#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:53:38 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252808 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557846.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_1557846 loop_ _publ_author_name 'Jost, Maximilian' 'Richter, Roman-Malte' 'Balmer, Markus' 'Peters, Bertram' 'Dankert, Fabian' 'von H\"anisch, Carsten' _publ_section_title ; Coordination polymers of alkali metal cyclosiloxazanides with one- and two-dimensional structures. ; _journal_issue 18 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 5787 _journal_page_last 5790 _journal_paper_doi 10.1039/d0dt01060j _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C24 H72 N2 Na2 O4 Si12' _chemical_formula_sum 'C24 H72 N2 Na2 O4 Si12' _chemical_formula_weight 835.89 _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 dual _audit_creation_date 2018-07-16 _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 92.488(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.2536(5) _cell_length_b 12.3598(5) _cell_length_c 18.9999(8) _cell_measurement_reflns_used 9086 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 26.47 _cell_measurement_theta_min 2.30 _cell_volume 2405.63(18) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'STOE X-AREA' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009) and MS-Word' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 8 _diffrn_detector_type 'Bruker APEX2 area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Quest' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_unetI/netI 0.0221 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 42047 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 2.146 _diffrn_source 'sealed tube' _diffrn_source_target Mo _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.7075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1147 before and 0.0509 after correction. The Ratio of minimum to maximum transmission is 0.9492. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.154 _exptl_crystal_description block _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.396 _exptl_crystal_size_mid 0.222 _exptl_crystal_size_min 0.217 _refine_diff_density_max 0.400 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 211 _refine_ls_number_reflns 4733 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0291 _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^)+(0.0422P)^2^+0.8831P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.0811 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4029 _reflns_number_total 4733 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; sk102p21n.res created by SHELXL-2014/7 TITL sk102p21n_a.res in P2(1)/n REM Old TITL SK102P21n in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.091, Rweak 0.005, Alpha 0.021, Orientation as input REM Formula found by SHELXT: C12 N O2 Na Si6 CELL 0.71073 10.2536 12.3598 18.9999 90 92.488 90 ZERR 2 0.0005 0.0005 0.0008 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Na