data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Keith Izod' _publ_contact_author_address ; School of Chemistry Bedson Building University of Newcastle Newcastle Upon Tyne NE1 7RU UNITED KINGDOM ; _publ_contact_author_email K.J.IZOD@NCL.AC.UK _publ_section_title ; Lanthanide(II) complexes of a phosphine-borane-stabilised carbanion ; loop_ _publ_author_name 'Keith Izod' W.Clegg 'Ross Harrington' data_ki405_compound5a _database_code_depnum_ccdc_archive 'CCDC 763178' #TrackingRef 'revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H62 B2 O P2 Si4 Sm' _chemical_formula_sum 'C22 H62 B2 O P2 Si4 Sm' _chemical_formula_weight 688.99 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9950(2) _cell_length_b 29.7059(5) _cell_length_c 12.4072(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.442(2) _cell_angle_gamma 90.00 _cell_volume 4412.99(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28996 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 29.49 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.523 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.751 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41414 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7755 _reflns_number_gt 7166 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+64.1049P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7755 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.351 _refine_ls_restrained_S_all 1.351 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.32421(4) 0.399828(16) 0.62930(4) 0.02620(15) Uani 1 1 d . . . P1 P 0.15381(19) 0.48145(8) 0.71204(18) 0.0241(5) Uani 1 1 d . . . P2 P 0.2818(3) 0.29727(8) 0.52148(19) 0.0362(6) Uani 1 1 d . . . Si1 Si 0.3158(2) 0.44983(10) 0.8932(2) 0.0299(6) Uani 1 1 d . . . Si2 Si 0.0885(2) 0.40119(9) 0.85278(19) 0.0288(5) Uani 1 1 d . . . Si3 Si 0.1456(2) 0.35813(9) 0.3611(2) 0.0314(6) Uani 1 1 d . . . Si4 Si 0.4040(2) 0.36116(9) 0.3734(2) 0.0321(6) Uani 1 1 d . . . B1 B 0.2410(10) 0.4898(4) 0.5847(9) 0.034(3) Uani 1 1 d . . . B2 B 0.3464(13) 0.3052(4) 0.6676(9) 0.045(3) Uani 1 1 d . . . O O 0.5346(5) 0.4139(2) 0.6606(6) 0.0351(16) Uani 1 1 d . . . C1 C 0.1964(7) 0.4360(3) 0.7956(6) 0.0222(18) Uani 1 1 d . . . C2 C 0.1449(9) 0.5341(3) 0.7839(8) 0.038(2) Uani 1 1 d . . . H2A H 0.1124 0.5572 0.7351 0.058 Uiso 1 1 calc R . . H2B H 0.2198 0.5435 0.8107 0.058 Uiso 1 1 calc R . . H2C H 0.0976 0.5302 0.8450 0.058 Uiso 1 1 calc R . . C3 C 0.0112(8) 0.4760(4) 0.6579(8) 0.039(2) Uani 1 1 d . . . H3A H -0.0388 0.4743 0.7174 0.059 Uiso 1 1 calc R . . H3B H 0.0037 0.4486 0.6142 0.059 Uiso 1 1 calc R . . H3C H -0.0087 0.5022 0.6128 0.059 Uiso 1 1 calc R . . C4 C 0.4034(9) 0.3988(5) 0.9284(9) 0.051(3) Uani 1 1 d . . . H4A H 0.4076 0.3797 0.8643 0.077 Uiso 1 1 calc R . . H4B H 0.3694 0.3818 0.9856 0.077 Uiso 1 1 calc R . . H4C H 0.4787 0.4083 0.9535 0.077 Uiso 1 1 calc R . . C5 C 0.2683(8) 0.4743(4) 1.0246(7) 0.043(3) Uani 1 1 d . . . H5A H 0.2142 0.4538 1.0550 0.064 Uiso 1 1 calc R . . H5B H 0.2332 0.5036 1.0104 0.064 Uiso 1 1 calc R . . H5C H 0.3329 0.4779 1.0760 0.064 Uiso 1 1 calc R . . C6 C 0.4169(8) 0.4920(4) 0.8428(8) 0.041(3) Uani 1 1 d . . . H6A H 0.4436 0.4816 0.7739 0.062 Uiso 1 1 calc R . . H6B H 0.4804 0.4952 0.8957 0.062 Uiso 1 1 calc R . . H6C H 0.3795 0.5211 0.8324 0.062 Uiso 1 1 calc R . . C7 C 0.0058(9) 0.3656(4) 0.7511(9) 0.044(3) Uani 1 1 d . . . H7A H -0.0339 0.3852 0.6980 0.066 Uiso 1 1 calc R . . H7B H -0.0483 0.3474 0.7881 0.066 Uiso 1 1 calc R . . H7C H 0.0565 0.3458 0.7143 0.066 Uiso 1 1 calc R . . C8 C 0.1469(10) 0.3579(4) 0.9508(9) 0.048(3) Uani 1 1 d . . . H8A H 0.1918 0.3362 0.9128 0.071 Uiso 1 1 calc R . . H8B H 0.0854 