#------------------------------------------------------------------------------ #$Date: 2020-04-22 02:01:23 +0300 (Wed, 22 Apr 2020) $ #$Revision: 251000 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557844.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_1557844 _journal_paper_doi 10.1039/D0DT01060J _chemical_formula_moiety '0.13(C64 H192 N8 Na8 O8 Si32)' _chemical_formula_sum 'C8 H24 N Na O Si4' _chemical_formula_weight 285.63 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2019-07-02 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-04-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.3280(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 12.9603(2) _cell_length_b 15.1185(2) _cell_length_c 17.6321(3) _cell_measurement_reflns_used 36895 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 76.416 _cell_measurement_theta_min 3.962 _cell_volume 3239.67(9) _computing_data_collection 'STOE X-AREA' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009) and MS-Word' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'STOE StadiVari' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54186 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_unetI/netI 0.0699 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 36084 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.686 _diffrn_reflns_theta_max 76.416 _diffrn_reflns_theta_min 3.962 _exptl_absorpt_coefficient_mu 3.514 _exptl_absorpt_correction_T_max 0.7795 _exptl_absorpt_correction_T_min 0.3672 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details 'X-Area LANA 1.68.2.0 (STOE, 2016)' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.171 _exptl_crystal_description plank _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.377 _exptl_crystal_size_mid 0.035 _exptl_crystal_size_min 0.035 _exptl_crystal_size_rad 0.058 _refine_diff_density_max 0.308 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 6672 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.786 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0255 _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^)+(0.0160P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.0555 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4501 _reflns_number_total 6672 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01060j2.cif _cod_data_source_block cvh-na-n(si2me4)2o _cod_database_code 1557844 _shelx_shelxl_version_number 2016/6 _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 0.887 _shelx_estimated_absorpt_t_max 0.351 _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups 2.a Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C00H(H00A,H00B,H00C), C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C4(H4A,H4B,H4C) ; _shelx_res_file ; TITL bp069c_a.res in P2(1)/n cvh-na-n(si2me4)2o.res created by SHELXL-2016/6 at 16:58:02 on 02-Jul-2019 REM Old TITL REM SHELXT solution in P2(1)/n REM R1 0.081, Rweak 0.003, Alpha 