O Si UNIT 48 144 4 4 8 24 EQIV $1 1-X,1-Y,1-Z L.S. 10 PLAN 20 SIZE 0.217 0.222 0.396 TEMP -173.15 FREE Si3 Na1 FREE Si2 Na1 FREE Si5 Na1 FREE Si6 Na1_$1 FREE Si6 Na1 FREE Si4 Na1 FREE Si1 Na1 FREE Na1 C11_$1 FREE Na1 Na1_$1 BOND $H list 4 fmap 2 53 acta OMIT 0 52 REM REM REM WGHT 0.042200 0.883100 FVAR 0.33226 SI5 6 0.695099 0.224274 0.524723 11.00000 0.01306 0.01681 = 0.01644 -0.00159 0.00098 0.00088 SI6 6 0.566446 0.301389 0.431211 11.00000 0.01449 0.01759 = 0.01376 -0.00014 0.00263 0.00041 SI1 6 0.284183 0.330994 0.475979 11.00000 0.01331 0.01745 = 0.01553 0.00105 0.00157 0.00032 SI2 6 0.265046 0.274155 0.594956 11.00000 0.01447 0.01921 = 0.01749 0.00243 0.00392 -0.00116 SI4 6 0.710230 0.293739 0.682123 11.00000 0.01865 0.01772 = 0.01500 0.00020 0.00048 -0.00028 SI3 6 0.490083 0.275537 0.712923 11.00000 0.01912 0.03126 = 0.01457 0.00457 0.00276 0.00352 O1 5 0.407318 0.303129 0.638010 11.00000 0.01754 0.02482 = 0.01645 0.00461 0.00091 -0.00204 O2 5 0.701532 0.308099 0.594607 11.00000 0.02513 0.01871 = 0.01680 -0.00074 0.00065 0.00225 N1 3 0.436560 0.372100 0.458277 11.00000 0.01498 0.01540 = 0.01661 0.00073 0.00308 0.00018 C1 1 0.160329 0.441586 0.459673 11.00000 0.02024 0.03002 = 0.03118 0.01010 0.00422 0.00617 AFIX 137 H1A 2 0.075941 0.418537 0.476815 11.00000 -1.50000 H1B 2 0.151238 0.456549 0.409046 11.00000 -1.50000 H1C 2 0.189322 0.507251 0.484670 11.00000 -1.50000 AFIX 0 C4 1 0.131970 0.341945 0.642882 11.00000 0.02002 0.03316 = 0.02576 -0.00084 0.00911 -0.00311 AFIX 137 H4A 2 0.147272 0.420204 0.644026 11.00000 -1.50000 H4B 2 0.131288 0.314113 0.691162 11.00000 -1.50000 H4C 2 0.047649 0.327023 0.618560 11.00000 -1.50000 AFIX 0 C3 1 0.232328 0.125045 0.600633 11.00000 0.02735 0.02437 = 0.03218 0.00628 0.00150 -0.00344 AFIX 137 H3A 2 0.153853 0.107184 0.571679 11.00000 -1.50000 H3B 2 0.219048 0.105172 0.649739 11.00000 -1.50000 H3C 2 0.307002 0.084935 0.583445 11.00000 -1.50000 AFIX 0 C10 1 0.620220 0.093922 0.553021 11.00000 0.02990 0.01923 = 0.02791 -0.00059 -0.00167 -0.00421 AFIX 137 H10A 2 0.534265 0.108334 0.571619 11.00000 -1.50000 H10B 2 0.676674 0.060193 0.589735 11.00000 -1.50000 H10C 2 0.610554 0.045055 0.512512 11.00000 -1.50000 AFIX 0 C8 1 0.818615 0.178904 0.709643 11.00000 0.02289 0.02318 = 0.02600 0.00325 0.00011 -0.00074 AFIX 137 H8A 2 0.824202 0.174250 0.761176 11.00000 -1.50000 H8B 2 0.905969 0.190785 0.692133 11.00000 -1.50000 H8C 2 0.782673 0.111284 0.690094 11.00000 -1.50000 AFIX 0 C12 1 0.536550 0.182923 0.370130 11.00000 0.02328 0.02974 = 0.02090 -0.00819 -0.00228 0.00531 AFIX 137 H12A 2 0.620345 0.151825 0.357600 11.00000 -1.50000 H12B 2 0.488576 0.207416 0.327322 11.00000 -1.50000 H12C 2 0.485188 0.127943 0.393714 11.00000 -1.50000 AFIX 0 C7 1 0.782747 0.419952 0.719252 11.00000 0.03774 0.02183 = 0.02235 -0.00297 -0.00073 -0.00130 AFIX 137 H7A 2 0.731211 0.482186 0.702252 11.00000 -1.50000 H7B 2 0.872625 0.427194 0.704328 11.00000 -1.50000 H7C 2 0.782730 0.417181 0.770800 11.00000 -1.50000 AFIX 0 C2 1 0.218058 0.214721 