#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:40:26 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267183 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/74/7707481.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7707481 loop_ _publ_author_name 'Dodonov, Vladimir A.' 'Kushnerova, Olga A.' 'Baranov, Evgeny V.' 'Novikov, Alexander S.' 'Fedushkin, Igor L.' _publ_section_title ; Activation and modification of carbon dioxide by redox-active low-valent gallium species. ; _journal_issue 25 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8899 _journal_page_last 8906 _journal_paper_doi 10.1039/d1dt01199e _journal_volume 50 _journal_year 2021 _chemical_formula_sum 'C102 H130 Ga2 N6 Na2 O12' _chemical_formula_weight 1817.53 _space_group_crystal_system tetragonal _space_group_IT_number 92 _space_group_name_Hall 'P 4abw 2nw' _space_group_name_H-M_alt 'P 41 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-05-04 deposited with the CCDC. 2021-05-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.1442(16) _cell_length_b 15.1442(16) _cell_length_c 43.794(5) _cell_measurement_reflns_used 9939 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 23.20 _cell_measurement_theta_min 2.69 _cell_volume 10044.0(19) _computing_cell_refinement SAINT _computing_data_collection APEX3 _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution SHELXT-2014/5 _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 Quest (CMOS)' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1388 _diffrn_reflns_av_unetI/netI 0.0787 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_number 91251 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 2.359 _diffrn_source 'microfocus tube' _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_correction_T_min 0.4475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS-2016/2 _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.202 _exptl_crystal_description prism _exptl_crystal_F_000 3856 _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.381 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 627 _refine_ls_number_reflns 9887 _refine_ls_number_restraints 864 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0617 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+3.3775P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1380 _refine_ls_wR_factor_ref 0.1515 _reflns_Friedel_coverage 0.747 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 7026 _reflns_number_total 9887 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01199e25.cif _cod_data_source_block biangaphnco2 _cod_depositor_comments 'Adding full bibliography for 7707480--7707489.cif.' _cod_original_cell_volume 10044(2) _cod_database_code 7707481 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.821 _shelx_estimated_absorpt_t_max 0.931 _shelx_res_file ; TITL biangaphnco2 in P4(1)2(1)2 biangaphnco2.res created by SHELXL-2018/3 at 18:39:27 on 29-Apr-2021 CELL 0.71073 15.14420 15.14420 43.79420 90.0000 90.0000 90.0000 ZERR 4.00 0.00160 0.00160 0.00500 0.0000 0.0000 0.0000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-Y, 0.5+X, 0.25+Z SYMM 0.5+Y, 0.5-X, 0.75+Z SYMM 0.5-X, 0.5+Y, 0.25-Z SYMM 0.5+X, 0.5-Y, 0.75-Z SYMM Y, X, -Z SYMM -Y, -X, 0.5-Z SFAC C H N O NA GA UNIT 408 520 24 48 8 8 SIZE 0.12 0.19 0.34 TEMP -123.00 L.S. 84 BOND $H LIST 4 FMAP 2 PLAN 20 TWIN OMIT 0 52 OMIT 0 1 3 ACTA RIGU ISOR 0.010 0.005 C20 C29 C33 C34 ISOR 0.010 0.005 C44 > C51 EADP O5 O5' EADP O6 O6' EADP C48 C48' EADP C49 C49' EADP C50 C50' EADP C51 C51' DFIX 31.0 0.005 O5 C48 O5' C48' O5 C49 O5' C49' DFIX 31.0 0.005 O6 C50 O6' C50' O6 C51 O6' C51' DFIX 41.0 0.005 C49 C50 C49' C50' SADI 0.01 C48 C49 C48' C49' C50 C51 C50' C51' EADP O3 O3' EADP O4 O4' EADP C44 C44' EADP C45 C45' EADP C46 C46' EADP C47 C47' DFIX 31.0 0.005 O3 C44 O3' C44' O3 C45 O3' C45' DFIX 31.0 0.005 O4 C46 O4' C46' O4 C47 O4' C47' DFIX 41.0 0.005 C45 C46 C45' C46' SADI 0.01 C44 C45 C44' C45' C46 C47 C46' C47' EADP C35 C35' EADP C36 C36' DFIX 71.0 0.005 C34 C35 C34 C36 C34 C35' C34 C36' DFIX 81.0 0.010 C35 C36 C35' C36' CONN 10 Na1 ISOR 0.005 c11 c24 c36 WGHT 0.076400 3.377500 BASF 0.06993 FVAR 0.07402 0.46133 1.39752 1.49200 0.67682 0.35586 1.53990 FVAR 2.52113 GA1 6 0.281528 0.315759 0.296992 11.00000 0.03765 0.03930 = 0.03981 0.00560 -0.00557 -0.00471 NA1 5 0.448548 0.634911 0.284329 11.00000 0.09472 0.06065 = 0.06938 -0.00094 0.02146 -0.02385 O1 4 0.359511 0.383550 0.271092 11.00000 0.04745 0.05260 = 0.05124 0.00668 0.00961 -0.01005 O2 4 0.342516 0.531308 0.268854 11.00000 0.07150 0.05006 = 0.06658 0.01826 0.00707 -0.01455 N1 3 0.319194 0.248982 0.330422 11.00000 0.04031 0.04658 = 0.03314 0.00728 -0.01067 -0.00353 N2 3 0.208089 0.224642 0.283837 11.00000 0.05034 0.04988 = 0.03799 0.00887 -0.01243 -0.01190 N3 3 0.253465 0.437835 0.298377 11.00000 0.04473 0.04798 = 0.05126 0.01790 0.00775 0.00020 C1 1 0.276505 0.168897 0.328381 11.00000 0.03282 0.03798 = 0.03794 0.00699 0.00242 -0.00059 C2 1 0.218582 0.156669 0.304600 11.00000 0.04259 0.04201 = 0.03562 0.00244 0.00128 -0.00572 C3 1 0.175631 0.070784 0.307725 11.00000 0.05487 0.04343 = 0.04622 -0.01081 0.01570 -0.01078 C4 1 0.212589 0.033391 0.334637 11.00000 0.06462 0.04056 = 0.06350 0.01016 0.02533 0.00315 C5 1 0.275939 0.091394 0.348040 11.00000 0.05132 0.05087 = 0.05392 0.02043 0.00795 0.00858 C6 1 0.317736 0.066248 0.374600 11.00000 0.08055 0.10814 = 0.08242 0.05387 -0.01105 0.00204 AFIX 43 H6A 2 0.358850 0.103851 0.384568 11.00000 -1.20000 AFIX 0 C7 1 0.296315 -0.019200 0.386479 11.00000 0.11764 0.12256 = 0.15723 0.10000 -0.02035 0.00320 AFIX 43 H7A 2 0.325363 -0.038261 0.404540 11.00000 -1.20000 AFIX 0 C8 