0.3421 0.9833 0.071 Uiso 1 1 calc R . . H8C H 0.1938 0.3728 1.0076 0.071 Uiso 1 1 calc R . . C9 C -0.0141(8) 0.4340(4) 0.9304(8) 0.038(2) Uani 1 1 d . . . H9A H -0.0564 0.4545 0.8813 0.057 Uiso 1 1 calc R . . H9B H 0.0263 0.4515 0.9872 0.057 Uiso 1 1 calc R . . H9C H -0.0656 0.4132 0.9632 0.057 Uiso 1 1 calc R . . C10 C 0.2760(8) 0.3465(3) 0.4436(7) 0.028(2) Uani 1 1 d . . . C11 C 0.3526(13) 0.2503(4) 0.4594(9) 0.058(4) Uani 1 1 d . . . H11A H 0.3561 0.2246 0.5091 0.087 Uiso 1 1 calc R . . H11B H 0.4285 0.2594 0.4438 0.087 Uiso 1 1 calc R . . H11C H 0.3111 0.2417 0.3921 0.087 Uiso 1 1 calc R . . C12 C 0.1434(11) 0.2736(4) 0.5360(9) 0.052(3) Uani 1 1 d . . . H12A H 0.1501 0.2455 0.5773 0.078 Uiso 1 1 calc R . . H12B H 0.1077 0.2674 0.4644 0.078 Uiso 1 1 calc R . . H12C H 0.0978 0.2950 0.5742 0.078 Uiso 1 1 calc R . . C13 C 0.1039(12) 0.3117(4) 0.2622(9) 0.060(4) Uani 1 1 d . . . H13A H 0.1578 0.3102 0.2060 0.090 Uiso 1 1 calc R . . H13B H 0.0294 0.3180 0.2289 0.090 Uiso 1 1 calc R . . H13C H 0.1029 0.2829 0.3005 0.090 Uiso 1 1 calc R . . C14 C 0.0195(10) 0.3698(4) 0.4406(9) 0.051(3) Uani 1 1 d . . . H14A H 0.0411 0.3891 0.5023 0.076 Uiso 1 1 calc R . . H14B H -0.0104 0.3413 0.4665 0.076 Uiso 1 1 calc R . . H14C H -0.0378 0.3850 0.3941 0.076 Uiso 1 1 calc R . . C15 C 0.1566(10) 0.4104(4) 0.2767(8) 0.044(3) Uani 1 1 d . . . H15A H 0.1762 0.4361 0.3237 0.065 Uiso 1 1 calc R . . H15B H 0.0847 0.4162 0.2373 0.065 Uiso 1 1 calc R . . H15C H 0.2145 0.4062 0.2252 0.065 Uiso 1 1 calc R . . C16 C 0.5374(9) 0.3396(4) 0.4422(9) 0.048(3) Uani 1 1 d . . . H16A H 0.5468 0.3078 0.4243 0.072 Uiso 1 1 calc R . . H16B H 0.5342 0.3430 0.5205 0.072 Uiso 1 1 calc R . . H16C H 0.6006 0.3569 0.4175 0.072 Uiso 1 1 calc R . . C17 C 0.4040(10) 0.3396(4) 0.2311(8) 0.047(3) Uani 1 1 d . . . H17A H 0.3942 0.3069 0.2310 0.070 Uiso 1 1 calc R . . H17B H 0.4753 0.3472 0.2008 0.070 Uiso 1 1 calc R . . H17C H 0.3427 0.3536 0.1874 0.070 Uiso 1 1 calc R . . C18 C 0.4266(10) 0.4236(3) 0.3667(9) 0.043(3) Uani 1 1 d . . . H18A H 0.4189 0.4368 0.4383 0.065 Uiso 1 1 calc R . . H18B H 0.3710 0.4369 0.3151 0.065 Uiso 1 1 calc R . . H18C H 0.5017 0.4297 0.3433 0.065 Uiso 1 1 calc R . . C19 C 0.6182(10) 0.3869(4) 0.7215(10) 0.054(3) Uani 1 1 d . . . H19A H 0.5852 0.3727 0.7845 0.065 Uiso 1 1 calc R . . H19B H 0.6467 0.3628 0.6753 0.065 Uiso 1 1 calc R . . C20 C 0.7041(14) 0.4157(6) 0.756(2) 0.134(10) Uani 1 1 d . . . H20A H 0.7769 0.4008 0.7469 0.161 Uiso 1 1 calc R . . H20B H 0.6986 0.4228 0.8330 0.161 Uiso 1 1 calc R . . C21 C 0.6978(10) 0.4574(4) 0.6922(10) 0.053(3) Uani 1 1 d . . . H21A H 0.7652 0.4612 0.6510 0.064 Uiso 1 1 calc R . . H21B H 0.6902 0.4839 0.7397 0.064 Uiso 1 1 calc R . . C22 C 0.5961(8) 0.4518(4) 0.6179(8) 0.041(2) Uani 1 1 d . . . H22A H 0.5500 0.4795 0.6167 0.049 Uiso 1 1 calc R . . H22B H 0.6173 0.4453 0.5436 0.049 Uiso 1 1 calc 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 Sm 0.0313(3) 0.0273(2) 0.0203(2) -0.00245(19) 0.00424(17) -0.0012(2) P1 0.0210(11) 0.0317(12) 0.0199(11) -0.0003(9) 0.0033(9) 0.0040(9) P2 0.0651(19) 0.0241(12) 0.0197(12) 0.0007(9) 0.0045(12) -0.0048(12) Si1 0.0210(13) 0.0501(16) 0.0189(12) -0.0023(11) 0.0023(10) -0.0023(12) Si2 0.0306(13) 0.0358(14) 0.0207(12) -0.0016(11) 0.0077(10) -0.0053(12) Si3 0.0326(15) 0.0409(15) 0.0206(12) -0.0024(11) 0.0009(11) -0.0039(12) Si4 0.0453(17) 0.0304(14) 0.0216(12) 0.0006(10) 0.0091(11) 0.0004(12) B1 0.046(7) 0.030(6) 0.028(5) 0.006(4) 0.015(5) 0.012(5) B2 0.092(11) 0.026(6) 0.017(5) 0.006(4) -0.003(6) -0.001(6) O 0.022(3) 0.038(4) 0.045(4) 0.004(3) 0.002(3) -0.003(3) C1 0.023(5) 0.032(5) 0.013(4) -0.001(3) 0.008(3) 0.001(4) C2 0.040(6) 0.038(6) 0.037(6) -0.005(4) 