 C 0.2954(4) 0.7258(2) 0.26593(17) 0.0533 1.0000 Uani . . . . . . C11 C 0.6249(3) 0.74466(15) 0.32486(13) 0.0351 1.0000 Uani . . . . . . O12 O 0.5884(3) 0.75299(14) 0.37863(9) 0.0536 1.0000 Uani . . . . . . N14 N 0.9372(2) 0.56938(10) 0.18802(8) 0.0183 1.0000 Uani D . . . . . C15 C 0.8841(3) 0.57736(12) 0.12229(10) 0.0197 1.0000 Uani . . . . . . C16 C 0.7506(3) 0.54418(13) 0.10507(11) 0.0233 1.0000 Uani . . . . . . C19 C 0.6935(3) 0.55687(14) 0.04273(12) 0.0309 1.0000 Uani . . . . . . C20 C 0.7646(3) 0.60082(15) -0.00034(11) 0.0323 1.0000 Uani . . . . . . C21 C 0.8959(3) 0.63192(15) 0.01702(11) 0.0304 1.0000 Uani . . . . . . C24 C 0.9598(3) 0.62045(13) 0.07830(10) 0.0234 1.0000 Uani . . . . . . C27 C 1.1050(3) 0.65545(13) 0.09559(11) 0.0261 1.0000 Uani . . . . . . C30 C 1.0768(4) 0.73823(15) 0.10349(15) 0.0392 1.0000 Uani . . . . . . C32 C 1.2296(3) 0.63837(16) 0.04476(13) 0.0357 1.0000 Uani . . . . . . C33 C 0.6698(3) 0.49762(14) 0.15308(12) 0.0278 1.0000 Uani . . . . . . C39 C 0.5057(3) 0.48602(18) 0.13465(16) 0.0422 1.0000 Uani . . . . . . C44 C 0.7531(3) 0.42222(16) 0.16418(16) 0.0402 1.0000 Uani . . . . . . C26 C 1.0467(3) 0.51734(12) 0.20150(11) 0.0204 1.0000 Uani . . . . . . C45 C 1.1189(3) 0.47242(14) 0.14714(11) 0.0270 1.0000 Uani . . . . . . C28 C 1.0976(3) 0.50117(13) 0.26406(11) 0.0231 1.0000 Uani . . . . . . C29 C 1.0339(3) 0.52785(12) 0.32210(11) 0.0213 1.0000 Uani . . . . . . N30 N 0.9240(2) 0.58172(10) 0.32502(8) 0.0197 1.0000 Uani D . . . . . C46 C 0.8503(3) 0.59702(13) 0.38652(10) 0.0220 1.0000 Uani . . . . . . C47 C 0.7174(3) 0.56307(14) 0.40024(11) 0.0268 1.0000 Uani . . . . . . C34 C 0.6446(3) 0.57950(16) 0.45916(12) 0.0355 1.0000 Uani . . . . . . C35 C 0.7021(4) 0.62805(17) 0.50214(12) 0.0385 1.0000 Uani . . . . . . C36 C 0.8332(4) 0.66116(16) 0.48743(12) 0.0359 1.0000 Uani . . . . . . C37 C 0.9107(3) 0.64661(14) 0.42970(11) 0.0266 1.0000 Uani . . . . . . C38 C 1.0543(3) 0.68410(16) 0.41533(13) 0.0356 1.0000 Uani . . . . . . C52 C 1.0200(4) 0.76659(17) 0.40958(16) 0.0467 1.0000 Uani . . . . . . C40 C 1.1773(4) 0.6679(2) 0.46713(18) 0.0538 1.0000 Uani . . . . . . C41 C 0.6498(3) 0.51017(16) 0.35344(12) 0.0341 1.0000 Uani . . . . . . C42 C 0.4930(4) 0.5384(2) 0.33093(19) 0.0577 1.0000 Uani . . . . . . C43 C 0.6483(5) 0.43354(18) 0.38122(17) 0.0535 1.0000 Uani . . . . . . C53 C 1.0892(3) 0.49047(14) 0.38357(12) 0.0315 1.0000 Uani . . . . . . Ga45 Ga 0.3318(3) 0.13704(7) 0.24884(3) 0.0188 0.925(11) Uani . . P 1 1 . Mn46 Mn 0.16386(4) 0.239002(19) 0.259034(16) 0.0246 1.0000 Uani D . . . . . C54 C 0.0038(3) 0.18512(15) 0.31809(13) 0.0342 1.0000 Uani . . . . . . C48 C 0.1069(3) 0.22008(15) 0.35822(12) 0.0343 1.0000 Uani . . . . . . C49 C 0.0894(4) 0.29534(15) 0.34431(12) 0.0361 1.0000 Uani . . . . . . C50 C -0.0231(3) 0.30729(15) 0.29558(12) 0.0358 1.0000 Uani . . . . . . C56 C -0.0779(3) 0.23874(16) 0.27981(13) 0.0366 1.0000 Uani . . . . . . C57 C -0.2049(4) 0.2257(2) 0.23423(17) 0.0531 1.0000 Uani . . . . . . C6 C 0.3155(3) 0.29597(15) 0.25177(13) 0.0337 1.0000 Uani . . . . . . O54 O 0.4091(3) 0.33778(12) 0.24850(12) 0.0508 1.0000 Uani . . . . . . C55 C 0.1253(3) 0.24441(15) 0.17521(13) 0.0344 1.0000 Uani . . . . . . O56 O 0.0886(3) 0.25314(14) 0.12139(9) 0.0540 1.0000 Uani . . . . . . N58 N 0.4371(2) 0.06946(10) 0.31198(8) 0.0177 1.0000 Uani D . . . . . C59 C 0.3838(3) 0.07720(12) 0.37791(10) 0.0206 1.0000 Uani . . . . . . C60 C 0.2503(3) 0.04414(13) 0.39492(11) 0.0228 1.0000 Uani . . . . . . C64 C 0.1934(3) 0.05677(14) 0.45715(12) 0.0301 1.0000 Uani . . . . . . C61 C 0.2650(3) 0.10075(15) 0.50050(11) 0.0323 1.0000 Uani . . . . . . C62 C 0.3953(3) 0.13200(15) 0.48300(11) 0.0297 1.0000 Uani . . . . . . C63 C 0.4597(3) 0.12047(13) 0.42162(10) 0.0232 1.0000 Uani . . . . . . C65 C 0.6051(3) 0.15525(14) 0.40433(11) 0.0268 1.0000 Uani . . . . . . C66 C 0.5766(4) 0.23791(15) 0.39664(14) 0.0382 1.0000 Uani . . . . . . C71 C 0.7293(3) 0.13819(16) 0.45518(13) 0.0358 1.0000 Uani . . . . . . C74 C 0.1697(3) -0.00251(14) 0.34687(12) 0.0280 1.0000 Uani . . . . . . C68 C 0.0061(3) -0.01360(17) 0.36549(15) 0.0404 1.0000 Uani . . . . . . C69 C 0.2525(3) -0.07771(16) 0.33541(16) 0.0400 1.0000 Uani . . . . . . C70 C 0.5466(3) 0.01729(12) 0.29864(11) 0.0208 1.0000 Uani . . . . . . C75 C 0.6190(3) -0.02751(14) 0.35292(11) 0.0271 1.0000 Uani . . . . . . C72 C 0.5974(3) 0.00085(13) 0.23577(11) 0.0225 1.0000 Uani . . . . . . C76 C 0.5339(3) 0.02756(12) 0.17798(10) 0.0212 1.0000 Uani . . . . . . N82 N 0.4243(2) 0.08172(10) 0.17488(8) 0.0196 1.0000 Uani D . . . . . C87 C 0.3507(3) 0.09720(13) 0.11360(10) 0.0220 1.0000 Uani . . . . . . C88 C 0.2170(3) 0.06316(14) 0.09975(11) 0.0281 1.0000 Uani . . . . . . C89 C 0.1446(3) 0.07968(17) 0.04090(12) 0.0362 1.0000 Uani . . . . . . C90 C 0.2023(3) 0.12806(16) -0.00221(12) 0.0375 1.0000 Uani . . . . . . C91 C 0.3330(3) 0.16125(15) 0.01254(12) 0.0346 1.0000 Uani . . . . . . C92 C 0.4107(3) 0.14650(14) 0.07030(11) 0.0269 1.0000 Uani . . . . . . C81 C 0.5545(3) 0.18407(16) 0.08464(13) 0.0350 1.0000 Uani . . . . . . C7 C 0.6775(4) 0.1679(2) 0.03284(18) 0.0547 1.0000 Uani . . . . . . C83 C 0.5195(4) 0.26652(17) 0.09047(16) 0.0476 1.0000 Uani . . . . . . C93 C 0.1496(3) 0.01017(16) 0.14653(12) 0.0337 1.0000 Uani . . . . . . C94 C -0.0074(4) 0.0384(2) 0.16877(19) 0.0577 1.0000 Uani . . . . . . C86 C 0.1485(5) -0.06658(18) 0.11877(17) 0.0547 1.0000 Uani . . . . . . C95 C 0.5891(3) -0.00982(14) 0.11648(12) 0.0310 1.0000 Uani . . . . . . Ga2 Ga 0.882(4) 0.6456(6) 0.2515(2) 0.0184 0.086(14) Uani D . P 2 2 . Ga3 Ga 0.384(4) 0.1459(5) 0.2483(2) 0.0164 0.075(11) Uani D . P 1 2 . H51 H 0.4879 0.6323 0.1822 0.0434 1.0000 Uiso R . . . . . H101 H 0.6748 0.6958 0.1097 0.0415 1.0000 Uiso R . . . . . H121 H 0.6451 0.8331 0.1341 0.0446 1.0000 Uiso R . . . . . H131 H 0.4426 0.8543 0.2229 0.0433 1.0000 Uiso R . . . . . H42 H 0.3109 0.7520 0.3055 0.0808 1.0000 Uiso R . . . . . H41 H 0.2940 0.6738 0.2758 0.0812 1.0000 Uiso R . . . . . H43 H 0.1995 0.7437 0.2469 0.0811 1.0000 Uiso R . . . . . H191 H 0.6047 0.5348 0.0293 0.0374 1.0000 Uiso R . . . . . H201 H 0.7236 0.6087 -0.0420 0.0381 1.0000 Uiso R . . . . . H211 H 0.9436 0.6621 -0.0126 0.0370 1.0000 Uiso R . . . . . H271 H 1.1430 0.6354 0.1373 0.0305 1.0000 Uiso R . . . . . H301 H 1.1710 0.7586 0.1158 0.0590 1.0000 Uiso R . . . . . H303 H 1.0410 0.7593 0.0625 0.0587 1.0000 Uiso R . . . . . H302 H 1.0018 0.7487 0.1368 0.0589 1.0000 Uiso R . . . . . H321 H 1.3231 0.6567 0.0604 0.0552 1.0000 Uiso R . . . . . H323 H 1.1993 0.6628 0.0050 0.0547 1.0000 Uiso R . . . . . H322 H 1.2433 0.5864 0.0384 0.0550 1.0000 Uiso R . . . . . H331 H 0.6671 0.5243 0.1953 0.0334 1.0000 Uiso R . . . . . H393 H 0.4554 0.4630 0.1703 0.0651 1.0000 Uiso R . . . . . H392 H 0.4500 0.5321 0.1243 0.0645 1.0000 Uiso R . . . . . H391 H 0.5048 0.4546 0.0972 0.0644 1.0000 Uiso R . . . . . H443 H 0.6913 0.3931 0.1906 0.0610 1.0000 Uiso R . . . . . H442 H 0.8497 0.4277 0.1857 0.0608 1.0000 Uiso R . . . . . H441 H 0.7696 0.3994 0.1226 0.0610 1.0000 Uiso R . . . . . H453 H 1.1789 0.4309 0.1644 0.0417 1.0000 Uiso R . . . . . H452 H 1.1847 0.5014 0.1227 0.0424 1.0000 Uiso R . . . . . H451 H 1.0417 0.4556 0.1192 0.0425 1.0000 Uiso R . . . . . H281 H 1.1822 0.4669 0.2680 0.0281 1.0000 Uiso R . . . . . H341 H 0.5548 0.5571 0.4692 0.0432 1.0000 Uiso R . . . . . H351 H 0.6520 0.6385 0.5415 0.0463 1.0000 Uiso R . . . . . H361 H 0.8717 0.6941 0.5172 0.0432 1.0000 Uiso R . . . . . H381 H 1.0963 0.6654 0.3739 0.0430 1.0000 Uiso R . . . . . H521 H 1.1098 0.7890 0.3961 0.0699 1.0000 Uiso R . . . . . H523 H 0.9859 0.7859 0.4515 0.0696 1.0000 Uiso R . . . . . H522 H 0.9402 0.7765 0.3778 0.0699 1.0000 Uiso R . . . . . H401 H 1.2691 0.6886 0.4533 0.0800 1.0000 Uiso R . . . . . H403 H 1.1420 0.6908 0.5073 0.0799 1.0000 Uiso R . . . . . H402 H 1.1949 0.6156 0.4723 0.0799 1.0000 Uiso R . . . . . H411 H 0.7154 0.5065 0.3144 0.0409 1.0000 Uiso R . . . . . H423 H 0.4540 0.5041 0.3010 0.0877 1.0000 Uiso R . . . . . H422 H 0.4980 0.5862 0.3107 0.0884 1.0000 Uiso R . . . . . H421 H 0.4281 0.5425 0.3687 0.0870 1.0000 Uiso R . . . . . H433 H 0.6104 0.4018 0.3487 0.0820 1.0000 Uiso R . . . . . H432 H 0.7509 0.4164 0.3937 0.0820 1.0000 Uiso R . . . . . H431 H 0.5819 0.4349 0.4189 0.0821 1.0000 Uiso R . . . . . H533 H 1.1035 0.5265 0.4161 0.0483 1.0000 Uiso R . . . . . H532 H 1.1835 0.4612 0.3759 0.0477 1.0000 Uiso R . . . . . H531 H 1.0124 0.4594 0.3979 0.0488 1.0000 Uiso R . . . . . H541 H -0.0096 0.1320 0.3170 0.0424 1.0000 Uiso R . . . . . H481 H 0.1757 0.1964 0.3905 0.0421 1.0000 Uiso R . . . . . H491 H 0.1447 0.3330 0.3656 0.0443 1.0000 Uiso R . . . . . H501 H -0.0591 0.3548 0.2771 0.0429 1.0000 Uiso R . . . . . H572 H -0.1882 0.2506 0.1939 0.0805 1.0000 Uiso R . . . . . H571 H -0.3011 0.2453 0.2521 0.0811 1.0000 Uiso R . . . . . H573 H -0.2096 0.1736 0.2256 0.0811 1.0000 Uiso R . . . . . H641 H 0.1042 0.0350 0.4705 0.0364 1.0000 Uiso R . . . . . H611 H 0.2232 0.1089 0.5424 0.0390 1.0000 Uiso R . . . . . H621 H 0.4439 0.1625 0.5125 0.0364 1.0000 Uiso R . . . . . H651 H 0.6434 0.1351 0.3624 0.0313 1.0000 Uiso R . . . . . H661 H 0.6701 0.2591 0.3846 0.0568 1.0000 Uiso R . . . . . H663 H 0.5399 0.2594 0.4373 0.0569 1.0000 Uiso R . . . . . H662 H 0.5013 0.2486 0.3636 0.0571 1.0000 Uiso R . . . . . H711 H 0.8219 0.1571 0.4406 0.0547 1.0000 Uiso R . . . . . H713 H 0.6987 0.1612 0.4952 0.0551 1.0000 Uiso R . . . . . H712 H 0.7445 0.0862 0.4612 0.0546 1.0000 Uiso R . . . . . H741 H 0.1658 0.0237 0.3046 0.0336 1.0000 Uiso R . . . . . H683 H -0.0432 -0.0371 0.3299 0.0619 1.0000 Uiso R . . . . . H682 H 0.0048 -0.0447 0.4031 0.0617 1.0000 Uiso R . . . . . H681 H -0.0493 0.0331 0.3751 0.0614 1.0000 Uiso