# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1174 data_compound7 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C37 H100 Cl P4 Si W' _chemical_formula_weight 916.44 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 8.977(9) _cell_length_b 30.300(30) _cell_length_c 16.449(20) _cell_angle_alpha 90.00 _cell_angle_beta 95.23(9) _cell_angle_gamma 90.00 _cell_volume 4455.4(82) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method ? _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 2.847 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P3' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5218 _diffrn_reflns_av_R_equivalents 0.1435 _diffrn_reflns_av_sigmaI/netI 0.1877 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4784 _reflns_number_observed 2117 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1406P)^2^+246.5966P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4781 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2602 _refine_ls_R_factor_obs 0.1279 _refine_ls_wR_factor_all 0.4043 _refine_ls_wR_factor_obs 0.2812 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max 0.237 _refine_ls_shift/esd_mean 0.034 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W W -0.9208(2) 0.83189(6) 0.15685(11) 0.0754(8) Uani 1 d . . P1 P -1.0744(17) 0.8824(6) 0.0723(11) 0.137(6) Uani 1 d . . P2 P -0.8323(17) 0.8134(5) 0.0272(8) 0.115(5) Uani 1 d . . P3 P -0.7364(16) 0.7924(4) 0.2461(8) 0.099(4) Uani 1 d . . P4 P -0.9806(16) 0.8612(5) 0.2870(8) 0.103(4) Uani 1 d . . Si Si -1.7747(17) 0.5907(4) 0.1314(8) 0.099(5) Uani 1 d . . C1 C -1.0709(34) 0.7863(9) 0.1532(17) 0.038(8) Uiso 1 d . . C2 C -1.1711(37) 0.7494(10) 0.1500(19) 0.046(8) Uiso 1 d . . C3 C -1.1961(48) 0.7238(13) 0.2128(25) 0.080(12) Uiso 1 d . . H3A H -1.1354(48) 0.7279(13) 0.2618(25) 0.096 Uiso 1 calc R . C4 C -1.3002(59) 0.6928(17) 0.2115(32) 0.118(17) Uiso 1 d . . H4A H -1.3064(59) 0.6752(17) 0.2580(32) 0.141 Uiso 1 calc R . C5 C -1.3980(50) 0.6857(13) 0.1451(25) 0.075(12) Uiso 1 d . . C6 C -1.3802(60) 0.7100(17) 0.0768(33) 0.121(18) Uiso 1 d . . H6A H -1.4404(60) 0.7048(17) 0.0280(33) 0.145 Uiso 1 calc R . C7 C -1.2691(50) 0.7433(14) 0.0814(27) 0.097(14) Uiso 1 d . . H7A H -1.2618(50) 0.7618(14) 0.0360(27) 0.116 Uiso 1 calc R . C8 C -1.5124(69) 0.6550(18) 0.1413(32) 0.119(18) Uiso 1 d . . C9 C -1.6082(56) 0.6275(16) 