0.421072 11.00000 0.02149 0.03462 = 0.02369 -0.00655 0.00252 -0.00816 AFIX 137 H2A 2 0.269930 0.149666 0.431629 11.00000 -1.50000 H2B 2 0.222938 0.232577 0.371001 11.00000 -1.50000 H2C 2 0.126921 0.201461 0.432035 11.00000 -1.50000 AFIX 0 C6 1 0.453467 0.137159 0.745907 11.00000 0.02444 0.04556 = 0.03236 0.02086 0.00515 0.00067 AFIX 137 H6A 2 0.474592 0.083543 0.710150 11.00000 -1.50000 H6B 2 0.360582 0.132093 0.755630 11.00000 -1.50000 H6C 2 0.505991 0.123138 0.789272 11.00000 -1.50000 AFIX 0 C11 1 0.675446 0.393705 0.380931 11.00000 0.02537 0.03209 = 0.03102 0.00881 0.01287 0.00236 AFIX 137 H11A 2 0.695263 0.458643 0.408996 11.00000 -1.50000 H11B 2 0.630917 0.414551 0.336297 11.00000 -1.50000 H11C 2 0.756802 0.355896 0.371371 11.00000 -1.50000 AFIX 0 C5 1 0.443099 0.377761 0.779839 11.00000 0.03593 0.05843 = 0.02018 -0.00567 0.00060 0.01767 AFIX 137 H5A 2 0.491221 0.363516 0.824572 11.00000 -1.50000 H5B 2 0.349129 0.372860 0.786769 11.00000 -1.50000 H5C 2 0.464328 0.450469 0.763240 11.00000 -1.50000 AFIX 0 C9 1 0.865896 0.194412 0.500567 11.00000 0.01802 0.04398 = 0.03430 -0.00524 0.00331 0.00541 AFIX 137 H9A 2 0.864393 0.147631 0.458894 11.00000 -1.50000 H9B 2 0.912272 0.157692 0.539923 11.00000 -1.50000 H9C 2 0.910701 0.262233 0.490199 11.00000 -1.50000 AFIX 0 NA1 4 0.530285 0.441308 0.571164 11.00000 0.01997 0.01671 = 0.01644 0.00187 0.00206 0.00057 HKLF 4 REM sk102p21n_a.res in P2(1)/n REM R1 = 0.0291 for 4029 Fo > 4sig(Fo) and 0.0391 for all 4733 data REM 211 parameters refined using 0 restraints END WGHT 0.0422 0.8831 REM Highest difference peak 0.400, deepest hole -0.253, 1-sigma level 0.080 Q1 1 0.4594 0.3340 0.7436 11.00000 0.05 0.40 Q2 1 0.6038 0.2848 0.7014 11.00000 0.05 0.36 Q3 1 0.7462 0.3647 0.7045 11.00000 0.05 0.36 Q4 1 0.4754 0.2055 0.7368 11.00000 0.05 0.35 Q5 1 0.2007 0.3065 0.6212 11.00000 0.05 0.33 Q6 1 0.5551 0.2378 0.3995 11.00000 0.05 0.30 Q7 1 0.7743 0.2417 0.6982 11.00000 0.05 0.29 Q8 1 0.7485 0.2200 0.6990 11.00000 0.05 0.29 Q9 1 0.4144 0.4397 0.7742 11.00000 0.05 0.28 Q10 1 0.2494 0.2591 0.4550 11.00000 0.05 0.24 Q11 1 0.3964 0.0981 0.7231 11.00000 0.05 0.24 Q12 1 0.4234 0.3565 0.7916 11.00000 0.05 0.24 Q13 1 0.7989 0.2217 0.5149 11.00000 0.05 0.24 Q14 1 0.4362 0.2804 0.6641 11.00000 0.05 0.23 Q15 1 0.7222 0.4463 0.7206 11.00000 0.05 0.23 Q16 1 0.2492 0.2027 0.6014 11.00000 0.05 0.22 Q17 1 0.6219 0.3381 0.3946 11.00000 0.05 0.21 Q18 1 0.3791 0.3440 0.4631 11.00000 0.05 0.21 Q19 1 0.2267 0.2791 0.4403 11.00000 0.05 0.21 Q20 1 0.5167 0.4013 0.8206 11.00000 0.05 0.20 REM The information below was added by Olex2. REM REM R1 = 0.0291 for 4029 Fo > 4sig(Fo) and 0.0391 for all 44573 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.40, deepest hole -0.25 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0391 REM R1_gt = 0.0291 REM wR_ref = 0.0811 REM GOOF = 1.102 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 44573 REM Reflections_gt = 4029 REM Parameters = n/a REM Hole = -0.25 REM Peak = 0.40 REM Flack = n/a ; _cod_data_source_file