0.019, Orientation as input REM Formula found by SHELXT: C8 Si4 N Na O CELL 1.54186 12.9603 15.1185 17.6321 90 110.328 90 ZERR 8 0.0002 0.0002 0.0003 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Na O Si UNIT 64 192 8 8 8 32 EQIV $1 1-X,1-Y,1-Z L.S. 7 PLAN 20 SIZE 0.035 0.035 0.377 TEMP -173.15 FREE Na1 C8_$1 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.016000 FVAR 0.34238 SI4 6 0.621366 0.687742 0.657930 11.00000 0.02100 0.02201 = 0.01855 0.00181 0.00892 0.00122 SI1 6 0.424814 0.691870 0.510593 11.00000 0.01862 0.01900 = 0.02044 0.00084 0.00848 -0.00073 SI5 6 0.205154 0.484043 0.649627 11.00000 0.02410 0.01775 = 0.01998 0.00007 0.01006 -0.00001 SI8 6 0.366377 0.504883 0.808603 11.00000 0.02223 0.01947 = 0.02192 -0.00063 0.00995 -0.00257 SI7 6 0.350794 0.351163 0.823564 11.00000 0.02206 0.01940 = 0.02253 0.00243 0.01012 -0.00014 SI6 6 0.125454 0.375718 0.710476 11.00000 0.02006 0.01931 = 0.02288 -0.00088 0.00979 -0.00212 SI3 6 0.675656 0.822269 0.614135 11.00000 0.01932 0.02245 = 0.02205 -0.00020 0.00841 -0.00267 SI2 6 0.451188 0.843702 0.487745 11.00000 0.02067 0.02033 = 0.02248 0.00331 0.00808 -0.00141 NA1 4 0.456609 0.514588 0.645507 11.00000 0.03578 0.02077 = 0.03368 0.00071 0.02167 0.00175 O1 5 0.564624 0.877708 0.559946 11.00000 0.02145 0.02115 = 0.02656 0.00123 0.00454 -0.00146 O2 5 0.218112 0.319012 0.786079 11.00000 0.02096 0.02154 = 0.02483 0.00321 0.00884 -0.00213 N1 3 0.485471 0.662468 0.609438 11.00000 0.01931 0.02150 = 0.01800 0.00075 0.00774 -0.00109 N2 3 0.323800 0.533569 0.708943 11.00000 0.02221 0.01910 = 0.02075 0.00034 0.00957 -0.00229 C8 1 0.472153 0.621202 0.439498 11.00000 0.02818 0.02752 = 0.02217 -0.00237 0.00990 0.00044 AFIX 137 H8A 2 0.435578 0.641249 0.383703 11.00000 -1.50000 H8B 2 0.453225 0.559188 0.444236 11.00000 -1.50000 H8C 2 0.552028 0.626786 0.453956 11.00000 -1.50000 AFIX 0 C10 1 0.225107 0.425255 0.560920 11.00000 0.03215 0.02714 = 0.02293 -0.00148 0.01195 -0.00177 AFIX 137 H10A 2 0.277157 0.376347 0.580799 11.00000 -1.50000 H10B 2 0.254164 0.467003 0.530833 11.00000 -1.50000 H10C 2 0.154328 0.401986 0.525208 11.00000 -1.50000 AFIX 0 C00H 1 0.654424 0.698945 0.770234 11.00000 0.02954 0.03812 = 0.02209 -0.00038 0.00986 0.00171 AFIX 137 H00A 2 0.731304 0.717220 0.795836 11.00000 -1.50000 H00B 2 0.643066 0.641944 0.792616 11.00000 -1.50000 H00C 2 0.606110 0.743502 0.780714 11.00000 -1.50000 AFIX 0 C1 1 0.271801 0.671383 0.475542 11.00000 0.02225 0.03128 = 0.03182 0.00628 0.01014 -0.00085 AFIX 137 H1A 2 0.238561 0.710359 0.505098 11.00000 -1.50000 H1B 2 0.258105 0.609567 0.485854 11.00000 -1.50000 H1C 2 0.239253 0.683579 0.417466 11.00000 -1.50000 AFIX 0 C13 1 0.408424 0.316313 0.931559 11.00000 0.02850 0.02956 = 0.02383 0.00517 0.00849 0.00231 AFIX 137 H13A 2 0.485838 0.334081 0.954478 11.00000 -1.50000 H13B 2 0.402882 0.251901 0.935071 11.00000 -1.50000 H13C 2 0.366857 0.344631 0.961917 11.00000 -1.50000 AFIX 0 C9 1 0.086931 