0.1377(27) 0.099(15) Uiso 1 d . . C10 C -1.7019(85) 0.5389(23) 0.0781(45) 0.174(27) Uiso 1 d . . H10A H -1.6100(85) 0.5299(23) 0.1119(45) 0.209 Uiso 1 calc R . C11 C -1.6531(119) 0.5511(35) 0.0000(69) 0.332(58) Uiso 1 d . . H11A H -1.5856(119) 0.5761(35) 0.0069(69) 0.498 Uiso 1 calc R . H11B H -1.7392(119) 0.5590(35) -0.0370(69) 0.498 Uiso 1 calc R . H11C H -1.6016(119) 0.5263(35) -0.0223(69) 0.498 Uiso 1 calc R . C12 C -1.8059(84) 0.5038(25) 0.0856(44) 0.205(31) Uiso 1 d . . H12A H -1.8278(84) 0.5012(25) 0.1420(44) 0.307 Uiso 1 calc R . H12B H -1.7631(84) 0.4764(25) 0.0682(44) 0.307 Uiso 1 calc R . H12C H -1.8975(84) 0.5100(25) 0.0515(44) 0.307 Uiso 1 calc R . C13 C -1.9326(70) 0.6277(21) 0.0791(41) 0.157(23) Uiso 1 d . . H13A H -1.9420(70) 0.6554(21) 0.1100(41) 0.189 Uiso 1 calc R . C14 C -1.9186(83) 0.6365(24) -0.0032(48) 0.210(33) Uiso 1 d . . H14A H -1.8294(83) 0.6540(24) -0.0081(48) 0.315 Uiso 1 calc R . H14B H -2.0058(83) 0.6527(24) -0.0262(48) 0.315 Uiso 1 calc R . H14C H -1.9108(83) 0.6089(24) -0.0326(48) 0.315 Uiso 1 calc R . C15 C -2.0878(69) 0.5964(20) 0.0818(37) 0.165(24) Uiso 1 d . . H15A H -2.1012(69) 0.5887(20) 0.1379(37) 0.247 Uiso 1 calc R . H15B H -2.0771(69) 0.5696(20) 0.0504(37) 0.247 Uiso 1 calc R . H15C H -2.1741(69) 0.6128(20) 0.0585(37) 0.247 Uiso 1 calc R . C16 C -1.8079(50) 0.5749(14) 0.2356(25) 0.089(13) Uiso 1 d . . H16A H -1.8880(50) 0.5523(14) 0.2308(25) 0.106 Uiso 1 calc R . C17 C -1.6740(57) 0.5539(16) 0.2849(31) 0.127(18) Uiso 1 d . . H17A H -1.6368(57) 0.5295(16) 0.2543(31) 0.190 Uiso 1 calc R . H17B H -1.7044(57) 0.5430(16) 0.3364(31) 0.190 Uiso 1 calc R . H17C H -1.5955(57) 0.5757(16) 0.2954(31) 0.190 Uiso 1 calc R . C18 C -1.8671(60) 0.6138(17) 0.2841(32) 0.138(20) Uiso 1 d . . H18A H -1.9527(60) 0.6269(17) 0.2528(32) 0.207 Uiso 1 calc R . H18B H -1.7889(60) 0.6357(17) 0.2941(32) 0.207 Uiso 1 calc R . H18C H -1.8970(60) 0.6031(17) 0.3358(32) 0.207 Uiso 1 calc R . C19 C -0.7574(37) 0.8823(10) 0.1621(18) 0.044(8) Uiso 1 d . . C20 C -0.6636(46) 0.9147(12) 0.1722(22) 0.070(11) Uiso 1 d . . C21 C -0.5521(45) 0.9493(12) 0.1798(23) 0.070(11) Uiso 1 d . . C22 C -0.4544(53) 0.9564(16) 0.2475(29) 0.102(15) Uiso 1 d . . H22A H -0.4548(53) 0.9366(16) 0.2916(29) 0.122 Uiso 1 calc R . C23 C -0.3537(53) 0.9919(15) 0.2535(29) 0.100(15) Uiso 1 d . . H23A H -0.2876(53) 0.9956(15) 0.3007(29) 