d0dt01060j2.cif _cod_data_source_block CvH-NaNSi6O2 _cod_depositor_comments 'Adding full bibliography for 1557842--1557846.cif.' _cod_database_code 1557846 _shelx_shelxl_version_number 2014/7 _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_max 0.924 _shelx_estimated_absorpt_t_min 0.868 _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: C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C), C6(H6A, H6B,H6C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C) ; _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 Si5 Si 0.69510(5) 0.22427(4) 0.52472(2) 0.01543(12) Uani 1 1 d . . . . . Si6 Si 0.56645(5) 0.30139(4) 0.43121(2) 0.01522(12) Uani 1 1 d . . . . . Si1 Si 0.28418(4) 0.33099(4) 0.47598(2) 0.01540(12) Uani 1 1 d . . . . . Si2 Si 0.26505(5) 0.27415(4) 0.59496(3) 0.01696(12) Uani 1 1 d . . . . . Si4 Si 0.71023(5) 0.29374(4) 0.68212(2) 0.01713(12) Uani 1 1 d . . . . . Si3 Si 0.49008(5) 0.27554(4) 0.71292(3) 0.02159(13) Uani 1 1 d . . . . . O1 O 0.40732(12) 0.30313(10) 0.63801(6) 0.0196(3) Uani 1 1 d . . . . . O2 O 0.70153(12) 0.30810(10) 0.59461(6) 0.0202(3) Uani 1 1 d . . . . . N1 N 0.43656(13) 0.37210(11) 0.45828(7) 0.0156(3) Uani 1 1 d . . . . . C1 C 0.16033(18) 0.44159(16) 0.45967(11) 0.0271(4) Uani 1 1 d . . . . . H1A H 0.0759 0.4185 0.4768 0.041 Uiso 1 1 calc GR . . . . H1B H 0.1512 0.4565 0.4090 0.041 Uiso 1 1 calc GR . . . . H1C H 0.1893 0.5073 0.4847 0.041 Uiso 1 1 calc GR . . . . C4 C 0.13197(18) 0.34194(17) 0.64288(10) 0.0261(4) Uani 1 1 d . . . . . H4A H 0.1473 0.4202 0.6440 0.039 Uiso 1 1 calc GR . . . . H4B H 0.1313 0.3141 0.6912 0.039 Uiso 1 1 calc GR . . . . H4C H 0.0476 0.3270 0.6186 0.039 Uiso 1 1 calc GR . . . . C3 C 0.2323(2) 0.12504(15) 0.60063(11) 0.0280(4) Uani 1 1 d . . . . . H3A H 0.1539 0.1072 0.5717 0.042 Uiso 1 1 calc GR . . . . H3B H 0.2190 0.1052 0.6497 0.042 Uiso 1 1 calc GR . . . . H3C H 0.3070 0.0849 0.5834 0.042 Uiso 1 1 calc GR . . . . C10 C 0.62022(19) 0.09392(15) 0.55302(10) 0.0258(4) Uani 1 1 d . . . . . H10A H 0.5343 0.1083 0.5716 0.039 Uiso 1 1 calc GR . . . . H10B H 0.6767 0.0602 0.5897 0.039 Uiso 1 1 calc GR . . . . H10C H 0.6106 0.0451 0.5125 0.039 Uiso 1 1 calc GR . . . . C8 C 0.81861(18) 0.17890(15) 0.70964(10) 0.0241(4) Uani 1 1 d . . . . . H8A H 0.8242 0.1743 0.7612 0.036 Uiso 1 1 calc GR . . . . H8B H 0.9060 0.1908 0.6921 0.036 Uiso 1 1 calc GR . . . . H8C H 0.7827 0.1113 0.6901 0.036 Uiso 1 1 calc GR . . . . C12 C 0.53655(19) 0.18292(16) 0.37013(10) 0.0247(4) Uani 1 1 d . . . . . H12A H 0.6203 0.1518 0.3576 0.037 Uiso 1 1 calc GR . . . . H12B H 0.4886 0.2074 0.3273 0.037 Uiso 1 1 calc GR . . . . H12C H 0.4852 0.1279 0.3937 0.037 Uiso 1 1 calc GR . . . . C7 C 0.7827(2) 0.41995(15) 0.71925(10) 0.0274(4) Uani 1 1 d . . . . . H7A H 0.7312 0.4822 0.7023 0.041 Uiso 1 1 calc GR . . . . H7B H 0.8726 0.4272 0.7043 0.041 Uiso 1 1 calc GR . . . . H7C H 0.7827 0.4172 0.7708 0.041 Uiso 1 1 calc GR . . . . C2 C 0.21806(19) 0.21472(16) 0.42107(10) 0.0266(4) Uani 1 1 d . . . . . H2A H 0.2699 