0.005(5) 0.016(5) C3 0.029(5) 0.056(7) 0.032(5) 0.004(5) -0.001(4) 0.007(5) C4 0.034(6) 0.082(9) 0.037(6) 0.017(6) -0.001(5) 0.011(6) C5 0.023(5) 0.089(9) 0.016(4) -0.011(5) 0.000(4) -0.013(5) C6 0.025(5) 0.070(8) 0.030(5) -0.014(5) 0.013(4) -0.011(5) C7 0.038(6) 0.053(7) 0.042(6) -0.009(5) 0.011(5) -0.018(5) C8 0.059(8) 0.047(6) 0.039(6) 0.010(5) 0.016(5) 0.004(6) C9 0.028(5) 0.052(6) 0.034(5) -0.003(5) 0.009(4) -0.003(5) C10 0.042(6) 0.022(4) 0.021(4) -0.001(3) 0.014(4) -0.003(4) C11 0.111(12) 0.026(5) 0.037(6) -0.001(5) 0.004(7) 0.004(6) C12 0.078(9) 0.041(6) 0.038(6) 0.006(5) 0.011(6) -0.025(6) C13 0.077(9) 0.069(8) 0.031(6) -0.014(6) -0.019(6) -0.024(7) C14 0.045(7) 0.067(8) 0.042(6) -0.001(6) 0.012(5) -0.010(6) C15 0.050(7) 0.051(7) 0.029(5) 0.008(5) 0.002(5) 0.009(5) C16 0.044(7) 0.057(7) 0.044(6) -0.006(5) 0.009(5) 0.012(6) C17 0.061(8) 0.054(7) 0.028(5) -0.002(5) 0.021(5) 0.003(6) C18 0.057(7) 0.038(6) 0.035(6) 0.005(5) 0.011(5) 0.006(5) C19 0.049(7) 0.053(7) 0.059(8) 0.013(6) -0.003(6) 0.000(6) C20 0.067(11) 0.073(11) 0.25(3) 0.052(14) -0.090(15) -0.024(9) C21 0.047(7) 0.067(8) 0.047(7) -0.005(6) 0.005(5) -0.021(6) C22 0.028(5) 0.056(7) 0.038(6) 0.006(5) 0.005(4) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Sm B1 2.895(11) . ? Sm B2 2.861(11) . ? Sm O 2.565(6) . ? Sm C1 2.853(8) . ? Sm C10 2.827(9) . ? P1 B1 1.962(11) . ? P1 C1 1.760(9) . ? P1 C2 1.808(10) . ? P1 C3 1.808(10) . ? P2 B2 1.943(12) . ? P2 C10 1.752(9) . ? P2 C11 1.827(12) . ? P2 C12 1.823(12) . ? Si1 C1 1.865(9) . ? Si1 C4 1.880(12) . ? Si1 C5 1.903(10) . ? Si1 C6 1.876(11) . ? Si2 C1 1.832(9) . ? Si2 C7 1.882(11) . ? Si2 C8 1.876(11) . ? Si2 C9 1.880(10) . ? Si3 C10 1.850(10) . ? Si3 C13 1.893(11) . ? Si3 C14 1.887(11) . ? Si3 C15 1.881(11) . ? Si4 C10 1.862(9) . ? Si4 C16 1.880(12) . ? Si4 C17 1.878(10) . ? Si4 C18 1.877(11) . ? O C19 1.460(13) . ? O C22 1.461(12) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.385(18) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.47(2) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.493(15) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? 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 B1 Sm B2 165.2(4) . . ? B1 Sm O 101.7(3) . . ? B1 Sm C1 66.2(3) . . ? B1 Sm C10 108.1(3) . . ? B2 Sm O 93.1(4) . . ? B2 Sm C1 107.4(3) . . ? B2 Sm C10 66.2(3) . . ? O Sm C1 113.3(2) . . ? O Sm C10 111.5(3) . . ? C1 Sm C10 135.0(3) . . ? B1 P1 C1 114.9(4) . . ? B1 P1 C2 109.8(5) . . ? B1 P1 C3 104.5(5) . . ? C1 P1 C2 113.4(4) . . ? C1 P1 C3 112.6(5) . . ? C2 P1 C3 100.3(5) . . ? B2 P2 C10 114.4(5) . . ? B2 P2 C11 108.4(6) . . ? B2 P2 C12 105.6(6) . . ? C10 P2 C11 114.2(5) . . ? C10 P2 C12 111.8(5) . . ? C11 P2 C12 101.3(6) . . ? C1 Si1 C4 111.7(5) . . ? C1 Si1 C5 112.5(4) . . ? C1 Si1 C6 114.7(4) . . ? C4 Si1 C5 107.5(5) . . ? C4 Si1 C6 104.6(5) . . ? C5 Si1 C6 105.3(5) . . ? C1 Si2 C7 114.4(4) . . ? C1 Si2 C8 113.1(5) . . ? C1 Si2 C9 113.9(4) . . ? C7 Si2 C8 102.2(6) . . ? C7 Si2 C9 107.4(5) . . ? C8 Si2 C9 104.7(5) . . ? C10 Si3 C13 113.9(5) . . ? C10 Si3 C14 115.0(5) . . ? C10 Si3 C15 112.2(5) . . ? C13 Si3 C14 106.5(6) . . ? C13 Si3 C15 105.4(5) . . ? C14 Si3 C15 103.0(5) . . ? C10 Si4 C16 114.3(5) . . ? C10 Si4 C17 114.0(5) . . ? C10 Si4 C18 112.2(5) . . ? C16 Si4 C17 105.2(5) . . ? C16 Si4 C18 103.6(6) . . ? C17 Si4 C18 106.6(5) . . ? Sm B1 P1 85.6(4) . . ? Sm B2 P2 86.3(4) . . ? Sm O C19 128.9(6) . . ? Sm O C22 125.8(6) . . ? C19 O C22 105.4(8) . . ? Sm C1 P1 90.7(3) . . ? Sm C1 Si1 97.3(3) . . ? Sm C1 Si2 119.4(4) . . ? P1 C1 Si1 113.4(5) . . ? P1 C1 Si2 118.3(5) . . ? Si1 C1 Si2 113.9(4) . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Sm C10 P2 91.1(3) . . ? Sm C10 Si3 118.1(4) . . ? Sm C10 Si4 96.7(4) . . ? P2 C10 Si3 117.7(5) . . ? P2 C10 Si4 116.5(5) . . ? Si3 C10 Si4 113.0(5) . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si4 C17 H17A 109.5 . . ? Si4 C17 H17B 109.5 . . ? Si4 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O C19 H19A 110.3 . . ? O C19 H19B 110.3 . . ? O C19 C20 107.0(11) . . ? H19A C19 H19B 108.6 . . ? H19A C19 C20 110.3 . . ? H19B C19 C20 110.3 . . ? C19 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C19 C20 C21 110.2(13) . . ? H20A C20 H20B 108.1 . . ? H20A C20 C21 109.6 . . ? H20B C20 C21 109.6 . . ? C20 C21 H21A 110.8 . . ? C20 C21 H21B 110.8 . . ? C20 C21 C22 104.5(10) . . ? H21A C21 H21B 108.9 . . ? H21A C21 C22 110.8 . . ? H21B C21 C22 110.8 . . ? O C22 C21 105.9(9) . . ? O C22 H22A 110.6 . . ? O C22 H22B 110.6 . . ? C21 C22 H22A 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.232 _refine_diff_density_min -1.652 _refine_diff_density_rms 0.153 # 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 0.250 0.750 0.158 577 125 ' ' 2 0.749 0.250 0.497 577 118 ' ' _platon_squeeze_details ; ; #===END data_ki423_compound5b _database_code_depnum_ccdc_archive 'CCDC 763179' #TrackingRef 'revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H78 B2 O3 P2 Si4 Sm' _chemical_formula_sum 'C30 H78 B2 O3 P2 Si4 Sm' _chemical_formula_weight 833.19 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7414(8) _cell_length_b 13.7832(7) _cell_length_c 15.9703(8) _cell_angle_alpha 66.697(5) _cell_angle_beta 88.844(5) _cell_angle_gamma 70.297(5) _cell_volume 2592.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12873 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 29.53 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_T_max 0.780 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27058 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10171 _reflns_number_gt 7815 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10171 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm -0.275317(12) 0.464597(13) 0.702430(10) 0.02387(5) Uani 1 1 d . . . P1 P -0.47984(7) 0.69404(7) 0.68788(5) 0.0384(2) Uani 1 1 d . . . P2 P 0.07020(6) 0.30092(7) 0.84866(5) 0.0332(2) Uani 1 1 d . . . Si1 Si -0.29825(8) 0.76439(7) 0.61078(5) 0.0384(2) Uani 1 1 d . . . Si2 Si -0.31828(8) 0.69314(7) 0.81780(6) 0.0399(2) Uani 1 1 d . . . Si3 Si 0.30183(6) 0.15756(8) 0.86804(6) 0.0375(2) Uani 1 1 d . . . Si4 Si 0.12572(7) 0.12710(7) 0.77011(5) 0.0334(2) Uani 1 1 d . . . O1 O -0.22144(15) 0.48343(18) 0.54302(12) 0.0350(5) Uani 1 1 d . . . O2 O -0.31581(15) 0.30318(17) 0.68152(13) 0.0372(5) Uani 1 1 d . . . O3 O -0.31448(15) 0.34170(17) 0.86155(12) 0.0351(5) Uani 1 1 d . . . B1 B -0.4969(3) 0.6021(4) 0.6277(3) 0.0387(9) Uani 1 1 d . . . H1A H -0.580(3) 0.637(3) 0.601(2) 0.050(9) Uiso 1 1 d . . . H1B H -0.443(2) 0.602(2) 0.5765(17) 0.029(7) Uiso 1 1 d . . . H1C H -0.471(2) 0.516(3) 0.685(2) 0.047(9) Uiso 1 1 d . . . B2 B -0.0693(3) 0.3626(3) 0.7854(2) 0.0310(8) Uani 1 1 d . . . H2A H -0.075(2) 0.416(2) 0.7102(18) 0.032(8) Uiso 1 1 d . . . H2B H -0.121(2) 0.417(2) 0.8160(16) 0.023(7) Uiso 1 1 d . . . H2C H -0.103(2) 0.296(2) 0.7899(17) 0.033(8) Uiso 1 1 d . . . C1 C -0.3507(2) 0.6815(2) 0.71081(18) 0.0321(7) Uani 1 1 d . . . C2 C -0.5693(3) 0.8403(3) 0.6280(2) 0.0629(11) Uani 1 1 d . . . H2D H -0.6401 0.8414 0.6195 0.094 Uiso 1 1 calc R . . H2E H -0.5477 0.8752 0.5679 0.094 Uiso 1 1 calc R . . H2F H -0.5679 0.8827 0.6645 0.094 Uiso 1 1 calc R . . C3 C -0.5393(3) 0.6484(3) 0.7927(2) 0.0561(10) Uani 1 1 d . . . H3A H -0.5418 0.6968 0.8248 0.084 Uiso 1 1 calc R . . H3B H -0.4977 0.5697 0.8327 0.084 Uiso 1 1 calc R . . H3C H -0.6102 0.6544 