1 0.236709 -0.074583 0.373345 11.00000 0.13318 0.08667 = 0.13410 0.06428 0.02879 0.00391 AFIX 43 H8A 2 0.225905 -0.130876 0.382158 11.00000 -1.20000 AFIX 0 C9 1 0.189894 -0.048619 0.346223 11.00000 0.09207 0.05158 = 0.10562 0.01969 0.03768 -0.00385 C10 1 0.125743 -0.095216 0.329488 11.00000 0.12746 0.05430 = 0.12343 -0.00238 0.05360 -0.03436 AFIX 43 H10A 2 0.107930 -0.152046 0.336302 11.00000 -1.20000 AFIX 0 C11 1 0.089482 -0.061891 0.304451 11.00000 0.10336 0.08185 = 0.10571 -0.02064 0.02817 -0.03486 AFIX 43 H11A 2 0.046273 -0.095657 0.293917 11.00000 -1.20000 AFIX 0 C12 1 0.113062 0.023015 0.292735 11.00000 0.08571 0.08100 = 0.07119 -0.01701 0.01641 -0.04519 AFIX 43 H12A 2 0.085627 0.045614 0.274861 11.00000 -1.20000 AFIX 0 C13 1 0.396298 0.258314 0.349060 11.00000 0.03338 0.05992 = 0.04482 -0.00049 -0.01001 -0.00046 C14 1 0.389857 0.306856 0.376689 11.00000 0.03754 0.10415 = 0.04281 -0.01012 -0.00379 -0.00193 C15 1 0.466320 0.318946 0.393834 11.00000 0.05289 0.15317 = 0.04992 -0.02740 -0.01022 -0.00022 AFIX 43 H15A 2 0.463040 0.351630 0.412315 11.00000 -1.20000 AFIX 0 C16 1 0.545910 0.285269 0.384907 11.00000 0.04318 0.12389 = 0.06105 -0.00942 -0.01999 -0.00945 AFIX 43 H16A 2 0.597129 0.294517 0.397016 11.00000 -1.20000 AFIX 0 C17 1 0.551040 0.237942 0.358260 11.00000 0.03859 0.08733 = 0.08210 -0.00910 -0.01642 0.01149 AFIX 43 H17A 2 0.606095 0.213656 0.352131 11.00000 -1.20000 AFIX 0 C18 1 0.476066 0.224830 0.339883 11.00000 0.04373 0.05596 = 0.05828 -0.00914 -0.01121 0.00524 C19 1 0.302538 0.345952 0.387946 11.00000 0.04277 0.15119 = 0.06551 -0.03024 -0.00741 -0.00220 AFIX 13 H19A 2 0.253925 0.321405 0.375033 11.00000 -1.20000 AFIX 0 C20 1 0.281323 0.328074 0.419810 11.00000 0.08041 0.13919 = 0.08321 -0.01886 0.00506 0.00065 AFIX 137 H20A 2 0.224753 0.355754 0.424953 11.00000 -1.50000 H20B 2 0.327822 0.352295 0.432927 11.00000 -1.50000 H20C 2 0.277129 0.264152 0.422977 11.00000 -1.50000 AFIX 0 C21 1 0.302952 0.448279 0.384023 11.00000 0.10207 0.12655 = 0.12698 -0.04660 -0.00489 0.02705 AFIX 137 H21A 2 0.243001 0.471153 0.386920 11.00000 -1.50000 H21B 2 0.323665 0.463309 0.363470 11.00000 -1.50000 H21C 2 0.342452 0.474692 0.399214 11.00000 -1.50000 AFIX 0 C22 1 0.484668 0.171931 0.310725 11.00000 0.05342 0.08350 = 0.07875 -0.02598 -0.01042 0.01422 AFIX 13 H22A 2 0.424501 0.167846 0.301424 11.00000 -1.20000 AFIX 0 C23 1 0.542802 0.218368 0.288294 11.00000 0.12397 0.07539 = 0.05533 -0.00778 -0.00222 0.02295 AFIX 137 H23A 2 0.519815 0.277884 0.284553 11.00000 -1.50000 H23B 2 0.543890 0.185232 0.269077 11.00000 -1.50000 H23C 2 0.602813 0.222433 0.296548 11.00000 -1.50000 AFIX 0 C24 1 0.516298 0.076756 0.317054 11.00000 0.10668 0.06794 = 0.13853 -0.02107 0.04568 -0.00204 AFIX 137 H24A 2 0.515811 0.042886 0.297987 11.00000 -1.50000 H24B 2 0.476737 0.048747 0.331879 