0.1497 0.4316 0.040 Uiso 1 1 calc GR . . . . H2B H 0.2229 0.2326 0.3710 0.040 Uiso 1 1 calc GR . . . . H2C H 0.1269 0.2015 0.4320 0.040 Uiso 1 1 calc GR . . . . C6 C 0.4535(2) 0.13716(18) 0.74591(11) 0.0340(5) Uani 1 1 d . . . . . H6A H 0.4746 0.0835 0.7101 0.051 Uiso 1 1 calc GR . . . . H6B H 0.3606 0.1321 0.7556 0.051 Uiso 1 1 calc GR . . . . H6C H 0.5060 0.1231 0.7893 0.051 Uiso 1 1 calc GR . . . . C11 C 0.67545(19) 0.39371(17) 0.38093(11) 0.0292(5) Uani 1 1 d . . . . . H11A H 0.6953 0.4586 0.4090 0.044 Uiso 1 1 calc GR . . . . H11B H 0.6309 0.4146 0.3363 0.044 Uiso 1 1 calc GR . . . . H11C H 0.7568 0.3559 0.3714 0.044 Uiso 1 1 calc GR . . . . C5 C 0.4431(2) 0.3778(2) 0.77984(11) 0.0382(5) Uani 1 1 d . . . . . H5A H 0.4912 0.3635 0.8246 0.057 Uiso 1 1 calc GR . . . . H5B H 0.3491 0.3729 0.7868 0.057 Uiso 1 1 calc GR . . . . H5C H 0.4643 0.4505 0.7632 0.057 Uiso 1 1 calc GR . . . . C9 C 0.86590(19) 0.19441(18) 0.50057(11) 0.0320(5) Uani 1 1 d . . . . . H9A H 0.8644 0.1476 0.4589 0.048 Uiso 1 1 calc GR . . . . H9B H 0.9123 0.1577 0.5399 0.048 Uiso 1 1 calc GR . . . . H9C H 0.9107 0.2622 0.4902 0.048 Uiso 1 1 calc GR . . . . Na1 Na 0.53029(6) 0.44131(5) 0.57116(3) 0.01767(16) 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 Si5 0.0131(2) 0.0168(2) 0.0164(2) -0.00159(18) 0.00098(18) 0.00088(19) Si6 0.0145(2) 0.0176(2) 0.0138(2) -0.00014(18) 0.00263(18) 0.00041(19) Si1 0.0133(2) 0.0175(2) 0.0155(2) 0.00105(18) 0.00157(18) 0.00032(18) Si2 0.0145(2) 0.0192(3) 0.0175(2) 0.00243(19) 0.00392(18) -0.00116(19) Si4 0.0187(3) 0.0177(2) 0.0150(2) 0.00020(18) 0.00048(19) -0.0003(2) Si3 0.0191(3) 0.0313(3) 0.0146(3) 0.0046(2) 0.00276(19) 0.0035(2) O1 0.0175(6) 0.0248(7) 0.0164(6) 0.0046(5) 0.0009(5) -0.0020(5) O2 0.0251(7) 0.0187(6) 0.0168(6) -0.0007(5) 0.0006(5) 0.0022(5) N1 0.0150(7) 0.0154(7) 0.0166(7) 0.0007(6) 0.0031(6) 0.0002(6) C1 0.0202(10) 0.0300(11) 0.0312(11) 0.0101(8) 0.0042(8) 0.0062(8) C4 0.0200(9) 0.0332(11) 0.0258(10) -0.0008(8) 0.0091(8) -0.0031(8) C3 0.0274(10) 0.0244(10) 0.0322(11) 0.0063(8) 0.0015(8) -0.0034(8) C10 0.0299(11) 0.0192(9) 0.0279(10) -0.0006(8) -0.0017(8) -0.0042(8) C8 0.0229(10) 0.0232(10) 0.0260(10) 0.0032(8) 0.0001(8) -0.0007(8) C12 0.0233(10) 0.0297(10) 0.0209(9) -0.0082(8) -0.0023(8) 0.0053(8) C7 0.0377(11) 0.0218(10) 0.0223(10) -0.0030(8) -0.0007(8) -0.0013(9) C2 0.0215(10) 0.0346(11) 0.0237(10) -0.0066(8) 0.0025(8) -0.0082(8) C6 0.0244(10) 0.0456(13) 0.0324(11) 0.0209(10) 0.0051(9) 0.0007(9) C11 0.0254(10) 0.0321(11) 0.0310(11) 0.0088(9) 0.0129(8) 0.0024(9) C5 0.0359(12) 0.0584(15) 0.0202(10) -0.0057(10) 0.0006(9) 0.0177(11) C9 0.0180(10) 0.0440(13) 0.0343(12) -0.0052(10) 0.0033(8) 0.0054(9) Na1 0.0200(4) 0.0167(3) 0.0164(3) 0.0019(3) 0.0021(3) 0.0006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 O2 Si5 Si6 110.23(5) . . ? O2 Si5 C10 107.78(8) . . ? O2 Si5 C9 108.10(8) . . ? C10 Si5 Si6 109.86(6) . . ? C9 Si5 Si6 113.16(7) . . ? C9 Si5 C10 107.52(10) . . ? N1 Si6 Si5 113.60(5) . . ? N1 Si6 C12 118.64(8) . . ? N1 Si6 C11 