0.562028 0.602734 11.00000 0.03090 0.02363 = 0.03293 0.00035 0.00878 0.00603 AFIX 137 H9A 2 0.019973 0.527938 0.575395 11.00000 -1.50000 H9B 2 0.103436 0.599981 0.563352 11.00000 -1.50000 H9C 2 0.075814 0.598776 0.645036 11.00000 -1.50000 AFIX 0 C16 1 0.291701 0.563754 0.868246 11.00000 0.03705 0.02917 = 0.02853 -0.00634 0.01724 -0.00411 AFIX 137 H16A 2 0.212402 0.553543 0.842993 11.00000 -1.50000 H16B 2 0.306769 0.627334 0.869046 11.00000 -1.50000 H16C 2 0.317047 0.541040 0.923756 11.00000 -1.50000 AFIX 0 C12 1 0.053745 0.292853 0.630692 11.00000 0.02964 0.02757 = 0.03334 -0.00513 0.01224 -0.00581 AFIX 137 H12A 2 -0.006792 0.321757 0.588143 11.00000 -1.50000 H12B 2 0.024429 0.245046 0.654838 11.00000 -1.50000 H12C 2 0.106054 0.268373 0.607326 11.00000 -1.50000 AFIX 0 C6 1 0.764308 0.804636 0.551106 11.00000 0.03020 0.03534 = 0.03218 -0.00095 0.01780 -0.00094 AFIX 137 H6A 2 0.829942 0.770918 0.582246 11.00000 -1.50000 H6B 2 0.786508 0.862054 0.536010 11.00000 -1.50000 H6C 2 0.722824 0.771716 0.502110 11.00000 -1.50000 AFIX 0 C3 1 0.335966 0.911809 0.496718 11.00000 0.02261 0.02488 = 0.04035 0.00302 0.00929 0.00160 AFIX 137 H3A 2 0.267183 0.895097 0.453931 11.00000 -1.50000 H3B 2 0.351049 0.974559 0.491287 11.00000 -1.50000 H3C 2 0.329129 0.901552 0.549650 11.00000 -1.50000 AFIX 0 C7 1 0.718658 0.598741 0.647864 11.00000 0.02573 0.02796 = 0.02950 0.00164 0.01098 0.00556 AFIX 137 H7A 2 0.709686 0.591258 0.590711 11.00000 -1.50000 H7B 2 0.701964 0.542838 0.669274 11.00000 -1.50000 H7C 2 0.794662 0.616079 0.678397 11.00000 -1.50000 AFIX 0 C15 1 0.516165 0.528364 0.863686 11.00000 0.02384 0.02792 = 0.03573 0.00124 0.00636 -0.00317 AFIX 137 H15A 2 0.537405 0.506231 0.919257 11.00000 -1.50000 H15B 2 0.528944 0.592307 0.864593 11.00000 -1.50000 H15C 2 0.560297 0.498805 0.835949 11.00000 -1.50000 AFIX 0 C11 1 0.022392 0.422809 0.751781 11.00000 0.02782 0.03330 = 0.03556 -0.00288 0.01796 -0.00078 AFIX 137 H11A 2 0.056422 0.470735 0.789631 11.00000 -1.50000 H11B 2 -0.002656 0.376354 0.780092 11.00000 -1.50000 H11C 2 -0.040597 0.446015 0.707266 11.00000 -1.50000 AFIX 0 C5 1 0.752212 0.896539 0.700351 11.00000 0.02340 0.03121 = 0.03058 -0.00521 0.00923 -0.00673 AFIX 137 H5A 2 0.710895 0.902119 0.737291 11.00000 -1.50000 H5B 2 0.760900 0.955056 0.679422 11.00000 -1.50000 H5C 2 0.824895 0.871301 0.729450 11.00000 -1.50000 AFIX 0 C14 1 0.423571 0.289305 0.764862 11.00000 0.03384 0.02974 = 0.03099 0.00310 0.01624 0.00474 AFIX 137 H14A 2 0.393442 0.306876 0.707864 11.00000 -1.50000 H14B 2 0.412991 0.225605 0.769427 11.00000 -1.50000 H14C 2 0.502327 0.303093 0.786607 11.00000 -1.50000 AFIX 0 C4 1 0.467796 0.868998 0.388591 11.00000 0.03262 0.04352 = 0.02621 0.00797 0.01009 -0.00868 AFIX 137 H4A 2 0.533801 0.839365 0.386111 11.00000 -1.50000 H4B 2 0.475157 0.933036 0.383510 11.00000 -1.50000 H4C 2 0.403116 0.847823 0.344290 11.00000 -1.50000 AFIX 0 NA2 4 0.352006 0.686283 0.677318 11.00000 0.02817 