R . . . . . H693 H 0.1898 -0.1068 0.3095 0.0598 1.0000 Uiso R . . . . . H692 H 0.2696 -0.1012 0.3767 0.0599 1.0000 Uiso R . . . . . H691 H 0.3486 -0.0733 0.3136 0.0599 1.0000 Uiso R . . . . . H753 H 0.6784 -0.0684 0.3356 0.0422 1.0000 Uiso R . . . . . H752 H 0.6838 0.0019 0.3776 0.0426 1.0000 Uiso R . . . . . H751 H 0.5431 -0.0451 0.3808 0.0424 1.0000 Uiso R . . . . . H721 H 0.6828 -0.0336 0.2319 0.0277 1.0000 Uiso R . . . . . H891 H 0.0539 0.0575 0.0309 0.0442 1.0000 Uiso R . . . . . H901 H 0.1524 0.1382 -0.0417 0.0453 1.0000 Uiso R . . . . . H911 H 0.3714 0.1942 -0.0171 0.0421 1.0000 Uiso R . . . . . H811 H 0.5955 0.1659 0.1264 0.0427 1.0000 Uiso R . . . . . H71 H 0.7689 0.1893 0.0469 0.0811 1.0000 Uiso R . . . . . H73 H 0.6419 0.1902 -0.0074 0.0811 1.0000 Uiso R . . . . . H72 H 0.6960 0.1158 0.0276 0.0808 1.0000 Uiso R . . . . . H831 H 0.6099 0.2892 0.1027 0.0719 1.0000 Uiso R . . . . . H833 H 0.4428 0.2769 0.1230 0.0720 1.0000 Uiso R . . . . . H832 H 0.4834 0.2865 0.0490 0.0719 1.0000 Uiso R . . . . . H931 H 0.2147 0.0063 0.1856 0.0409 1.0000 Uiso R . . . . . H943 H -0.0461 0.0050 0.1997 0.0878 1.0000 Uiso R . . . . . H942 H -0.0031 0.0866 0.1882 0.0885 1.0000 Uiso R . . . . . H941 H -0.0727 0.0419 0.1309 0.0869 1.0000 Uiso R . . . . . H863 H 0.1092 -0.0979 0.1512 0.0828 1.0000 Uiso R . . . . . H862 H 0.2504 -0.0843 0.1068 0.0832 1.0000 Uiso R . . . . . H861 H 0.0838 -0.0653 0.0810 0.0831 1.0000 Uiso R . . . . . H953 H 0.6043 0.0259 0.0845 0.0482 1.0000 Uiso R . . . . . H952 H 0.6836 -0.0391 0.1245 0.0475 1.0000 Uiso R . . . . . H951 H 0.5123 -0.0409 0.1018 0.0485 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 Ga1 0.0221(6) 0.01787(18) 0.01549(16) 0.00001(12) -0.00046(16) -0.0004(3) Mn2 0.0332(2) 0.02156(18) 0.01856(16) -0.00089(13) -0.00066(14) 0.00542(15) C3 0.0456(16) 0.0260(13) 0.0298(12) -0.0004(10) -0.0013(11) 0.0023(12) O4 0.0594(15) 0.0374(12) 0.0582(14) -0.0039(10) -0.0020(11) -0.0154(11) C5 0.0376(15) 0.0327(14) 0.0336(13) -0.0029(11) -0.0102(11) 0.0060(11) C10 0.0434(16) 0.0366(14) 0.0200(11) -0.0030(10) -0.0040(10) 0.0112(12) C12 0.0519(17) 0.0333(14) 0.0215(11) 0.0071(10) -0.0040(11) 0.0091(12) C13 0.0438(16) 0.0319(14) 0.0288(12) 0.0005(10) -0.0043(11) 0.0156(12) C9 0.0331(14) 0.0452(16) 0.0306(13) -0.0003(11) -0.0030(11) 0.0099(12) C4 0.0387(18) 0.066(2) 0.0538(19) 0.0070(16) 0.0057(14) 0.0068(16) C11 0.0440(16) 0.0310(14) 0.0290(13) -0.0030(10) -0.0010(11) 0.0062(12) O12 0.0729(17) 0.0635(15) 0.0215(9) -0.0061(9) 0.0061(10) 0.0137(13) N14 0.0203(9) 0.0195(9) 0.0151(8) -0.0002(7) -0.0009(7) -0.0022(7) C15 0.0209(11) 0.0220(11) 0.0160(9) -0.0032(8) -0.0001(8) 0.0009(9) C16 0.0257(12) 0.0225(11) 0.0219(10) -0.0030(8) -0.0046(9) -0.0023(9) C19 0.0349(14) 0.0326(13) 0.0249(12) -0.0060(10) -0.0090(10) -0.0014(11) C20 0.0396(15) 0.0383(14) 0.0176(10) -0.0020(10) -0.0060(10) 0.0059(12) C21 0.0370(14) 0.0352(14) 0.0182(10) 0.0025(9) 0.0026(9) 0.0019(11) C24 0.0271(12) 0.0243(11) 0.0181(10) -0.0003(8) 0.0021(8) 0.0017(9) C27 0.0300(13) 0.0268(12) 0.0221(11) 0.0039(9) 0.0026(9) -0.0057(10) C30 0.0462(17) 0.0307(14) 0.0412(15) -0.0021(11) 0.0062(12) -0.0056(12) C32 0.0354(15) 0.0387(15) 0.0330(13) 0.0051(11) 0.0095(11) -0.0020(12) C33 0.0272(12) 0.0280(12) 0.0295(12) 0.0012(9) -0.0048(9) -0.0096(10) C39 0.0306(15) 0.0438(17) 0.0537(18) 0.0061(14) -0.0107(13) -0.0125(13) C44 0.0384(16) 0.0307(14) 0.0526(17) 0.0108(12) -0.0094(13) -0.0095(12) C26 0.0189(10) 0.0191(10) 0.0233(10) -0.0022(8) 0.0032(8) -0.0020(8) C45 0.0252(12) 0.0302(13) 0.0248(11) -0.0012(9) 0.0017(9) 0.0032(10) C28 0.0218(11) 0.0234(11) 0.0239(11) 0.0011(9) -0.0040(8) -0.0011(9) C29 0.0225(11) 0.0194(10) 0.0225(10) 0.0021(8) -0.0060(8) -0.0044(9) N30 0.0239(10) 0.0198(9) 0.0153(8) -0.0009(7) -0.0006(7) -0.0018(7) C46 0.0292(12) 0.0231(11) 0.0137(9) 0.0025(8) -0.0015(8) -0.0007(9) C47 0.0319(13) 0.0291(12) 0.0199(10) 0.0043(9) 0.0014(9) -0.0052(10) C34 0.0378(15) 0.0431(16) 0.0258(12) 0.0061(11) 0.0082(10) -0.0038(12) C35 0.0506(17) 0.0447(16) 0.0190(11) 0.0009(10) 0.0091(11) 0.0035(13) C36 0.0509(17) 0.0362(14) 0.0200(11) -0.0061(10) 0.0013(11) -0.0004(13) C37 0.0354(13) 0.0266(12) 0.0178(10) -0.0007(9) -0.0014(9) -0.0017(10) C38 0.0402(15) 0.0390(15) 0.0288(12) -0.0104(11) -0.0029(11) -0.0114(12) C52 0.059(2) 0.0401(17) 0.0433(16) 0.0026(13) -0.0082(14) -0.0186(15) C40 0.0456(19) 0.0485(19) 0.068(2) -0.0142(16) -0.0215(16) -0.0053(15) C41 0.0380(15) 0.0403(15) 0.0259(12) 0.0043(10) 0.0018(10) -0.0153(12) C42 0.0435(19) 0.064(2) 0.067(2) 0.0015(18) -0.0185(16) -0.0158(17) C43 0.074(3) 0.0395(17) 0.0490(18) 0.0021(14) -0.0018(17) -0.0161(17) C53 0.0397(15) 0.0292(13) 0.0243(11) 0.0041(9) -0.0066(10) 0.0055(11) Ga45 0.0227(5) 0.01797(17) 0.01560(16) 0.00034(11) 0.00018(16) 0.0000(3) Mn46 0.0327(2) 0.02122(18) 0.01879(16) 0.00106(13) 0.00024(13) 0.00541(15) C54 0.0389(15) 0.0307(13) 0.0319(13) 0.0033(10) 0.0096(11) 0.0038(11) C48 0.0434(16) 0.0380(15) 0.0192(11) 0.0042(10) 0.0030(10) 0.0124(12) C49 0.0507(17) 0.0322(14) 0.0236(12) -0.0056(10) 0.0010(11) 0.0092(12) C50 0.0446(16) 0.0328(14) 0.0270(12) 0.0005(10) 0.0035(11) 0.0179(12) C56 0.0342(15) 0.0412(15) 0.0324(13) -0.0021(11) 0.0031(11) 0.0101(12) C57 0.0356(17) 0.070(2) 0.0520(19) -0.0052(17) -0.0076(14) 0.0058(16) C6 0.0438(16) 0.0272(13) 0.0289(12) 0.0006(10) 0.0009(11) 0.0045(12) O54 0.0564(15) 0.0379(12) 0.0598(14) 0.0027(10) 0.0027(11) -0.0143(11) C55 0.0437(16) 0.0300(13) 0.0281(12) 0.0046(10) 0.0004(11) 0.0065(12) O56 0.0713(16) 0.0653(16) 0.0228(10) 0.0059(9) -0.0065(10) 0.0127(13) N58 0.0192(9) 0.0192(9) 0.0147(8) -0.0001(6) 0.0001(6) -0.0018(7) C59 0.0248(11) 0.0216(11) 0.0151(9) 0.0033(8) 0.0001(8) 0.0008(9) C60 0.0262(12) 0.0211(11) 0.0211(10) 0.0050(8) 0.0025(8) -0.0013(9) C64 0.0319(13) 0.0339(13) 0.0241(11) 0.0078(10) 0.0085(10) 0.0001(11) C61 0.0384(14) 0.0405(15) 0.0169(10) 0.0018(10) 0.0055(9) 0.0052(12) C62 0.0367(14) 0.0336(13) 0.0180(10) -0.0013(9) -0.0020(9) 0.0027(11) C63 0.0277(12) 0.0247(11) 0.0166(10) 0.0011(8) -0.0029(8) 0.0007(9) C65 0.0297(13) 0.0294(12) 0.0218(11) -0.0040(9) -0.0022(9) -0.0056(10) C66 0.0461(17) 0.0280(14) 0.0415(15) 0.0029(11) -0.0085(12) -0.0091(12) C71 0.0316(14) 0.0419(16) 0.0341(13) -0.0029(11) -0.0084(11) -0.0041(12) C74 0.0281(13) 0.0287(13) 0.0281(12) 0.0001(9) 0.0061(9) -0.0090(10) C68 0.0302(14) 0.0409(16) 0.0516(17) -0.0046(13) 0.0081(12) -0.0122(12) C69 0.0365(15) 0.0321(14) 0.0527(17) -0.0099(12) 0.0068(13) -0.0108(12) C70 0.0191(10) 0.0202(10) 0.0232(10) 0.0038(8) -0.0034(8) -0.0030(8) C75 0.0279(12) 0.0288(12) 0.0238(11) 0.0041(9) -0.0020(9) 0.0028(10) C72 0.0228(11) 0.0214(11) 0.0229(11) -0.0008(8) 0.0031(8) 0.0007(9) C76 0.0237(11) 0.0194(10) 0.0206(10) -0.0026(8) 0.0050(8) -0.0030(9) N82 0.0238(10) 0.0204(9) 0.0145(8) 0.0003(7) 0.0010(7) -0.0020(7) C87 0.0294(12) 0.0234(11) 0.0131(9) -0.0025(8) 0.0003(8) -0.0006(9) C88 0.0328(13) 0.0306(13) 0.0213(11) -0.0045(9) -0.0012(9) -0.0047(10) C89 0.0358(15) 0.0467(16) 0.0265(12) -0.0074(11) -0.0075(10) -0.0048(12) C90 0.0473(17) 0.0438(16) 0.0202(11) -0.0002(10) -0.0090(11) 0.0044(13) C91 0.0499(17) 0.0357(14) 0.0179(11) 0.0041(10) -0.0007(10) -0.0015(12) C92 0.0355(14) 0.0278(12) 0.0175(10) 0.0002(9) 0.0017(9) -0.0037(10) C81 0.0415(15) 0.0363(14) 0.0285(12) 0.0096(10) 0.0033(11) -0.0117(12) C7 0.051(2) 0.0478(19) 0.066(2) 0.0109(16) 0.0214(17) -0.0080(16) C83 0.060(2) 0.0397(17) 0.0450(17) -0.0031(13) 0.0094(15) -0.0187(15) C93 0.0364(15) 0.0415(15) 0.0255(12) -0.0041(10) 0.0000(10) -0.0176(12) C94 0.0446(19) 0.063(2) 0.067(2) -0.0030(18) 0.0181(17) -0.0151(17) C86 0.077(3) 0.0370(17) 0.0516(19) -0.0012(14) 0.0030(17) -0.0154(17) C95 0.0395(15) 0.0295(13) 0.0231(11) -0.0033(9) 0.0064(10) 0.0036(11) Ga2 0.032(8) 0.0133(19) 0.0092(16) -0.0013(11) -0.0010(19) 0.001(3) Ga3 0.030(7) 0.011(2) 0.0071(17) 0.0010(12) 0.003(2) 0.003(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.32307(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 Ga1 . Mn2 . 2.3111(9) yes Ga1 . N14 . 1.9857(19) yes Ga1 . N30 . 1.976(2) yes Mn2 . C3 . 1.760(3) yes Mn2 . C5 . 2.162(3) yes Mn2 . C10 . 2.147(2) yes Mn2 . C12 . 2.129(2) yes Mn2 . C13 . 2.132(3) yes Mn2 . C9 . 2.173(3) yes Mn2 . C11 . 1.770(3) yes Mn2 . C3 . 1.760(3) yes Mn2 . C5 . 2.162(3) yes Mn2 . C10 . 2.147(2) yes Mn2 . C12 . 2.129(2) yes Mn2 . C13 . 2.132(3) yes Mn2 . C9 . 2.173(3) yes Mn2 . C11 . 1.770(3) yes Mn2 . Ga2 . 2.49(2) yes C3 . O4 . 1.174(4) yes C5 . C10 . 1.416(4) yes C5 . C9 . 1.420(4) yes C5 . H51 . 0.990 no C10 . C12 . 1.416(4) yes C10 . H101 . 0.980 no C12 . C13 . 1.417(4) yes C12 . H121 . 0.983 no C13 . C9 . 1.415(4) yes C13 . H131 . 0.978 no C9 . C4 . 1.500(4) yes C4 . H42 . 0.965 no C4 . H41 . 0.977 no C4 . H43 . 0.969 no C11 . O12 . 1.165(3) yes N14 . C15 . 1.442(3) yes N14 . C26 . 1.338(3) yes N14 . C15 . 1.442(3) yes N14 . C26 . 1.338(3) yes N14 . Ga2 . 1.954(4) yes C15 . C16 . 1.413(3) yes C15 . C24 . 1.407(3) yes C16 . C19 . 1.397(3) yes C16 . C33 . 1.522(3) yes C19 . C20 . 1.384(4) yes C19 . H191 . 0.950 no C20 . C21 . 1.378(4) yes C20 . H201 . 0.941 no C21 . C24 . 1.396(3) yes C21 . H211 . 0.946 no C24 . C27 . 1.520(3) yes C27 . C30 . 1.532(4) yes C27 . C32 . 1.537(3) yes C27 . H271 . 0.988 no C30 . H301 . 0.971 no C30 . H303 . 0.975 no C30 . H302 . 0.965 no C32 . H321 . 0.970 no C32 . H323 . 0.965 no C32 . H322 . 0.963 no C33 . C39 . 1.529(4) yes C33 . C44 . 1.537(4) yes C33 . H331 . 1.000 no C39 . H393 . 0.974 no C39 . H392 . 0.970 no C39 . H391 . 0.966 no C44 . H443 . 0.963 no C44 . H442 . 0.974 no C44 . H441 . 0.963 no C26 . C45 . 1.508(3) yes C26 . C28 . 1.394(3) yes C45 . H453 . 0.964 no C45 . H452 . 0.962 no C45 . H451 . 0.962 no C28 . C29 . 1.398(3) yes C28 . H281 . 