0.7769 0.084 Uiso 1 1 calc R . . C4 C -0.1528(3) 0.6988(3) 0.6173(2) 0.0479(9) Uani 1 1 d . . . H4A H -0.1336 0.6187 0.6296 0.072 Uiso 1 1 calc R . . H4B H -0.1185 0.7054 0.6669 0.072 Uiso 1 1 calc R . . H4C H -0.1306 0.7381 0.5587 0.072 Uiso 1 1 calc R . . C5 C -0.3520(3) 0.7808(3) 0.49662(19) 0.0468(9) Uani 1 1 d . . . H5A H -0.3327 0.7062 0.4954 0.070 Uiso 1 1 calc R . . H5B H -0.3230 0.8283 0.4473 0.070 Uiso 1 1 calc R . . H5C H -0.4281 0.8166 0.4877 0.070 Uiso 1 1 calc R . . C6 C -0.3250(3) 0.9135(3) 0.5970(2) 0.0606(11) Uani 1 1 d . . . H6A H -0.4004 0.9531 0.5907 0.091 Uiso 1 1 calc R . . H6B H -0.2975 0.9532 0.5419 0.091 Uiso 1 1 calc R . . H6C H -0.2911 0.9119 0.6512 0.091 Uiso 1 1 calc R . . C7 C -0.4092(3) 0.8253(3) 0.8270(2) 0.0587(11) Uani 1 1 d . . . H7A H -0.4794 0.8223 0.8320 0.088 Uiso 1 1 calc R . . H7B H -0.4111 0.8919 0.7721 0.088 Uiso 1 1 calc R . . H7C H -0.3842 0.8302 0.8817 0.088 Uiso 1 1 calc R . . C8 C -0.1848(3) 0.6972(3) 0.8292(2) 0.0564(10) Uani 1 1 d . . . H8A H -0.1334 0.6309 0.8242 0.085 Uiso 1 1 calc R . . H8B H -0.1697 0.6966 0.8891 0.085 Uiso 1 1 calc R . . H8C H -0.1814 0.7663 0.7802 0.085 Uiso 1 1 calc R . . C9 C -0.3141(3) 0.5685(3) 0.9266(2) 0.0496(9) Uani 1 1 d . . . H9A H -0.3828 0.5612 0.9298 0.074 Uiso 1 1 calc R . . H9B H -0.2956 0.5802 0.9799 0.074 Uiso 1 1 calc R . . H9C H -0.2619 0.4994 0.9267 0.074 Uiso 1 1 calc R . . C10 C 0.1673(2) 0.2113(3) 0.81575(19) 0.0318(7) Uani 1 1 d . . . C11 C 0.0583(3) 0.2379(3) 0.97113(19) 0.0530(10) Uani 1 1 d . . . H11A H 0.1257 0.2126 1.0074 0.080 Uiso 1 1 calc R . . H11B H 0.0365 0.1731 0.9843 0.080 Uiso 1 1 calc R . . H11C H 0.0061 0.2944 0.9873 0.080 Uiso 1 1 calc R . . C12 C 0.0940(3) 0.4264(3) 0.8389(2) 0.0501(9) Uani 1 1 d . . . H12A H 0.1556 0.4043 0.8817 0.075 Uiso 1 1 calc R . . H12B H 0.0334 0.4762 0.8540 0.075 Uiso 1 1 calc R . . H12C H 0.1060 0.4665 0.7759 0.075 Uiso 1 1 calc R . . C13 C 0.3375(3) 0.2518(3) 0.9105(2) 0.0555(10) Uani 1 1 d . . . H13A H 0.2934 0.2639 0.9571 0.083 Uiso 1 1 calc R . . H13B H 0.3269 0.3247 0.8590 0.083 Uiso 1 1 calc R . . H13C H 0.4109 0.2159 0.9377 0.083 Uiso 1 1 calc R . . C14 C 0.4019(2) 0.1343(3) 0.7885(2) 0.0517(10) Uani 1 1 d . . . H14A H 0.4024 0.0706 0.7751 0.078 Uiso 1 1 calc R . . H14B H 0.4710 0.1175 0.8180 0.078 Uiso 1 1 calc R . . H14C H 0.3842 0.2028 0.7310 0.078 Uiso 1 1 calc R . . C15 C 0.3369(3) 0.0192(3) 0.9722(2) 0.0621(11) Uani 1 1 d . . . H15A H 0.3203 -0.0356 0.9562 0.093 Uiso 1 1 calc R . . H15B H 0.2970 0.0308 1.0212 0.093 Uiso 1 1 calc R . . H15C H 0.4116 -0.0097 0.9936 0.093 Uiso 1 1 calc R . . C16 C 0.0514(3) 0.0433(3) 0.8501(2) 0.0481(9) Uani 1 1 d . . . H16A H -0.0103 0.0952 0.8621 0.072 Uiso 1 1 calc R . . H16B H 0.0963 -0.0102 0.9081 0.072 Uiso 1 1 calc R . . H16C H 0.0296 0.0016 0.8213 0.072 Uiso 1 1 calc R . . C17 C 0.2386(3) 0.0186(3) 0.7492(2) 0.0493(9) Uani 1 1 d . . . H17A H 0.2713 0.0571 0.6977 0.074 Uiso 1 1 calc R . . H17B H 0.2132 -0.0319 0.7345 0.074 Uiso 1 1 calc R . . H17C H 0.2900 -0.0256 0.8046 0.074 Uiso 1 1 calc R . . C18 C 0.0430(3) 0.2091(3) 0.6548(2) 0.0410(8) Uani 1 1 d . . . H18A H -0.0228 0.2623 0.6599 0.062 Uiso 1 1 calc R . . H18B H 0.0286 0.1566 0.6340 0.062 Uiso 1 1 calc R . . H18C H 0.0802 0.2510 0.6102 0.062 Uiso 1 1 calc R . . C19 C -0.2814(3) 0.4701(3) 0.4772(2) 0.0463(9) Uani 1 1 d . . . H19A H -0.3571 0.5080 0.4760 0.056 Uiso 1 1 calc R . . H19B H -0.2667 0.3890 0.4932 0.056 Uiso 1 1 calc R . . C20 C -0.2475(3) 0.5240(4) 0.3869(2) 0.0680(12) Uani 1 1 d . . . H20A H -0.2880 0.6063 0.3571 0.082 Uiso 1 1 calc R . . H20B H -0.2551 0.4891 0.3450 0.082 Uiso 1 1 calc R . . C21 C -0.1338(3) 0.5009(4) 0.4127(2) 0.0681(13) Uani 