0.120 Uiso 1 calc R . C24 C -0.3528(54) 1.0197(15) 0.1929(30) 0.095(14) Uiso 1 d . . C25 C -0.4390(56) 1.0171(16) 0.1269(31) 0.112(17) Uiso 1 d . . H25A H -0.4315(56) 1.0381(16) 0.0854(31) 0.134 Uiso 1 calc R . C26 C -0.5524(62) 0.9807(17) 0.1154(34) 0.128(19) Uiso 1 d . . H26A H -0.6199(62) 0.9788(17) 0.0683(34) 0.154 Uiso 1 calc R . C27 C -0.2331(78) 1.0619(22) 0.2009(42) 0.199(30) Uiso 1 d . . H27A H -0.1737(78) 1.0605(22) 0.2531(42) 0.298 Uiso 1 calc R . H27B H -0.2882(78) 1.0895(22) 0.1970(42) 0.298 Uiso 1 calc R . H27C H -0.1677(78) 1.0603(22) 0.1571(42) 0.298 Uiso 1 calc R . C28 C -1.0534(72) 0.9422(20) 0.0801(39) 0.173(26) Uiso 1 d . . H28A H -0.9479(72) 0.9497(20) 0.0874(39) 0.260 Uiso 1 calc R . H28B H -1.1024(72) 0.9528(20) 0.1265(39) 0.260 Uiso 1 calc R . H28C H -1.0987(72) 0.9559(20) 0.0306(39) 0.260 Uiso 1 calc R . C29 C -1.2750(66) 0.8785(20) 0.0606(37) 0.166(24) Uiso 1 d . . H29A H -1.3043(66) 0.8477(20) 0.0548(37) 0.249 Uiso 1 calc R . H29B H -1.3135(66) 0.8947(20) 0.0123(37) 0.249 Uiso 1 calc R . H29C H -1.3154(66) 0.8909(20) 0.1082(37) 0.249 Uiso 1 calc R . C30 C -1.0074(95) 0.8726(28) -0.0353(48) 0.223(36) Uiso 1 d . . H30A H -1.0894(95) 0.8815(28) -0.0754(48) 0.267 Uiso 1 calc R . H30B H -0.9244(95) 0.8930(28) -0.0413(48) 0.267 Uiso 1 calc R . C31 C -0.9616(111) 0.8316(31) -0.0573(60) 0.266(44) Uiso 1 d . . H31A H -0.9118(111) 0.8331(31) -0.1078(60) 0.319 Uiso 1 calc R . H31B H -1.0469(111) 0.8114(31) -0.0655(60) 0.319 Uiso 1 calc R . C32 C -0.8476(72) 0.7597(20) -0.0087(38) 0.174(26) Uiso 1 d . . H32A H -0.7860(72) 0.7404(20) 0.0276(38) 0.261 Uiso 1 calc R . H32B H -0.8141(72) 0.7583(20) -0.0630(38) 0.261 Uiso 1 calc R . H32C H -0.9511(72) 0.7503(20) -0.0106(38) 0.261 Uiso 1 calc R . C33 C -0.6416(61) 0.8308(18) 0.0041(35) 0.149(21) Uiso 1 d . . H33A H -0.6238(61) 0.8609(18) 0.0221(35) 0.223 Uiso 1 calc R . H33B H -0.6341(61) 0.8288(18) -0.0542(35) 0.223 Uiso 1 calc R . H33C H -0.5678(61) 0.8115(18) 0.0325(35) 0.223 Uiso 1 calc R . C34 C -0.7406(55) 0.7339(14) 0.2479(29) 0.112(16) Uiso 1 d . . H34A H -0.8433(55) 0.7239(14) 0.2478(29) 0.168 Uiso 1 calc R . H34B H -0.6830(55) 0.7233(14) 0.2968(29) 0.168 Uiso 1 calc R . H34C H -0.6978(55) 0.7224(14) 0.2001(29) 0.168 Uiso 1 calc R . C35 C -0.5352(58) 0.7996(18) 0.2479(33) 0.140(20) Uiso 1 d . . H35A H -0.5118(58) 0.8308(18) 0.2465(33) 