0.01836 = 0.02907 0.00002 0.01587 0.00125 HKLF 4 REM bp069c_a.res in P2(1)/n REM R1 = 0.0255 for 4501 Fo > 4sig(Fo) and 0.0405 for all 6672 data REM 287 parameters refined using 0 restraints END WGHT 0.0160 0.0000 REM Highest difference peak 0.308, deepest hole -0.260, 1-sigma level 0.050 Q1 1 0.7307 0.8131 0.5852 11.00000 0.05 0.31 Q2 1 0.3503 0.4250 0.8167 11.00000 0.05 0.29 Q3 1 0.6411 0.7605 0.6353 11.00000 0.05 0.28 Q4 1 0.1693 0.4251 0.6794 11.00000 0.05 0.27 Q5 1 0.3916 0.3192 0.8011 11.00000 0.05 0.27 Q6 1 0.3611 0.5245 0.7369 11.00000 0.05 0.25 Q7 1 0.4589 0.7582 0.4857 11.00000 0.05 0.25 Q8 1 0.5126 0.6643 0.6365 11.00000 0.05 0.24 Q9 1 0.0785 0.4036 0.7392 11.00000 0.05 0.24 Q10 1 0.3292 0.5437 0.8388 11.00000 0.05 0.23 Q11 1 0.1236 0.5234 0.6120 11.00000 0.05 0.23 Q12 1 0.2752 0.5207 0.6833 11.00000 0.05 0.23 Q13 1 0.3405 0.6811 0.4973 11.00000 0.05 0.22 Q14 1 0.4127 0.8804 0.5004 11.00000 0.05 0.21 Q15 1 0.0635 0.3349 0.6535 11.00000 0.05 0.21 Q16 1 0.6981 0.6466 0.6670 11.00000 0.05 0.21 Q17 1 0.4597 0.5110 0.8238 11.00000 0.05 0.21 Q18 1 0.2657 0.3184 0.7952 11.00000 0.05 0.21 Q19 1 0.2165 0.4592 0.5855 11.00000 0.05 0.21 Q20 1 0.4370 0.6630 0.5855 11.00000 0.05 0.20 ; _shelx_res_checksum 67695 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si4 Si 0.62137(5) 0.68774(4) 0.65793(3) 0.01998(11) Uani 1 1 d . . . . . Si1 Si 0.42481(5) 0.69187(3) 0.51059(3) 0.01891(11) Uani 1 1 d . . . . . Si5 Si 0.20515(5) 0.48404(3) 0.64963(3) 0.01997(11) Uani 1 1 d . . . . . Si8 Si 0.36638(5) 0.50488(3) 0.80860(3) 0.02061(12) Uani 1 1 d . . . . . Si7 Si 0.35079(5) 0.35116(3) 0.82356(3) 0.02070(12) Uani 1 1 d . . . . . Si6 Si 0.12545(5) 0.37572(3) 0.71048(3) 0.02014(12) Uani 1 1 d . . . . . Si3 Si 0.67566(5) 0.82227(4) 0.61413(3) 0.02095(12) Uani 1 1 d . . . . . Si2 Si 0.45119(5) 0.84370(3) 0.48774(3) 0.02101(12) Uani 1 1 d . . . . . Na1 Na 0.45661(7) 0.51459(5) 0.64551(5) 0.02754(19) Uani 1 1 d . . . . . O1 O 0.56462(12) 0.87771(9) 0.55995(8) 0.0241(3) Uani 1 1 d . . . . . O2 O 0.21811(11) 0.31901(9) 0.78608(8) 0.0222(3) Uani 1 1 d . . . . . N1 N 0.48547(13) 0.66247(10) 0.60944(9) 0.0193(3) Uani 1 1 d . . . . . N2 N 0.32380(14) 0.53357(10) 0.70894(9) 0.0201(4) Uani 1 1 d . . . . . C8 C 0.47215(17) 0.62120(13) 0.43950(11) 0.0257(5) Uani 1 1 d . . . . . H8A H 0.435578 0.641249 0.383703 0.038 Uiso 1 1 calc GR . . . . H8B H 0.453225 0.559188 0.444236 0.038 Uiso 1 1 calc GR . . . . H8C H 0.552028 0.626786 0.453956 0.038 Uiso 1 1 calc GR . . . . C10 C 0.22511(17) 0.42526(13) 0.56092(11) 0.0268(5) Uani 1 1 d . . . . . H10A H 0.277157 0.376347 0.580799 0.040 Uiso 1 1 calc GR . . . . H10B H 0.254164 0.467003 0.530833 0.040 Uiso 1 1 calc GR . . . . H10C H 0.154328 0.401986 0.525208 0.040 Uiso 1 1 calc GR . . . . C00H C 0.65442(17) 0.69894(14) 0.77023(11) 0.0297(5) Uani 1 1 d . . . . . H00A H 0.731304 0.717220 0.795836 0.045 Uiso 1 1 calc GR . . . . H00B H 0.643066 0.641944 0.792616 0.045 