1 1 d . . . H21A H -0.0892 0.4234 0.4214 0.082 Uiso 1 1 calc R . . H21B H -0.1089 0.5562 0.3654 0.082 Uiso 1 1 calc R . . C22 C -0.1353(3) 0.5141(3) 0.5002(2) 0.0408(8) Uani 1 1 d . . . H22A H -0.0686 0.4639 0.5407 0.049 Uiso 1 1 calc R . . H22B H -0.1459 0.5933 0.4884 0.049 Uiso 1 1 calc R . . C23 C -0.2379(3) 0.1918(3) 0.7179(3) 0.0634(11) Uani 1 1 d . . . H23A H -0.2078 0.1713 0.7810 0.076 Uiso 1 1 calc R . . H23B H -0.1811 0.1879 0.6789 0.076 Uiso 1 1 calc R . . C24 C -0.2915(3) 0.1133(3) 0.7185(3) 0.0700(12) Uani 1 1 d . . . H24A H -0.3188 0.0843 0.7776 0.084 Uiso 1 1 calc R . . H24B H -0.2436 0.0485 0.7078 0.084 Uiso 1 1 calc R . . C25 C -0.3786(3) 0.1864(3) 0.6407(2) 0.0505(9) Uani 1 1 d . . . H25A H -0.3543 0.1907 0.5810 0.061 Uiso 1 1 calc R . . H25B H -0.4370 0.1580 0.6497 0.061 Uiso 1 1 calc R . . C26 C -0.4100(2) 0.2987(3) 0.6458(2) 0.0409(8) Uani 1 1 d . . . H26A H -0.4382 0.3609 0.5840 0.049 Uiso 1 1 calc R . . H26B H -0.4640 0.3055 0.6872 0.049 Uiso 1 1 calc R . . C27 C -0.4057(3) 0.3119(3) 0.8804(2) 0.0434(9) Uani 1 1 d . . . H27A H -0.3946 0.2385 0.8775 0.052 Uiso 1 1 calc R . . H27B H -0.4669 0.3707 0.8356 0.052 Uiso 1 1 calc R . . C28 C -0.4214(3) 0.3040(3) 0.9767(2) 0.0509(10) Uani 1 1 d . . . H28A H -0.4510 0.2451 1.0100 0.061 Uiso 1 1 calc R . . H28B H -0.4685 0.3774 0.9751 0.061 Uiso 1 1 calc R . . C29 C -0.3118(3) 0.2724(3) 1.0221(2) 0.0472(9) Uani 1 1 d . . . H29A H -0.3094 0.3286 1.0452 0.057 Uiso 1 1 calc R . . H29B H -0.2890 0.1967 1.0739 0.057 Uiso 1 1 calc R . . C30 C -0.2438(3) 0.2729(3) 0.94587(19) 0.0415(8) Uani 1 1 d . . . H30A H -0.1908 0.3057 0.9490 0.050 Uiso 1 1 calc R . . H30B H -0.2079 0.1951 0.9506 0.050 Uiso 1 1 calc 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 Sm 0.02107(8) 0.02665(9) 0.02169(8) -0.00960(6) 0.00322(5) -0.00644(6) P1 0.0339(5) 0.0372(5) 0.0290(4) -0.0129(4) 0.0003(3) 0.0044(4) P2 0.0220(4) 0.0505(5) 0.0279(4) -0.0215(4) 0.0023(3) -0.0074(4) Si1 0.0539(6) 0.0290(5) 0.0279(4) -0.0097(4) 0.0020(4) -0.0119(5) Si2 0.0558(6) 0.0290(5) 0.0271(4) -0.0145(4) -0.0029(4) -0.0019(5) Si3 0.0212(5) 0.0439(6) 0.0374(5) -0.0108(4) -0.0007(4) -0.0069(4) Si4 0.0293(5) 0.0373(5) 0.0329(4) -0.0145(4) 0.0071(4) -0.0112(4) O1 0.0324(12) 0.0529(14) 0.0279(10) -0.0202(10) 0.0096(9) -0.0210(11) O2 0.0310(12) 0.0376(13) 0.0462(12) -0.0185(10) 0.0014(10) -0.0146(11) O3 0.0348(12) 0.0430(13) 0.0238(10) -0.0080(9) 0.0051(9) -0.0167(11) B1 0.026(2) 0.049(3) 0.034(2) -0.0172(18) 0.0012(17) -0.0039(19) B2 0.0211(19) 0.039(2) 0.0299(19) -0.0166(17) 0.0040(15) -0.0052(18) C1 0.0402(19) 0.0223(16) 0.0236(15) -0.0072(12) -0.0010(13) -0.0014(14) C2 0.050(2) 0.051(2) 0.056(2) -0.0183(19) -0.0075(18) 0.0157(19) C3 0.048(2) 0.071(3) 0.045(2) -0.0305(19) 0.0161(17) -0.010(2) C4 0.057(2) 0.052(2) 0.0447(19) -0.0244(17) 0.0106(17) -0.027(2) C5 0.061(2) 0.045(2) 0.0284(17) -0.0095(15) 0.0040(15) -0.0181(19) C6 0.092(3) 0.032(2) 0.048(2) -0.0091(17) 0.004(2) -0.019(2) C7 0.085(3) 0.038(2) 0.042(2) -0.0238(17) 0.0022(19) 0.001(2) C8 0.069(3) 0.056(2) 0.050(2) -0.0289(19) -0.0054(18) -0.019(2) C9 0.066(3) 0.038(2) 0.0305(17) -0.0141(15) -0.0046(16) -0.0022(19) C10 0.0212(16) 0.0415(19) 0.0300(15) -0.0166(14) 0.0030(12) -0.0057(14) C11 0.036(2) 0.088(3) 0.0292(17) -0.0278(18) 0.0031(14) -0.010(2) C12 0.038(2) 0.064(3) 0.060(2) -0.042(2) 0.0045(17) -0.0112(19) C13 0.0297(19) 0.070(3) 0.066(2) -0.029(2) -0.0099(17) -0.0142(19) C14 0.0277(19) 0.054(2) 0.064(2) -0.0183(19) 0.0115(16) -0.0115(18) C15 0.041(2) 0.063(3) 0.055(2) -0.0013(19) -0.0094(17) -0.013(2) C16 0.043(2) 0.048(2) 0.047(2) -0.0137(17) 0.0097(16) -0.0175(18) C17 0.048(2) 0.044(2) 0.060(2) -0.0275(18) 