0.210 Uiso 1 calc R . H35B H -0.4996(58) 0.7852(18) 0.2007(33) 0.210 Uiso 1 calc R . H35C H -0.4869(58) 0.7866(18) 0.2973(33) 0.210 Uiso 1 calc R . C36 C -0.7617(78) 0.8024(23) 0.3581(40) 0.180(27) Uiso 1 d . . H36A H -0.8203(78) 0.7782(23) 0.3785(40) 0.216 Uiso 1 calc R . H36B H -0.6635(78) 0.8025(23) 0.3894(40) 0.216 Uiso 1 calc R . C37 C -0.8390(63) 0.8451(18) 0.3711(33) 0.135(20) Uiso 1 d . . H37A H -0.7636(63) 0.8685(18) 0.3783(33) 0.161 Uiso 1 calc R . H37B H -0.8882(63) 0.8431(18) 0.4218(33) 0.161 Uiso 1 calc R . C38 C -0.9788(76) 0.9197(21) 0.3094(41) 0.184(28) Uiso 1 d . . H38A H -0.8908(76) 0.9331(21) 0.2896(41) 0.277 Uiso 1 calc R . H38B H -0.9766(76) 0.9240(21) 0.3679(41) 0.277 Uiso 1 calc R . H38C H -1.0680(76) 0.9334(21) 0.2827(41) 0.277 Uiso 1 calc R . C39 C -1.1529(67) 0.8437(19) 0.3289(37) 0.164(24) Uiso 1 d . . H39A H -1.1669(67) 0.8122(19) 0.3204(37) 0.245 Uiso 1 calc R . H39B H -1.2371(67) 0.8595(19) 0.3016(37) 0.245 Uiso 1 calc R . H39C H -1.1460(67) 0.8501(19) 0.3869(37) 0.245 Uiso 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 W 0.0684(14) 0.0858(12) 0.0715(11) -0.0040(11) 0.0044(8) -0.0053(13) P1 0.081(12) 0.167(15) 0.160(15) 0.042(12) -0.008(10) 0.021(11) P2 0.111(12) 0.152(13) 0.084(9) -0.021(8) 0.028(8) -0.025(10) P3 0.090(11) 0.098(10) 0.109(10) 0.011(8) 0.012(8) -0.005(8) P4 0.100(11) 0.124(11) 0.089(9) -0.019(8) 0.026(8) -0.001(9) Si 0.120(13) 0.076(8) 0.098(10) -0.001(7) 0.000(9) -0.026(9) _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 W C1 1.93(3) . ? W C19 2.11(3) . ? W P1 2.41(2) . ? W P2 2.409(13) . ? W P4 2.422(13) . ? W P3 2.425(14) . ? P1 C29 1.80(6) . ? P1 C28 1.83(6) . ? P1 C30 1.94(8) . ? P2 C32 1.73(6) . ? P2 C31 1.81(9) . ? P2 C33 1.86(5) . ? P3 C34 1.77(4) . ? P3 C35 1.82(5) . ? P3 C36 1.90(7) . ? P4 C38 1.81(6) . ? P4 C39 1.83(6) . ? P4 C37 1.86(5) . ? Si C16 1.83(4) . ? Si C9 1.86(5) . ? Si C10 1.94(7) . ? Si C13 1.94(6) . ? C1 C2 1.43(4) . ? C2 C3 1.33(4) . ? C2 C7 1.38(5) . ? C3 C4 1.32(5) . ? C4 C5 1.35(6) . ? C5 C6 1.36(6) . ? C5 C8 1.38(6) . ? C6 C7 1.41(6) . ? C8 C9 1.20(6) . ? C10 C12 1.43(8) . ? C10 C11 1.44(11) . ? C13 C14 1.40(8) . ? C13 C15 1.69(7) . ? C16 C18 1.54(6) . ? C16 C17 1.53(6) . ? C19 C20 1.29(4) . ? C20 C21 1.45(5) . ? C21 C22 1.37(5) . ? C21 C26 1.42(6) . ? C22 C23 1.40(6) . ? C23 C24 1.31(5) . ? C24 C25 1.28(6) . ? C24 C27 1.67(7) . ? C25 C26 1.50(6) . ? C30 C31 1.37(10) . ? C36 C37 1.49(7) . ? 