Uiso 1 1 calc GR . . . . H00C H 0.606110 0.743502 0.780714 0.045 Uiso 1 1 calc GR . . . . C1 C 0.27180(16) 0.67138(13) 0.47554(12) 0.0283(5) Uani 1 1 d . . . . . H1A H 0.238561 0.710359 0.505098 0.042 Uiso 1 1 calc GR . . . . H1B H 0.258105 0.609567 0.485854 0.042 Uiso 1 1 calc GR . . . . H1C H 0.239253 0.683579 0.417466 0.042 Uiso 1 1 calc GR . . . . C13 C 0.40842(17) 0.31631(14) 0.93156(11) 0.0275(5) Uani 1 1 d . . . . . H13A H 0.485838 0.334081 0.954478 0.041 Uiso 1 1 calc GR . . . . H13B H 0.402882 0.251901 0.935071 0.041 Uiso 1 1 calc GR . . . . H13C H 0.366857 0.344631 0.961917 0.041 Uiso 1 1 calc GR . . . . C9 C 0.08693(17) 0.56203(13) 0.60273(12) 0.0298(5) Uani 1 1 d . . . . . H9A H 0.019973 0.527938 0.575395 0.045 Uiso 1 1 calc GR . . . . H9B H 0.103436 0.599981 0.563352 0.045 Uiso 1 1 calc GR . . . . H9C H 0.075814 0.598776 0.645036 0.045 Uiso 1 1 calc GR . . . . C16 C 0.29170(18) 0.56375(14) 0.86825(12) 0.0300(5) Uani 1 1 d . . . . . H16A H 0.212402 0.553543 0.842993 0.045 Uiso 1 1 calc GR . . . . H16B H 0.306769 0.627334 0.869046 0.045 Uiso 1 1 calc GR . . . . H16C H 0.317047 0.541040 0.923756 0.045 Uiso 1 1 calc GR . . . . C12 C 0.05374(18) 0.29285(13) 0.63069(12) 0.0298(5) Uani 1 1 d . . . . . H12A H -0.006792 0.321757 0.588143 0.045 Uiso 1 1 calc GR . . . . H12B H 0.024429 0.245046 0.654838 0.045 Uiso 1 1 calc GR . . . . H12C H 0.106054 0.268373 0.607326 0.045 Uiso 1 1 calc GR . . . . C6 C 0.76431(17) 0.80464(14) 0.55111(12) 0.0307(5) Uani 1 1 d . . . . . H6A H 0.829942 0.770918 0.582246 0.046 Uiso 1 1 calc GR . . . . H6B H 0.786508 0.862054 0.536010 0.046 Uiso 1 1 calc GR . . . . H6C H 0.722824 0.771716 0.502110 0.046 Uiso 1 1 calc GR . . . . C3 C 0.33597(17) 0.91181(13) 0.49672(13) 0.0297(5) Uani 1 1 d . . . . . H3A H 0.267183 0.895097 0.453931 0.045 Uiso 1 1 calc GR . . . . H3B H 0.351049 0.974559 0.491287 0.045 Uiso 1 1 calc GR . . . . H3C H 0.329129 0.901552 0.549650 0.045 Uiso 1 1 calc GR . . . . C7 C 0.71866(17) 0.59874(13) 0.64786(12) 0.0274(5) Uani 1 1 d . . . . . H7A H 0.709686 0.591258 0.590711 0.041 Uiso 1 1 calc GR . . . . H7B H 0.701964 0.542838 0.669274 0.041 Uiso 1 1 calc GR . . . . H7C H 0.794662 0.616079 0.678397 0.041 Uiso 1 1 calc GR . . . . C15 C 0.51616(17) 0.52836(14) 0.86369(13) 0.0302(5) Uani 1 1 d . . . . . H15A H 0.537405 0.506231 0.919257 0.045 Uiso 1 1 calc GR . . . . H15B H 0.528944 0.592307 0.864593 0.045 Uiso 1 1 calc GR . . . . H15C H 0.560297 0.498805 0.835949 0.045 Uiso 1 1 calc GR . . . . C11 C 0.02239(17) 0.42281(14) 0.75178(13) 0.0304(5) Uani 1 1 d . . . . . H11A H 0.056422 0.470735 0.789631 0.046 Uiso 1 1 calc GR . . . . H11B H -0.002656 0.376354 0.780092 0.046 Uiso 1 1 calc GR . . . . H11C H -0.040597 0.446015 0.707266 0.046 Uiso 1 1 calc GR . . . . C5 C 0.75221(17) 0.89654(14) 0.70035(12) 0.0284(5) Uani 1 1 d . . . . . H5A H 0.710895 0.902119 0.737291 0.043 Uiso 1 1 calc GR . . . . H5B H 0.760900 0.955056 0.679422 0.043 