0.0165(17) -0.0148(18) C18 0.042(2) 0.048(2) 0.0378(17) -0.0233(16) 0.0015(15) -0.0147(17) C19 0.039(2) 0.080(3) 0.0359(18) -0.0333(18) 0.0097(15) -0.029(2) C20 0.085(3) 0.103(4) 0.0316(19) -0.029(2) 0.0095(19) -0.050(3) C21 0.077(3) 0.120(4) 0.055(2) -0.058(2) 0.041(2) -0.067(3) C22 0.043(2) 0.056(2) 0.0337(17) -0.0198(16) 0.0177(15) -0.0288(18) C23 0.045(2) 0.048(2) 0.101(3) -0.041(2) -0.008(2) -0.008(2) C24 0.074(3) 0.051(3) 0.093(3) -0.035(2) -0.011(2) -0.025(2) C25 0.051(2) 0.065(3) 0.057(2) -0.036(2) 0.0090(18) -0.033(2) C26 0.0339(19) 0.056(2) 0.0412(18) -0.0227(16) 0.0046(14) -0.0227(18) C27 0.044(2) 0.057(2) 0.0356(17) -0.0156(16) 0.0120(15) -0.0296(19) C28 0.053(2) 0.063(3) 0.0385(19) -0.0171(17) 0.0175(17) -0.029(2) C29 0.065(3) 0.053(2) 0.0283(17) -0.0113(16) 0.0098(16) -0.034(2) C30 0.043(2) 0.043(2) 0.0287(16) -0.0050(14) 0.0001(14) -0.0152(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Sm O1 2.5743(18) . ? Sm O2 2.608(2) . ? Sm O3 2.6020(17) . ? Sm B1 2.959(4) . ? Sm H1C 2.53(3) . ? Sm B2 2.783(3) . ? Sm H2A 2.60(3) . ? Sm H2B 2.55(2) . ? Sm H2C 2.61(3) . ? Sm C1 2.873(3) . ? P1 B1 1.939(4) . ? P1 C1 1.756(3) . ? P1 C2 1.827(3) . ? P1 C3 1.823(3) . ? P2 B2 1.928(3) . ? P2 C10 1.719(3) . ? P2 C11 1.829(3) . ? P2 C12 1.814(4) . ? Si1 C1 1.855(3) . ? Si1 C4 1.881(4) . ? Si1 C5 1.880(3) . ? Si1 C6 1.883(4) . ? Si2 C1 1.855(3) . ? Si2 C7 1.889(4) . ? Si2 C8 1.868(4) . ? Si2 C9 1.884(3) . ? Si3 C10 1.820(3) . ? Si3 C13 1.878(4) . ? Si3 C14 1.887(3) . ? Si3 C15 1.881(3) . ? Si4 C10 1.827(3) . ? Si4 C16 1.893(3) . ? Si4 C17 1.888(3) . ? Si4 C18 1.880(3) . ? O1 C19 1.452(3) . ? O1 C22 1.457(3) . ? O2 C23 1.432(4) . ? O2 C26 1.455(3) . ? O3 C27 1.437(3) . ? O3 C30 1.441(3) . ? B1 H1A 1.09(3) . ? B1 H1B 1.09(3) . ? B1 H1C 1.11(3) . ? B2 H2A 1.12(3) . ? B2 H2B 1.11(3) . ? B2 H2C 1.14(3) . ? C2 H2D 0.980 . ? C2 H2E 0.980 . ? C2 H2F 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.486(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.516(5) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.478(4) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.498(5) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 C25 1.499(5) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C25 C26 1.496(5) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.515(4) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 C29 1.528(5) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C29 C30 1.519(4) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? 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 O1 Sm O2 77.21(6) . . ? O1 Sm O3 149.05(7) . . ? O1 Sm H1C 105.7(7) . . ? O1 Sm H2A 71.1(6) . . ? O1 Sm H2B 111.8(6) . . ? O1 Sm H2C 93.4(6) . . ? O1 Sm C1 110.73(7) . . ? O2 Sm O3 73.71(6) . . ? O2 Sm H1C 71.8(7) . . ? O2 Sm H2A 107.8(6) . . ? O2 Sm H2B 120.2(6) . . ? O2 Sm H2C 80.8(6) . . ? O2 Sm C1 148.84(8) . . ? O3 Sm H1C 75.0(7) . . ? O3 Sm H2A 108.1(6) . . ? O3 Sm H2B 75.2(5) . . ? O3 Sm H2C 71.8(6) . . ? O3 Sm C1 99.68(7) . . ? H1C Sm H2A 176.7(9) . . ? H1C Sm H2B 142.3(9) . . ? H1C Sm H2C 141.7(9) . . ? H1C Sm C1 77.1(7) . . ? H2A Sm H2B 40.9(8) . . ? H2A Sm H2C 40.5(8) . . ? H2A Sm C1 103.3(6) . . ? H2B Sm H2C 41.2(9) . . ? H2B Sm C1 85.8(6) . . ? H2C Sm C1 127.0(7) . . ? B1 P1 C1 115.18(16) . . ? B1 P1 C2 110.48(18) . . ? B1 P1 C3 103.33(18) . . ? C1 P1 C2 113.65(17) . . ? C1 P1 C3 112.17(15) . . ? C2 P1 C3 100.59(18) . . ? B2 P2 C10 118.58(15) . . ? B2 P2 C11 105.69(15) . . ? B2 P2 C12 102.68(17) . . ? C10 P2 C11 112.79(16) . . ? C10 P2 C12 113.97(16) . . ? C11 P2 C12 101.22(17) . . ? C1 Si1 C4 112.72(14) . . ? C1 Si1 C5 114.40(15) . . ? C1 Si1 C6 113.68(15) . . ? C4 Si1 C5 104.83(16) . . ? C4 