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 C1 W C19 179.3(12) . . ? C1 W P1 94.3(10) . . ? C19 W P1 85.6(9) . . ? C1 W P2 95.3(9) . . ? C19 W P2 85.4(9) . . ? P1 W P2 81.6(6) . . ? C1 W P4 94.5(9) . . ? C19 W P4 84.7(9) . . ? P1 W P4 96.7(6) . . ? P2 W P4 170.1(5) . . ? C1 W P3 95.9(9) . . ? C19 W P3 84.2(9) . . ? P1 W P3 169.7(5) . . ? P2 W P3 99.2(5) . . ? P4 W P3 80.8(5) . . ? C29 P1 C28 99.7(30) . . ? C29 P1 C30 106.4(33) . . ? C28 P1 C30 100.2(33) . . ? C29 P1 W 122.3(22) . . ? C28 P1 W 122.6(22) . . ? C30 P1 W 102.8(26) . . ? C32 P2 C31 90.0(37) . . ? C32 P2 C33 103.9(29) . . ? C31 P2 C33 107.1(37) . . ? C32 P2 W 119.8(22) . . ? C31 P2 W 111.6(33) . . ? C33 P2 W 119.9(19) . . ? C34 P3 C35 98.1(25) . . ? C34 P3 C36 97.9(26) . . ? C35 P3 C36 99.9(28) . . ? C34 P3 W 119.2(17) . . ? C35 P3 W 125.0(18) . . ? C36 P3 W 111.9(22) . . ? C38 P4 C39 101.5(30) . . ? C38 P4 C37 96.4(28) . . ? C39 P4 C37 100.9(27) . . ? C38 P4 W 122.7(23) . . ? C39 P4 W 119.4(20) . . ? C37 P4 W 111.8(19) . . ? C16 Si C9 107.7(21) . . ? C16 Si C10 107.5(27) . . ? C9 Si C10 102.0(28) . . ? C16 Si C13 113.0(25) . . ? C9 Si C13 103.3(24) . . ? C10 Si C13 121.9(30) . . ? C2 C1 W 174.5(24) . . ? C3 C2 C7 114.7(37) . . ? C3 C2 C1 125.3(32) . . ? C7 C2 C1 119.1(31) . . ? C4 C3 C2 124.9(45) . . ? C3 C4 C5 122.0(51) . . ? C4 C5 C6 117.5(49) . . ? C4 C5 C8 124.6(46) . . ? C6 C5 C8 117.9(47) . . ? C5 C6 C7 118.4(50) . . ? C2 C7 C6 122.2(43) . . ? C9 C8 C5 178.0(57) . . ? C8 C9 Si 172.5(46) . . ? C12 C10 C11 121.4(77) . . ? C12 C10 Si 108.3(55) . . ? C11 C10 Si 109.7(65) . . ? C14 C13 C15 106.3(57) . . ? C14 C13 Si 114.4(53) . . ? C15 C13 Si 103.6(39) . . ? C18 C16 C17 109.6(39) . . ? C18 C16 Si 112.1(31) . . ? C17 C16 Si 114.8(33) . . ? C20 C19 W 173.8(27) . . ? C19 C20 C21 175.9(38) . . ? C22 C21 C26 117.3(44) . . ? C22 C21 C20 124.7(39) . . ? C26 C21 C20 117.8(40) . . ? C21 C22 C23 122.5(46) . . ? C24 C23 C22 119.4(49) . . ? C25 C24 C23 124.3(54) . . ? C25 C24 C27 116.8(49) . . ? C23 C24 C27 119.0(49) . . ? C24 C25 C26 120.3(52) . . ? C21 C26 C25 116.2(48) . . ? C31 C30 P1 120.3(71) . . ? C30 C31 P2 105.1(73) . . ? C37 C36 P3 112.0(45) . . ? C36 C37 P4 114.5(43) . . ? _refine_diff_density_max 2.076 _refine_diff_density_min -2.202 _refine_diff_density_rms 0.227