11.00000 -1.50000 H24C 2 0.576423 0.078225 0.325313 11.00000 -1.50000 AFIX 0 C25 1 0.174563 0.204182 0.253649 11.00000 0.06701 0.07695 = 0.03859 0.01128 -0.01549 -0.04121 C26 1 0.227349 0.156343 0.233185 11.00000 0.12241 0.08545 = 0.03910 -0.00191 -0.00344 -0.03139 C27 1 0.192776 0.135858 0.204857 11.00000 0.17189 0.15073 = 0.05588 -0.02579 -0.01714 -0.04800 AFIX 43 H27A 2 0.227348 0.102852 0.190808 11.00000 -1.20000 AFIX 0 C28 1 0.111753 0.161573 0.196871 11.00000 0.14961 0.22974 = 0.06180 -0.01139 -0.03009 -0.08048 AFIX 43 H28A 2 0.090201 0.147370 0.177100 11.00000 -1.20000 AFIX 0 C29 1 0.058351 0.208515 0.216762 11.00000 0.09838 0.19254 = 0.07483 0.02252 -0.03835 -0.04842 AFIX 43 H29A 2 0.000891 0.226278 0.210597 11.00000 -1.20000 AFIX 0 C30 1 0.089352 0.229751 0.246035 11.00000 0.05600 0.16350 = 0.05611 0.02692 -0.02025 -0.03731 C31 1 0.318583 0.129794 0.240423 11.00000 0.14417 0.10562 = 0.05578 -0.00689 0.02518 0.02404 AFIX 13 H31A 2 0.332452 0.153407 0.261201 11.00000 -1.20000 AFIX 0 C32 1 0.387457 0.165021 0.219029 11.00000 0.13863 0.17688 = 0.11829 0.01873 0.00824 -0.02753 AFIX 137 H32A 2 0.445203 0.140420 0.224472 11.00000 -1.50000 H32B 2 0.389540 0.229540 0.220591 11.00000 -1.50000 H32C 2 0.372622 0.148113 0.198046 11.00000 -1.50000 AFIX 0 C33 1 0.328998 0.032195 0.241837 11.00000 0.17295 0.14981 = 0.18236 0.01852 0.03117 0.01471 AFIX 137 H33A 2 0.277046 0.006131 0.251674 11.00000 -1.50000 H33B 2 0.381940 0.017566 0.253669 11.00000 -1.50000 H33C 2 0.334869 0.008598 0.221100 11.00000 -1.50000 AFIX 0 C34 1 0.031724 0.279401 0.267806 11.00000 0.06674 0.17844 = 0.08567 0.03529 -0.02142 0.00284 PART 1 AFIX 13 H34A 2 0.061807 0.269773 0.287858 61.00000 -1.20000 AFIX 13 PART 2 H34B 2 0.055136 0.269030 0.288853 -61.00000 -1.20000 AFIX 0 PART 1 C35 1 0.056317 0.375652 0.260070 61.00000 0.05834 0.18063 = 0.14291 0.03714 -0.02184 0.02753 AFIX 137 H35A 2 0.117160 0.387279 0.266544 61.00000 -1.50000 H35B 2 0.016172 0.415913 0.270756 61.00000 -1.50000 H35C 2 0.051248 0.384930 0.237993 61.00000 -1.50000 AFIX 0 C36 1 -0.066824 0.275063 0.276395 61.00000 0.08642 0.18717 = 0.14425 -0.00818 0.01973 -0.00633 AFIX 137 H36A 2 -0.088732 0.214857 0.273249 61.00000 -1.50000 H36B 2 -0.100283 0.316053 0.263512 61.00000 -1.50000 H36C 2 -0.074148 0.291520 0.297888 61.00000 -1.50000 AFIX 0 PART 2 C35' 1 0.023545 0.379549 0.263324 -61.00000 0.05834 0.18063 = 0.14291 0.03714 -0.02184 0.02753 AFIX 137 H35D 2 -0.015665 0.404029 0.278985 -61.00000 -1.50000 H35E 2 -0.000942 0.391783 0.243048 -61.00000 -1.50000 H35F 2 0.082018 0.406803 0.265078 -61.00000 -1.50000 AFIX 0 C36' 1 -0.059701 0.234855 0.265809 -61.00000 0.08642 0.18717 = 0.14425 -0.00818 0.01973 -0.00633 AFIX 137 H36D 2 -0.052161 0.170997 0.263293 -61.00000 -1.50000 H36E 2 -0.092132 0.258658 0.248281 -61.00000 -1.50000 H36F 2 -0.092891 