Si1 C6 105.83(18) . . ? C5 Si1 C6 104.50(16) . . ? C1 Si2 C7 113.39(15) . . ? C1 Si2 C8 113.08(16) . . ? C1 Si2 C9 114.17(15) . . ? C7 Si2 C8 105.19(18) . . ? C7 Si2 C9 107.61(16) . . ? C8 Si2 C9 102.44(17) . . ? C10 Si3 C13 115.31(16) . . ? C10 Si3 C14 114.37(15) . . ? C10 Si3 C15 112.98(15) . . ? C13 Si3 C14 102.84(17) . . ? C13 Si3 C15 103.92(18) . . ? C14 Si3 C15 106.27(17) . . ? C10 Si4 C16 113.20(15) . . ? C10 Si4 C17 112.84(15) . . ? C10 Si4 C18 115.25(15) . . ? C16 Si4 C17 105.09(16) . . ? C16 Si4 C18 106.69(15) . . ? C17 Si4 C18 102.75(16) . . ? Sm O1 C19 122.41(16) . . ? Sm O1 C22 129.19(16) . . ? C19 O1 C22 108.3(2) . . ? Sm O2 C23 118.62(18) . . ? Sm O2 C26 132.38(18) . . ? C23 O2 C26 108.7(2) . . ? Sm O3 C27 126.86(16) . . ? Sm O3 C30 127.89(17) . . ? C27 O3 C30 104.4(2) . . ? P1 B1 H1A 106.1(17) . . ? P1 B1 H1B 109.2(14) . . ? P1 B1 H1C 102.4(16) . . ? H1A B1 H1B 115(2) . . ? H1A B1 H1C 114(2) . . ? H1B B1 H1C 109(2) . . ? P2 B2 H2A 113.1(14) . . ? P2 B2 H2B 108.6(13) . . ? P2 B2 H2C 114.0(14) . . ? H2A B2 H2B 107.3(19) . . ? H2A B2 H2C 105.8(19) . . ? H2B B2 H2C 107.7(19) . . ? Sm C1 P1 90.41(12) . . ? Sm C1 Si1 100.69(12) . . ? Sm C1 Si2 119.64(12) . . ? P1 C1 Si1 114.70(15) . . ? P1 C1 Si2 116.04(16) . . ? Si1 C1 Si2 112.80(16) . . ? P1 C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? P1 C2 H2F 109.5 . . ? H2D C2 H2E 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C10 Si3 120.52(17) . . ? P2 C10 Si4 115.55(16) . . ? Si3 C10 Si4 118.58(17) . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si4 C17 H17A 109.5 . . ? Si4 C17 H17B 109.5 . . ? Si4 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 H19A 110.7 . . ? O1 C19 H19B 110.7 . . ? O1 C19 C20 105.4(3) . . ? H19A C19 H19B 108.8 . . ? H19A C19 C20 110.7 . . ? H19B C19 C20 110.7 . . ? C19 C20 H20A 111.2 . . ? C19 C20 H20B 111.2 . . ? C19 C20 C21 102.8(3) . . ? H20A C20 H20B 109.1 . . ? H20A C20 C21 111.2 . . ? H20B C20 C21 111.2 . . ? C20 C21 H21A 111.3 . . ? C20 C21 H21B 111.3 . . ? C20 C21 C22 102.4(3) . . ? H21A C21 H21B 109.2 . . ? H21A C21 C22 111.3 . . ? H21B C21 C22 111.3 . . ? O1 C22 C21 106.6(3) . . ? O1 C22 H22A 110.4 . . ? O1 C22 H22B 110.4 . . ? C21 C22 H22A 110.4 . . ? C21 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? O2 C23 H23A 110.4 . . ? O2 C23 H23B 110.4 . . ? O2 C23 C24 106.4(3) . . ? H23A C23 H23B 108.6 . . ? H23A C23 C24 110.4 . . ? H23B C23 C24 110.4 . . ? C23 C24 H24A 111.1 . . ? C23 C24 H24B 111.1 . . ? C23 C24 C25 103.4(3) . . ? H24A C24 H24B 109.0 . . ? H24A C24 C25 111.1 . . ? H24B C24 C25 111.1 . . ? C24 C25 H25A 111.3 . . ? C24 C25 H25B 111.3 . . ? C24 C25 C26 102.4(3) . . ? H25A C25 H25B 109.2 . . ? H25A C25 C26 111.3 . . ? H25B C25 C26 111.3 . . ? O2 C26 C25 106.0(3) . . ? O2 C26 H26A 110.5 . . ? O2 C26 H26B 110.5 . . ? C25 C26 H26A 110.5 . . ? C25 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? O3 C27 H27A 110.8 . . ? O3 C27 H27B 110.8 . . ? O3 C27 C28 104.6(2) . . ? H27A C27 H27B 108.9 . . ? H27A C27 C28 110.8 . . ? H27B C27 C28 110.8 . . ? C27 C28 H28A 110.9 . . ? C27 C28 H28B 110.9 . . ? C27 C28 C29 104.1(3) . . ? H28A C28 H28B 109.0 . . ? H28A C28 C29 110.9 . . ? H28B C28 C29 110.9 . . ? C28 C29 H29A 110.9 . . ? C28 C29 H29B 110.9 . . ? C28 C29 C30 104.4(2) . . ? H29A C29 H29B 108.9 . . ? H29A C29 C30 110.9 . . ? H29B C29 C30 110.9 . . ? O3 C30 C29 105.2(3) . . ? O3 C30 H30A 110.7 . . ? O3 C30 H30B 110.7 . . ? C29 C30 H30A 110.7 . . ? C29 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.446 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.070 # 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 0.026 0.474 452 55 ' ' _platon_squeeze_details ; ; #===END