0.945 no C29 . N30 . 1.336(3) yes C29 . C53 . 1.508(3) yes N30 . C46 . 1.447(3) yes N30 . C46 . 1.447(3) yes N30 . Ga2 . 1.940(4) yes C46 . C47 . 1.399(3) yes C46 . C37 . 1.408(3) yes C47 . C34 . 1.400(3) yes C47 . C41 . 1.524(4) yes C34 . C35 . 1.382(4) yes C34 . H341 . 0.943 no C35 . C36 . 1.381(4) yes C35 . H351 . 0.939 no C36 . C37 . 1.392(3) yes C36 . H361 . 0.944 no C37 . C38 . 1.517(4) yes C38 . C52 . 1.529(4) yes C38 . C40 . 1.538(4) yes C38 . H381 . 0.984 no C52 . H521 . 0.962 no C52 . H523 . 0.975 no C52 . H522 . 0.970 no C40 . H401 . 0.964 no C40 . H403 . 0.971 no C40 . H402 . 0.968 no C41 . C42 . 1.515(4) yes C41 . C43 . 1.522(4) yes C41 . H411 . 0.993 no C42 . H423 . 0.965 no C42 . H422 . 0.977 no C42 . H421 . 0.969 no C43 . H433 . 0.967 no C43 . H432 . 0.972 no C43 . H431 . 0.973 no C53 . H533 . 0.959 no C53 . H532 . 0.970 no C53 . H531 . 0.964 no Ga45 . Mn46 . 2.3118(8) yes Ga45 . N58 . 1.9849(18) yes Ga45 . N82 . 1.9786(19) yes Mn46 . C54 . 2.163(3) yes Mn46 . C48 . 2.146(2) yes Mn46 . C49 . 2.124(3) yes Mn46 . C50 . 2.137(3) yes Mn46 . C56 . 2.178(3) yes Mn46 . C6 . 1.767(3) yes Mn46 . C55 . 1.767(3) yes Mn46 . C54 . 2.163(3) yes Mn46 . C48 . 2.146(2) yes Mn46 . C49 . 2.124(3) yes Mn46 . C50 . 2.137(3) yes Mn46 . C56 . 2.178(3) yes Mn46 . C6 . 1.767(3) yes Mn46 . C55 . 1.767(3) yes Mn46 . Ga3 . 2.50(2) yes C54 . C48 . 1.421(4) yes C54 . C56 . 1.419(4) yes C54 . H541 . 0.991 no C48 . C49 . 1.410(4) yes C48 . H481 . 0.981 no C49 . C50 . 1.420(4) yes C49 . H491 . 0.980 no C50 . C56 . 1.421(4) yes C50 . H501 . 0.984 no C56 . C57 . 1.497(4) yes C57 . H572 . 0.967 no C57 . H571 . 0.971 no C57 . H573 . 0.979 no C6 . O54 . 1.171(4) yes C55 . O56 . 1.167(3) yes N58 . C59 . 1.446(3) yes N58 . C70 . 1.339(3) yes N58 . C59 . 1.446(3) yes N58 . C70 . 1.339(3) yes N58 . Ga3 . 1.956(4) yes C59 . C60 . 1.411(3) yes C59 . C63 . 1.406(3) yes C60 . C64 . 1.394(3) yes C60 . C74 . 1.523(3) yes C64 . C61 . 1.390(4) yes C64 . H641 . 0.951 no C61 . C62 . 1.373(4) yes C61 . H611 . 0.950 no C62 . C63 . 1.400(3) yes C62 . H621 . 0.953 no C63 . C65 . 1.519(3) yes C65 . C66 . 1.530(4) yes C65 . C71 . 1.535(3) yes C65 . H651 . 0.993 no C66 . H661 . 0.972 no C66 . H663 . 0.973 no C66 . H662 . 0.963 no C71 . H711 . 0.961 no C71 . H713 . 0.959 no C71 . H712 . 0.963 no C74 . C68 . 1.524(4) yes C74 . C69 . 1.533(4) yes C74 . H741 . 0.997 no C68 . H683 . 0.972 no C68 . H682 . 0.965 no C68 . H681 . 0.976 no C69 . H693 . 0.961 no C69 . H692 . 0.963 no C69 . H691 . 0.970 no C70 . C75 . 1.506(3) yes C70 . C72 . 1.401(3) yes C75 . H753 . 0.954 no C75 . H752 . 0.962 no C75 . H751 . 0.958 no C72 . C76 . 1.394(3) yes C72 . H721 . 0.952 no C76 . N82 . 1.337(3) yes C76 . C95 . 1.509(3) yes N82 . C87 . 1.442(3) yes N82 . C87 . 1.442(3) yes N82 . Ga3 . 1.940(4) yes C87 . C88 . 1.407(3) yes C87 . C92 . 1.405(3) yes C88 . C89 . 1.397(3) yes C88 . C93 . 1.525(4) yes C89 . C90 . 1.383(4) yes C89 . H891 . 0.948 no C90 . C91 . 1.380(4) yes C90 . H901 . 0.939 no C91 . C92 . 1.394(3) yes C91 . H911 . 0.943 no C92 . C81 . 1.520(4) yes C81 . C7 . 1.539(4) yes C81 . C83 . 1.529(4) yes C81 . H811 . 0.984 no C7 . H71 . 0.969 no C7 . H73 . 0.970 no C7 . H72 . 0.964 no C83 . H831 . 0.961 no C83 . H833 . 0.963 no C83 . H832 . 0.977 no C93 . C94 . 1.515(4) yes C93 . C86 . 1.523(4) yes C93 . H931 . 0.991 no C94 . H943 . 0.967 no C94 . H942 . 0.976 no C94 . H941 . 0.972 no C86 . H863 . 0.966 no C86 . H862 . 0.966 no C86 . H861 . 0.966 no C95 . H953 . 0.949 no C95 . H952 . 0.973 no C95 . H951 . 0.968 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 Mn2 . Ga1 . N14 . 133.67(6) yes Mn2 . Ga1 . N30 . 134.61(6) yes N14 . Ga1 . N30 . 91.72(8) yes Ga1 . Mn2 . C3 . 90.30(12) yes Ga1 . Mn2 . C5 . 94.66(10) yes C3 . Mn2 . C5 . 150.33(12) yes Ga1 . Mn2 . C10 . 95.69(8) yes C3 . Mn2 . C10 . 112.05(12) yes C5 . Mn2 . C10 . 38.37(11) yes Ga1 . Mn2 . C12 . 128.90(8) yes C3 . Mn2 . C12 . 90.02(12) yes C5 . Mn2 . C12 . 64.31(11) yes C10 . Mn2 . C12 . 38.69(10) yes Ga1 . Mn2 . C13 . 158.27(10) yes C3 . Mn2 . C13 . 105.58(12) yes C5 . Mn2 . C13 . 64.23(11) yes C10 . Mn2 . C13 . 64.86(10) yes C12 . Mn2 . C13 . 38.86(11) yes Ga1 . Mn2 . C9 . 125.92(12) yes C3 . Mn2 . C9 . 143.45(12) yes C5 . Mn2 . C9 . 38.23(10) yes C10 . Mn2 . C9 . 64.47(11) yes C12 . Mn2 . C9 . 64.52(12) yes Ga1 . Mn2 . C11 . 93.97(9) yes C3 . Mn2 . C11 . 92.03(13) yes C5 . Mn2 . C11 . 116.70(13) yes C10 . Mn2 . C11 . 153.93(13) yes C12 . Mn2 . C11 . 137.08(12) yes C13 . Mn2 . C9 . 38.35(11) yes C13 . Mn2 . C11 . 100.07(12) yes C9 . Mn2 . C11 . 90.35(12) yes C3 . Mn2 . C5 . 150.33(12) yes C3 . Mn2 . C10 . 112.05(12) yes C5 . Mn2 . C10 . 38.37(11) yes C3 . Mn2 . C12 . 90.02(12) yes C5 . Mn2 . C12 . 64.31(11) yes C10 . Mn2 . C12 . 38.69(10) yes C3 . Mn2 . C13 . 105.58(12) yes C5 . Mn2 . C13 . 64.23(11) yes C10 . Mn2 . C13 . 64.86(10) yes C12 . Mn2 . C13 . 38.86(11) yes C3 . Mn2 . C9 . 143.45(12) yes C5 . Mn2 . C9 . 38.23(10) yes C10 . Mn2 . C9 . 64.47(11) yes C12 . Mn2 . C9 . 64.52(12) yes C13 . Mn2 . C9 . 38.35(11) yes C3 . Mn2 . C11 . 92.03(13) yes C5 . Mn2 . C11 . 116.70(13) yes C10 . Mn2 . C11 . 153.93(13) yes C12 . Mn2 . C11 . 137.08(12) yes C13 . Mn2 . C11 . 100.07(12) yes C3 . Mn2 . Ga2 . 79.6(8) yes C5 . Mn2 . Ga2 . 103.4(6) yes C10 . Mn2 . Ga2 . 98.6(2) yes C12 . Mn2 . Ga2 . 127.1(2) yes C13 . Mn2 . Ga2 . 163.5(2) yes C9 . Mn2 . C11 . 90.35(12) yes C9 . Mn2 . Ga2 . 136.4(8) yes C11 . Mn2 . Ga2 . 95.33(18) yes Mn2 . C3 . O4 . 175.3(3) yes Mn2 . C5 . C10 . 70.24(16) yes Mn2 . C5 . C9 . 71.34(16) yes C10 . C5 . C9 . 108.7(3) yes Mn2 . C5 . H51 . 126.2 no C10 . C5 . H51 . 126.1 no C9 . C5 . H51 . 125.1 no Mn2 . C10 . C5 . 71.39(15) yes Mn2 . C10 . C12 . 69.97(14) yes C5 . C10 . C12 . 107.5(2) yes Mn2 . C10 . H101 . 125.2 no C5 . C10 . H101 . 125.8 no C12 . C10 . H101 . 126.7 no Mn2 . C12 . C10 . 71.34(14) yes Mn2 . C12 . C13 . 70.71(14) yes C10 . C12 . C13 . 108.1(3) yes Mn2 . C12 . H121 . 124.4 no C10 . C12 . H121 . 125.2 no C13 . C12 . H121 . 126.7 no Mn2 . C13 . C12 . 70.43(15) yes Mn2 . C13 . C9 . 72.40(15) yes C12 . C13 . C9 . 108.4(2) yes Mn2 . C13 . H131 . 124.0 no C12 . C13 . H131 . 125.5 no C9 . C13 . H131 . 126.1 no Mn2 . C9 . C5 . 70.43(16) yes Mn2 . C9 . C13 . 69.25(16) yes C5 . C9 . C13 . 107.3(3) yes Mn2 . C9 . C4 . 128.5(2) yes C5 . C9 . C4 . 125.9(3) yes C13 . C9 . C4 . 126.7(3) yes C9 . C4 . H42 . 108.6 no C9 . C4 . H41 . 110.6 no H42 . C4 . H41 . 108.9 no C9 . C4 . H43 . 109.7 no H42 . C4 . H43 . 109.1 no H41 . C4 . H43 . 109.9 no Mn2 . C11 . O12 . 173.8(3) yes Ga1 . N14 . C15 . 114.96(14) yes Ga1 . N14 . C26 . 126.22(15) yes C15 . N14 . C26 . 118.79(18) yes C15 . N14 . C26 . 118.79(18) yes C15 . N14 . Ga2 . 119.9(4) yes C26 . N14 . Ga2 . 120.0(7) yes N14 . C15 . C16 . 117.98(19) yes N14 . C15 . C24 . 120.1(2) yes C16 . C15 . C24 . 121.8(2) yes C15 . C16 . C19 . 117.6(2) yes C15 . C16 . C33 . 121.3(2) yes C19 . C16 . C33 . 121.2(2) yes C16 . C19 . C20 . 121.2(2) yes C16 . C19 . H191 . 119.8 no C20 . C19 . H191 . 119.1 no C19 . C20 . C21 . 120.5(2) yes C19 . C20 . H201 . 119.5 no C21 . C20 . H201 . 120.0 no C20 . C21 . C24 . 121.1(2) yes C20 . C21 . H211 . 120.0 no C24 . C21 . H211 . 118.9 no C15 . C24 . C21 . 117.9(2) yes C15 . C24 . C27 . 122.5(2) yes C21 . C24 . C27 . 119.6(2) yes C24 . C27 . C30 . 111.4(2) yes C24 . C27 . C32 . 111.5(2) yes C30 . C27 . C32 . 109.7(2) yes C24 . C27 . H271 . 108.8 no C30 . C27 . H271 . 107.6 no C32 . C27 . H271 . 107.6 no C27 . C30 . H301 . 109.3 no C27 . C30 . H303 . 109.1 no H301 . C30 . H303 . 109.6 no C27 . C30 . H302 . 109.4 no H301 . C30 . H302 . 109.4 no H303 . C30 . H302 . 110.1 no C27 . C32 . H321 . 108.4 no C27 . C32 . H323 . 108.5 no H321 . C32 . H323 . 109.8 no C27 . C32 . H322 . 109.3 no H321 . C32 . H322 . 110.0 no H323 . C32 . H322 . 110.8 no C16 . C33 . C39 . 113.9(2) yes C16 . C33 . C44 . 113.0(2) yes C39 . C33 . C44 . 107.9(2) yes C16 . C33 . H331 . 106.8 no C39 . C33 . H331 . 107.3 no C44 . C33 . H331 . 107.8 no C33 . C39 . H393 . 109.8 no C33 . C39 . H392 . 111.0 no H393 . C39 . H392 . 109.1 no C33 . C39 . H391 . 109.5 no H393 . C39 . H391 . 108.8 no H392 . C39 . H391 . 108.7 no C33 . C44 . H443 . 109.5 no C33 . C44 . H442 . 109.8 no H443 . C44 . H442 . 109.6 no C33 . C44 . H441 . 107.8 no H443 . C44 . H441 . 109.7 no H442 . C44 . H441 . 110.4 no N14 . C26 . C45 . 119.34(19) yes N14 . C26 . C28 . 123.4(2) yes C45 . C26 . C28 . 117.3(2) yes C26 . C45 . H453 . 110.0 no C26 . C45 . H452 . 109.7 no H453 . C45 . H452 . 108.3 no C26 . C45 . H451 . 110.1 no H453 . C45 . H451 . 109.2 no H452 . C45 . H451 . 109.5 no C26 . C28 . C29 . 127.3(2) yes C26 . C28 . H281 . 116.7 no C29 . C28 . H281 . 115.9 no C28 . C29 . N30 . 123.4(2) yes C28 . C29 . C53 . 117.1(2) yes N30 . C29 . C53 . 119.5(2) yes Ga1 . N30 . C29 . 126.55(15) yes Ga1 . N30 . C46 . 114.64(15) yes C29 . N30 . C46 . 118.40(18) yes C29 . N30 . C46 . 118.40(18) yes C29 . N30 . Ga2 . 120.5(7) yes C46 . N30 . Ga2 . 120.6(5) yes N30 . C46 . C47 . 118.2(2) yes N30 . C46 . C37 . 119.8(2) yes C47 . C46 . C37 . 122.1(2) yes C46 . C47 . C34 . 117.9(2) yes C46 . C47 . C41 . 122.5(2) yes C34 . C47 . C41 . 119.6(2) yes C47 . C34 . C35 . 120.9(3) yes C47 . C34 . H341 . 119.0 no C35 . C34 . H341 . 120.1 no C34 . C35 . C36 . 120.2(2) yes C34 . C35 . H351 . 119.9 no C36 . C35 . H351 . 119.9 no C35 . C36 . C37 . 121.4(3) yes C35 . C36 . H361 . 119.5 no C37 . C36 . H361 . 119.1 no C46 . C37 . C36 . 117.6(2) yes C46 . C37 . C38 . 122.6(2) yes C36 . C37 . C38 . 119.8(2) yes C37 . C38 . C52 . 110.8(3) yes C37 . C38 . C40 . 112.2(3) yes C52 . C38 . C40 . 109.4(2) yes C37 . C38 . H381 . 108.5 no C52 . C38 . H381 . 108.7 no C40 . C38 . H381 . 107.2 no C38 . C52 . H521 . 