109.46(8) . . ? C12 Si6 Si5 102.70(6) . . ? C12 Si6 C11 104.02(9) . . ? C11 Si6 Si5 107.50(7) . . ? N1 Si1 Si2 113.09(5) . . ? N1 Si1 C1 111.83(8) . . ? N1 Si1 C2 115.62(8) . . ? C1 Si1 Si2 106.70(6) . . ? C1 Si1 C2 103.81(9) . . ? C2 Si1 Si2 104.94(7) . . ? O1 Si2 Si1 107.07(5) . . ? O1 Si2 C4 107.69(8) . . ? O1 Si2 C3 109.57(8) . . ? C4 Si2 Si1 114.92(7) . . ? C4 Si2 C3 106.01(9) . . ? C3 Si2 Si1 111.48(7) . . ? O2 Si4 Si3 104.23(5) . . ? O2 Si4 C8 111.44(8) . . ? O2 Si4 C7 107.01(8) . . ? C8 Si4 Si3 114.94(6) . . ? C7 Si4 Si3 110.91(7) . . ? C7 Si4 C8 108.04(9) . . ? O1 Si3 Si4 103.06(5) . . ? O1 Si3 C6 111.93(9) . . ? O1 Si3 C5 107.87(8) . . ? C6 Si3 Si4 112.22(7) . . ? C6 Si3 C5 109.24(11) . . ? C5 Si3 Si4 112.36(8) . . ? Si2 O1 Na1 110.15(6) . . ? Si3 O1 Si2 140.74(8) . . ? Si3 O1 Na1 108.98(6) . . ? Si5 O2 Na1 105.59(6) . . ? Si4 O2 Si5 135.91(8) . . ? Si4 O2 Na1 105.12(6) . . ? Si6 N1 Na1 107.71(7) . 3_666 ? Si6 N1 Na1 99.29(6) . . ? Si1 N1 Si6 130.68(9) . . ? Si1 N1 Na1 105.07(7) . . ? Si1 N1 Na1 118.46(7) . 3_666 ? Na1 N1 Na1 79.37(5) 3_666 . ? 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 . . ? 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 . . ? 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 . . ? 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 C8 H8A 109.5 . . ? Si4 C8 H8B 109.5 . . ? Si4 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 . . ? 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 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 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 . . ? Si6 C11 H11A 109.5 . . ? Si6 C11 H11B 109.5 . . ? Si6 C11 H11C 109.5 . . ? Si6 C11 Na1 79.83(6) . 3_666 ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Na1 C11 H11A 55.2 3_666 . ? Na1 C11 H11B 77.5 3_666 . ? Na1 C11 H11C 164.6 3_666 . ? 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 . . ? 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 . . ? O1 Na1 Si6 120.15(4) . 3_666 ? O2 Na1 Si6 149.35(4) . 3_666 ? O2 Na1 O1 79.68(4) . . ? O2 Na1 N1 100.10(5) . . ? N1 Na1 Si6 102.41(4) . 3_666 ? N1 Na1 Si6 28.93(3) 3_666 3_666 ? N1 Na1 O1 148.61(5) 3_666 . ? N1 Na1 O1 91.08(5) . . ? N1 Na1 O2 125.74(5) 3_666 . ? N1 Na1 N1 100.63(5) 3_666 . ? 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 Si5 Si6 2.3668(7) . ? Si5 O2 1.6832(12) . ? Si5 C10 1.8735(19) . ? Si5 C9 1.866(2) . ? Si6 N1 1.6916(14) . ? Si6 C12 1.8852(19) . ? Si6 C11 1.8858(19) . ? Si1 Si2 2.3834(7) . ? Si1 N1 1.6906(14) . ? Si1 C1 1.8823(19) . ? Si1 C2 1.8847(19) . ? Si2 O1 1.6798(13) . ? Si2 C4 1.8711(19) . ? Si2 C3 1.877(2) . ? Si4 Si3 2.3671(7) . ? Si4 O2 1.6708(12) . ? Si4 C8 1.8635(19) . ? Si4 C7 1.8543(19) . ? Si3 O1 1.6606(13) . ? Si3 C6 1.865(2) . ? Si3 C5 1.870(2) . ? O1 Na1 2.5017(14) . ? O2 Na1 2.4340(14) . ? N1 Na1 2.4651(15) . ? N1 Na1 2.4008(15) 3_666 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 Na1 3.099(2) 3_666 ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? Na1 Si6 3.3310(8) 3_666 ? Na1 N1 2.4008(15) 3_666 ?