0.246609 0.284584 -61.00000 -1.50000 AFIX 0 PART 0 C37 1 0.320072 0.457392 0.278890 11.00000 0.04878 0.04489 = 0.04828 0.01081 -0.00338 -0.01584 C38 1 0.192228 0.494612 0.312450 11.00000 0.04633 0.05427 = 0.06873 0.01275 0.00875 0.00968 C39 1 0.192066 0.583823 0.309343 11.00000 0.07863 0.05262 = 0.12862 0.00628 0.01759 0.01004 AFIX 43 H39A 2 0.234568 0.611190 0.296498 11.00000 -1.20000 AFIX 0 C40 1 0.131483 0.635054 0.324463 11.00000 0.11553 0.06426 = 0.19424 -0.00664 0.03461 0.02450 AFIX 43 H40A 2 0.133304 0.697475 0.322406 11.00000 -1.20000 AFIX 0 C41 1 0.068429 0.596669 0.342497 11.00000 0.09832 0.12216 = 0.13561 -0.00603 0.02360 0.04827 AFIX 43 H41A 2 0.025867 0.632338 0.352586 11.00000 -1.20000 AFIX 0 C42 1 0.066749 0.508004 0.345944 11.00000 0.08545 0.11985 = 0.11486 0.03232 0.04534 0.04159 AFIX 43 H42A 2 0.023655 0.480957 0.358632 11.00000 -1.20000 AFIX 0 C43 1 0.127563 0.458018 0.331007 11.00000 0.07082 0.07936 = 0.08940 0.02849 0.02664 0.01457 AFIX 43 H43A 2 0.125720 0.395686 0.333363 11.00000 -1.20000 AFIX 0 PART 1 O3 4 0.410307 0.612733 0.337901 51.00000 0.09437 0.11045 = 0.07414 -0.00032 -0.00311 0.00380 O4 4 0.549861 0.541083 0.305598 51.00000 0.08541 0.08145 = 0.08758 0.01307 0.00853 -0.01486 C44 1 0.366987 0.674812 0.356149 51.00000 0.10868 0.11275 = 0.09944 -0.00477 0.00433 0.00677 AFIX 137 H44A 2 0.315297 0.697622 0.345239 51.00000 -1.50000 H44B 2 0.407320 0.723600 0.360795 51.00000 -1.50000 H44C 2 0.347964 0.646749 0.375209 51.00000 -1.50000 AFIX 0 C45 1 0.484143 0.576742 0.352414 51.00000 0.09422 0.09252 = 0.07784 0.00886 -0.00361 -0.00473 AFIX 23 H45A 2 0.466891 0.553132 0.372632 51.00000 -1.20000 H45B 2 0.529065 0.623320 0.355620 51.00000 -1.20000 AFIX 0 C46 1 0.522353 0.504175 0.333311 51.00000 0.10326 0.07673 = 0.09391 0.01578 0.00290 -0.00347 AFIX 23 H46A 2 0.573121 0.476810 0.343954 51.00000 -1.20000 H46B 2 0.477346 0.458001 0.329590 51.00000 -1.20000 AFIX 0 C47 1 0.591356 0.478164 0.287115 51.00000 0.10615 0.09979 = 0.11437 0.00208 0.00622 0.00111 AFIX 137 H47A 2 0.550137 0.429847 0.282824 51.00000 -1.50000 H47B 2 0.643381 0.454814 0.297693 51.00000 -1.50000 H47C 2 0.609610 0.505766 0.267885 51.00000 -1.50000 AFIX 0 PART 2 O3' 4 0.439074 0.593693 0.338936 -51.00000 0.09437 0.11045 = 0.07414 -0.00032 -0.00311 0.00380 O4' 4 0.571006 0.520375 0.303338 -51.00000 0.08541 0.08145 = 0.08758 0.01307 0.00853 -0.01486 C44' 1 0.412208 0.656395 0.360444 -51.00000 0.10868 0.11275 = 0.09944 -0.00477 0.00433 0.00677 AFIX 137 H44D 2 0.419631 0.715771 0.351925 -51.00000 -1.50000 H44E 2 0.448217 0.650561 0.378927 -51.00000 -1.50000 H44F 2 0.349942 0.646806 0.365557 -51.00000 -1.50000 AFIX 0 C45' 1 0.506364 0.539942 0.350398 -51.00000 0.09422 0.09252 = 0.07784 0.00886 -0.00361 -0.00473 AFIX 23 H45C 2 0.483130 0.508373 0.368489 -51.00000 -1.20000 H45D 2 0.554853 