109.8 no C38 . C52 . H523 . 108.9 no H521 . C52 . H523 . 110.2 no C38 . C52 . H522 . 109.0 no H521 . C52 . H522 . 109.5 no H523 . C52 . H522 . 109.4 no C38 . C40 . H401 . 108.7 no C38 . C40 . H403 . 108.2 no H401 . C40 . H403 . 109.5 no C38 . C40 . H402 . 109.1 no H401 . C40 . H402 . 110.3 no H403 . C40 . H402 . 111.0 no C47 . C41 . C42 . 111.6(3) yes C47 . C41 . C43 . 112.4(2) yes C42 . C41 . C43 . 111.2(3) yes C47 . C41 . H411 . 107.8 no C42 . C41 . H411 . 106.7 no C43 . C41 . H411 . 106.8 no C41 . C42 . H423 . 109.5 no C41 . C42 . H422 . 109.8 no H423 . C42 . H422 . 110.7 no C41 . C42 . H421 . 107.4 no H423 . C42 . H421 . 109.3 no H422 . C42 . H421 . 110.0 no C41 . C43 . H433 . 108.9 no C41 . C43 . H432 . 109.1 no H433 . C43 . H432 . 110.2 no C41 . C43 . H431 . 109.0 no H433 . C43 . H431 . 109.7 no H432 . C43 . H431 . 110.0 no C29 . C53 . H533 . 109.4 no C29 . C53 . H532 . 110.5 no H533 . C53 . H532 . 110.2 no C29 . C53 . H531 . 108.1 no H533 . C53 . H531 . 109.1 no H532 . C53 . H531 . 109.6 no Mn46 . Ga45 . N58 . 133.62(6) yes Mn46 . Ga45 . N82 . 134.63(6) yes N58 . Ga45 . N82 . 91.75(8) yes Ga45 . Mn46 . C54 . 94.73(9) yes Ga45 . Mn46 . C48 . 95.73(8) yes C54 . Mn46 . C48 . 38.49(11) yes Ga45 . Mn46 . C49 . 128.88(8) yes C54 . Mn46 . C49 . 64.23(11) yes C48 . Mn46 . C49 . 38.56(10) yes Ga45 . Mn46 . C50 . 158.42(9) yes C54 . Mn46 . C50 . 64.30(11) yes C48 . Mn46 . C50 . 64.98(10) yes C49 . Mn46 . C50 . 38.95(10) yes Ga45 . Mn46 . C56 . 125.90(11) yes C54 . Mn46 . C56 . 38.14(10) yes C48 . Mn46 . C56 . 64.51(11) yes C49 . Mn46 . C56 . 64.48(11) yes C50 . Mn46 . C56 . 38.43(11) yes Ga45 . Mn46 . C6 . 90.19(11) yes C54 . Mn46 . C6 . 150.40(12) yes C48 . Mn46 . C6 . 111.99(12) yes C49 . Mn46 . C6 . 90.16(12) yes C50 . Mn46 . C6 . 105.60(12) yes Ga45 . Mn46 . C55 . 93.75(9) yes C54 . Mn46 . C55 . 116.72(13) yes C48 . Mn46 . C55 . 154.11(13) yes C49 . Mn46 . C55 . 137.31(12) yes C50 . Mn46 . C55 . 100.17(11) yes C56 . Mn46 . C6 . 143.57(12) yes C56 . Mn46 . C55 . 90.51(12) yes C6 . Mn46 . C55 . 91.98(13) yes C54 . Mn46 . C48 . 38.49(11) yes C54 . Mn46 . C49 . 64.23(11) yes C48 . Mn46 . C49 . 38.56(10) yes C54 . Mn46 . C50 . 64.30(11) yes C48 . Mn46 . C50 . 64.98(10) yes C49 . Mn46 . C50 . 38.95(10) yes C54 . Mn46 . C56 . 38.14(10) yes C48 . Mn46 . C56 . 64.51(11) yes C49 . Mn46 . C56 . 64.48(11) yes C50 . Mn46 . C56 . 38.43(11) yes C54 . Mn46 . C6 . 150.40(12) yes C48 . Mn46 . C6 . 111.99(12) yes C49 . Mn46 . C6 . 90.16(12) yes C50 . Mn46 . C6 . 105.60(12) yes C56 . Mn46 . C6 . 143.57(12) yes C54 . Mn46 . C55 . 116.72(13) yes C48 . Mn46 . C55 . 154.11(13) yes C49 . Mn46 . C55 . 137.31(12) yes C50 . Mn46 . C55 . 100.17(11) yes C56 . Mn46 . C55 . 90.51(12) yes C54 . Mn46 . Ga3 . 103.8(6) yes C48 . Mn46 . Ga3 . 98.8(2) yes C49 . Mn46 . Ga3 . 127.1(2) yes C50 . Mn46 . Ga3 . 163.79(19) yes C56 . Mn46 . Ga3 . 136.8(7) yes C6 . Mn46 . C55 . 91.98(13) yes C6 . Mn46 . Ga3 . 79.2(7) yes C55 . Mn46 . Ga3 . 95.08(18) yes Mn46 . C54 . C48 . 70.11(15) yes Mn46 . C54 . C56 . 71.52(16) yes C48 . C54 . C56 . 108.8(2) yes Mn46 . C54 . H541 . 124.6 no C48 . C54 . H541 . 125.8 no C56 . C54 . H541 . 125.4 no Mn46 . C48 . C54 . 71.40(14) yes Mn46 . C48 . C49 . 69.88(14) yes C54 . C48 . C49 . 107.3(2) yes Mn46 . C48 . H481 . 125.2 no C54 . C48 . H481 . 126.4 no C49 . C48 . H481 . 126.3 no Mn46 . C49 . C48 . 71.57(14) yes Mn46 . C49 . C50 . 71.01(14) yes C48 . C49 . C50 . 108.7(3) yes Mn46 . C49 . H491 . 124.3 no C48 . C49 . H491 . 125.2 no C50 . C49 . H491 . 126.1 no Mn46 . C50 . C49 . 70.05(15) yes Mn46 . C50 . C56 . 72.38(15) yes C49 . C50 . C56 . 107.8(2) yes Mn46 . C50 . H501 . 124.6 no C49 . C50 . H501 . 126.1 no C56 . C50 . H501 . 126.0 no Mn46 . C56 . C50 . 69.20(16) yes Mn46 . C56 . C54 . 70.34(16) yes C50 . C56 . C54 . 107.4(3) yes Mn46 . C56 . C57 . 128.5(2) yes C50 . C56 . C57 . 126.5(3) yes C54 . C56 . C57 . 126.0(3) yes C56 . C57 . H572 . 108.9 no C56 . C57 . H571 . 110.3 no H572 . C57 . H571 . 108.1 no C56 . C57 . H573 . 111.0 no H572 . C57 . H573 . 109.0 no H571 . C57 . H573 . 109.4 no Mn46 . C6 . O54 . 175.2(2) yes Mn46 . C55 . O56 . 173.3(3) yes Ga45 . N58 . C59 . 115.13(14) yes Ga45 . N58 . C70 . 126.33(15) yes C59 . N58 . C70 . 118.50(18) yes C59 . N58 . C70 . 118.50(18) yes C59 . N58 . Ga3 . 120.3(4) yes C70 . N58 . Ga3 . 119.8(6) yes N58 . C59 . C60 . 117.99(19) yes N58 . C59 . C63 . 119.7(2) yes C60 . C59 . C63 . 122.1(2) yes C59 . C60 . C64 . 117.4(2) yes C59 . C60 . C74 . 121.4(2) yes C64 . C60 . C74 . 121.2(2) yes C60 . C64 . C61 . 121.2(2) yes C60 . C64 . H641 . 119.8 no C61 . C64 . H641 . 119.0 no C64 . C61 . C62 . 120.3(2) yes C64 . C61 . H611 . 119.5 no C62 . C61 . H611 . 120.2 no C61 . C62 . C63 . 121.3(2) yes C61 . C62 . H621 . 120.4 no C63 . C62 . H621 . 118.3 no C59 . C63 . C62 . 117.5(2) yes C59 . C63 . C65 . 122.7(2) yes C62 . C63 . C65 . 119.8(2) yes C63 . C65 . C66 . 111.1(2) yes C63 . C65 . C71 . 111.5(2) yes C66 . C65 . C71 . 109.7(2) yes C63 . C65 . H651 . 108.9 no C66 . C65 . H651 . 107.8 no C71 . C65 . H651 . 107.7 no C65 . C66 . H661 . 110.0 no C65 . C66 . H663 . 109.8 no H661 . C66 . H663 . 109.1 no C65 . C66 . H662 . 109.7 no H661 . C66 . H662 . 109.3 no H663 . C66 . H662 . 108.9 no C65 . C71 . H711 . 109.0 no C65 . C71 . H713 . 109.1 no H711 . C71 . H713 . 109.3 no C65 . C71 . H712 . 109.7 no H711 . C71 . H712 . 109.8 no H713 . C71 . H712 . 109.9 no C60 . C74 . C68 . 113.5(2) yes C60 . C74 . C69 . 113.4(2) yes C68 . C74 . C69 . 108.2(2) yes C60 . C74 . H741 . 107.5 no C68 . C74 . H741 . 106.7 no C69 . C74 . H741 . 107.3 no C74 . C68 . H683 . 109.2 no C74 . C68 . H682 . 109.6 no H683 . C68 . H682 . 108.7 no C74 . C68 . H681 . 110.6 no H683 . C68 . H681 . 109.4 no H682 . C68 . H681 . 109.3 no C74 . C69 . H693 . 109.4 no C74 . C69 . H692 . 108.4 no H693 . C69 . H692 . 108.8 no C74 . C69 . H691 . 111.0 no H693 . C69 . H691 . 109.3 no H692 . C69 . H691 . 109.9 no N58 . C70 . C75 . 119.5(2) yes N58 . C70 . C72 . 123.2(2) yes C75 . C70 . C72 . 117.2(2) yes C70 . C75 . H753 . 109.7 no C70 . C75 . H752 . 109.5 no H753 . C75 . H752 . 109.0 no C70 . C75 . H751 . 110.7 no H753 . C75 . H751 . 108.6 no H752 . C75 . H751 . 109.3 no C70 . C72 . C76 . 127.3(2) yes C70 . C72 . H721 . 116.6 no C76 . C72 . H721 . 116.1 no C72 . C76 . N82 . 123.6(2) yes C72 . C76 . C95 . 117.0(2) yes N82 . C76 . C95 . 119.4(2) yes Ga45 . N82 . C76 . 126.42(15) yes Ga45 . N82 . C87 . 114.51(15) yes C76 . N82 . C87 . 118.64(18) yes C76 . N82 . C87 . 118.64(18) yes C76 . N82 . Ga3 . 120.3(6) yes C87 . N82 . Ga3 . 120.6(5) yes N82 . C87 . C88 . 118.1(2) yes N82 . C87 . C92 . 120.1(2) yes C88 . C87 . C92 . 121.8(2) yes C87 . C88 . C89 . 117.8(2) yes C87 . C88 . C93 . 122.4(2) yes C89 . C88 . C93 . 119.8(2) yes C88 . C89 . C90 . 121.1(3) yes C88 . C89 . H891 . 118.9 no C90 . C89 . H891 . 119.9 no C89 . C90 . C91 . 120.1(2) yes C89 . C90 . H901 . 119.8 no C91 . C90 . H901 . 120.0 no C90 . C91 . C92 . 121.3(2) yes C90 . C91 . H911 . 119.5 no C92 . C91 . H911 . 119.2 no C87 . C92 . C91 . 117.9(2) yes C87 . C92 . C81 . 122.4(2) yes C91 . C92 . C81 . 119.6(2) yes C92 . C81 . C7 . 112.2(2) yes C92 . C81 . C83 . 110.6(3) yes C7 . C81 . C83 . 109.5(2) yes C92 . C81 . H811 . 108.4 no C7 . C81 . H811 . 107.9 no C83 . C81 . H811 . 108.0 no C81 . C7 . H71 . 108.0 no C81 . C7 . H73 . 108.3 no H71 . C7 . H73 . 109.8 no C81 . C7 . H72 . 109.6 no H71 . C7 . H72 . 110.6 no H73 . C7 . H72 . 110.4 no C81 . C83 . H831 . 109.7 no C81 . C83 . H833 . 109.8 no H831 . C83 . H833 . 109.0 no C81 . C83 . H832 . 109.8 no H831 . C83 . H832 . 109.0 no H833 . C83 . H832 . 109.4 no C88 . C93 . C94 . 111.4(3) yes C88 . C93 . C86 . 112.5(2) yes C94 . C93 . C86 . 111.3(3) yes C88 . C93 . H931 . 108.1 no C94 . C93 . H931 . 106.7 no C86 . C93 . H931 . 106.5 no C93 . C94 . H943 . 109.9 no C93 . C94 . H942 . 109.8 no H943 . C94 . H942 . 110.2 no C93 . C94 . H941 . 107.6 no H943 . C94 . H941 . 109.9 no H942 . C94 . H941 . 109.5 no C93 . C86 . H863 . 108.5 no C93 . C86 . H862 . 109.8 no H863 . C86 . H862 . 110.2 no C93 . C86 . H861 . 109.0 no H863 . C86 . H861 . 109.7 no H862 . C86 . H861 . 109.6 no C76 . C95 . H953 . 109.3 no C76 . C95 . H952 . 110.1 no H953 . C95 . H952 . 110.0 no C76 . C95 . H951 . 108.4 no H953 . C95 . H951 . 109.3 no H952 . C95 . H951 . 109.7 no N14 . Ga2 . N30 . 93.79(7) yes N14 . Ga2 . Mn2 . 125.0(11) yes N30 . Ga2 . Mn2 . 125.9(12) yes N58 . Ga3 . N82 . 93.81(7) yes N58 . Ga3 . Mn46 . 124.3(10) yes N82 . Ga3 . Mn46 . 125.6(11) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C44 . H442 . C26 . 141.64 0.974 2.504 3.324(4) yes C69 . H691 . C70 . 139.99 0.970 2.522 3.324(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 01/07/13 at 15:34:09 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) EQUIV PART(2001,OCC) PART(2002,OCC) WEIGHT -1 PART(2002,OCC) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 4,X'S) H ( 42,X'S) H ( 41,X'S) H ( 43,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 303,X'S) H ( 302,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 323,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 39,X'S) H ( 393,X'S) H ( 392,X'S) H ( 391,X'S) RIDE C ( 44,X'S) H ( 443,X'S) H ( 442,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 453,X'S) H ( 452,X'S) H ( 451,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 523,X'S) H ( 522,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 403,X'S) H ( 402,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 423,X'S) H ( 422,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 433,X'S) H ( 432,X'S) H ( 431,X'S) RIDE C ( 53,X'S) H ( 533,X'S) H ( 532,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 57,X'S) H ( 572,X'S) H ( 571,X'S) H ( 573,X'S) RIDE C ( 64,X'S) H ( 641,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 65,X'S) H ( 651,X'S) RIDE C ( 66,X'S) H ( 661,X'S) H ( 663,X'S) H ( 662,X'S) RIDE C ( 71,X'S) H ( 711,X'S) H ( 713,X'S) H ( 712,X'S) RIDE C ( 74,X'S) H ( 741,X'S) RIDE C ( 68,X'S) H ( 683,X'S) H ( 682,X'S) H ( 681,X'S) RIDE C ( 69,X'S) H ( 693,X'S) H ( 692,X'S) H ( 691,X'S) RIDE C ( 75,X'S) H ( 753,X'S) H ( 752,X'S) H ( 751,X'S) RIDE C ( 72,X'S) H ( 721,X'S) RIDE C ( 89,X'S) H ( 891,X'S) RIDE C ( 90,X'S) H ( 901,X'S) RIDE C ( 91,X'S) H ( 911,X'S) RIDE C ( 81,X'S) H ( 811,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 73,X'S) H ( 72,X'S) RIDE C ( 83,X'S) H ( 831,X'S) H ( 833,X'S) H ( 832,X'S) RIDE C ( 93,X'S) H ( 931,X'S) RIDE C ( 94,X'S) H ( 943,X'S) H ( 942,X'S) H ( 941,X'S) RIDE C ( 86,X'S) H ( 863,X'S) H ( 862,X'S) H ( 861,X'S) RIDE C ( 95,X'S) H ( 953,X'S) H ( 952,X'S) H ( 951,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 01/07/13 at 15:34:09 # #LIST 16 SAME GA(2) N(14) N(30) AND CONT GA(2) N(30) N(14) AND CONT GA(3) N(82) N(58) AND CONT GA(3) N(58) N(82) SIMU 0.01 GA(2) MN(2) AND CONT GA(3) MN(46) DELU 0.01 GA(2) MN(2) AND CONT GA(3) MN(46) END ; _database_code_depnum_ccdc_archive 'CCDC 952954' ####################################################################### # # 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_079jart13 _audit_creation_date 13-07-28 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '079JART13 in P -1' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 12.5663(2) _cell_length_b 13.2686(3) _cell_length_c 20.7262(4) _cell_angle_alpha 78.4857(19) _cell_angle_beta 83.9447(17) _cell_angle_gamma 83.4912(18) _cell_volume 3352.25(12) _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 0.0181 0.0091 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 0.0311 0.0180 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' Ga -1.2846 0.7763 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co -2.3653 3.6143 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' B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 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 2 # Given Formula = C70 H40 B1 Co1 F24 Ga1 N2 O4 # Dc = 1.55 Fooo = 1536.00 Mu = 34.88 M = 1568.51 # Found Formula = C65 H53 B1 Co1 F24 Ga1 N2 O4 # Dc = 1.51 FOOO = 1536.00 Mu = 34.62 M = 1521.56 _chemical_formula_sum 'C65 H53 B1 Co1 F24 Ga1 N2 O4' _chemical_formula_moiety 'C65 H53 B1 Co1 F24 Ga1 N2 O4' _chemical_compound_source . _chemical_formula_weight 1521.56 _cell_measurement_reflns_used 17796 _cell_measurement_theta_min 3 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.060 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_max 0.230 _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 3.462 # Sheldrick geometric approximatio 0.52 0.81 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.81 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _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 150 _diffrn_reflns_number 13907 _reflns_number_total 13907 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 13907 # Theoretical number of reflections is about 28155 _diffrn_reflns_theta_min 3.415 _diffrn_reflns_theta_max 76.432 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 74.139 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 2.49 _oxford_diffrn_Wilson_scale 0.12 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.09 _refine_diff_density_max 1.74 # 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>0.0\s(I) _refine_ls_number_reflns 13849 _refine_ls_number_restraints 486 _refine_ls_number_parameters 974 _oxford_refine_ls_R_factor_ref 0.0521 _refine_ls_wR_factor_ref 0.1228 _refine_ls_goodness_of_fit_ref 0.9839 _refine_ls_shift/su_max 0.0005839 _refine_ls_shift/su_mean 0.0000194 # The values computed with all filters except I/sigma _oxford_reflns_number_all 13849 _refine_ls_R_factor_all 0.0521 _refine_ls_wR_factor_all 0.1228 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12839 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_gt 0.1201 # 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^) + ( 0.06P)^2^ + 4.47P] ,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 C98 C 0.6793(5) 0.5286(4) 0.0626(3) 0.0594 0.503(5) Uani D . P 1 2 . C99 C 0.6766(4) 0.5288(3) 0.0599(2) 0.0639 0.497(5) Uani D . P 1 1 . F1 F 1.0996(5) 0.3508(3) 0.3931(2) 0.0927 0.633(5) Uani D . P 1 1 . F2 F 1.2224(3) 0.2553(5) 0.3563(2) 0.1070 0.633(5) Uani D . P 1 1 . F3 F 1.0864(4) 0.1930(3) 0.41361(17) 0.0579 0.633(5) Uani D . P 1 1 . F4 F 0.6167(6) 0.6085(4) 0.0784(3) 0.1034 0.633(5) Uani D . P 1 1 . F5 F 0.6548(5) 0.5290(4) -0.0017(2) 0.0698 0.633(5) Uani D . P 1 1 . F6 F 0.7774(4) 0.5508(5) 0.0559(3) 0.0826 0.633(5) Uani D . P 1 1 . F7 F 0.4248(3) 0.3654(4) 0.48456(16) 0.0654 0.633(5) Uani D . P 1 1 . F8 F 0.4004(3) 0.2843(3) 0.4089(2) 0.0501 0.633(5) Uani D . P 1 1 . F9 F 0.3563(3) 0.4451(3) 0.3976(2) 0.0613 0.633(5) Uani D . P 1 1 . F43 F 0.51184(15) 0.11938(14) 0.12123(11) 0.0481 1.0000 Uani . . . . . . F45 F 0.42846(18) 0.25299(17) 0.06595(10) 0.0567 1.0000 Uani . . . . . . F46 F 0.39140(14) 0.20972(17) 0.17027(11) 0.0515 1.0000 Uani . . . . . . F51 F 1.0493(4) 0.3213(5) 0.4095(3) 0.0648 0.367(5) Uani D . P 1 2 . F52 F 1.1995(5) 0.3302(6) 0.3492(2) 0.0656 0.367(5) Uani D . P 1 2 . F53 F 1.1519(5) 0.1913(4) 0.3995(3) 0.0781 0.367(5) Uani D . P 1 2 . F54 F 0.6690(7) 0.6064(6) 0.0942(4) 0.0806 0.367(5) Uani D . P 1 2 . F55 F 0.6207(7) 0.5581(7) 0.0119(5) 0.0779 0.367(5) Uani D . P 1 2 . F56 F 0.7817(6) 0.5209(7) 0.0372(5) 0.0700 0.367(5) Uani D . P 1 2 . F57 F 0.4040(5) 0.4239(6) 0.4689(3) 0.0665 0.367(5) Uani D . P 1 2 . F58 F 0.4112(5) 0.2796(4) 0.4417(4) 0.0709 0.367(5) Uani D . P 1 2 . F59 F 0.3611(4) 0.4107(6) 0.3745(3) 0.0623 0.367(5) Uani D . P 1 2 . F65 F 0.7322(3) -0.14561(18) 0.48396(12) 0.0784 1.0000 Uani . . . . . . F66 F 0.6176(2) -0.0133(3) 0.48903(13) 0.1015 1.0000 Uani . . . . . . F67 F 0.7796(3) -0.0070(2) 0.50074(12) 0.0861 1.0000 Uani . . . . . . F69 F 0.71137(17) -0.17708(16) 0.24568(12) 0.0560 1.0000 Uani . . . . . . F70 F 0.87942(17) -0.17445(16) 0.24609(13) 0.0618 1.0000 Uani . . . . . . F71 F 0.7956(3) -0.06625(17) 0.17440(11) 0.0804 1.0000 Uani . . . . . . F84 F 1.20397(15) 0.35881(16) 0.11715(10) 0.0479 1.0000 Uani . . . . . . F85 F 1.06005(16) 0.3509(2) 0.07379(10) 0.0637 1.0000 Uani . . . . . . F86 F 1.1626(2) 0.21129(19) 0.10912(14) 0.0741 1.0000 Uani . . . . . . F98 F 0.78914(19) 0.56324(17) 0.43567(11) 0.0578 1.0000 Uani . . . . . . F99 F 0.81938(19) 0.61406(16) 0.33118(11) 0.0582 1.0000 Uani . . . . . . F100 F 0.67299(18) 0.66771(14) 0.38212(12) 0.0578 1.0000 Uani . . . . . . Ga1 Ga 0.20164(2) 0.77234(2) 0.220106(15) 0.0240 1.0000 Uani . . . . . . Co2 Co 0.28646(4) 0.60769(3) 0.22556(2) 0.0325 1.0000 Uani . . . . . . C4 C 0.1532(3) 0.5712(2) 0.25360(16) 0.0397 1.0000 Uani . . . . . . C6 C 0.3473(3) 0.4755(3) 0.23483(18) 0.0447 1.0000 Uani . . . . . . C8 C 0.3739(3) 0.6408(2) 0.28043(17) 0.0435 1.0000 Uani . . . . . . C10 C 0.3252(3) 0.6369(3) 0.13722(17) 0.0432 1.0000 Uani . . . . . . C11 C 0.0947(2) 0.7578(2) 0.06836(14) 0.0294 1.0000 Uani . . . . . . C13 C 0.1511(2) 0.8332(2) 0.08488(12) 0.0252 1.0000 Uani . . . . . . C15 C 0.1191(2) 0.7348(2) 0.00509(15) 0.0366 1.0000 Uani . . . . . . C16 C 0.1947(2) 0.7848(3) -0.03929(14) 0.0378 1.0000 Uani . . . . . . C17 C 0.2491(2) 0.8583(3) -0.02180(14) 0.0364 1.0000 Uani . . . . . . C18 C 0.2292(2) 0.8839(2) 0.04077(13) 0.0297 1.0000 Uani . . . . . . C19 C 0.2962(2) 0.9605(2) 0.05968(15) 0.0369 1.0000 Uani . . . . . . C20 C 0.4060(3) 0.9058(3) 0.0775(2) 0.0630 1.0000 Uani . . . . . . C21 C 0.3101(4) 1.0557(3) 0.00551(19) 0.0566 1.0000 Uani . . . . . . C22 C 0.0075(2) 0.7040(2) 0.11402(15) 0.0355 1.0000 Uani . . . . . . C23 C 0.0190(3) 0.5869(3) 0.1166(2) 0.0504 1.0000 Uani . . . . . . C24 C -0.1035(2) 0.7498(3) 0.09276(19) 0.0465 1.0000 Uani . . . . . . C25 C 0.07326(19) 0.94782(19) 0.15841(12) 0.0244 1.0000 Uani . . . . . . C26 C 0.0605(2) 0.98378(19) 0.21750(13) 0.0260 1.0000 Uani . . . . . . C28 C 0.1064(2) 0.94263(19) 0.27683(12) 0.0251 1.0000 Uani . . . . . . C29 C 0.2258(2) 0.8218(2) 0.34678(12) 0.0267 1.0000 Uani . . . . . . C30 C 0.1852(2) 0.7428(2) 0.39553(13) 0.0308 1.0000 Uani . . . . . . C31 C 0.0821(2) 0.6963(2) 0.39072(14) 0.0331 1.0000 Uani . . . . . . C32 C 0.0857(3) 0.5814(2) 0.42147(19) 0.0477 1.0000 Uani . . . . . . C33 C -0.0144(3) 0.7552(3) 0.4214(2) 0.0545 1.0000 Uani . . . . . . C34 C 0.2415(3) 0.7109(3) 0.45194(15) 0.0428 1.0000 Uani . . . . . . C35 C 0.3324(3) 0.7553(3) 0.45881(16) 0.0494 1.0000 Uani . . . . . . C36 C 0.3702(3) 0.8331(3) 0.41011(16) 0.0430 1.0000 Uani . . . . . . C37 C 0.3176(2) 0.8691(2) 0.35275(13) 0.0320 1.0000 Uani . . . . . . C38 C 0.3621(2) 0.9544(2) 0.30005(15) 0.0375 1.0000 Uani . . . . . . C39 C 0.3986(5) 1.0404(4) 0.3290(2) 0.0765 1.0000 Uani . . . . . . C40 C 0.4560(5) 0.9098(4) 0.2583(3) 0.0885 1.0000 Uani . . . . . . C41 C 0.0826(3) 1.0024(2) 0.33144(14) 0.0369 1.0000 Uani . . . . . . C42 C 0.0198(2) 1.0130(2) 0.10050(14) 0.0330 1.0000 Uani . . . . . . C44 C 0.4720(2) 0.2176(2) 0.12236(14) 0.0323 1.0000 Uani . . . . . . C47 C 0.55625(19) 0.2814(2) 0.13445(12) 0.0256 1.0000 Uani . . . . . . C48 C 0.61470(19) 0.24580(19) 0.18945(12) 0.0234 1.0000 Uani . . . . . . C49 C 0.69591(19) 0.29938(18) 0.20400(12) 0.0224 1.0000 Uani . . . . . . C50 C 0.7127(2) 0.39310(19) 0.16077(13) 0.0272 1.0000 Uani . . . . . . C51 C 0.6545(2) 0.4286(2) 0.10579(14) 0.0320 1.0000 Uani . . . . . . C52 C 0.5756(2) 0.3729(2) 0.09199(13) 0.0302 1.0000 Uani . . . . . . C58 C 0.75270(19) 0.14017(19) 0.30170(12) 0.0242 1.0000 Uani . . . . . . C59 C 0.7715(2) 0.06732(19) 0.25996(13) 0.0263 1.0000 Uani . . . . . . C60 C 0.7690(2) -0.0382(2) 0.28381(14) 0.0309 1.0000 Uani . . . . . . C61 C 0.7497(2) -0.0761(2) 0.35101(15) 0.0341 1.0000 Uani . . . . . . C62 C 0.7343(2) -0.0065(2) 0.39315(14) 0.0333 1.0000 Uani . . . . . . C63 C 0.7349(2) 0.0996(2) 0.36905(13) 0.0281 1.0000 Uani . . . . . . C64 C 0.7141(3) -0.0444(3) 0.46631(17) 0.0502 1.0000 Uani . . . . . . C68 C 0.7874(3) -0.1130(2) 0.23741(17) 0.0427 1.0000 Uani . . . . . . C72 C 0.88960(19) 0.27577(18) 0.25769(12) 0.0231 1.0000 Uani . . . . . . C73 C 0.9490(2) 0.28623(19) 0.19610(12) 0.0255 1.0000 Uani . . . . . . C74 C 1.0597(2) 0.2922(2) 0.18934(13) 0.0286 1.0000 Uani . . . . . . C75 C 1.1159(2) 0.2878(2) 0.24397(14) 0.0311 1.0000 Uani . . . . . . C76 C 1.0587(2) 0.2771(2) 0.30537(14) 0.0311 1.0000 Uani . . . . . . C77 C 0.9488(2) 0.27068(19) 0.31214(13) 0.0272 1.0000 Uani . . . . . . C78 C 1.1152(2) 0.2726(2) 0.36544(11) 0.0572 1.0000 Uani D . . . . . C83 C 1.1211(2) 0.3027(3) 0.12280(16) 0.0399 1.0000 Uani . . . . . . C87 C 0.70140(19) 0.33856(18) 0.32038(12) 0.0234 1.0000 Uani . . . . . . C88 C 0.7452(2) 0.42628(19) 0.32989(12) 0.0260 1.0000 Uani . . . . . . C89 C 0.6895(2) 0.49449(19) 0.36760(13) 0.0278 1.0000 Uani . . . . . . C90 C 0.5876(2) 0.4780(2) 0.39731(13) 0.0291 1.0000 Uani . . . . . . C91 C 0.5421(2) 0.3916(2) 0.38804(12) 0.0273 1.0000 Uani . . . . . . C92 C 0.5975(2) 0.3238(2) 0.35027(12) 0.0254 1.0000 Uani . . . . . . C93 C 0.43130(13) 0.37296(19) 0.41899(11) 0.0407 1.0000 Uani D . . . . . C97 C 0.7424(3) 0.5844(2) 0.37851(16) 0.0372 1.0000 Uani . . . . . . O5 O 0.0711(2) 0.54359(19) 0.27107(13) 0.0506 1.0000 Uani . . . . . . O7 O 0.3855(2) 0.39388(19) 0.24068(16) 0.0625 1.0000 Uani . . . . . . O9 O 0.4344(2) 0.6546(2) 0.31385(15) 0.0598 1.0000 Uani . . . . . . O11 O 0.3549(2) 0.6461(2) 0.08334(13) 0.0602 1.0000 Uani . . . . . . N12 N 0.13111(16) 0.85840(16) 0.15042(10) 0.0230 1.0000 Uani . . . . . . N28 N 0.17156(17) 0.85388(16) 0.28604(10) 0.0239 1.0000 Uani . . . . . . B57 B 0.7601(2) 0.2629(2) 0.27090(13) 0.0229 1.0000 Uani . . . . . . H151 H 0.0831 0.6834 -0.0074 0.0445 1.0000 Uiso R . . . . . H161 H 0.2096 0.7697 -0.0824 0.0456 1.0000 Uiso R . . . . . H171 H 0.3004 0.8928 -0.0534 0.0443 1.0000 Uiso R . . . . . H191 H 0.2600 0.9835 0.0989 0.0443 1.0000 Uiso R . . . . . H201 H 0.3976 0.8489 0.1152 0.0951 1.0000 Uiso R . . . . . H202 H 0.4429 0.8789 0.0401 0.0955 1.0000 Uiso R . . . . . H203 H 0.4499 0.9547 0.0885 0.0947 1.0000 Uiso R . . . . . H211 H 0.3518 1.0341 -0.0316 0.0860 1.0000 Uiso R . . . . . H212 H 0.2394 1.0858 -0.0074 0.0860 1.0000 Uiso R . . . . . H213 H 0.3474 1.1047 0.0209 0.0860 1.0000 Uiso R . . . . . H221 H 0.0135 0.7147 0.1589 0.0428 1.0000 Uiso R . . . . . H231 H 0.0919 0.5582 0.1247 0.0746 1.0000 Uiso R . . . . . H232 H -0.0303 0.5549 0.1517 0.0749 1.0000 Uiso R . . . . . H233 H 0.0009 0.5732 0.0751 0.0749 1.0000 Uiso R . . . . . H241 H -0.1124 0.7378 0.0493 0.0685 1.0000 Uiso R . . . . . H242 H -0.1141 0.8237 0.0921 0.0687 1.0000 Uiso R . . . . . H243 H -0.1587 0.7176 0.1232 0.0686 1.0000 Uiso R . . . . . H261 H 0.0151 1.0449 0.2179 0.0311 1.0000 Uiso R . . . . . H311 H 0.0715 0.7062 0.3426 0.0398 1.0000 Uiso R . . . . . H321 H 0.0243 0.5527 0.4099 0.0726 1.0000 Uiso R . . . . . H322 H 0.1527 0.5469 0.4060 0.0727 1.0000 Uiso R . . . . . H323 H 0.0817 0.5742 0.4691 0.0728 1.0000 Uiso R . . . . . H331 H -0.0791 0.7211 0.4205 0.0840 1.0000 Uiso R . . . . . H332 H -0.0221 0.8251 0.3968 0.0839 1.0000 Uiso R . . . . . H333 H -0.0018 0.7548 0.4668 0.0841 1.0000 Uiso R . . . . . H341 H 0.2162 0.6585 0.4866 0.0512 1.0000 Uiso R . . . . . H351 H 0.3697 0.7321 0.4975 0.0573 1.0000 Uiso R . . . . . H361 H 0.4329 0.8633 0.4156 0.0513 1.0000 Uiso R . . . . . H381 H 0.3041 0.9845 0.2712 0.0459 1.0000 Uiso R . . . . . H391 H 0.4139 1.0972 0.2932 0.1149 1.0000 Uiso R . . . . . H392 H 0.4618 1.0152 0.3512 0.1154 1.0000 Uiso R . . . . . H393 H 0.3409 1.0627 0.3595 0.1152 1.0000 Uiso R . . . . . H401 H 0.4857 0.9655 0.2267 0.1296 1.0000 Uiso R . . . . . H402 H 0.4295 0.8610 0.2359 0.1302 1.0000 Uiso R . . . . . H403 H 0.5100 0.8745 0.2870 0.1303 1.0000 Uiso R . . . . . H411 H 0.0870 0.9585 0.3748 0.0563 1.0000 Uiso R . . . . . H412 H 0.0116 1.0394 0.3292 0.0566 1.0000 Uiso R . . . . . H413 H 0.1334 1.0525 0.3263 0.0563 1.0000 Uiso R . . . . . H421 H -0.0306 1.0649 0.1156 0.0512 1.0000 Uiso R . . . . . H422 H 0.0730 1.0456 0.0690 0.0513 1.0000 Uiso R . . . . . H423 H -0.0169 0.9702 0.0799 0.0514 1.0000 Uiso R . . . . . H481 H 0.5982 0.1822 0.2179 0.0285 1.0000 Uiso R . . . . . H501 H 0.7651 0.4340 0.1682 0.0319 1.0000 Uiso R . . . . . H521 H 0.5373 0.3972 0.0545 0.0366 1.0000 Uiso R . . . . . H591 H 0.7860 0.0913 0.2136 0.0307 1.0000 Uiso R . . . . . H611 H 0.7470 -0.1480 0.3670 0.0414 1.0000 Uiso R . . . . . H631 H 0.7238 0.1448 0.3997 0.0342 1.0000 Uiso R . . . . . H731 H 0.9126 0.2900 0.1577 0.0314 1.0000 Uiso R . . . . . H751 H 1.1914 0.2918 0.2393 0.0371 1.0000 Uiso R . . . . . H771 H 0.9123 0.2613 0.3551 0.0331 1.0000 Uiso R . . . . . H881 H 0.8143 0.4411 0.3106 0.0317 1.0000 Uiso R . . . . . H901 H 0.5499 0.5239 0.4232 0.0353 1.0000 Uiso R . . . . . H921 H 0.5641 0.2652 0.3443 0.0310 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 C98 0.063(3) 0.037(3) 0.077(4) 0.028(3) -0.050(3) -0.027(3) C99 0.081(4) 0.038(3) 0.069(3) 0.021(3) -0.032(3) -0.021(3) F1 0.169(4) 0.0355(18) 0.094(3) -0.0229(19) -0.089(3) -0.006(2) F2 0.048(2) 0.194(5) 0.069(3) 0.009(3) -0.0318(19) -0.006(3) F3 0.073(2) 0.061(2) 0.0432(17) 0.0003(14) -0.0411(18) -0.0042(19) F4 0.135(4) 0.036(2) 0.119(4) 0.019(2) -0.007(3) 0.013(3) F5 0.095(3) 0.053(3) 0.055(2) 0.0256(19) -0.026(2) -0.027(2) F6 0.086(3) 0.065(3) 0.094(4) 0.044(2) -0.057(3) -0.057(2) F7 0.0438(19) 0.117(3) 0.0364(17) -0.017(2) 0.0094(14) -0.019(2) F8 0.0421(17) 0.0487(18) 0.059(2) -0.0142(17) 0.0225(17) -0.0203(14) F9 0.0266(15) 0.0476(19) 0.098(3) 0.0002(19) 0.0065(18) 0.0111(14) F43 0.0435(10) 0.0324(9) 0.0737(13) -0.0154(9) -0.0118(9) -0.0098(7) F45 0.0686(13) 0.0552(12) 0.0507(11) 0.0079(9) -0.0357(10) -0.0278(10) F46 0.0310(9) 0.0685(13) 0.0591(12) -0.0178(10) 0.0038(8) -0.0199(9) F51 0.057(3) 0.101(5) 0.051(3) -0.032(3) -0.021(3) -0.025(3) F52 0.055(3) 0.090(4) 0.056(3) 0.008(3) -0.041(3) -0.031(3) F53 0.109(5) 0.047(3) 0.087(4) -0.014(3) -0.080(4) 0.021(3) F54 0.105(5) 0.026(3) 0.108(5) 0.017(3) -0.037(4) -0.023(4) F55 0.078(4) 0.051(4) 0.099(6) 0.047(4) -0.075(4) -0.028(3) F56 0.071(4) 0.058(4) 0.076(5) 0.027(3) -0.020(3) -0.044(3) F57 0.050(3) 0.100(4) 0.060(4) -0.044(3) 0.020(3) -0.020(3) F58 0.054(3) 0.058(3) 0.076(4) 0.025(3) 0.034(3) -0.004(3) F59 0.026(3) 0.100(5) 0.055(3) -0.005(3) -0.003(2) 0.002(3) F65 0.133(2) 0.0420(12) 0.0480(13) 0.0159(10) 0.0020(14) -0.0069(13) F66 0.0815(19) 0.146(3) 0.0458(13) 0.0191(16) 0.0253(13) 0.0274(19) F67 0.134(3) 0.0854(19) 0.0383(12) 0.0085(12) -0.0263(14) -0.0253(18) F69 0.0511(11) 0.0465(11) 0.0783(15) -0.0307(10) 0.0041(10) -0.0140(9) F70 0.0471(11) 0.0400(11) 0.1009(18) -0.0335(11) 0.0164(11) 0.0002(9) F71 0.161(3) 0.0369(11) 0.0424(12) -0.0170(9) 0.0144(14) -0.0076(14) F84 0.0343(9) 0.0580(12) 0.0491(11) -0.0029(9) 0.0051(8) -0.0152(8) F85 0.0399(10) 0.119(2) 0.0319(10) -0.0095(11) -0.0002(8) -0.0175(12) F86 0.0795(16) 0.0615(14) 0.0860(17) -0.0433(13) 0.0427(14) -0.0207(12) F98 0.0704(14) 0.0530(12) 0.0585(12) -0.0130(10) -0.0218(11) -0.0232(10) F99 0.0714(14) 0.0416(11) 0.0655(13) -0.0204(9) 0.0225(11) -0.0299(10) F100 0.0627(13) 0.0266(9) 0.0859(16) -0.0204(9) 0.0007(11) -0.0010(8) Ga1 0.02644(16) 0.02053(15) 0.02459(15) -0.00472(11) -0.00400(11) 0.00236(11) Co2 0.0360(2) 0.0239(2) 0.0362(3) -0.00711(18) -0.00517(19) 0.00788(18) C4 0.0501(18) 0.0244(13) 0.0438(16) -0.0086(12) -0.0048(14) 0.0046(12) C6 0.0473(17) 0.0352(16) 0.0515(19) -0.0134(14) -0.0061(14) 0.0074(13) C8 0.0471(17) 0.0294(14) 0.0520(18) -0.0062(13) -0.0137(15) 0.0121(13) C10 0.0427(16) 0.0396(16) 0.0451(18) -0.0114(13) -0.0054(14) 0.0131(13) C11 0.0258(12) 0.0318(13) 0.0335(13) -0.0121(11) -0.0066(10) -0.0003(10) C13 0.0247(11) 0.0271(12) 0.0251(12) -0.0079(9) -0.0064(9) 0.0014(9) C15 0.0333(14) 0.0435(16) 0.0388(15) -0.0194(13) -0.0088(12) -0.0023(12) C16 0.0336(14) 0.0534(18) 0.0297(14) -0.0187(13) -0.0045(11) 0.0026(13) C17 0.0309(13) 0.0497(17) 0.0285(13) -0.0098(12) 0.0000(10) -0.0021(12) C18 0.0268(12) 0.0356(14) 0.0278(12) -0.0085(10) -0.0039(10) -0.0021(10) C19 0.0364(14) 0.0442(16) 0.0325(14) -0.0091(12) 0.0021(11) -0.0159(12) C20 0.045(2) 0.064(2) 0.088(3) -0.018(2) -0.026(2) -0.0151(18) C21 0.071(2) 0.054(2) 0.0472(19) -0.0038(16) -0.0007(17) -0.0290(19) C22 0.0349(14) 0.0375(15) 0.0387(15) -0.0139(12) -0.0033(11) -0.0109(12) C23 0.058(2) 0.0380(17) 0.060(2) -0.0146(15) -0.0079(17) -0.0137(15) C24 0.0305(14) 0.0542(19) 0.062(2) -0.0288(17) 0.0008(14) -0.0077(13) C25 0.0220(11) 0.0230(11) 0.0279(12) -0.0035(9) -0.0037(9) -0.0018(9) C26 0.0283(12) 0.0188(11) 0.0296(12) -0.0037(9) -0.0033(10) 0.0026(9) C28 0.0279(12) 0.0206(11) 0.0261(12) -0.0042(9) -0.0003(9) -0.0022(9) C29 0.0315(12) 0.0258(12) 0.0219(11) -0.0030(9) -0.0052(9) 0.0005(10) C30 0.0364(14) 0.0274(13) 0.0265(12) -0.0013(10) -0.0023(10) -0.0015(10) C31 0.0364(14) 0.0279(13) 0.0322(14) -0.0003(11) 0.0006(11) -0.0049(11) C32 0.0505(18) 0.0327(16) 0.055(2) 0.0063(14) -0.0046(15) -0.0105(14) C33 0.0398(17) 0.049(2) 0.077(3) -0.0230(18) 0.0064(17) -0.0061(15) C34 0.0514(18) 0.0414(16) 0.0311(15) 0.0082(12) -0.0097(13) -0.0067(14) C35 0.059(2) 0.054(2) 0.0336(16) 0.0051(14) -0.0217(15) -0.0060(16) C36 0.0431(16) 0.0507(18) 0.0368(16) -0.0018(13) -0.0167(13) -0.0109(14) C37 0.0344(13) 0.0334(14) 0.0279(13) -0.0038(11) -0.0048(10) -0.0037(11) C38 0.0400(15) 0.0400(16) 