Uiso 1 1 calc GR . . . . H5C H 0.824895 0.871301 0.729450 0.043 Uiso 1 1 calc GR . . . . C14 C 0.42357(18) 0.28930(14) 0.76486(12) 0.0302(5) Uani 1 1 d . . . . . H14A H 0.393442 0.306876 0.707864 0.045 Uiso 1 1 calc GR . . . . H14B H 0.412991 0.225605 0.769427 0.045 Uiso 1 1 calc GR . . . . H14C H 0.502327 0.303093 0.786607 0.045 Uiso 1 1 calc GR . . . . C4 C 0.46780(19) 0.86900(15) 0.38859(12) 0.0342(5) Uani 1 1 d . . . . . H4A H 0.533801 0.839365 0.386111 0.051 Uiso 1 1 calc GR . . . . H4B H 0.475157 0.933036 0.383510 0.051 Uiso 1 1 calc GR . . . . H4C H 0.403116 0.847823 0.344290 0.051 Uiso 1 1 calc GR . . . . Na2 Na 0.35201(7) 0.68628(5) 0.67732(5) 0.02364(18) Uani 1 1 d . . . . . 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 Si4 0.0210(3) 0.0220(2) 0.0186(3) 0.0018(2) 0.0089(2) 0.0012(2) Si1 0.0186(3) 0.0190(2) 0.0204(3) 0.0008(2) 0.0085(2) -0.0007(2) Si5 0.0241(3) 0.0177(2) 0.0200(3) 0.0001(2) 0.0101(2) 0.0000(2) Si8 0.0222(3) 0.0195(2) 0.0219(3) -0.0006(2) 0.0099(3) -0.0026(2) Si7 0.0221(3) 0.0194(2) 0.0225(3) 0.0024(2) 0.0101(3) -0.0001(2) Si6 0.0201(3) 0.0193(2) 0.0229(3) -0.0009(2) 0.0098(2) -0.0021(2) Si3 0.0193(3) 0.0224(3) 0.0221(3) -0.0002(2) 0.0084(2) -0.0027(2) Si2 0.0207(3) 0.0203(2) 0.0225(3) 0.0033(2) 0.0081(2) -0.0014(2) Na1 0.0358(5) 0.0208(4) 0.0337(5) 0.0007(3) 0.0217(4) 0.0017(4) O1 0.0215(8) 0.0211(7) 0.0266(8) 0.0012(6) 0.0045(7) -0.0015(6) O2 0.0210(8) 0.0215(7) 0.0248(8) 0.0032(6) 0.0088(6) -0.0021(6) N1 0.0193(9) 0.0215(8) 0.0180(8) 0.0007(6) 0.0077(7) -0.0011(7) N2 0.0222(9) 0.0191(8) 0.0207(9) 0.0003(6) 0.0096(8) -0.0023(7) C8 0.0282(12) 0.0275(10) 0.0222(11) -0.0024(8) 0.0099(10) 0.0004(9) C10 0.0322(13) 0.0271(10) 0.0229(11) -0.0015(8) 0.0120(10) -0.0018(9) C00H 0.0295(13) 0.0381(12) 0.0221(11) -0.0004(9) 0.0099(10) 0.0017(10) C1 0.0223(12) 0.0313(11) 0.0318(12) 0.0063(9) 0.0101(10) -0.0008(9) C13 0.0285(12) 0.0296(10) 0.0238(11) 0.0052(9) 0.0085(10) 0.0023(10) C9 0.0309(13) 0.0236(10) 0.0329(13) 0.0003(9) 0.0088(11) 0.0060(9) C16 0.0371(14) 0.0292(11) 0.0285(12) -0.0063(9) 0.0172(11) -0.0041(10) C12 0.0296(13) 0.0276(11) 0.0333(13) -0.0051(9) 0.0122(11) -0.0058(9) C6 0.0302(13) 0.0353(11) 0.0322(12) -0.0009(10) 0.0178(11) -0.0009(10) C3 0.0226(12) 0.0249(10) 0.0404(13) 0.0030(9) 0.0093(11) 0.0016(9) C7 0.0257(12) 0.0280(10) 0.0295(12) 0.0016(9) 0.0110(10) 0.0056(9) C15 0.0238(12) 0.0279(11) 0.0357(13) 0.0012(9) 0.0064(10) -0.0032(9) C11 0.0278(13) 0.0333(11) 0.0356(13) -0.0029(9) 0.0180(11) -0.0008(10) C5 0.0234(12) 0.0312(11) 0.0306(12) -0.0052(9) 0.0092(10) -0.0067(9) C14 0.0338(13) 0.0297(11) 0.0310(12) 0.0031(9) 0.0162(11) 0.0047(10) C4 0.0326(14) 0.0435(13) 0.0262(12) 0.0080(10) 0.0101(11) -0.0087(11) Na2 0.0282(5) 0.0184(3) 0.0291(4) 0.0000(3) 0.0159(4) 0.0013(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si3 Si4 Na1 155.28(3) . . ? N1 Si4 Si3 113.54(6) . . ? N1 Si4 Na1 42.99(5) . . ? N1 Si4 C00H 111.35(9) . . ? N1 Si4 C7 