0.578626 0.357534 -51.00000 -1.20000 AFIX 0 C46' 1 0.544645 0.473199 0.329186 -51.00000 0.10326 0.07673 = 0.09391 0.01578 0.00290 -0.00347 AFIX 23 H46C 2 0.595817 0.443284 0.338718 -51.00000 -1.20000 H46D 2 0.499976 0.428154 0.323728 -51.00000 -1.20000 AFIX 0 C47' 1 0.636671 0.475071 0.287281 -51.00000 0.10615 0.09979 = 0.11437 0.00208 0.00622 0.00111 AFIX 137 H47D 2 0.652892 0.421444 0.298479 -51.00000 -1.50000 H47E 2 0.688704 0.513021 0.285094 -51.00000 -1.50000 H47F 2 0.614452 0.458988 0.267013 -51.00000 -1.50000 AFIX 0 PART 1 O5 4 0.386569 0.784745 0.291529 21.00000 0.13872 0.08027 = 0.16489 0.00303 0.03153 0.00767 O6 4 0.555213 0.746141 0.302060 21.00000 0.14817 0.07764 = 0.15243 -0.01659 0.00873 -0.01588 C48 1 0.312708 0.828504 0.303028 21.00000 0.14505 0.14657 = 0.16230 0.00930 0.02207 0.00919 AFIX 137 H48A 2 0.292919 0.799272 0.321782 21.00000 -1.50000 H48B 2 0.265176 0.827007 0.287851 21.00000 -1.50000 H48C 2 0.328112 0.889991 0.307531 21.00000 -1.50000 AFIX 0 C49 1 0.455493 0.840755 0.282600 21.00000 0.15280 0.08851 = 0.16945 0.01156 0.02552 -0.00127 AFIX 23 H49A 2 0.433592 0.902334 0.282125 21.00000 -1.20000 H49B 2 0.474371 0.824878 0.261665 21.00000 -1.20000 AFIX 0 C50 1 0.533157 0.835574 0.303456 21.00000 0.15874 0.08041 = 0.16750 -0.01626 0.01371 -0.01660 AFIX 23 H50A 2 0.582268 0.873136 0.296115 21.00000 -1.20000 H50B 2 0.517216 0.853388 0.324496 21.00000 -1.20000 AFIX 0 C51 1 0.645069 0.729543 0.306062 21.00000 0.12888 0.12912 = 0.14822 -0.00590 0.00787 -0.01620 AFIX 137 H51A 2 0.679514 0.773903 0.294947 21.00000 -1.50000 H51B 2 0.659222 0.670626 0.298207 21.00000 -1.50000 H51C 2 0.659600 0.732437 0.327845 21.00000 -1.50000 AFIX 0 PART 2 O5' 4 0.358093 0.774145 0.286147 -21.00000 0.13872 0.08027 = 0.16489 0.00303 0.03153 0.00767 O6' 4 0.544227 0.763575 0.296500 -21.00000 0.14817 0.07764 = 0.15243 -0.01659 0.00873 -0.01588 C48' 1 0.278805 0.786478 0.270684 -21.00000 0.14505 0.14657 = 0.16230 0.00930 0.02207 0.00919 AFIX 137 H48D 2 0.236290 0.815634 0.284210 -21.00000 -1.50000 H48E 2 0.255295 0.729083 0.264302 -21.00000 -1.50000 H48F 2 0.288974 0.823405 0.252647 -21.00000 -1.50000 AFIX 0 C49' 1 0.406755 0.851034 0.291330 -21.00000 0.15280 0.08851 = 0.16945 0.01156 0.02552 -0.00127 AFIX 23 H49C 2 0.370961 0.892977 0.303473 -21.00000 -1.20000 H49D 2 0.420872 0.879383 0.271554 -21.00000 -1.20000 AFIX 0 C50' 1 0.490136 0.830883 0.307948 -21.00000 0.15874 0.08041 = 0.16750 -0.01626 0.01371 -0.01660 AFIX 23 H50C 2 0.525630 0.885731 0.308741 -21.00000 -1.20000 H50D 2 0.474486 0.815473 0.329240 -21.00000 -1.20000 AFIX 0 C51' 1 0.621763 0.752348 0.313574 -21.00000 0.12888 0.12912 = 0.14822 -0.00590 0.00787 -0.01620 AFIX 137 H51D 2 0.623677 0.796309 0.329981 -21.00000 -1.50000 H51E 2 0.673177 0.759966 0.300243 -21.00000 -1.50000 H51F 2 0.622616 0.692924 0.322428 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM biangaphnco2 in P4(1)2(1)2 REM wR2 = 0.151501, GooF = S = 1.02875, Restrained GooF = 1.04174 for all data REM R1 = 0.061658 for 7026 Fo > 4sig(Fo) and 0.104606 for all 9887 data REM 627 parameters refined using 864 restraints END WGHT 0.0763 3.7579 REM Highest difference peak 0.381, deepest hole -0.450, 1-sigma level 0.059 Q1 1 0.3562 0.3141 0.2843 11.00000 0.05 0.38 Q2 1 0.2862 0.2131 0.4163 11.00000 0.05 0.37 Q3 1 0.3560 0.0462 0.2556 11.00000 0.05 0.32 Q4 1 0.3070 0.2733 0.3941 11.00000 0.05 0.31 Q5 1 0.2955 0.0230 0.2216 11.00000 0.05 0.31 Q6 1 0.1958 0.2719 0.3007 11.00000 0.05 0.30 Q7 1 0.2436 0.7564 0.2500 10.50000 0.05 0.29 Q8 1 0.2819 0.3083 0.3187 11.00000 0.05 0.28 Q9 1 0.2922 0.3906 0.4062 11.00000 0.05 0.25 Q10 1 0.5011 0.4989 0.2500 10.50000 0.05 0.24 Q11 1 0.4787 0.1000 0.2977 11.00000 0.05 0.23 Q12 1 0.5528 0.5351 0.2489 11.00000 0.05 0.22 Q13 1 0.2895 0.8302 0.2842 11.00000 0.05 0.22 Q14 1 0.3582 0.8226 0.3241 11.00000 0.05 0.22 Q15 1 0.0570 -0.0441 0.2965 11.00000 0.05 0.22 Q16 1 0.2266 0.8116 0.2369 11.00000 0.05 0.21 Q17 1 0.1918 0.3636 0.2934 11.00000 0.05 0.21 Q18 1 0.2346 0.2639 0.3302 11.00000 0.05 0.21 Q19 1 0.5439 0.5144 0.2473 11.00000 0.05 0.20 Q20 1 0.6186 0.2821 0.3522 11.00000 0.05 0.20 ; _shelx_res_checksum 96839 _shelx_hkl_file ; 2 1 0 13.23 1.24 -2 -1 0 14.04 1.15 1 -2 0 14.92 1.31 -2 0 0 271.90 22.16 0 -2 0 283.78 22.16 1 2 0 13.44 1.15 2 -1 0 10.16 0.98 -1 -2 0 11.28 0.95 -2 1 0 10.69 0.98 2 -1 0 11.88 1.02 -2 2 0 130.48 10.67 2 2 0 126.59 10.75 2 2 0 137.04 10.61 -2 -2 0 135.65 10.79 2 -2 0 130.81 10.71 -2 2 0 133.99 10.76 -2 -2 0 135.02 10.61 -2 3 0 10.93 1.23 2 -3 0 10.47 1.18 -3 -2 0 10.62 1.19 3 2 0 9.55 1.13 -3 -1 0 21.85 1.79 -3 -1 0 19.49 1.67 -1 3 0 20.69 1.93 3 1 0 19.02 1.67 -1 3 0 21.14 1.94 3 1 0 19.59 1.75 0 3 0 -0.17 0.42 3 0 0 0.06 0.14 -3 0 0 -0.08 0.20 3 0 0 0.01 0.21 0 3 0 0.08 0.16 -3 0 0 0.18 0.16 3 -1 0 14.38 1.32 -3 1 0 15.87 1.34 -1 -3 0 15.64 1.32 3 -2 0 10.04 1.17 2 3 0 13.55 1.03 -3 2 0 12.27 1.19 -2 -3 0 11.44 1.38 3 -2 0 11.21 1.09 2 3 0 9.72 1.29 -3 2 0 13.11 1.27 -2 -3 0 13.07 1.04 -3 3 0 335.19 28.04 3 3 0 347.62 28.10 3 -3 0 371.17 28.04 -3 -3 0 341.26 27.88 3 3 0 352.94 27.88 -4 -3 0 4.15 0.50 4 3 0 5.90 0.92 4 3 0 4.50 0.49 -4 -3 0 4.95 0.88 4 2 0 -0.19 0.42 4 2 0 0.41 0.18 -4 -2 0 -0.37 0.48 -2 4 0 -0.09 0.66 -4 -1 0 198.34 16.03 4 1 0 193.62 15.94 -1 4 0 203.67 16.20 -1 4 0 204.29 15.99 4 1 0 195.53 16.00 -1 4 0 200.84 16.23 4 0 0 158.12 13.23 -4 0 0 170.85 13.22 0 4 0 150.68 13.46 0 -4 0 190.66 13.25 4 0 0 152.68 13.22 -4 0 0 146.37 13.21 0 4 0 185.63 13.24 0 4 0 164.43 13.47 -1 -4 0 189.12 15.82 -1 -4 0 215.42 15.56 -4 1 0 201.32 15.54 -4 1 0 182.50 15.55 1 4 0 196.73 15.80 4 -1 0 200.23 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