0.0328(14) -0.0007(12) -0.0062(12) -0.0129(12) C39 0.121(4) 0.066(3) 0.051(2) 0.0026(19) -0.019(2) -0.059(3) C40 0.092(4) 0.066(3) 0.085(3) 0.010(2) 0.045(3) -0.005(3) C41 0.0515(17) 0.0283(13) 0.0311(14) -0.0104(11) -0.0035(12) 0.0036(12) C42 0.0360(14) 0.0306(13) 0.0314(13) -0.0044(11) -0.0101(11) 0.0047(11) C44 0.0295(13) 0.0328(14) 0.0355(14) -0.0039(11) -0.0080(11) -0.0064(11) C47 0.0225(11) 0.0277(12) 0.0272(12) -0.0056(10) -0.0032(9) -0.0027(9) C48 0.0232(11) 0.0221(11) 0.0238(11) -0.0022(9) -0.0004(9) -0.0022(9) C49 0.0213(11) 0.0211(11) 0.0244(11) -0.0053(9) -0.0012(9) 0.0005(9) C50 0.0262(12) 0.0218(11) 0.0336(13) -0.0019(10) -0.0073(10) -0.0041(9) C51 0.0313(13) 0.0243(12) 0.0385(14) 0.0032(11) -0.0107(11) -0.0035(10) C52 0.0284(12) 0.0297(13) 0.0312(13) 0.0011(10) -0.0104(10) -0.0015(10) C58 0.0211(11) 0.0242(11) 0.0259(12) -0.0013(9) -0.0026(9) -0.0014(9) C59 0.0260(12) 0.0227(12) 0.0282(12) -0.0019(9) 0.0001(9) -0.0011(9) C60 0.0313(13) 0.0234(12) 0.0362(14) -0.0048(10) 0.0030(10) -0.0021(10) C61 0.0352(14) 0.0216(12) 0.0409(15) 0.0017(11) 0.0025(11) -0.0022(10) C62 0.0358(14) 0.0294(13) 0.0300(13) 0.0034(10) -0.0004(11) -0.0007(11) C63 0.0311(13) 0.0258(12) 0.0261(12) -0.0020(10) -0.0033(10) -0.0010(10) C64 0.067(2) 0.0404(17) 0.0345(16) 0.0065(13) 0.0047(15) 0.0012(16) C68 0.0518(18) 0.0250(13) 0.0493(18) -0.0090(12) 0.0100(14) -0.0055(12) C72 0.0249(11) 0.0174(10) 0.0269(12) -0.0033(9) -0.0051(9) -0.0001(9) C73 0.0249(12) 0.0248(12) 0.0272(12) -0.0052(9) -0.0053(9) -0.0007(9) C74 0.0261(12) 0.0268(12) 0.0336(13) -0.0072(10) -0.0025(10) -0.0026(10) C75 0.0237(12) 0.0289(13) 0.0418(15) -0.0066(11) -0.0075(11) -0.0032(10) C76 0.0322(13) 0.0282(13) 0.0342(14) -0.0027(10) -0.0132(11) -0.0038(10) C77 0.0300(12) 0.0238(12) 0.0278(12) -0.0024(9) -0.0065(10) -0.0024(10) C78 0.0585(17) 0.0681(18) 0.0516(16) -0.0092(14) -0.0328(14) -0.0117(15) C83 0.0288(13) 0.0511(18) 0.0417(16) -0.0141(14) 0.0028(12) -0.0078(12) C87 0.0246(11) 0.0217(11) 0.0231(11) -0.0016(9) -0.0053(9) -0.0007(9) C88 0.0266(12) 0.0220(11) 0.0282(12) -0.0022(9) -0.0021(9) -0.0024(9) C89 0.0335(13) 0.0208(11) 0.0284(12) -0.0026(9) -0.0042(10) -0.0023(10) C90 0.0330(13) 0.0267(12) 0.0271(12) -0.0070(10) -0.0037(10) 0.0037(10) C91 0.0250(12) 0.0316(13) 0.0238(11) -0.0022(10) -0.0039(9) 0.0002(10) C92 0.0259(12) 0.0266(12) 0.0242(11) -0.0036(9) -0.0056(9) -0.0030(9) C93 0.0278(12) 0.0560(15) 0.0402(14) -0.0153(12) 0.0014(10) -0.0045(11) C97 0.0438(16) 0.0258(13) 0.0432(16) -0.0110(11) 0.0020(12) -0.0061(11) O5 0.0521(14) 0.0407(12) 0.0580(15) -0.0089(11) 0.0043(11) -0.0099(11) O7 0.0696(17) 0.0321(12) 0.083(2) -0.0165(12) -0.0068(14) 0.0182(12) O9 0.0587(15) 0.0476(14) 0.0771(18) -0.0163(13) -0.0367(14) 0.0144(12) O11 0.0621(16) 0.0705(18) 0.0409(14) -0.0122(12) 0.0019(11) 0.0203(13) N12 0.0229(9) 0.0227(10) 0.0242(10) -0.0061(8) -0.0042(8) -0.0005(8) N28 0.0273(10) 0.0210(9) 0.0225(10) -0.0020(8) -0.0035(8) -0.0011(8) B57 0.0237(12) 0.0214(12) 0.0231(12) -0.0020(10) -0.0033(10) -0.0022(10) _refine_ls_extinction_coef 10.177 _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 3.24(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 C98 . F54 . 1.317(6) yes C98 . F55 . 1.317(5) yes C98 . F56 . 1.338(6) yes C98 . C51 . 1.489(5) yes C99 . F4 . 1.324(5) yes C99 . F5 . 1.332(5) yes C99 . F6 . 1.323(5) yes C99 . C51 . 1.507(4) yes F1 . C78 . 1.269(4) yes F2 . C78 . 1.340(4) yes F3 . C78 . 1.353(4) yes F7 . C93 . 1.337(4) yes F8 . C93 . 1.340(4) yes F9 . C93 . 1.310(4) yes F43 . C44 . 1.346(3) yes F45 . C44 . 1.321(3) yes F46 . C44 . 1.339(3) yes F51 . C78 . 1.375(5) yes F52 . C78 . 1.352(5) yes F53 . C78 . 1.236(5) yes F57 . C93 . 1.340(5) yes F58 . C93 . 1.278(5) yes F59 . C93 . 1.330(5) yes F65 . C64 . 1.320(4) yes F66 . C64 . 1.306(5) yes F67 . C64 . 1.338(5) yes F69 . C68 . 1.325(4) yes F70 . C68 . 1.344(4) yes F71 . C68 . 1.328(4) yes F84 . C83 . 1.330(4) yes F85 . C83 . 1.350(4) yes F86 . C83 . 1.337(4) yes F98 . C97 . 1.343(4) yes F99 . C97 . 1.336(4) yes F100 . C97 . 1.337(4) yes Ga1 . Co2 . 2.3066(5) yes Ga1 . N12 . 1.886(2) yes Ga1 . N28 . 1.889(2) yes Co2 . C4 . 1.800(4) yes Co2 . C6 . 1.813(3) yes Co2 . C8 . 1.807(3) yes Co2 . C10 . 1.820(3) yes C4 . O5 . 1.133(4) yes C6 . O7 . 1.123(4) yes C8 . O9 . 1.133(4) yes C10 . O11 . 1.127(4) yes C11 . C13 . 1.404(4) yes C11 . C15 . 1.400(4) yes C11 . C22 . 1.515(4) yes C13 . C18 . 1.402(4) yes C13 . N12 . 1.453(3) yes C15 . C16 . 1.380(5) yes C15 . H151 . 0.950 no C16 . C17 . 1.377(4) yes C16 . H161 . 0.949 no C17 . C18 . 1.395(4) yes C17 . H171 . 0.954 no C18 . C19 . 1.523(4) yes C19 . C20 . 1.530(5) yes C19 . C21 . 1.525(5) yes C19 . H191 . 0.975 no C20 . H201 . 0.978 no C20 . H202 . 0.970 no C20 . H203 . 0.972 no C21 . H211 . 0.958 no C21 . H212 . 0.973 no C21 . H213 . 0.964 no C22 . C23 . 1.536(4) yes C22 . C24 . 1.529(4) yes C22 . H221 . 0.981 no C23 . H231 . 0.971 no C23 . H232 . 0.966 no C23 . H233 . 0.966 no C24 . H241 . 0.965 no C24 . H242 . 0.971 no C24 . H243 . 0.964 no C25 . C26 . 1.388(4) yes C25 . C42 . 1.505(3) yes C25 . N12 . 1.350(3) yes C26 . C28 . 1.398(4) yes C26 . H261 . 0.938 no C28 . C41 . 1.494(4) yes C28 . N28 . 1.348(3) yes C29 . C30 . 1.403(4) yes C29 . C37 . 1.402(4) yes C29 . N28 . 1.460(3) yes C30 . C31 . 1.517(4) yes C30 . C34 . 1.398(4) yes C31 . C32 . 1.528(4) yes C31 . C33 . 1.519(4) yes C31 . H311 . 1.002 no C32 . H321 . 0.969 no C32 . H322 . 0.968 no C32 . H323 . 0.970 no C33 . H331 . 0.978 no C33 . H332 . 0.965 no C33 . H333 . 0.969 no C34 . C35 . 1.376(5) yes C34 . H341 . 0.950 no C35 . C36 . 1.380(5) yes C35 . H351 . 0.952 no C36 . C37 . 1.395(4) yes C36 . H361 . 0.949 no C37 . C38 . 1.520(4) yes C38 . C39 . 1.524(5) yes C38 . C40 . 1.523(6) yes C38 . H381 . 0.990 no C39 . H391 . 0.968 no C39 . H392 . 0.952 no C39 . H393 . 0.971 no C40 . H401 . 0.966 no C40 . H402 . 0.974 no C40 . H403 . 0.966 no C41 . H411 . 0.971 no C41 . H412 . 0.969 no C41 . H413 . 0.956 no C42 . H421 . 0.958 no C42 . H422 . 0.960 no C42 . H423 . 0.957 no C44 . C47 . 1.498(3) yes C47 . C48 . 1.395(3) yes C47 . C52 . 1.379(4) yes C48 . C49 . 1.398(3) yes C48 . H481 . 0.958 no C49 . C50 . 1.403(3) yes C49 . B57 . 1.640(3) yes C50 . C51 . 1.392(4) yes C50 . H501 . 0.943 no C51 . C52 . 1.387(4) yes C51 . C52 . 1.387(4) yes C52 . H521 . 0.941 no C58 . C59 . 1.406(4) yes C58 . C63 . 1.396(3) yes C58 . B57 . 1.636(4) yes C59 . C60 . 1.392(4) yes C59 . H591 . 0.956 no C60 . C61 . 1.389(4) yes C60 . C68 . 1.498(4) yes C61 . C62 . 1.378(4) yes C61 . H611 . 0.948 no C62 . C63 . 1.397(4) yes C62 . C64 . 1.503(4) yes C63 . H631 . 0.947 no C72 . C73 . 1.399(4) yes C72 . C77 . 1.403(3) yes C72 . B57 . 1.643(4) yes C73 . C74 . 1.394(4) yes C73 . H731 . 0.949 no C74 . C75 . 1.385(4) yes C74 . C83 . 1.496(4) yes C75 . C76 . 1.384(4) yes C75 . H751 . 0.949 no C76 . C77 . 1.384(4) yes C76 . C78 . 1.484(3) yes C77 . H771 . 0.949 no C87 . C88 . 1.399(3) yes C87 . C92 . 1.402(3) yes C87 . B57 . 1.639(4) yes C88 . C89 . 1.394(4) yes C88 . H881 . 0.942 no C89 . C90 . 1.382(4) yes C89 . C97 . 1.495(4) yes C90 . C91 . 1.392(4) yes C90 . H901 . 0.946 no C91 . C92 . 1.390(4) yes C91 . C93 . 1.496(3) yes C92 . H921 . 0.959 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 F54 . C98 . F55 . 106.16(6) yes F54 . C98 . F56 . 106.16(6) yes F55 . C98 . F56 . 106.21(6) yes F54 . C98 . C51 . 113.4(5) yes F55 . C98 . C51 . 114.8(5) yes F56 . C98 . C51 . 109.5(5) yes F4 . C99 . F5 . 106.19(6) yes F4 . C99 . F6 . 106.16(6) yes F5 . C99 . F6 . 106.19(6) yes F4 . C99 . C51 . 111.8(4) yes F5 . C99 . C51 . 112.0(4) yes F6 . C99 . C51 . 114.0(4) yes Co2 . Ga1 . N12 . 129.41(6) yes Co2 . Ga1 . N28 . 130.15(6) yes N12 . Ga1 . N28 . 100.21(9) yes Ga1 . Co2 . C4 . 82.74(9) yes Ga1 . Co2 . C6 . 176.14(12) yes C4 . Co2 . C6 . 94.18(15) yes Ga1 . Co2 . C8 . 86.93(9) yes C4 . Co2 . C8 . 122.06(16) yes C6 . Co2 . C8 . 92.78(15) yes Ga1 . Co2 . C10 . 90.00(10) yes C4 . Co2 . C10 . 119.08(15) yes C6 . Co2 . C10 . 93.54(15) yes C8 . Co2 . C10 . 117.74(16) yes Co2 . C4 . O5 . 176.7(3) yes Co2 . C6 . O7 . 179.6(3) yes Co2 . C8 . O9 . 174.3(3) yes Co2 . C10 . O11 . 173.4(3) yes C13 . C11 . C15 . 117.1(3) yes C13 . C11 . C22 . 123.6(2) yes C15 . C11 . C22 . 119.2(2) yes C11 . C13 . C18 . 122.3(2) yes C11 . C13 . N12 . 119.6(2) yes C18 . C13 . N12 . 118.1(2) yes C11 . C15 . C16 . 121.4(3) yes C11 . C15 . H151 . 119.2 no C16 . C15 . H151 . 119.4 no C15 . C16 . C17 . 120.3(3) yes C15 . C16 . H161 . 120.8 no C17 . C16 . H161 . 118.9 no C16 . C17 . C18 . 121.0(3) yes C16 . C17 . H171 . 119.1 no C18 . C17 . H171 . 119.9 no C13 . C18 . C17 . 117.8(3) yes C13 . C18 . C19 . 122.7(2) yes C17 . C18 . C19 . 119.3(3) yes C18 . C19 . C20 . 109.2(3) yes C18 . C19 . C21 . 113.0(3) yes C20 . C19 . C21 . 110.3(3) yes C18 . C19 . H191 . 108.2 no C20 . C19 . H191 . 107.9 no C21 . C19 . H191 . 108.1 no C19 . C20 . H201 . 110.4 no C19 . C20 . H202 . 110.0 no H201 . C20 . H202 . 109.2 no C19 . C20 . H203 . 109.6 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 108.0 no C19 . C21 . H211 . 108.2 no C19 . C21 . H212 . 108.6 no H211 . C21 . H212 . 109.4 no C19 . C21 . H213 . 110.3 no H211 . C21 . H213 . 109.0 no H212 . C21 . H213 . 111.1 no C11 . C22 . C23 . 112.5(3) yes C11 . C22 . C24 . 110.3(3) yes C23 . C22 . C24 . 109.5(3) yes C11 . C22 . H221 . 108.4 no C23 . C22 . H221 . 107.1 no C24 . C22 . H221 . 108.9 no C22 . C23 . H231 . 110.3 no C22 . C23 . H232 . 109.2 no H231 . C23 . H232 . 109.3 no C22 . C23 . H233 . 109.3 no H231 . C23 . H233 . 110.1 no H232 . C23 . H233 . 108.7 no C22 . C24 . H241 . 110.4 no C22 . C24 . H242 . 111.5 no H241 . C24 . H242 . 108.8 no C22 . C24 . H243 . 109.9 no H241 . C24 . H243 . 108.1 no H242 . C24 . H243 . 108.0 no C26 . C25 . C42 . 117.7(2) yes C26 . C25 . N12 . 123.5(2) yes C42 . C25 . N12 . 118.8(2) yes C25 . C26 . C28 . 129.4(2) yes C25 . C26 . H261 . 115.9 no C28 . C26 . H261 . 114.8 no C26 . C28 . C41 . 117.3(2) yes C26 . C28 . N28 . 123.2(2) yes C41 . C28 . N28 . 119.5(2) yes C30 . C29 . C37 . 123.2(2) yes C30 . C29 . N28 . 118.3(2) yes C37 . C29 . N28 . 118.5(2) yes C29 . C30 . C31 . 123.0(2) yes C29 . C30 . C34 . 116.9(3) yes C31 . C30 . C34 . 120.0(3) yes C30 . C31 . C32 . 112.9(2) yes C30 . C31 . C33 . 111.1(3) yes C32 . C31 . C33 . 110.1(3) yes C30 . C31 . H311 . 106.8 no C32 . C31 . H311 . 109.6 no C33 . C31 . H311 . 106.1 no C31 . C32 . H321 . 109.6 no C31 . C32 . H322 . 108.9 no H321 . C32 . H322 . 111.5 no C31 . C32 . H323 . 108.5 no H321 . C32 . H323 . 108.6 no H322 . C32 . H323 . 109.7 no C31 . C33 . H331 . 109.6 no C31 . C33 . H332 . 109.0 no H331 . C33 . H332 . 110.2 no C31 . C33 . H333 . 107.9 no H331 . C33 . H333 . 109.7 no H332 . C33 . H333 . 110.4 no C30 . C34 . C35 . 121.1(3) yes C30 . C34 . H341 . 119.8 no C35 . C34 . H341 . 119.1 no C34 . C35 . C36 . 120.7(3) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 119.6 no C35 . C36 . C37 . 121.1(3) yes C35 . C36 . H361 . 119.8 no C37 . C36 . H361 . 119.1 no C29 . C37 . C36 . 116.9(3) yes C29 . C37 . C38 . 123.5(2) yes C36 . C37 . C38 . 119.6(3) yes C37 . C38 . C39 . 112.7(3) yes C37 . C38 . C40 . 110.1(3) yes C39 . C38 . C40 . 109.3(4) yes C37 . C38 . H381 . 107.6 no C39 . C38 . H381 . 108.4 no C40 . C38 . H381 . 108.7 no C38 . C39 . H391 . 108.4 no C38 . C39 . H392 . 109.4 no H391 . C39 . H392 . 109.9 no C38 . C39 . H393 . 108.5 no H391 . C39 . H393 . 109.9 no H392 . C39 . H393 . 110.8 no C38 . C40 . H401 . 108.9 no C38 . C40 . H402 . 108.3 no H401 . C40 . H402 . 110.6 no C38 . C40 . H403 . 108.9 no H401 . C40 . H403 . 110.1 no H402 . C40 . H403 . 109.9 no C28 . C41 . H411 . 112.3 no C28 . C41 . H412 . 110.4 no H411 . C41 . H412 . 109.0 no C28 . C41 . H413 . 108.9 no H411 . C41 . H413 . 108.6 no H412 . C41 . H413 . 107.5 no C25 . C42 . H421 . 109.4 no C25 . C42 . H422 . 109.6 no H421 . C42 . H422 . 109.4 no C25 . C42 . H423 . 109.5 no H421 . C42 . H423 . 109.7 no H422 . C42 . H423 . 109.2 no F43 . C44 . F46 . 104.6(2) yes F43 . C44 . F45 . 106.6(2) yes F46 . C44 . F45 . 107.1(2) yes F43 . C44 . C47 . 111.7(2) yes F46 . C44 . C47 . 112.7(2) yes F45 . C44 . C47 . 113.5(2) yes C44 . C47 . C48 . 118.4(2) yes C44 . C47 . C52 . 120.6(2) yes C48 . C47 . C52 . 121.0(2) yes C47 . C48 . C49 . 122.3(2) yes C47 . C48 . H481 . 118.3 no C49 . C48 . H481 . 119.4 no C48 . C49 . C50 . 115.6(2) yes C48 . C49 . B57 . 123.1(2) yes C50 . C49 . B57 . 121.1(2) yes C49 . C50 . C51 . 122.1(2) yes C49 . C50 . H501 . 120.2 no C51 . C50 . H501 . 117.7 no C99 . C51 . C50 . 120.4(3) yes C99 . C51 . C52 . 118.7(3) yes C50 . C51 . C52 . 120.9(2) yes C98 . C51 . C50 . 117.9(3) yes C98 . C51 . C52 . 121.2(3) yes C50 . C51 . C52 . 120.9(2) yes C51 . C52 . C47 . 118.0(2) yes C51 . C52 . H521 . 120.3 no C47 . C52 . H521 . 121.7 no C59 . C58 . C63 . 115.7(2) yes C59 . C58 . B57 . 120.0(2) yes C63 . C58 . B57 . 124.2(2) yes C58 . C59 . C60 . 122.3(2) yes C58 . C59 . H591 . 118.8 no C60 . C59 . H591 . 118.9 no C59 . C60 . C61 . 120.6(3) yes C59 . C60 . C68 . 120.5(3) yes C61 . C60 . C68 . 118.8(2) yes C60 . C61 . C62 . 118.2(2) yes C60 . C61 . H611 . 120.3 no C62 . C61 . H611 . 121.5 no C61 . C62 . C63 . 121.2(3) yes C61 . C62 . C64 . 119.9(3) yes C63 . C62 . C64 . 118.9(3) yes C62 . C63 . C58 . 122.0(3) yes C62 . C63 . H631 . 118.5 no C58 . C63 . H631 . 119.5 no C62 . C64 . F67 . 112.0(3) yes C62 . C64 . F65 . 113.1(3) yes F67 . C64 . F65 . 104.3(3) yes C62 . C64 . F66 . 112.3(3) yes F67 . C64 . F66 . 104.4(4) yes F65 . C64 . F66 . 110.1(3) yes C60 . C68 . F70 . 112.2(3) yes C60 . C68 . F71 . 112.7(2) yes F70 . C68 . F71 . 105.3(3) yes C60 . C68 . F69 . 112.9(3) yes F70 . C68 . F69 . 104.9(2) yes F71 . C68 . F69 . 108.2(3) yes C73 . C72 . C77 . 115.7(2) yes C73 . C72 . B57 . 125.5(2) yes C77 . C72 . B57 . 118.7(2) yes C72 . C73 . C74 . 122.0(2) yes C72 . C73 . H731 . 119.0 no C74 . C73 . H731 . 119.0 no C73 . C74 . C75 . 120.9(2) yes C73 . C74 . C83 . 120.8(2) yes C75 . C74 . C83 . 118.3(2) yes C74 . C75 . C76 . 117.9(2) yes C74 . C75 . H751 . 120.9 no C76 . C75 . H751 . 121.2 no C75 . C76 . C77 . 121.2(2) yes C75 . C76 . C78 . 120.0(2) yes C77 . C76 . C78 . 118.8(3) yes C72 . C77 . C76 . 122.2(2) yes C72 . C77 . H771 . 118.7 no C76 . C77 . H771 . 119.1 no C76 . C78 . F3 . 111.0(2) yes C76 . C78 . F2 . 114.1(3) yes F3 . C78 . F2 . 104.11(6) yes C76 . C78 . F1 . 117.3(3) yes F3 . C78 . F1 . 104.44(6) yes F2 . C78 . F1 . 104.55(6) yes C76 . C78 . F51 . 109.4(3) yes C76 . C78 . F52 . 108.9(3) yes F51 . C78 . F52 . 104.20(6) yes C76 . C78 . F53 . 123.7(3) yes F51 . C78 . F53 . 104.45(6) yes F52 . C78 . F53 . 104.53(6) yes C74 . C83 . F85 . 112.3(2) yes C74 . C83 . F86 . 112.1(3) yes F85 . C83 . F86 . 108.3(3) yes C74 . C83 . F84 . 113.1(3) yes F85 . C83 . F84 . 104.9(3) yes F86 . C83 . F84 . 105.6(2) yes C88 . C87 . C92 . 116.2(2) yes C88 . C87 . B57 . 123.1(2) yes C92 . C87 . B57 . 120.4(2) yes C87 . C88 . C89 . 122.0(2) yes C87 . C88 . H881 . 120.4 no C89 . C88 . H881 . 117.6 no C88 . C89 . C90 . 121.0(2) yes C88 . C89 . C97 . 119.6(2) yes C90 . C89 . C97 . 119.4(2) yes C89 . C90 . C91 . 117.9(2) yes C89 . C90 . H901 . 121.1 no C91 . C90 . H901 . 120.9 no C90 . C91 . C92 . 121.1(2) yes C90 . C91 . C93 . 118.9(2) yes C92 . C91 . C93 . 120.1(2) yes C87 . C92 . C91 . 121.8(2) yes C87 . C92 . H921 . 118.8 no C91 . C92 . H921 . 119.4 no C91 . C93 . F8 . 112.2(2) yes C91 . C93 . F7 . 111.9(2) yes F8 . C93 . F7 . 105.75(6) yes C91 . C93 . F9 . 114.5(2) yes F8 . C93 . F9 . 105.87(6) yes F7 . C93 . F9 . 106.01(6) yes C91 . C93 . F57 . 111.6(3) yes C91 . C93 . F59 . 108.9(3) yes F57 . C93 . F59 . 105.79(6) yes C91 . C93 . F58 . 117.9(3) yes F57 . C93 . F58 . 105.96(6) yes F59 . C93 . F58 . 105.91(6) yes C89 . C97 . F98 . 111.9(2) yes C89 . C97 . F100 . 112.8(3) yes F98 . C97 . F100 . 105.5(3) yes C89 . C97 . F99 . 113.3(2) yes F98 . C97 . F99 . 106.2(3) yes F100 . C97 . F99 . 106.7(2) yes C13 . N12 . C25 . 119.6(2) yes C13 . N12 . Ga1 . 118.32(15) yes C25 . N12 . Ga1 . 121.69(17) yes C29 . N28 . Ga1 . 118.30(16) yes C29 . N28 . C28 . 119.8(2) yes Ga1 . N28 . C28 . 121.77(17) yes C72 . B57 . C49 . 113.3(2) yes C72 . B57 . C87 . 110.9(2) yes C49 . B57 . C87 . 103.57(18) yes C72 . B57 . C58 . 104.74(19) yes C49 . B57 . C58 . 111.5(2) yes C87 . B57 . C58 . 113.1(2) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C19 . H191 . C25 . 129.74 0.975 2.580 3.290(4) yes C38 . H381 . C28 . 130.82 0.990 2.592 3.324(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 28/07/13 at 16:30:07 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) 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) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 203,X'S) H ( 202,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 213,X'S) H ( 212,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 232,X'S) H ( 231,X'S) H ( 233,X'S) RIDE C ( 24,X'S) H ( 243,X'S) H ( 242,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 323,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 333,X'S) H ( 332,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 393,X'S) H ( 392,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 403,X'S) H ( 402,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 413,X'S) H ( 412,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 63,X'S) H ( 631,X'S) RIDE C ( 73,X'S) H ( 731,X'S) RIDE C ( 75,X'S) H ( 751,X'S) RIDE C ( 77,X'S) H ( 771,X'S) RIDE C ( 88,X'S) H ( 881,X'S) RIDE C ( 90,X'S) H ( 901,X'S) RIDE C ( 92,X'S) H ( 921,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 28/07/13 at 16:30:07 # #LIST 16 SAME C(78) F(1) F(2) F(3) AND CONT C(78) F(2) F(3) F(1) AND CONT C(78) F(3) F(1) F(2) AND CONT C(78) F(51) F(52) F(53) AND CONT C(78) F(52) F(53) F(51) AND CONT C(78) F(53) F(51) F(52) SIMU 0.01 C(78) F(1) F(2) F(3) AND CONT C(78) F(2) F(3) F(1) AND CONT C(78) F(3) F(1) F(2) AND CONT C(78) F(51) F(52) F(53) AND CONT C(78) F(52) F(53) F(51) AND CONT C(78) F(53) F(51) F(52) DELU 0.01 C(78) F(1) F(2) F(3) AND CONT C(78) F(2) F(3) F(1) AND CONT C(78) F(3) F(1) F(2) AND CONT C(78) F(51) F(52) F(53) AND CONT C(78) F(52) F(53) F(51) AND CONT C(78) F(53) F(51) F(52) SAME C(99) F(4) F(5) F(6) AND CONT C(99) F(5) F(6) F(4) AND CONT C(99) F(6) F(4) F(5) AND CONT C(98) F(54) F(55) F(56) AND CONT C(98) F(55) F(56) F(54) AND CONT C(98) F(56) F(54) F(55) SIMU 0.01 C(99) F(4) F(5) F(6) AND CONT C(99) F(5) F(6) F(4) AND CONT C(99) F(6) F(4) F(5) AND CONT C(98) F(54) F(55) F(56) AND CONT C(98) F(55) F(56) F(54) AND CONT C(98) F(56) F(54) F(55) DELU 0.01 C(99) F(4) F(5) F(6) AND CONT C(99) F(5) F(6) F(4) AND CONT C(99) F(6) F(4) F(5) AND CONT C(98) F(54) F(55) F(56) AND CONT C(98) F(55) F(56) F(54) AND CONT C(98) F(56) F(54) F(55) SAME C(93) F(7) F(8) F(9) AND CONT C(93) F(8) F(9) F(7) AND CONT C(93) F(9) F(7) F(8) AND CONT C(93) F(57) F(58) F(59) AND CONT C(93) F(58) F(59) F(57) AND CONT C(93) F(59) F(57) F(58) SIMU 0.01 C(93) F(7) F(8) F(9) AND CONT C(93) F(8) F(9) F(7) AND CONT C(93) F(9) F(7) F(8) AND CONT C(93) F(57) F(58) F(59) AND CONT C(93) F(58) F(59) F(57) AND CONT C(93) F(59) F(57) F(58) DELU 0.01 C(93) F(7) F(8) F(9) AND CONT C(93) F(8) F(9) F(7) AND CONT C(93) F(9) F(7) F(8) AND CONT C(93) F(57) F(58) F(59) AND CONT C(93) F(58) F(59) F(57) AND CONT C(93) F(59) F(57) F(58) 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 0.500 18 0 ' ' 2 0.378 0.321 0.808 46 1 ' ' 3 0.622 0.678 0.192 46 1 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952955'