113.41(9) . . ? C00H Si4 Si3 106.32(7) . . ? C00H Si4 Na1 92.65(7) . . ? C00H Si4 C7 104.29(9) . . ? C7 Si4 Si3 107.26(7) . . ? C7 Si4 Na1 82.43(7) . . ? Si2 Si1 Na1 149.59(3) . . ? Si2 Si1 Na2 105.74(3) . . ? N1 Si1 Si2 112.53(6) . . ? N1 Si1 Na1 37.23(5) . . ? N1 Si1 C8 112.80(8) . . ? N1 Si1 C1 110.57(9) . . ? N1 Si1 Na2 43.44(6) . . ? C8 Si1 Si2 109.41(7) . . ? C8 Si1 Na1 91.66(6) . . ? C8 Si1 Na2 143.94(7) . . ? C1 Si1 Si2 107.45(7) . . ? C1 Si1 Na1 87.66(6) . . ? C1 Si1 C8 103.57(9) . . ? C1 Si1 Na2 72.67(7) . . ? Na2 Si1 Na1 52.799(19) . . ? Si6 Si5 Na1 133.54(3) . . ? N2 Si5 Si6 117.78(6) . . ? N2 Si5 Na1 42.95(5) . . ? N2 Si5 C10 111.12(9) . . ? N2 Si5 C9 114.70(9) . . ? C10 Si5 Si6 104.74(7) . . ? C10 Si5 Na1 68.29(7) . . ? C9 Si5 Si6 102.38(7) . . ? C9 Si5 Na1 124.01(7) . . ? C9 Si5 C10 104.78(9) . . ? Si7 Si8 Na1 101.63(3) . . ? N2 Si8 Si7 110.90(6) . . ? N2 Si8 Na1 38.30(6) . . ? N2 Si8 C16 114.24(9) . . ? N2 Si8 C15 113.03(9) . . ? C16 Si8 Si7 108.86(7) . . ? C16 Si8 Na1 146.25(7) . . ? C15 Si8 Si7 104.00(7) . . ? C15 Si8 Na1 80.50(7) . . ? C15 Si8 C16 105.16(10) . . ? O2 Si7 Si8 110.86(6) . . ? O2 Si7 C13 108.14(8) . . ? O2 Si7 C14 106.27(9) . . ? C13 Si7 Si8 111.95(7) . . ? C13 Si7 C14 108.86(9) . . ? C14 Si7 Si8 110.56(7) . . ? Si5 Si6 Na2 150.40(3) . 2_546 ? O2 Si6 Si5 113.87(5) . . ? O2 Si6 C12 106.57(9) . . ? O2 Si6 C11 107.13(8) . . ? O2 Si6 Na2 39.28(5) . 2_546 ? C12 Si6 Si5 107.55(7) . . ? C12 Si6 Na2 78.20(7) . 2_546 ? C11 Si6 Si5 113.20(7) . . ? C11 Si6 C12 108.19(10) . . ? C11 Si6 Na2 91.29(7) . 2_546 ? O1 Si3 Si4 109.06(6) . . ? O1 Si3 C6 108.62(9) . . ? O1 Si3 C5 105.94(9) . . ? C6 Si3 Si4 112.58(7) . . ? C5 Si3 Si4 112.58(7) . . ? C5 Si3 C6 107.79(10) . . ? O1 Si2 Si1 108.12(5) . . ? O1 Si2 C3 106.64(9) . . ? O1 Si2 C4 107.14(9) . . ? C3 Si2 Si1 110.63(7) . . ? C3 Si2 C4 108.74(10) . . ? C4 Si2 Si1 115.17(8) . . ? Si4 Na1 Si1 50.767(17) . . ? Si4 Na1 Si8 111.82(3) . . ? Si5 Na1 Si4 135.96(3) . . ? Si5 Na1 Si1 103.66(3) . . ? Si5 Na1 Si8 50.077(17) . . ? Si8 Na1 Si1 126.93(3) . . ? N1 Na1 Si4 29.26(4) . . ? N1 Na1 Si1 25.55(4) . . ? N1 Na1 Si5 112.45(5) . . ? N1 Na1 Si8 112.95(4) . . ? N1 Na1 Na2 51.47(4) . . ? N2 Na1 Si4 115.24(5) . . ? N2 Na1 Si1 107.06(5) . . ? N2 Na1 Si5 29.27(4) . . ? N2 Na1 Si8 26.43(4) . . ? N2 Na1 N1 102.62(6) . . ? N2 Na1 Na2 51.17(4) . . ? Na2 Na1 Si4 68.76(2) . . ? Na2 Na1 Si1 61.50(2) . . ? Na2 Na1 Si5 67.30(2) . . ? Na2 Na1 Si8 65.55(2) . . ? Si3 O1 Si2 130.45(9) . . ? Si7 O2 Si6 120.86(8) . . ? Si7 O2 Na2 124.74(7) . 2_546 ? Si6 O2 Na2 114.11(7) . 2_546 ? Si4 N1 Na1 107.75(8) . . ? Si4 N1 Na2 120.13(8) . . ? Si1 N1 Si4 118.80(9) . . ? Si1 N1 Na1 117.21(8) . . ? Si1 N1 Na2 107.97(8) . . ? Na1 N1 Na2 78.75(5) . . ? Si5 N2 Si8 114.89(9) . . ? Si5 N2 Na1 107.77(8) . . ? Si5 N2 Na2 116.87(8) . . ? Si8 N2 Na1 115.27(9) . . ? Si8 N2 Na2 117.20(8) . . ? Na1 N2 Na2 79.36(5) . . ? Si1 C8 Na1 168.20(10) . 3_666 ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? Na1 C8 H8A 80.1 3_666 . ? Na1 C8 H8B 59.8 3_666 . ? Na1 C8 H8C 72.3 3_666 . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C10 H10A 109.5 . . ? Si5 C10 H10B 109.5 . . ? Si5 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C00H H00A 109.5 . . ? Si4 C00H H00B 109.5 . . ? Si4 C00H H00C 109.5 . . ? H00A C00H H00B 109.5 . . ? H00A C00H H00C 109.5 . . ? H00B C00H H00C 109.5 . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si7 C13 H13A 109.5 . . ? Si7 C13 H13B 109.5 . . ? Si7 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si5 C9 H9A 109.5 . . ? Si5 C9 H9B 109.5 . . ? Si5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si8 C16 H16A 109.5 . . ? Si8 C16 H16B 109.5 . . ? Si8 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si6 C12 H12A 109.5 . . ? Si6 C12 H12B 109.5 . . ? Si6 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si4 C7 H7A 109.5 . . ? Si4 C7 H7B 109.5 . . ? Si4 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si8 C15 H15A 109.5 . . ? Si8 C15 H15B 109.5 . . ? Si8 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si6 C11 H11A 109.5 . . ? Si6 C11 H11B 109.5 . . ? Si6 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C5 H5A 109.5 . . ? Si3 C5 H5B 109.5 . . ? Si3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si7 C14 H14A 109.5 . . ? Si7 C14 H14B 109.5 . . ? Si7 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 Na2 Si6 119.05(3) . 2_556 ? Na1 Na2 Si1 65.70(2) . . ? Na1 Na2 Si6 148.85(3) . 2_556 ? O2 Na2 Si1 117.50(4) 2_556 . ? O2 Na2 Si6 26.61(4) 2_556 2_556 ? O2 Na2 Na1 174.96(5) 2_556 . ? O2 Na2 N1 131.08(6) 2_556 . ? O2 Na2 N2 129.46(6) 2_556 . ? N1 Na2 Si1 28.58(4) . . ? N1 Na2 Si6 118.10(5) . 2_556 ? N1 Na2 Na1 49.78(4) . . ? N2 Na2 Si1 109.39(4) . . ? N2 Na2 Si6 130.45(5) . 2_556 ? N2 Na2 Na1 49.47(4) . . ? N2 Na2 N1 99.23(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si4 Si3 2.3676(7) . ? Si4 Na1 3.3370(10) . ? Si4 N1 1.7125(17) . ? Si4 C00H 1.8825(19) . ? Si4 C7 1.8941(19) . ? Si1 Si2 2.3757(7) . ? Si1 Na1 3.5116(10) . ? Si1 N1 1.7033(16) . ? Si1 C8 1.9036(19) . ? Si1 C1 1.887(2) . ? Si1 Na2 3.3863(9) . ? Si5 Si6 2.3812(7) . ? Si5 Na1 3.3172(10) . ? Si5 N2 1.7034(17) . ? Si5 C10 1.8932(19) . ? Si5 C9 1.882(2) . ? Si8 Si7 2.3555(7) . ? Si8 Na1 3.4635(9) . ? Si8 N2 1.7049(16) . ? Si8 C16 1.8820(19) . ? Si8 C15 1.878(2) . ? Si7 O2 1.6854(14) . ? Si7 C13 1.8637(19) . ? Si7 C14 1.875(2) . ? Si6 O2 1.6858(14) . ? Si6 C12 1.872(2) . ? Si6 C11 1.870(2) . ? Si6 Na2 3.4351(9) 2_546 ? Si3 O1 1.6525(14) . ? Si3 C6 1.8744(19) . ? Si3 C5 1.873(2) . ? Si2 O1 1.6571(14) . ? Si2 C3 1.865(2) . ? Si2 C4 1.8736(19) . ? Na1 N1 2.3892(17) . ? Na1 N2 2.3736(17) . ? Na1 Na2 3.0690(10) . ? O2 Na2 2.3825(15) 2_546 ? N1 Na2 2.4480(16) . ? N2 Na2 2.4324(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C00H H00A 0.9800 . ? C00H H00B 0.9800 . ? C00H H00C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ?