Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Sun, Duoli' 'Linderman, Sergey V.' 'Rathore, Rajendra' 'Kochi, J.' _publ_contact_author_name 'Dr J Kochi' _publ_contact_author_address ; Dr J Kochi Department of Chemistry University of Houston Houston Texas 77204-5641 UNITED STATES OF AMERICA ; _publ_contact_author_email 'JKOCHI@POP.UH.EDU' data_juerpsx _database_code_CSD 162395 _audit_creation_method SHELXL _chemical_name_systematic ; 1,4-dimethoxy-2,5-dimethylbenzene ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H14 O2' _chemical_formula_weight 166.21 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' '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 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 6.4943(4) _cell_length_b 8.9209(5) _cell_length_c 8.0240(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.817(2) _cell_angle_gamma 90.00 _cell_volume 455.02(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2081 _cell_measurement_theta_min 2 _cell_measurement_theta_max 36 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method ? _exptl_crystal_F_000 180 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.963 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4073 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 36.25 _reflns_number_total 1987 _reflns_number_observed 1593 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 4 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.1420P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1983 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_obs 0.0489 _refine_ls_wR_factor_all 0.1405 _refine_ls_wR_factor_obs 0.1200 _refine_ls_goodness_of_fit_all 1.108 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.130 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.04747(14) 0.91831(10) 0.86519(11) 0.0143(2) Uani 1 d . . O11 O 0.08445(11) 0.84348(8) 0.72369(9) 0.0192(2) Uani 1 d . . C12 C 0.2708(2) 0.75498(12) 0.74458(13) 0.0233(2) Uani 1 d . . H12A H 0.2826(8) 0.7117(9) 0.6347(3) 0.035 Uiso 1 calc R . H12B H 0.2641(7) 0.6742(7) 0.8261(10) 0.035 Uiso 1 calc R . H12C H 0.3937(2) 0.8182(3) 0.7873(12) 0.035 Uiso 1 calc R . C2 C -0.13038(13) 1.01104(10) 0.83633(11) 0.0149(2) Uani 1 d . . C21 C -0.2647(2) 1.02521(12) 0.66047(12) 0.0215(2) Uani 1 d . . H21A H -0.3725(10) 1.1020(8) 0.6608(3) 0.032 Uiso 1 calc R . H21B H -0.3326(12) 0.9289(3) 0.6258(5) 0.032 Uiso 1 calc R . H21C H -0.1764(3) 1.0540(11) 0.5802(3) 0.032 Uiso 1 calc R . C3 C -0.17573(14) 1.09225(10) 0.97306(11) 0.0152(2) Uani 1 d . . H3 H -0.29575(14) 1.15566(10) 0.95569(11) 0.018 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 C1 0.0151(4) 0.0125(3) 0.0152(3) -0.0004(2) 0.0031(3) 0.0001(3) O11 0.0210(3) 0.0201(3) 0.0165(3) -0.0031(2) 0.0038(2) 0.0047(2) C12 0.0261(5) 0.0225(5) 0.0231(4) 0.0008(3) 0.0093(4) 0.0088(4) C2 0.0142(3) 0.0142(3) 0.0154(3) 0.0004(3) 0.0012(3) 0.0006(3) C21 0.0208(4) 0.0252(4) 0.0163(4) -0.0012(3) -0.0013(3) 0.0045(4) C3 0.0136(3) 0.0141(3) 0.0174(4) 0.0013(3) 0.0019(3) 0.0018(3) _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 C1 O11 1.3799(11) . ? C1 C3 1.3944(12) 3_577 ? C1 C2 1.4009(12) . ? O11 C12 1.4256(12) . ? C2 C3 1.3955(12) . ? C2 C21 1.5046(13) . ? C3 C1 1.3944(12) 3_577 ? 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 O11 C1 C3 124.18(8) . 3_577 ? O11 C1 C2 115.23(8) . . ? C3 C1 C2 120.59(8) 3_577 . ? C1 O11 C12 117.24(7) . . ? C3 C2 C1 118.44(8) . . ? C3 C2 C21 121.24(8) . . ? C1 C2 C21 120.30(8) . . ? C1 C3 C2 120.98(8) 3_577 . ? _refine_diff_density_max 0.532 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.056 data_pier-rsy _database_code_CSD 162396 _audit_creation_method SHELXL _chemical_name_systematic ; 1,3-Bis(2',5'-dimethoxy-4'-methyl)propane ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H28 O4' _chemical_formula_weight 344.43 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.8130(5) _cell_length_b 7.9994(5) _cell_length_c 29.763(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1860.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 4661 _cell_measurement_theta_min 2 _cell_measurement_theta_max 34 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method none _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.963 _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number 216 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 23294 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 35.90 _reflns_number_total 4699 _reflns_number_observed 4102 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS (Sheldrick, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 9 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.1120P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(71) _refine_ls_number_reflns 4690 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_obs 0.0386 _refine_ls_wR_factor_all 0.1055 _refine_ls_wR_factor_obs 0.0943 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.110 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.67130(13) 0.71089(12) -0.06297(3) 0.0214(2) Uani 1 d . . O2 O 0.76392(12) 0.27387(11) 0.07907(3) 0.0195(2) Uani 1 d . . O3 O 0.60843(13) 0.95814(11) 0.18331(3) 0.0207(2) Uani 1 d . . O4 O 0.89649(13) 0.57283(11) 0.31801(3) 0.0206(2) Uani 1 d . . C1 C 0.69033(14) 0.60474(14) -0.02688(3) 0.0155(2) Uani 1 d . . C2 C 0.79890(14) 0.46875(15) -0.03387(4) 0.0162(2) Uani 1 d . . C3 C 0.8235(2) 0.35516(14) 0.00116(4) 0.0170(2) Uani 1 d . . C4 C 0.74142(15) 0.37725(13) 0.04256(4) 0.0151(2) Uani 1 d . . C5 C 0.62992(14) 0.51199(14) 0.04924(3) 0.0137(2) Uani 1 d . . C6 C 0.60600(14) 0.62533(14) 0.01418(4) 0.0153(2) Uani 1 d . . C7 C 0.5762(2) 0.8598(2) -0.05525(5) 0.0259(3) Uani 1 d . . C8 C 0.8695(2) 0.1303(2) 0.07334(5) 0.0292(3) Uani 1 d . . C9 C 0.8857(2) 0.4457(2) -0.07876(4) 0.0231(2) Uani 1 d . . C10 C 0.54215(14) 0.53757(15) 0.09376(4) 0.0153(2) Uani 1 d . . C11 C 0.65933(15) 0.61284(15) 0.12983(4) 0.0159(2) Uani 1 d . . C12 C 0.5676(2) 0.61496(15) 0.17518(4) 0.0169(2) Uani 1 d . . C13 C 0.6668(2) 0.69226(14) 0.21350(3) 0.0155(2) Uani 1 d . . C14 C 0.6804(2) 0.86644(15) 0.21749(3) 0.0164(2) Uani 1 d . . C15 C 0.7611(2) 0.93662(15) 0.25461(4) 0.0175(2) Uani 1 d . . C16 C 0.8314(2) 0.83677(14) 0.28847(4) 0.0169(2) Uani 1 d . . C17 C 0.8234(2) 0.66271(14) 0.28372(4) 0.0162(2) Uani 1 d . . C18 C 0.7415(2) 0.59238(14) 0.24668(4) 0.0169(2) Uani 1 d . . C19 C 0.6307(2) 1.1353(2) 0.18497(4) 0.0209(2) Uani 1 d . . C20 C 0.9090(2) 0.9128(2) 0.32991(4) 0.0233(2) Uani 1 d . . C21 C 0.8734(2) 0.3961(2) 0.31753(4) 0.0222(2) Uani 1 d . . H3 H 0.8993(23) 0.2602(24) -0.0042(6) 0.015(4) Uiso 1 d . . H6 H 0.5319(25) 0.7204(23) 0.0193(6) 0.021(4) Uiso 1 d . . H7A H 0.5808(30) 0.9279(29) -0.0845(7) 0.040(6) Uiso 1 d . . H7B H 0.6264(27) 0.9255(27) -0.0313(7) 0.036(5) Uiso 1 d . . H7C H 0.4612(26) 0.8360(23) -0.0484(6) 0.024(4) Uiso 1 d . . H8A H 0.8653(30) 0.0696(31) 0.1014(7) 0.042(6) Uiso 1 d . . H8B H 0.9821(33) 0.1621(29) 0.0656(7) 0.039(6) Uiso 1 d . . H8C H 0.8150(24) 0.0575(24) 0.0512(6) 0.024(4) Uiso 1 d . . H9A H 0.9679(29) 0.3482(28) -0.0788(7) 0.030(5) Uiso 1 d . . H9B H 0.9436(30) 0.5528(28) -0.0863(7) 0.038(6) Uiso 1 d . . H9C H 0.8150(27) 0.4140(26) -0.1008(6) 0.029(5) Uiso 1 d . . H10A H 0.4961(22) 0.4335(22) 0.1031(5) 0.018(4) Uiso 1 d . . H10B H 0.4374(23) 0.6200(22) 0.0896(5) 0.014(4) Uiso 1 d . . H11A H 0.7593(24) 0.5481(21) 0.1315(5) 0.018(4) Uiso 1 d . . H11B H 0.6932(25) 0.7271(22) 0.1204(5) 0.021(4) Uiso 1 d . . H12A H 0.4588(24) 0.6702(22) 0.1719(5) 0.018(4) Uiso 1 d . . H12B H 0.5312(23) 0.4993(22) 0.1839(6) 0.017(4) Uiso 1 d . . H15 H 0.7744(25) 1.0594(24) 0.2578(6) 0.022(4) Uiso 1 d . . H18 H 0.7288(22) 0.4721(20) 0.2436(5) 0.010(4) Uiso 1 d . . H19A H 0.5773(27) 1.1788(24) 0.1583(7) 0.029(5) Uiso 1 d . . H19B H 0.7501(26) 1.1646(22) 0.1864(6) 0.024(4) Uiso 1 d . . H19C H 0.5758(30) 1.1922(30) 0.2099(7) 0.043(6) Uiso 1 d . . H20A H 1.0222(36) 0.8693(32) 0.3368(8) 0.056(7) Uiso 1 d . . H20B H 0.8432(33) 0.8915(30) 0.3577(8) 0.049(6) Uiso 1 d . . H20C H 0.9192(31) 1.0331(28) 0.3284(7) 0.038(6) Uiso 1 d . . H21A H 0.9227(28) 0.3586(25) 0.3440(6) 0.029(5) Uiso 1 d . . H21B H 0.9241(25) 0.3443(25) 0.2922(6) 0.024(4) Uiso 1 d . . H21C H 0.7562(27) 0.3715(24) 0.3175(6) 0.028(5) Uiso 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 O1 0.0236(4) 0.0249(4) 0.0156(3) 0.0028(3) 0.0028(3) 0.0067(4) O2 0.0226(4) 0.0169(4) 0.0190(4) 0.0016(3) 0.0017(3) 0.0059(3) O3 0.0296(4) 0.0149(4) 0.0175(4) -0.0004(3) -0.0052(3) 0.0017(3) O4 0.0283(4) 0.0164(4) 0.0173(4) 0.0022(3) -0.0055(3) -0.0021(3) C1 0.0157(4) 0.0181(5) 0.0127(4) -0.0019(3) 0.0000(3) 0.0014(4) C2 0.0154(4) 0.0186(5) 0.0145(4) -0.0036(4) 0.0009(3) 0.0017(4) C3 0.0164(4) 0.0164(5) 0.0182(4) -0.0039(3) 0.0017(4) 0.0020(4) C4 0.0153(4) 0.0140(4) 0.0161(4) -0.0014(3) -0.0005(3) 0.0008(4) C5 0.0131(4) 0.0147(4) 0.0134(4) -0.0030(3) -0.0005(3) 0.0008(3) C6 0.0147(4) 0.0170(4) 0.0142(4) -0.0026(3) -0.0004(3) 0.0026(4) C7 0.0277(6) 0.0280(6) 0.0221(5) 0.0072(5) 0.0058(5) 0.0103(5) C8 0.0359(7) 0.0242(6) 0.0275(6) 0.0030(5) 0.0040(5) 0.0148(6) C9 0.0240(5) 0.0274(6) 0.0180(5) -0.0038(4) 0.0053(4) 0.0047(5) C10 0.0150(4) 0.0174(5) 0.0133(4) -0.0027(3) 0.0004(3) 0.0007(4) C11 0.0162(4) 0.0184(5) 0.0132(4) -0.0026(3) 0.0001(3) 0.0001(4) C12 0.0194(5) 0.0183(5) 0.0131(4) -0.0028(3) 0.0000(4) -0.0013(4) C13 0.0185(5) 0.0151(4) 0.0128(4) -0.0022(3) 0.0015(4) -0.0004(4) C14 0.0198(5) 0.0152(4) 0.0141(4) -0.0017(3) 0.0006(4) 0.0004(4) C15 0.0223(5) 0.0147(4) 0.0156(4) -0.0028(3) -0.0006(4) 0.0000(4) C16 0.0189(5) 0.0162(5) 0.0155(4) -0.0032(3) 0.0000(4) -0.0010(4) C17 0.0189(5) 0.0160(4) 0.0136(4) 0.0001(3) 0.0000(4) -0.0005(4) C18 0.0207(5) 0.0149(4) 0.0151(4) -0.0014(3) 0.0014(4) -0.0009(4) C19 0.0284(6) 0.0153(5) 0.0191(5) 0.0015(4) -0.0004(4) -0.0002(4) C20 0.0291(6) 0.0206(5) 0.0203(5) -0.0048(4) -0.0071(5) -0.0012(5) C21 0.0282(6) 0.0167(5) 0.0218(5) 0.0030(4) -0.0011(5) -0.0023(4) _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 O1 C1 1.3774(14) . ? O1 C7 1.423(2) . ? O2 C4 1.3768(14) . ? O2 C8 1.424(2) . ? O3 C14 1.3747(14) . ? O3 C19 1.428(2) . ? O4 C17 1.3729(14) . ? O4 C21 1.425(2) . ? C1 C2 1.395(2) . ? C1 C6 1.3981(14) . ? C2 C3 1.396(2) . ? C2 C9 1.510(2) . ? C3 C4 1.4000(15) . ? C3 H3 0.98(2) . ? C4 C5 1.4001(15) . ? C5 C6 1.395(2) . ? C5 C10 1.5059(15) . ? C6 H6 0.97(2) . ? C7 H7A 1.03(2) . ? C7 H7B 0.97(2) . ? C7 H7C 0.94(2) . ? C8 H8A 0.97(2) . ? C8 H8B 0.94(2) . ? C8 H8C 0.98(2) . ? C9 H9A 1.01(2) . ? C9 H9B 0.99(2) . ? C9 H9C 0.89(2) . ? C10 C11 1.534(2) . ? C10 H10A 0.95(2) . ? C10 H10B 1.06(2) . ? C11 C12 1.528(2) . ? C11 H11A 0.94(2) . ? C11 H11B 0.99(2) . ? C12 C13 1.511(2) . ? C12 H12A 0.96(2) . ? C12 H12B 1.00(2) . ? C13 C18 1.398(2) . ? C13 C14 1.402(2) . ? C14 C15 1.390(2) . ? C15 C16 1.398(2) . ? C15 H15 0.99(2) . ? C16 C17 1.401(2) . ? C16 C20 1.503(2) . ? C17 C18 1.393(2) . ? C18 H18 0.97(2) . ? C19 H19A 0.96(2) . ? C19 H19B 0.96(2) . ? C19 H19C 0.97(2) . ? C20 H20A 0.97(3) . ? C20 H20B 0.99(2) . ? C20 H20C 0.97(2) . ? C21 H21A 0.93(2) . ? C21 H21B 0.95(2) . ? C21 H21C 0.94(2) . ? 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 O1 C7 116.53(9) . . ? C4 O2 C8 117.62(9) . . ? C14 O3 C19 116.99(10) . . ? C17 O4 C21 117.34(10) . . ? O1 C1 C2 115.46(9) . . ? O1 C1 C6 123.94(10) . . ? C2 C1 C6 120.59(10) . . ? C1 C2 C3 118.66(9) . . ? C1 C2 C9 120.05(10) . . ? C3 C2 C9 121.29(10) . . ? C2 C3 C4 120.80(10) . . ? C2 C3 H3 117.9(10) . . ? C4 C3 H3 121.3(10) . . ? O2 C4 C3 124.08(10) . . ? O2 C4 C5 115.45(9) . . ? C3 C4 C5 120.47(10) . . ? C6 C5 C4 118.52(10) . . ? C6 C5 C10 120.59(10) . . ? C4 C5 C10 120.86(9) . . ? C5 C6 C1 120.94(10) . . ? C5 C6 H6 118.3(10) . . ? C1 C6 H6 120.7(10) . . ? O1 C7 H7A 106.8(13) . . ? O1 C7 H7B 111.2(13) . . ? H7A C7 H7B 108.8(17) . . ? O1 C7 H7C 111.3(12) . . ? H7A C7 H7C 108.9(17) . . ? H7B C7 H7C 109.7(17) . . ? O2 C8 H8A 106.4(14) . . ? O2 C8 H8B 110.6(14) . . ? H8A C8 H8B 112.3(19) . . ? O2 C8 H8C 108.0(11) . . ? H8A C8 H8C 105.5(17) . . ? H8B C8 H8C 113.7(17) . . ? C2 C9 H9A 112.4(11) . . ? C2 C9 H9B 107.4(13) . . ? H9A C9 H9B 112.1(17) . . ? C2 C9 H9C 114.0(13) . . ? H9A C9 H9C 100.0(18) . . ? H9B C9 H9C 111.0(18) . . ? C5 C10 C11 113.42(9) . . ? C5 C10 H10A 108.2(10) . . ? C11 C10 H10A 111.4(10) . . ? C5 C10 H10B 109.4(9) . . ? C11 C10 H10B 107.4(9) . . ? H10A C10 H10B 106.8(14) . . ? C12 C11 C10 110.05(9) . . ? C12 C11 H11A 110.5(10) . . ? C10 C11 H11A 108.5(10) . . ? C12 C11 H11B 111.4(10) . . ? C10 C11 H11B 108.8(10) . . ? H11A C11 H11B 107.5(15) . . ? C13 C12 C11 115.52(10) . . ? C13 C12 H12A 110.0(10) . . ? C11 C12 H12A 109.2(10) . . ? C13 C12 H12B 109.1(10) . . ? C11 C12 H12B 110.6(10) . . ? H12A C12 H12B 101.5(15) . . ? C18 C13 C14 118.44(10) . . ? C18 C13 C12 120.89(10) . . ? C14 C13 C12 120.64(10) . . ? O3 C14 C15 123.93(10) . . ? O3 C14 C13 115.87(9) . . ? C15 C14 C13 120.20(10) . . ? C14 C15 C16 121.34(10) . . ? C14 C15 H15 121.5(10) . . ? C16 C15 H15 117.1(11) . . ? C15 C16 C17 118.52(10) . . ? C15 C16 C20 121.25(10) . . ? C17 C16 C20 120.20(11) . . ? O4 C17 C18 124.59(10) . . ? O4 C17 C16 115.28(10) . . ? C18 C17 C16 120.11(10) . . ? C17 C18 C13 121.33(10) . . ? C17 C18 H18 121.5(9) . . ? C13 C18 H18 117.1(9) . . ? O3 C19 H19A 106.1(12) . . ? O3 C19 H19B 111.2(11) . . ? H19A C19 H19B 111.5(17) . . ? O3 C19 H19C 116.0(14) . . ? H19A C19 H19C 105.6(17) . . ? H19B C19 H19C 106.3(18) . . ? C16 C20 H20A 113.3(15) . . ? C16 C20 H20B 114.0(14) . . ? H20A C20 H20B 103.6(19) . . ? C16 C20 H20C 113.4(13) . . ? H20A C20 H20C 106.9(22) . . ? H20B C20 H20C 104.7(19) . . ? O4 C21 H21A 105.1(13) . . ? O4 C21 H21B 112.9(12) . . ? H21A C21 H21B 111.1(17) . . ? O4 C21 H21C 109.4(12) . . ? H21A C21 H21C 109.8(18) . . ? H21B C21 H21C 108.4(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 O1 C1 C2 -173.46(11) . . . . ? C7 O1 C1 C6 7.9(2) . . . . ? O1 C1 C2 C3 -179.58(11) . . . . ? C6 C1 C2 C3 -0.9(2) . . . . ? O1 C1 C2 C9 -0.2(2) . . . . ? C6 C1 C2 C9 178.47(11) . . . . ? C1 C2 C3 C4 -0.2(2) . . . . ? C9 C2 C3 C4 -179.59(11) . . . . ? C8 O2 C4 C3 -3.8(2) . . . . ? C8 O2 C4 C5 176.98(11) . . . . ? C2 C3 C4 O2 -177.70(11) . . . . ? C2 C3 C4 C5 1.4(2) . . . . ? O2 C4 C5 C6 177.68(10) . . . . ? C3 C4 C5 C6 -1.5(2) . . . . ? O2 C4 C5 C10 -0.29(15) . . . . ? C3 C4 C5 C10 -179.51(10) . . . . ? C4 C5 C6 C1 0.4(2) . . . . ? C10 C5 C6 C1 178.40(10) . . . . ? O1 C1 C6 C5 179.36(11) . . . . ? C2 C1 C6 C5 0.8(2) . . . . ? C6 C5 C10 C11 -100.67(12) . . . . ? C4 C5 C10 C11 77.27(13) . . . . ? C5 C10 C11 C12 -173.15(9) . . . . ? C10 C11 C12 C13 -177.81(10) . . . . ? C11 C12 C13 C18 -105.01(13) . . . . ? C11 C12 C13 C14 77.41(15) . . . . ? C19 O3 C14 C15 4.9(2) . . . . ? C19 O3 C14 C13 -175.84(11) . . . . ? C18 C13 C14 O3 178.36(10) . . . . ? C12 C13 C14 O3 -4.0(2) . . . . ? C18 C13 C14 C15 -2.4(2) . . . . ? C12 C13 C14 C15 175.26(11) . . . . ? O3 C14 C15 C16 179.73(12) . . . . ? C13 C14 C15 C16 0.5(2) . . . . ? C14 C15 C16 C17 1.8(2) . . . . ? C14 C15 C16 C20 -176.23(12) . . . . ? C21 O4 C17 C18 -5.8(2) . . . . ? C21 O4 C17 C16 172.50(12) . . . . ? C15 C16 C17 O4 179.38(11) . . . . ? C20 C16 C17 O4 -2.6(2) . . . . ? C15 C16 C17 C18 -2.2(2) . . . . ? C20 C16 C17 C18 175.81(11) . . . . ? O4 C17 C18 C13 178.60(11) . . . . ? C16 C17 C18 C13 0.4(2) . . . . ? C14 C13 C18 C17 1.9(2) . . . . ? C12 C13 C18 C17 -175.70(11) . . . . ? _refine_diff_density_max 0.401 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.047 data_pier-psy _database_code_CSD 162397 _audit_creation_method SHELXL _chemical_name_systematic ; 1,3-Bis(2',5'-dimethoxy-4'-methyl)propane dication-biradical bis(hexachloroantimonate) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H28 Cl12 O4 Sb2' _chemical_formula_weight 1013.33 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 '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' 'Sb' 'Sb' -0.5866 1.5461 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.073(2) _cell_length_b 26.577(5) _cell_length_c 8.445(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.99(3) _cell_angle_gamma 90.00 _cell_volume 1789.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 34 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method none _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.432 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.407 _exptl_absorpt_correction_T_max 0.668 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number 198 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 22003 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 36.04 _reflns_number_total 8082 _reflns_number_observed 5945 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS (Sheldrick, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 33 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+2.8898P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent carbon atom (1.5Uiso/eq for Me-hydrogens ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8049 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_obs 0.0472 _refine_ls_wR_factor_all 0.1081 _refine_ls_wR_factor_obs 0.0928 _refine_ls_goodness_of_fit_all 1.152 _refine_ls_goodness_of_fit_obs 1.258 _refine_ls_restrained_S_all 1.256 _refine_ls_restrained_S_obs 1.258 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sb1 Sb 0.52001(3) 0.2500 0.84127(3) 0.01835(7) Uani 1 d S . Cl1 Cl 0.2226(2) 0.2500 0.7991(2) 0.0467(4) Uani 1 d S . Cl2 Cl 0.52083(14) 0.16076(4) 0.84440(12) 0.0396(2) Uani 1 d . . Cl3 Cl 0.81597(13) 0.2500 0.87400(14) 0.0292(2) Uani 1 d S . Cl4 Cl 0.51756(15) 0.2500 0.55820(14) 0.0324(3) Uani 1 d S . Cl5 Cl 0.5311(2) 0.2500 1.12524(14) 0.0281(2) Uani 1 d S . Sb2 Sb 0.0000 0.0000 0.0000 0.01445(6) Uani 1 d S . Cl6 Cl -0.29386(9) -0.01368(3) -0.03617(10) 0.0285(2) Uani 1 d . . Cl7 Cl 0.00859(10) 0.00604(3) 0.28280(9) 0.02305(15) Uani 1 d . . Cl8 Cl 0.04850(12) -0.08797(3) 0.02390(10) 0.0294(2) Uani 1 d . . O1 O 0.5402(3) 0.08332(8) -0.6326(3) 0.0240(4) Uani 1 d . . O2 O -0.0577(3) 0.16069(9) -0.5404(3) 0.0232(4) Uani 1 d . . C1 C 0.0892(4) 0.14078(11) -0.5563(3) 0.0178(5) Uani 1 d . . C2 C 0.1773(4) 0.10622(11) -0.4483(4) 0.0200(5) Uani 1 d . . H2A H 0.1321(4) 0.09625(11) -0.3558(4) 0.024 Uiso 1 calc R . C3 C 0.3274(4) 0.08682(11) -0.4752(4) 0.0207(5) Uani 1 d . . C4 C 0.3929(4) 0.10336(10) -0.6165(4) 0.0180(5) Uani 1 d . . C5 C 0.3063(4) 0.13837(10) -0.7242(3) 0.0177(5) Uani 1 d . . H5A H 0.3514(4) 0.14828(10) -0.8167(3) 0.021 Uiso 1 calc R . C6 C 0.1565(4) 0.15825(10) -0.6956(3) 0.0167(5) Uani 1 d . . C7 C 0.0725(4) 0.20099(10) -0.7949(3) 0.0179(5) Uani 1 d . . H7A H -0.0509(4) 0.19725(10) -0.8089(3) 0.022 Uiso 1 calc R . H7B H 0.1075(4) 0.20132(10) -0.9021(3) 0.022 Uiso 1 calc R . C8 C 0.1269(6) 0.2500 -0.7042(5) 0.0208(8) Uani 1 d S . H8A H 0.0807(6) 0.2500 -0.6023(5) 0.025 Uiso 1 calc SR . H8B H 0.2507(6) 0.2500 -0.6767(5) 0.025 Uiso 1 calc SR . C16 C 0.6211(4) 0.09791(13) -0.7682(4) 0.0268(6) Uani 1 d . . H16A H 0.7261(17) 0.0792(8) -0.7647(18) 0.040 Uiso 1 calc R . H16B H 0.6451(31) 0.1341(2) -0.7627(18) 0.040 Uiso 1 calc R . H16C H 0.5464(14) 0.0903(9) -0.8684(4) 0.040 Uiso 1 calc R . C17 C 0.4233(5) 0.04943(12) -0.3628(4) 0.0282(7) Uani 1 d . . H17A H 0.3811(24) 0.0500(7) -0.2601(12) 0.042 Uiso 1 calc R . H17B H 0.5427(7) 0.0583(6) -0.3453(26) 0.042 Uiso 1 calc R . H17C H 0.4089(28) 0.0157(2) -0.4095(15) 0.042 Uiso 1 calc R . C18 C -0.1355(5) 0.14697(14) -0.4021(4) 0.0308(7) Uani 1 d . . H18A H -0.2448(16) 0.1636(9) -0.4095(18) 0.046 Uiso 1 calc R . H18B H -0.0633(18) 0.1577(10) -0.3037(5) 0.046 Uiso 1 calc R . H18C H -0.1509(33) 0.1104(2) -0.4001(20) 0.046 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 Sb1 0.01547(12) 0.02518(14) 0.01377(13) 0.000 0.00036(9) 0.000 Cl1 0.0170(5) 0.0860(12) 0.0380(7) 0.000 0.0067(5) 0.000 Cl2 0.0618(6) 0.0247(4) 0.0324(5) -0.0067(3) 0.0082(4) -0.0090(4) Cl3 0.0165(4) 0.0491(7) 0.0195(5) 0.000 -0.0049(4) 0.000 Cl4 0.0251(5) 0.0555(8) 0.0136(5) 0.000 -0.0061(4) 0.000 Cl5 0.0393(6) 0.0309(6) 0.0163(5) 0.000 0.0115(4) 0.000 Sb2 0.01520(11) 0.01590(11) 0.01206(11) -0.00017(9) 0.00151(8) -0.00108(9) Cl6 0.0167(3) 0.0434(5) 0.0250(4) -0.0038(3) 0.0020(3) -0.0053(3) Cl7 0.0288(4) 0.0267(4) 0.0137(3) -0.0009(3) 0.0033(3) -0.0028(3) Cl8 0.0467(5) 0.0165(3) 0.0231(4) 0.0004(3) -0.0005(3) 0.0032(3) O1 0.0256(11) 0.0211(10) 0.0259(11) 0.0016(9) 0.0064(9) 0.0060(8) O2 0.0250(11) 0.0254(11) 0.0200(10) 0.0012(9) 0.0060(9) 0.0031(8) C1 0.0211(13) 0.0161(12) 0.0159(12) -0.0010(10) 0.0018(10) -0.0016(9) C2 0.0298(15) 0.0141(12) 0.0160(12) 0.0013(10) 0.0036(11) 0.0000(10) C3 0.0300(15) 0.0133(12) 0.0185(13) 0.0006(10) 0.0025(11) -0.0002(10) C4 0.0220(13) 0.0114(11) 0.0199(13) -0.0021(10) 0.0014(10) 0.0000(9) C5 0.0236(13) 0.0154(12) 0.0138(12) 0.0003(9) 0.0018(10) -0.0007(10) C6 0.0225(13) 0.0126(11) 0.0141(11) -0.0013(9) -0.0005(10) -0.0011(9) C7 0.0221(13) 0.0152(12) 0.0152(12) -0.0006(9) -0.0014(10) -0.0009(9) C8 0.026(2) 0.017(2) 0.017(2) 0.000 -0.005(2) 0.000 C16 0.026(2) 0.029(2) 0.026(2) -0.0019(13) 0.0081(13) 0.0030(12) C17 0.039(2) 0.0214(15) 0.024(2) 0.0073(12) 0.0050(14) 0.0074(12) C18 0.033(2) 0.037(2) 0.025(2) 0.0021(14) 0.0118(14) 0.0027(14) _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 Sb1 Cl3 2.3618(12) . ? Sb1 Cl1 2.3718(14) . ? Sb1 Cl2 2.3718(10) 4_565 ? Sb1 Cl2 2.3719(10) . ? Sb1 Cl5 2.3857(13) . ? Sb1 Cl4 2.3875(13) . ? Sb2 Cl6 2.3721(9) . ? Sb2 Cl6 2.3721(9) 3 ? Sb2 Cl8 2.3738(9) 3 ? Sb2 Cl8 2.3740(9) . ? Sb2 Cl7 2.3837(9) 3 ? Sb2 Cl7 2.3838(9) . ? O1 C4 1.329(4) . ? O1 C16 1.457(4) . ? O2 C1 1.324(4) . ? O2 C18 1.457(4) . ? C1 C2 1.407(4) . ? C1 C6 1.447(4) . ? C2 C3 1.369(4) . ? C3 C4 1.447(4) . ? C3 C17 1.503(4) . ? C4 C5 1.408(4) . ? C5 C6 1.375(4) . ? C6 C7 1.508(4) . ? C7 C8 1.540(3) . ? C8 C7 1.540(4) 4_565 ? 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 Cl3 Sb1 Cl1 178.11(5) . . ? Cl3 Sb1 Cl2 89.87(3) . 4_565 ? Cl1 Sb1 Cl2 90.15(3) . 4_565 ? Cl3 Sb1 Cl2 89.87(3) . . ? Cl1 Sb1 Cl2 90.15(3) . . ? Cl2 Sb1 Cl2 178.73(5) 4_565 . ? Cl3 Sb1 Cl5 90.24(5) . . ? Cl1 Sb1 Cl5 91.65(6) . . ? Cl2 Sb1 Cl5 89.38(2) 4_565 . ? Cl2 Sb1 Cl5 89.38(2) . . ? Cl3 Sb1 Cl4 88.11(5) . . ? Cl1 Sb1 Cl4 90.00(6) . . ? Cl2 Sb1 Cl4 90.62(2) 4_565 . ? Cl2 Sb1 Cl4 90.61(2) . . ? Cl5 Sb1 Cl4 178.35(5) . . ? Cl6 Sb2 Cl6 180.0 . 3 ? Cl6 Sb2 Cl8 89.52(3) . 3 ? Cl6 Sb2 Cl8 90.48(3) 3 3 ? Cl6 Sb2 Cl8 90.48(3) . . ? Cl6 Sb2 Cl8 89.52(3) 3 . ? Cl8 Sb2 Cl8 180.0 3 . ? Cl6 Sb2 Cl7 89.36(4) . 3 ? Cl6 Sb2 Cl7 90.64(4) 3 3 ? Cl8 Sb2 Cl7 90.15(3) 3 3 ? Cl8 Sb2 Cl7 89.85(3) . 3 ? Cl6 Sb2 Cl7 90.64(4) . . ? Cl6 Sb2 Cl7 89.36(4) 3 . ? Cl8 Sb2 Cl7 89.85(3) 3 . ? Cl8 Sb2 Cl7 90.15(3) . . ? Cl7 Sb2 Cl7 180.0 3 . ? C4 O1 C16 119.5(2) . . ? C1 O2 C18 119.2(3) . . ? O2 C1 C2 124.4(3) . . ? O2 C1 C6 114.2(3) . . ? C2 C1 C6 121.4(3) . . ? C3 C2 C1 120.6(3) . . ? C2 C3 C4 118.0(3) . . ? C2 C3 C17 121.8(3) . . ? C4 C3 C17 120.2(3) . . ? O1 C4 C5 124.1(3) . . ? O1 C4 C3 114.2(3) . . ? C5 C4 C3 121.7(3) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 C1 118.1(3) . . ? C5 C6 C7 121.5(3) . . ? C1 C6 C7 120.0(3) . . ? C6 C7 C8 107.0(2) . . ? C7 C8 C7 115.5(3) 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 O2 C1 C2 0.6(4) . . . . ? C18 O2 C1 C6 -178.3(3) . . . . ? O2 C1 C2 C3 179.0(3) . . . . ? C6 C1 C2 C3 -2.2(4) . . . . ? C1 C2 C3 C4 0.7(4) . . . . ? C1 C2 C3 C17 -179.3(3) . . . . ? C16 O1 C4 C5 0.4(4) . . . . ? C16 O1 C4 C3 -178.6(3) . . . . ? C2 C3 C4 O1 179.1(3) . . . . ? C17 C3 C4 O1 -0.9(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C17 C3 C4 C5 -179.9(3) . . . . ? O1 C4 C5 C6 -178.2(3) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C4 C5 C6 C1 -2.2(4) . . . . ? C4 C5 C6 C7 171.3(3) . . . . ? O2 C1 C6 C5 -178.1(3) . . . . ? C2 C1 C6 C5 2.9(4) . . . . ? O2 C1 C6 C7 8.3(4) . . . . ? C2 C1 C6 C7 -170.7(3) . . . . ? C5 C6 C7 C8 -94.9(3) . . . . ? C1 C6 C7 C8 78.5(3) . . . . ? C6 C7 C8 C7 172.8(3) . . . 4_565 ? _refine_diff_density_max 1.372 _refine_diff_density_min -2.193 _refine_diff_density_rms 0.160 data_raj-usx _database_code_CSD 162398 _audit_creation_method SHELXL _chemical_name_systematic ; 2,2',5,5'-tetramethoxy-4,4'-dimethylbiphenyl ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H22 O4' _chemical_formula_weight 302.36 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.1995(12) _cell_length_b 5.8270(3) _cell_length_c 12.6965(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.848(2) _cell_angle_gamma 90.00 _cell_volume 1544.81(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3151 _cell_measurement_theta_min 2 _cell_measurement_theta_max 36 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method none _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10207 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 36.07 _reflns_number_total 3439 _reflns_number_observed 1847 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 13 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.7019P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3426 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_obs 0.0584 _refine_ls_wR_factor_all 0.1851 _refine_ls_wR_factor_obs 0.1374 _refine_ls_goodness_of_fit_all 0.982 _refine_ls_goodness_of_fit_obs 1.040 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.040 _refine_ls_shift/esd_max 0.009 _refine_ls_shift/esd_mean 0.001 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 O2 O 0.02347(4) 0.0820(2) 0.14679(8) 0.0252(2) Uani 1 d . . O5 O 0.18021(4) -0.5821(2) 0.41563(8) 0.0292(2) Uani 1 d . . C1 C 0.03519(5) -0.2460(2) 0.26131(10) 0.0176(2) Uani 1 d . . C2 C 0.06372(5) -0.0769(2) 0.21525(10) 0.0196(2) Uani 1 d . . C3 C 0.12997(5) -0.0772(2) 0.24006(11) 0.0236(3) Uani 1 d . . H3A H 0.14898(5) 0.0389(2) 0.20909(11) 0.028 Uiso 1 calc R . C4 C 0.16891(5) -0.2435(2) 0.30916(11) 0.0233(3) Uani 1 d . . C5 C 0.14004(5) -0.4163(2) 0.35131(10) 0.0211(2) Uani 1 d . . C6 C 0.07374(5) -0.4167(2) 0.32762(10) 0.0202(2) Uani 1 d . . H6A H 0.05472(5) -0.5351(2) 0.35716(10) 0.024 Uiso 1 calc R . C7 C 0.04984(7) 0.2250(2) 0.08223(12) 0.0284(3) Uani 1 d . . H7A H 0.01527(9) 0.3087(14) 0.0264(6) 0.043 Uiso 1 calc R . H7B H 0.0726(4) 0.1299(3) 0.0442(7) 0.043 Uiso 1 calc R . H7C H 0.0798(4) 0.3346(12) 0.1317(2) 0.043 Uiso 1 calc R . C8 C 0.24075(6) -0.2320(3) 0.33956(14) 0.0341(3) Uani 1 d . . H8A H 0.25186(12) -0.2390(75) 0.2712(3) 0.051 Uiso 0.50 calc PR . H8B H 0.26044(14) -0.3617(41) 0.3882(30) 0.051 Uiso 0.50 calc PR . H8C H 0.2566(2) -0.0878(34) 0.3790(32) 0.051 Uiso 0.50 calc PR . H8D H 0.26074(12) -0.2200(75) 0.4210(3) 0.051 Uiso 0.50 calc PR . H8E H 0.25216(14) -0.0973(42) 0.3041(30) 0.051 Uiso 0.50 calc PR . H8F H 0.2560(2) -0.3712(34) 0.3133(32) 0.051 Uiso 0.50 calc PR . C9 C 0.15450(7) -0.7334(3) 0.47762(12) 0.0312(3) Uani 1 d . . H9A H 0.18837(14) -0.8353(13) 0.5235(7) 0.047 Uiso 1 calc R . H9B H 0.1201(4) -0.8252(14) 0.42578(12) 0.047 Uiso 1 calc R . H9C H 0.1373(5) -0.6437(3) 0.5262(7) 0.047 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 O2 0.0182(4) 0.0237(5) 0.0351(5) 0.0084(4) 0.0109(4) 0.0027(3) O5 0.0161(4) 0.0268(5) 0.0415(6) 0.0073(4) 0.0056(4) 0.0057(4) C1 0.0119(4) 0.0179(5) 0.0232(5) -0.0018(4) 0.0061(4) -0.0008(4) C2 0.0141(5) 0.0191(5) 0.0255(6) 0.0002(4) 0.0068(4) 0.0004(4) C3 0.0145(5) 0.0249(6) 0.0332(7) 0.0013(5) 0.0102(4) -0.0023(5) C4 0.0116(5) 0.0261(6) 0.0313(6) -0.0027(5) 0.0060(4) -0.0006(5) C5 0.0135(5) 0.0207(6) 0.0271(6) -0.0007(5) 0.0044(4) 0.0028(4) C6 0.0142(5) 0.0194(6) 0.0268(6) 0.0006(4) 0.0065(4) 0.0002(4) C7 0.0291(6) 0.0241(7) 0.0351(7) 0.0069(6) 0.0151(5) 0.0007(5) C8 0.0127(5) 0.0397(8) 0.0486(8) -0.0002(7) 0.0088(5) -0.0007(6) C9 0.0268(7) 0.0274(7) 0.0362(7) 0.0079(6) 0.0065(5) 0.0063(6) _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 O2 C2 1.3725(15) . ? O2 C7 1.426(2) . ? O5 C5 1.3789(15) . ? O5 C9 1.424(2) . ? C1 C6 1.393(2) . ? C1 C2 1.402(2) . ? C1 C1 1.490(2) 2 ? C2 C3 1.396(2) . ? C3 C4 1.393(2) . ? C4 C5 1.394(2) . ? C4 C8 1.510(2) . ? C5 C6 1.399(2) . ? 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 C2 O2 C7 116.88(10) . . ? C5 O5 C9 117.46(10) . . ? C6 C1 C2 118.82(10) . . ? C6 C1 C1 120.35(9) . 2 ? C2 C1 C1 120.82(9) . 2 ? O2 C2 C3 123.58(11) . . ? O2 C2 C1 116.69(10) . . ? C3 C2 C1 119.73(11) . . ? C4 C3 C2 121.58(12) . . ? C3 C4 C5 118.45(10) . . ? C3 C4 C8 120.39(12) . . ? C5 C4 C8 121.14(12) . . ? O5 C5 C4 116.39(10) . . ? O5 C5 C6 123.22(11) . . ? C4 C5 C6 120.39(11) . . ? C1 C6 C5 120.95(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 O2 C2 C3 12.2(2) . . . . ? C7 O2 C2 C1 -167.77(11) . . . . ? C6 C1 C2 O2 177.38(11) . . . . ? C1 C1 C2 O2 -1.7(2) 2 . . . ? C6 C1 C2 C3 -2.6(2) . . . . ? C1 C1 C2 C3 178.33(12) 2 . . . ? O2 C2 C3 C4 -179.33(12) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? C2 C3 C4 C5 1.8(2) . . . . ? C2 C3 C4 C8 -176.68(12) . . . . ? C9 O5 C5 C4 167.85(12) . . . . ? C9 O5 C5 C6 -12.4(2) . . . . ? C3 C4 C5 O5 177.51(12) . . . . ? C8 C4 C5 O5 -4.0(2) . . . . ? C3 C4 C5 C6 -2.2(2) . . . . ? C8 C4 C5 C6 176.24(13) . . . . ? C2 C1 C6 C5 2.1(2) . . . . ? C1 C1 C6 C5 -178.75(12) 2 . . . ? O5 C5 C6 C1 -179.44(11) . . . . ? C4 C5 C6 C1 0.3(2) . . . . ? _refine_diff_density_max 0.391 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.065 data_raj-ssy _database_code_CSD 162399 _audit_creation_method SHELXL _chemical_name_systematic ; 2,2',5,5'-tetramethoxy-4,4'-dimethylbiphenyl hexachloroantimonate ; _chemical_name_common ? _chemical_formula_moiety '(C18 H22 O4)^+^, (Cl6 Sb)^-^' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H22 Cl6 O4 Sb' _chemical_formula_weight 636.81 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 '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' 'Sb' 'Sb' -0.5866 1.5461 '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 7.6596(2) _cell_length_b 12.8575(3) _cell_length_c 13.7700(3) _cell_angle_alpha 62.3690(10) _cell_angle_beta 83.1900(10) _cell_angle_gamma 83.5670(10) _cell_volume 1190.47(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7842 _cell_measurement_theta_min 2 _cell_measurement_theta_max 36 _exptl_crystal_description 'prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method none _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 1.855 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 0.862 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17125 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 36.10 _reflns_number_total 10303 _reflns_number_observed 7229 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 13 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.1818P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10290 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.0872 _refine_ls_wR_factor_obs 0.0696 _refine_ls_goodness_of_fit_all 1.076 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_restrained_S_all 1.127 _refine_ls_restrained_S_obs 1.076 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sb1 Sb 0.5000 0.0000 0.5000 0.01236(5) Uani 1 d S . Sb2 Sb 0.0000 0.5000 0.0000 0.01645(6) Uani 1 d S . Cl1 Cl 0.20882(8) 0.00183(6) 0.45882(6) 0.02283(14) Uani 1 d . . Cl2 Cl 0.54885(11) 0.16690(6) 0.32852(6) 0.0299(2) Uani 1 d . . Cl3 Cl 0.40068(9) 0.12546(7) 0.58166(6) 0.0259(2) Uani 1 d . . Cl4 Cl 0.24731(10) 0.37352(6) 0.08382(6) 0.0283(2) Uani 1 d . . Cl5 Cl 0.00430(11) 0.41795(6) -0.12338(6) 0.0287(2) Uani 1 d . . Cl6 Cl -0.18954(10) 0.35663(6) 0.12654(6) 0.0277(2) Uani 1 d . . O12 O -0.0992(2) 0.0574(2) -0.2543(2) 0.0192(4) Uani 1 d . . O15 O -0.7794(2) 0.0348(2) -0.0750(2) 0.0179(4) Uani 1 d . . O22 O -0.4383(3) 0.3749(2) -0.2289(2) 0.0209(4) Uani 1 d . . O25 O -0.0818(3) 0.3939(2) -0.6058(2) 0.0213(4) Uani 1 d . . C11 C -0.3697(3) 0.1597(2) -0.2403(2) 0.0141(5) Uani 1 d . . C12 C -0.2679(3) 0.0497(2) -0.2137(2) 0.0146(5) Uani 1 d . . C13 C -0.3436(3) -0.0576(2) -0.1467(2) 0.0163(5) Uani 1 d . . H13A H -0.2756(3) -0.1290(2) -0.1324(2) 0.020 Uiso 1 calc R . C14 C -0.5143(3) -0.0619(2) -0.1009(2) 0.0152(5) Uani 1 d . . C15 C -0.6119(3) 0.0471(2) -0.1214(2) 0.0148(5) Uani 1 d . . C16 C -0.5401(3) 0.1535(2) -0.1875(2) 0.0148(5) Uani 1 d . . H16A H -0.6071(3) 0.2242(2) -0.1978(2) 0.018 Uiso 1 calc R . C17 C 0.0092(4) -0.0509(2) -0.2294(2) 0.0233(6) Uani 1 d . . H17A H 0.1285(8) -0.0321(2) -0.2641(15) 0.035 Uiso 1 calc R . H17B H -0.0420(16) -0.0970(9) -0.2577(16) 0.035 Uiso 1 calc R . H17C H 0.0143(24) -0.0967(9) -0.1496(3) 0.035 Uiso 1 calc R . C18 C -0.5990(4) -0.1757(2) -0.0342(2) 0.0194(5) Uani 1 d . . H18A H -0.5094(5) -0.2411(2) -0.0178(13) 0.029 Uiso 1 calc R . H18B H -0.6886(18) -0.1825(8) -0.0758(7) 0.029 Uiso 1 calc R . H18C H -0.6544(22) -0.1781(7) 0.0346(7) 0.029 Uiso 1 calc R . C19 C -0.8885(4) 0.1410(2) -0.0963(2) 0.0227(6) Uani 1 d . . H19A H -1.0046(10) 0.1206(2) -0.0568(14) 0.034 Uiso 1 calc R . H19B H -0.9021(24) 0.1861(10) -0.1754(3) 0.034 Uiso 1 calc R . H19C H -0.8331(14) 0.1885(9) -0.0713(16) 0.034 Uiso 1 calc R . C21 C -0.3093(3) 0.2715(2) -0.3265(2) 0.0149(5) Uani 1 d . . C22 C -0.3573(3) 0.3817(2) -0.3236(2) 0.0164(5) Uani 1 d . . C23 C -0.3182(3) 0.4883(2) -0.4157(2) 0.0173(5) Uani 1 d . . H23A H -0.3536(3) 0.5603(2) -0.4132(2) 0.021 Uiso 1 calc R . C24 C -0.2293(3) 0.4908(2) -0.5098(2) 0.0172(5) Uani 1 d . . C25 C -0.1725(3) 0.3819(2) -0.5108(2) 0.0154(5) Uani 1 d . . C26 C -0.2116(3) 0.2756(2) -0.4216(2) 0.0167(5) Uani 1 d . . H26A H -0.1721(3) 0.2042(2) -0.4244(2) 0.020 Uiso 1 calc R . C27 C -0.4810(4) 0.4825(3) -0.2188(3) 0.0266(6) Uani 1 d . . H27A H -0.5339(27) 0.4633(3) -0.1445(6) 0.040 Uiso 1 calc R . H27B H -0.5647(23) 0.5335(9) -0.2728(13) 0.040 Uiso 1 calc R . H27C H -0.3733(6) 0.5233(10) -0.2322(18) 0.040 Uiso 1 calc R . C28 C -0.1931(4) 0.6041(2) -0.6108(2) 0.0224(6) Uani 1 d . . H28A H -0.2437(24) 0.6704(2) -0.5978(6) 0.034 Uiso 1 calc R . H28B H -0.2465(23) 0.6060(8) -0.6729(4) 0.034 Uiso 1 calc R . H28C H -0.0656(4) 0.6099(9) -0.6276(10) 0.034 Uiso 1 calc R . C29 C -0.0054(4) 0.2887(2) -0.6111(2) 0.0251(6) Uani 1 d . . H29A H 0.0684(23) 0.3104(2) -0.6800(8) 0.038 Uiso 1 calc R . H29B H -0.0996(4) 0.2414(9) -0.6081(18) 0.038 Uiso 1 calc R . H29C H 0.0669(23) 0.2430(10) -0.5487(10) 0.038 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 Sb1 0.01013(11) 0.01375(11) 0.01428(12) -0.00736(9) 0.00076(8) -0.00238(8) Sb2 0.02004(13) 0.01057(11) 0.01780(13) -0.00713(10) 0.00519(10) -0.00130(9) Cl1 0.0123(3) 0.0267(3) 0.0357(4) -0.0190(3) -0.0047(3) -0.0008(2) Cl2 0.0318(4) 0.0244(3) 0.0216(3) -0.0004(3) 0.0028(3) -0.0073(3) Cl3 0.0209(3) 0.0328(4) 0.0366(4) -0.0273(3) -0.0033(3) 0.0027(3) Cl4 0.0273(4) 0.0214(3) 0.0343(4) -0.0128(3) -0.0027(3) 0.0060(3) Cl5 0.0423(4) 0.0219(3) 0.0264(4) -0.0161(3) 0.0009(3) 0.0006(3) Cl6 0.0305(4) 0.0185(3) 0.0294(4) -0.0086(3) 0.0116(3) -0.0086(3) O12 0.0160(9) 0.0190(9) 0.0213(10) -0.0088(8) -0.0007(7) 0.0014(7) O15 0.0158(9) 0.0133(8) 0.0216(10) -0.0061(7) 0.0022(7) -0.0022(7) O22 0.0266(11) 0.0162(9) 0.0212(10) -0.0105(8) 0.0034(8) -0.0027(8) O25 0.0271(11) 0.0159(9) 0.0176(9) -0.0061(8) 0.0046(8) -0.0026(8) C11 0.0152(11) 0.0140(11) 0.0152(11) -0.0085(9) -0.0020(9) -0.0002(9) C12 0.0152(11) 0.0154(11) 0.0143(11) -0.0079(9) -0.0016(9) -0.0004(9) C13 0.0178(12) 0.0128(11) 0.0175(12) -0.0064(10) -0.0024(10) 0.0012(9) C14 0.0171(12) 0.0142(11) 0.0157(12) -0.0073(10) -0.0040(9) -0.0006(9) C15 0.0148(11) 0.0163(11) 0.0150(11) -0.0086(10) -0.0012(9) -0.0005(9) C16 0.0179(12) 0.0129(11) 0.0141(11) -0.0069(9) -0.0003(9) -0.0005(9) C17 0.0174(13) 0.0242(14) 0.0250(14) -0.0100(12) -0.0020(11) 0.0068(11) C18 0.0199(13) 0.0130(11) 0.0226(14) -0.0060(10) -0.0009(10) -0.0014(9) C19 0.0182(13) 0.0177(12) 0.0255(15) -0.0066(11) 0.0058(11) 0.0011(10) C21 0.0135(11) 0.0153(11) 0.0149(11) -0.0063(9) -0.0007(9) -0.0006(9) C22 0.0148(11) 0.0190(12) 0.0187(12) -0.0109(10) -0.0016(9) -0.0019(9) C23 0.0167(12) 0.0132(11) 0.0223(13) -0.0082(10) -0.0031(10) -0.0004(9) C24 0.0157(12) 0.0146(11) 0.0187(13) -0.0044(10) -0.0053(10) -0.0018(9) C25 0.0152(11) 0.0152(11) 0.0164(12) -0.0074(10) -0.0012(9) -0.0020(9) C26 0.0187(12) 0.0142(11) 0.0184(12) -0.0084(10) -0.0019(10) -0.0005(9) C27 0.037(2) 0.0200(13) 0.028(2) -0.0171(12) 0.0043(13) -0.0010(12) C28 0.0234(14) 0.0170(12) 0.0223(14) -0.0053(11) -0.0017(11) -0.0017(10) C29 0.033(2) 0.0203(13) 0.0223(14) -0.0113(12) 0.0042(12) -0.0018(12) _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 Sb1 Cl1 2.3605(7) . ? Sb1 Cl1 2.3606(7) 2_656 ? Sb1 Cl2 2.3646(7) . ? Sb1 Cl2 2.3646(7) 2_656 ? Sb1 Cl3 2.3769(6) . ? Sb1 Cl3 2.3770(6) 2_656 ? Sb2 Cl6 2.3585(7) . ? Sb2 Cl6 2.3585(7) 2_565 ? Sb2 Cl5 2.3753(7) 2_565 ? Sb2 Cl5 2.3753(7) . ? Sb2 Cl4 2.3774(7) 2_565 ? Sb2 Cl4 2.3774(7) . ? O12 C12 1.341(3) . ? O12 C17 1.453(3) . ? O15 C15 1.356(3) . ? O15 C19 1.442(3) . ? O22 C22 1.344(3) . ? O22 C27 1.452(3) . ? O25 C25 1.356(3) . ? O25 C29 1.442(3) . ? C11 C16 1.408(4) . ? C11 C12 1.444(3) . ? C11 C21 1.458(4) . ? C12 C13 1.400(4) . ? C13 C14 1.378(4) . ? C14 C15 1.432(3) . ? C14 C18 1.493(4) . ? C15 C16 1.377(4) . ? C21 C26 1.410(4) . ? C21 C22 1.442(3) . ? C22 C23 1.402(4) . ? C23 C24 1.379(4) . ? C24 C25 1.425(3) . ? C24 C28 1.501(4) . ? C25 C26 1.383(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 Cl1 Sb1 Cl1 180.0 . 2_656 ? Cl1 Sb1 Cl2 89.70(3) . . ? Cl1 Sb1 Cl2 90.30(3) 2_656 . ? Cl1 Sb1 Cl2 90.30(3) . 2_656 ? Cl1 Sb1 Cl2 89.70(3) 2_656 2_656 ? Cl2 Sb1 Cl2 180.0 . 2_656 ? Cl1 Sb1 Cl3 89.65(2) . . ? Cl1 Sb1 Cl3 90.35(2) 2_656 . ? Cl2 Sb1 Cl3 89.78(3) . . ? Cl2 Sb1 Cl3 90.22(3) 2_656 . ? Cl1 Sb1 Cl3 90.35(2) . 2_656 ? Cl1 Sb1 Cl3 89.65(2) 2_656 2_656 ? Cl2 Sb1 Cl3 90.22(3) . 2_656 ? Cl2 Sb1 Cl3 89.78(3) 2_656 2_656 ? Cl3 Sb1 Cl3 180.0 . 2_656 ? Cl6 Sb2 Cl6 180.0 . 2_565 ? Cl6 Sb2 Cl5 90.01(3) . 2_565 ? Cl6 Sb2 Cl5 89.99(3) 2_565 2_565 ? Cl6 Sb2 Cl5 89.99(3) . . ? Cl6 Sb2 Cl5 90.01(3) 2_565 . ? Cl5 Sb2 Cl5 180.0 2_565 . ? Cl6 Sb2 Cl4 90.24(3) . 2_565 ? Cl6 Sb2 Cl4 89.76(3) 2_565 2_565 ? Cl5 Sb2 Cl4 90.74(3) 2_565 2_565 ? Cl5 Sb2 Cl4 89.26(3) . 2_565 ? Cl6 Sb2 Cl4 89.76(3) . . ? Cl6 Sb2 Cl4 90.24(3) 2_565 . ? Cl5 Sb2 Cl4 89.26(3) 2_565 . ? Cl5 Sb2 Cl4 90.74(3) . . ? Cl4 Sb2 Cl4 179.999(1) 2_565 . ? C12 O12 C17 118.4(2) . . ? C15 O15 C19 117.3(2) . . ? C22 O22 C27 118.8(2) . . ? C25 O25 C29 117.9(2) . . ? C16 C11 C12 116.9(2) . . ? C16 C11 C21 120.6(2) . . ? C12 C11 C21 122.2(2) . . ? O12 C12 C13 123.2(2) . . ? O12 C12 C11 116.2(2) . . ? C13 C12 C11 120.6(2) . . ? C14 C13 C12 121.5(2) . . ? C13 C14 C15 118.0(2) . . ? C13 C14 C18 121.8(2) . . ? C15 C14 C18 120.2(2) . . ? O15 C15 C16 124.5(2) . . ? O15 C15 C14 114.1(2) . . ? C16 C15 C14 121.4(2) . . ? C15 C16 C11 121.4(2) . . ? C26 C21 C22 117.4(2) . . ? C26 C21 C11 119.8(2) . . ? C22 C21 C11 122.6(2) . . ? O22 C22 C23 123.4(2) . . ? O22 C22 C21 116.2(2) . . ? C23 C22 C21 120.4(2) . . ? C24 C23 C22 121.3(2) . . ? C23 C24 C25 118.5(2) . . ? C23 C24 C28 122.0(2) . . ? C25 C24 C28 119.5(2) . . ? O25 C25 C26 124.9(2) . . ? O25 C25 C24 113.9(2) . . ? C26 C25 C24 121.2(2) . . ? C25 C26 C21 121.0(2) . . ? _refine_diff_density_max 0.820 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.154 data_raj-tsx _database_code_CSD 162400 _audit_creation_method SHELXL _chemical_name_systematic ; 2,2",5,5"-tetramethoxy-4,4"-dimethylterphenyl ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H26 O4' _chemical_formula_weight 378.45 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 '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 5.0760(3) _cell_length_b 13.9623(9) _cell_length_c 14.3411(9) _cell_angle_alpha 77.796(2) _cell_angle_beta 88.587(2) _cell_angle_gamma 88.641(2) _cell_volume 992.94(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2359 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method none _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.928 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10726 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.1480 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.68 _reflns_number_total 5993 _reflns_number_observed 2535 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 20 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1437P)^2^+0.0000P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5973 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2170 _refine_ls_R_factor_obs 0.0986 _refine_ls_wR_factor_all 0.3313 _refine_ls_wR_factor_obs 0.2325 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_goodness_of_fit_obs 1.200 _refine_ls_restrained_S_all 1.115 _refine_ls_restrained_S_obs 1.200 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.001 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 O12 O 0.1565(5) -0.0705(2) 0.7452(2) 0.0311(6) Uani 1 d . . O15 O 0.8435(5) -0.3873(2) 0.7642(2) 0.0350(7) Uani 1 d . . C1 C 0.4958(6) -0.0721(2) 0.5853(2) 0.0189(7) Uani 1 d . . C2A C 0.7342(12) -0.0337(5) 0.5450(5) 0.0220(14) Uani 0.50 d P 1 H2AA H 0.8955(12) -0.0569(5) 0.5746(5) 0.026 Uiso 0.50 calc PR 1 C3A C 0.7361(12) 0.0388(5) 0.4612(4) 0.0208(13) Uani 0.50 d P 1 H3AA H 0.8991(12) 0.0658(5) 0.4356(4) 0.025 Uiso 0.50 calc PR 1 C2B C 0.5014(12) -0.0989(5) 0.4984(4) 0.0207(13) Uani 0.50 d P 2 H2BA H 0.5029(12) -0.1664(5) 0.4960(4) 0.025 Uiso 0.50 calc PR 2 C3B C 0.5048(11) -0.0284(5) 0.4138(4) 0.0177(12) Uani 0.50 d P 2 H3BA H 0.5076(11) -0.0485(5) 0.3545(4) 0.021 Uiso 0.50 calc PR 2 C11 C 0.4953(6) -0.1508(2) 0.6735(2) 0.0199(7) Uani 1 d . . C12 C 0.3229(6) -0.1504(2) 0.7503(2) 0.0233(7) Uani 1 d . . C13 C 0.3263(6) -0.2290(3) 0.8291(2) 0.0269(8) Uani 1 d . . H13A H 0.2082(6) -0.2281(3) 0.8814(2) 0.032 Uiso 1 calc R . C14 C 0.4996(7) -0.3084(3) 0.8323(2) 0.0258(8) Uani 1 d . . C15 C 0.6758(6) -0.3072(2) 0.7571(2) 0.0241(7) Uani 1 d . . C16 C 0.6740(6) -0.2293(2) 0.6780(2) 0.0222(7) Uani 1 d . . H16A H 0.7957(6) -0.2296(2) 0.6266(2) 0.027 Uiso 1 calc R . C17 C -0.0335(7) -0.0720(3) 0.8201(3) 0.0340(9) Uani 1 d . . H17A H -0.1426(35) -0.0120(9) 0.8062(10) 0.051 Uiso 1 calc R . H17B H 0.0569(7) -0.0758(19) 0.8804(4) 0.051 Uiso 1 calc R . H17C H -0.1456(33) -0.1292(11) 0.8252(12) 0.051 Uiso 1 calc R . C18 C 0.4899(8) -0.3951(3) 0.9148(3) 0.0397(10) Uani 1 d . . H18A H 0.3900(47) -0.3772(7) 0.9681(7) 0.060 Uiso 1 calc R . H18B H 0.6697(8) -0.4152(13) 0.9349(13) 0.060 Uiso 1 calc R . H18C H 0.4037(49) -0.4495(7) 0.8951(6) 0.060 Uiso 1 calc R . C19 C 1.0332(9) -0.3864(3) 0.6897(3) 0.0433(11) Uani 1 d . . H19A H 1.1386(40) -0.4472(10) 0.7030(11) 0.065 Uiso 1 calc R . H19B H 1.1487(37) -0.3303(13) 0.6855(14) 0.065 Uiso 1 calc R . H19C H 0.9431(9) -0.3809(22) 0.6290(4) 0.065 Uiso 1 calc R . O22 O -0.8349(5) 0.2590(2) 0.6104(2) 0.0299(6) Uani 1 d . . O25 O -0.1666(5) 0.2853(2) 0.9023(2) 0.0351(7) Uani 1 d . . C4 C -0.5060(6) 0.4235(2) 0.5819(2) 0.0184(7) Uani 1 d . . C5A C -0.4835(11) 0.5249(5) 0.5872(4) 0.0174(12) Uani 0.50 d P 1 H5AA H -0.4707(11) 0.5421(5) 0.6476(4) 0.021 Uiso 0.50 calc PR 1 C6A C -0.4803(11) 0.5975(5) 0.5047(4) 0.0207(13) Uani 0.50 d P 1 H6AA H -0.4680(11) 0.6640(5) 0.5097(4) 0.025 Uiso 0.50 calc PR 1 C5B C -0.2689(12) 0.4584(5) 0.5400(4) 0.0205(13) Uani 0.50 d P 2 H5BA H -0.1089(12) 0.4287(5) 0.5657(4) 0.025 Uiso 0.50 calc PR 2 C6B C -0.2594(12) 0.5350(5) 0.4622(4) 0.0223(14) Uani 0.50 d P 2 H6BA H -0.0937(12) 0.5604(5) 0.4377(4) 0.027 Uiso 0.50 calc PR 2 C21 C -0.5079(6) 0.3450(2) 0.6705(2) 0.0192(7) Uani 1 d . . C22 C -0.6733(6) 0.2644(2) 0.6836(2) 0.0236(7) Uani 1 d . . C23 C -0.6628(7) 0.1934(3) 0.7682(2) 0.0277(8) Uani 1 d . . H23A H -0.7751(7) 0.1387(3) 0.7766(2) 0.033 Uiso 1 calc R . C24 C -0.4928(7) 0.2010(3) 0.8400(2) 0.0301(8) Uani 1 d . . C25 C -0.3284(6) 0.2815(3) 0.8280(2) 0.0256(8) Uani 1 d . . C26 C -0.3377(6) 0.3528(3) 0.7438(2) 0.0238(7) Uani 1 d . . H26A H -0.2264(6) 0.4078(3) 0.7360(2) 0.029 Uiso 1 calc R . C27 C -1.0146(8) 0.1799(3) 0.6239(3) 0.0373(9) Uani 1 d . . H27A H -1.1229(36) 0.1863(11) 0.5672(8) 0.056 Uiso 1 calc R . H27B H -1.1286(35) 0.1814(12) 0.6797(12) 0.056 Uiso 1 calc R . H27C H -0.9156(8) 0.1176(3) 0.6340(18) 0.056 Uiso 1 calc R . C28 C -0.4858(9) 0.1245(3) 0.9321(3) 0.0465(11) Uani 1 d . . H28A H -0.5925(49) 0.0686(10) 0.9260(8) 0.070 Uiso 1 calc R . H28B H -0.5571(56) 0.1530(7) 0.9845(5) 0.070 Uiso 1 calc R . H28C H -0.3034(11) 0.1023(17) 0.9455(12) 0.070 Uiso 1 calc R . C29 C 0.0123(8) 0.3644(3) 0.8892(3) 0.0354(9) Uani 1 d . . H29A H 0.1066(36) 0.3618(11) 0.9485(6) 0.053 Uiso 1 calc R . H29B H -0.0857(9) 0.4267(3) 0.8723(17) 0.053 Uiso 1 calc R . H29C H 0.1392(30) 0.3589(10) 0.8379(12) 0.053 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 O12 0.0292(13) 0.0282(15) 0.0347(13) -0.0039(12) 0.0023(10) -0.0021(11) O15 0.0390(15) 0.0235(14) 0.0410(15) -0.0026(12) -0.0055(12) -0.0005(11) C1 0.020(2) 0.014(2) 0.023(2) -0.0041(13) 0.0001(12) -0.0045(12) C2A 0.022(3) 0.016(3) 0.028(3) -0.004(3) -0.007(3) -0.003(2) C3A 0.021(3) 0.019(3) 0.023(3) -0.004(3) 0.000(2) -0.008(2) C2B 0.022(3) 0.015(3) 0.025(3) -0.005(3) -0.005(2) -0.005(2) C3B 0.022(3) 0.016(3) 0.018(3) -0.007(3) 0.001(2) -0.003(2) C11 0.0197(15) 0.015(2) 0.023(2) 0.0028(13) -0.0023(12) -0.0063(12) C12 0.021(2) 0.021(2) 0.026(2) -0.0019(15) -0.0022(13) -0.0057(13) C13 0.024(2) 0.029(2) 0.024(2) 0.001(2) 0.0020(13) -0.0062(14) C14 0.027(2) 0.019(2) 0.028(2) 0.0042(15) -0.0051(13) -0.0102(13) C15 0.028(2) 0.014(2) 0.030(2) -0.0020(14) -0.0082(14) -0.0042(13) C16 0.023(2) 0.017(2) 0.027(2) -0.0048(14) -0.0030(13) -0.0093(12) C17 0.036(2) 0.033(2) 0.035(2) -0.014(2) 0.005(2) -0.005(2) C18 0.046(2) 0.034(2) 0.033(2) 0.009(2) -0.004(2) -0.013(2) C19 0.056(3) 0.035(2) 0.040(2) -0.014(2) -0.008(2) 0.014(2) O22 0.0323(13) 0.0211(13) 0.0362(14) -0.0038(11) -0.0038(10) -0.0118(10) O25 0.0421(15) 0.033(2) 0.0286(13) -0.0029(12) -0.0071(11) -0.0036(12) C4 0.0182(15) 0.012(2) 0.024(2) 0.0002(13) -0.0011(12) -0.0034(12) C5A 0.018(3) 0.014(3) 0.022(3) -0.007(3) 0.003(2) -0.004(2) C6A 0.017(3) 0.021(3) 0.024(3) -0.004(3) -0.003(2) -0.007(2) C5B 0.017(3) 0.018(3) 0.027(3) -0.005(3) -0.006(2) -0.005(2) C6B 0.021(3) 0.025(4) 0.023(3) -0.009(3) -0.002(2) -0.005(3) C21 0.022(2) 0.013(2) 0.022(2) -0.0014(13) 0.0049(12) -0.0025(12) C22 0.026(2) 0.015(2) 0.028(2) -0.0010(14) 0.0028(13) -0.0026(13) C23 0.033(2) 0.018(2) 0.030(2) 0.0019(15) 0.0047(14) -0.0031(14) C24 0.034(2) 0.024(2) 0.028(2) 0.004(2) 0.0021(15) -0.0008(15) C25 0.028(2) 0.026(2) 0.022(2) -0.0027(15) -0.0012(13) 0.0016(14) C26 0.020(2) 0.024(2) 0.028(2) -0.0059(15) 0.0011(13) -0.0014(13) C27 0.046(2) 0.027(2) 0.042(2) -0.012(2) 0.003(2) -0.017(2) C28 0.068(3) 0.029(2) 0.036(2) 0.008(2) -0.002(2) -0.012(2) C29 0.041(2) 0.031(2) 0.036(2) -0.011(2) -0.009(2) -0.002(2) _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 O12 C12 1.373(4) . ? O12 C17 1.423(4) . ? O15 C15 1.377(4) . ? O15 C19 1.419(5) . ? C1 C2B 1.375(7) . ? C1 C3A 1.389(7) 2_656 ? C1 C2A 1.397(7) . ? C1 C3B 1.405(7) 2_656 ? C1 C11 1.490(4) . ? C2A C3A 1.398(8) . ? C3A C1 1.389(7) 2_656 ? C2B C3B 1.391(8) . ? C3B C1 1.404(7) 2_656 ? C11 C12 1.391(4) . ? C11 C16 1.398(5) . ? C12 C13 1.399(4) . ? C13 C14 1.393(5) . ? C14 C15 1.382(5) . ? C14 C18 1.504(5) . ? C15 C16 1.396(4) . ? O22 C22 1.363(4) . ? O22 C27 1.428(4) . ? O25 C25 1.372(4) . ? O25 C29 1.424(5) . ? C4 C6A 1.338(7) 2_466 ? C4 C5B 1.384(7) . ? C4 C6B 1.415(7) 2_466 ? C4 C5A 1.442(7) . ? C4 C21 1.492(4) . ? C5A C6A 1.386(8) . ? C6A C4 1.338(7) 2_466 ? C5B C6B 1.374(9) . ? C6B C4 1.415(7) 2_466 ? C21 C22 1.398(4) . ? C21 C26 1.400(4) . ? C22 C23 1.396(4) . ? C23 C24 1.382(5) . ? C24 C25 1.394(5) . ? C24 C28 1.515(5) . ? C25 C26 1.394(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 C12 O12 C17 118.1(3) . . ? C15 O15 C19 117.5(3) . . ? C3A C1 C2A 118.5(4) 2_656 . ? C2B C1 C3B 118.1(4) . 2_656 ? C2B C1 C11 118.4(4) . . ? C3A C1 C11 121.4(3) 2_656 . ? C2A C1 C11 120.0(3) . . ? C3B C1 C11 123.5(4) 2_656 . ? C3A C2A C1 120.2(5) . . ? C1 C3A C2A 121.2(5) 2_656 . ? C1 C2B C3B 120.8(6) . . ? C2B C3B C1 121.1(5) . 2_656 ? C12 C11 C16 118.9(3) . . ? C12 C11 C1 123.0(3) . . ? C16 C11 C1 118.1(3) . . ? O12 C12 C11 117.4(3) . . ? O12 C12 C13 122.7(3) . . ? C11 C12 C13 119.8(3) . . ? C14 C13 C12 121.2(3) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 C18 120.6(3) . . ? C13 C14 C18 120.6(3) . . ? O15 C15 C14 116.3(3) . . ? O15 C15 C16 123.1(3) . . ? C14 C15 C16 120.6(3) . . ? C15 C16 C11 120.7(3) . . ? C22 O22 C27 118.0(3) . . ? C25 O25 C29 117.3(3) . . ? C5B C4 C6B 117.6(4) . 2_466 ? C6A C4 C5A 117.8(4) 2_466 . ? C6A C4 C21 121.7(4) 2_466 . ? C5B C4 C21 120.0(3) . . ? C6B C4 C21 122.4(4) 2_466 . ? C5A C4 C21 120.5(4) . . ? C6A C5A C4 120.3(5) . . ? C4 C6A C5A 121.9(6) 2_466 . ? C6B C5B C4 121.6(5) . . ? C5B C6B C4 120.6(5) . 2_466 ? C22 C21 C26 118.7(3) . . ? C22 C21 C4 122.7(3) . . ? C26 C21 C4 118.6(3) . . ? O22 C22 C23 123.4(3) . . ? O22 C22 C21 117.0(3) . . ? C23 C22 C21 119.6(3) . . ? C24 C23 C22 121.5(3) . . ? C23 C24 C25 119.4(3) . . ? C23 C24 C28 121.2(4) . . ? C25 C24 C28 119.5(3) . . ? O25 C25 C26 123.9(3) . . ? O25 C25 C24 116.5(3) . . ? C26 C25 C24 119.5(3) . . ? C25 C26 C21 121.3(3) . . ? _refine_diff_density_max 0.596 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.095 data_raj-rsy _database_code_CSD 162401 _audit_creation_method SHELXL _chemical_name_systematic ; 2,2",5,5"-tetramethoxy-4,4"-dimethylterphenyl hexachloroantimonate ; _chemical_name_common ? _chemical_formula_moiety '(C24 H26 O4)^+^, (Cl6 Sb)^-^' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H26 Cl6 O4 Sb' _chemical_formula_weight 712.90 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 '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' 'Sb' 'Sb' -0.5866 1.5461 '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)/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 13.4765(2) _cell_length_b 15.5512(2) _cell_length_c 13.8393(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.9440(10) _cell_angle_gamma 90.00 _cell_volume 2788.81(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7410 _cell_measurement_theta_min 2 _cell_measurement_theta_max 36 _exptl_crystal_description 'prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method none _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 1.594 _exptl_absorpt_correction_type 'Semi-empirical (SADABs procedure)' _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 0.75 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34861 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 36.23 _reflns_number_total 12599 _reflns_number_observed 9054 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 10 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.0312P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12589 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_obs 0.0367 _refine_ls_wR_factor_all 0.0853 _refine_ls_wR_factor_obs 0.0712 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.065 _refine_ls_restrained_S_obs 1.052 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sb1 Sb 0.853242(8) -0.228218(8) 0.436968(9) 0.01656(3) Uani 1 d . . Cl1 Cl 0.76887(4) -0.15714(5) 0.28683(4) 0.0416(2) Uani 1 d . . Cl2 Cl 0.87191(5) -0.35407(4) 0.34676(5) 0.04057(15) Uani 1 d . . Cl3 Cl 0.69146(3) -0.27937(3) 0.45018(4) 0.02477(10) Uani 1 d . . Cl4 Cl 0.93385(4) -0.29998(3) 0.58907(4) 0.02677(10) Uani 1 d . . Cl5 Cl 1.01506(4) -0.17726(4) 0.42347(4) 0.03154(12) Uani 1 d . . Cl6 Cl 0.83668(4) -0.10407(3) 0.53048(5) 0.03117(12) Uani 1 d . . O12 O 0.18749(10) 0.59274(8) 0.26024(10) 0.0193(3) Uani 1 d . . O15 O 0.39384(10) 0.89736(8) 0.33971(10) 0.0172(2) Uani 1 d . . O32 O 0.73468(9) 0.40362(8) 0.44913(10) 0.0173(2) Uani 1 d . . O35 O 0.49110(9) 0.11229(8) 0.38364(9) 0.0160(2) Uani 1 d . . C11 C 0.34488(12) 0.66415(11) 0.32834(12) 0.0129(3) Uani 1 d . . C12 C 0.23455(13) 0.66776(11) 0.28686(13) 0.0148(3) Uani 1 d . . C13 C 0.18269(13) 0.74750(12) 0.27159(13) 0.0161(3) Uani 1 d . . H13A H 0.10954(13) 0.74860(12) 0.24755(13) 0.019 Uiso 1 calc R . C14 C 0.23642(13) 0.82379(11) 0.29098(13) 0.0156(3) Uani 1 d . . C15 C 0.34701(13) 0.82023(11) 0.32596(12) 0.0138(3) Uani 1 d . . C16 C 0.39836(13) 0.74211(11) 0.34469(12) 0.0131(3) Uani 1 d . . H16A H 0.47148(13) 0.74161(11) 0.36916(12) 0.016 Uiso 1 calc R . C17 C 0.07908(14) 0.59061(14) 0.2058(2) 0.0260(4) Uani 1 d . . H17A H 0.0582(3) 0.5311(2) 0.1875(10) 0.039 Uiso 1 calc R . H17B H 0.0676(2) 0.6254(8) 0.1447(6) 0.039 Uiso 1 calc R . H17C H 0.0381(2) 0.6138(9) 0.2483(4) 0.039 Uiso 1 calc R . C18 C 0.18279(15) 0.90925(12) 0.27458(14) 0.0201(4) Uani 1 d . . H18A H 0.1080(2) 0.90031(12) 0.2511(10) 0.030 Uiso 1 calc R . H18B H 0.2057(8) 0.9419(4) 0.2241(8) 0.030 Uiso 1 calc R . H18C H 0.1996(9) 0.9414(4) 0.3379(3) 0.030 Uiso 1 calc R . C19 C 0.50527(13) 0.89867(12) 0.37061(14) 0.0181(3) Uani 1 d . . H19A H 0.52948(14) 0.95838(12) 0.3767(10) 0.027 Uiso 1 calc R . H19B H 0.53164(14) 0.8688(7) 0.3204(5) 0.027 Uiso 1 calc R . H19C H 0.53032(14) 0.8697(8) 0.4357(5) 0.027 Uiso 1 calc R . C21 C 0.40085(12) 0.58237(11) 0.34825(12) 0.0126(3) Uani 1 d . . C22 C 0.35931(13) 0.50831(11) 0.38103(12) 0.0133(3) Uani 1 d . . H22A H 0.29198(13) 0.51008(11) 0.39009(12) 0.016 Uiso 1 calc R . C23 C 0.41585(12) 0.43325(11) 0.40004(12) 0.0131(3) Uani 1 d . . H23A H 0.38677(12) 0.38443(11) 0.42327(12) 0.016 Uiso 1 calc R . C24 C 0.51508(12) 0.42656(11) 0.38620(12) 0.0120(3) Uani 1 d . . C25 C 0.55740(13) 0.50146(11) 0.35532(12) 0.0135(3) Uani 1 d . . H25A H 0.62497(13) 0.49982(11) 0.34682(12) 0.016 Uiso 1 calc R . C26 C 0.50151(12) 0.57691(11) 0.33743(12) 0.0130(3) Uani 1 d . . H26A H 0.53178(12) 0.62654(11) 0.31726(12) 0.016 Uiso 1 calc R . C31 C 0.56725(12) 0.34231(11) 0.40028(12) 0.0125(3) Uani 1 d . . C32 C 0.67568(13) 0.33112(11) 0.43135(12) 0.0134(3) Uani 1 d . . C33 C 0.71804(13) 0.24840(11) 0.44455(13) 0.0148(3) Uani 1 d . . H33A H 0.79094(13) 0.24196(11) 0.46512(13) 0.018 Uiso 1 calc R . C34 C 0.65606(13) 0.17523(11) 0.42829(12) 0.0139(3) Uani 1 d . . C35 C 0.54809(13) 0.18642(11) 0.39794(12) 0.0132(3) Uani 1 d . . C36 C 0.50530(13) 0.26787(11) 0.38334(12) 0.0133(3) Uani 1 d . . H36A H 0.43238(13) 0.27375(11) 0.36135(12) 0.016 Uiso 1 calc R . C37 C 0.84387(13) 0.39453(13) 0.4906(2) 0.0219(4) Uani 1 d . . H37A H 0.8759(2) 0.45157(13) 0.5018(10) 0.033 Uiso 1 calc R . H37B H 0.8725(2) 0.3621(8) 0.4438(5) 0.033 Uiso 1 calc R . H37C H 0.85794(14) 0.3637(8) 0.5547(5) 0.033 Uiso 1 calc R . C38 C 0.70189(14) 0.08632(11) 0.44109(14) 0.0184(3) Uani 1 d . . H38A H 0.7772(2) 0.09043(12) 0.4660(10) 0.028 Uiso 1 calc R . H38B H 0.6833(9) 0.0565(3) 0.3762(2) 0.028 Uiso 1 calc R . H38C H 0.6751(8) 0.0541(3) 0.4894(8) 0.028 Uiso 1 calc R . C39 C 0.38082(13) 0.12036(12) 0.35058(14) 0.0186(3) Uani 1 d . . H39A H 0.34941(14) 0.06304(12) 0.3432(10) 0.028 Uiso 1 calc R . H39B H 0.36083(15) 0.1502(8) 0.2857(5) 0.028 Uiso 1 calc R . H39C H 0.3569(2) 0.1533(8) 0.4002(5) 0.028 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 Sb1 0.00954(5) 0.02082(6) 0.01777(5) 0.00138(5) 0.00113(4) 0.00109(4) Cl1 0.0257(3) 0.0620(4) 0.0306(3) 0.0236(3) -0.0033(2) -0.0023(3) Cl2 0.0314(3) 0.0473(4) 0.0425(3) -0.0238(3) 0.0092(2) 0.0020(2) Cl3 0.0137(2) 0.0279(2) 0.0315(2) 0.0015(2) 0.0042(2) -0.0043(2) Cl4 0.0211(2) 0.0297(3) 0.0247(2) 0.0077(2) -0.0017(2) 0.0033(2) Cl5 0.0135(2) 0.0458(3) 0.0357(3) 0.0072(2) 0.0073(2) -0.0026(2) Cl6 0.0221(2) 0.0212(2) 0.0484(3) -0.0077(2) 0.0067(2) 0.0021(2) O12 0.0127(6) 0.0164(6) 0.0253(7) -0.0013(5) -0.0009(5) -0.0012(4) O15 0.0167(6) 0.0112(6) 0.0220(6) -0.0001(5) 0.0025(5) 0.0001(4) O32 0.0101(5) 0.0153(6) 0.0247(6) -0.0004(5) 0.0017(5) -0.0007(4) O35 0.0150(6) 0.0120(6) 0.0194(6) -0.0010(5) 0.0022(5) 0.0005(4) C11 0.0127(7) 0.0139(8) 0.0116(7) 0.0003(6) 0.0024(5) 0.0016(5) C12 0.0136(7) 0.0144(8) 0.0157(7) 0.0001(6) 0.0030(6) 0.0000(6) C13 0.0123(7) 0.0170(8) 0.0181(8) 0.0015(6) 0.0028(6) 0.0031(6) C14 0.0160(7) 0.0161(8) 0.0140(7) 0.0011(6) 0.0030(6) 0.0046(6) C15 0.0161(7) 0.0119(7) 0.0130(7) 0.0004(6) 0.0033(6) 0.0012(6) C16 0.0125(7) 0.0124(7) 0.0138(7) 0.0003(6) 0.0028(6) 0.0005(5) C17 0.0125(8) 0.0266(10) 0.0335(11) -0.0016(8) -0.0024(7) -0.0019(7) C18 0.0204(8) 0.0164(8) 0.0225(9) 0.0017(7) 0.0039(7) 0.0061(6) C19 0.0174(8) 0.0154(8) 0.0196(8) 0.0001(7) 0.0018(6) -0.0016(6) C21 0.0125(7) 0.0123(7) 0.0114(7) -0.0008(6) 0.0008(5) 0.0003(5) C22 0.0127(7) 0.0130(7) 0.0139(7) -0.0010(6) 0.0033(6) 0.0003(5) C23 0.0133(7) 0.0123(7) 0.0132(7) -0.0002(6) 0.0026(6) -0.0001(5) C24 0.0124(7) 0.0122(7) 0.0107(6) -0.0010(6) 0.0017(5) 0.0007(5) C25 0.0131(7) 0.0135(7) 0.0138(7) 0.0001(6) 0.0033(6) 0.0017(6) C26 0.0137(7) 0.0115(7) 0.0130(7) -0.0004(6) 0.0025(6) -0.0007(5) C31 0.0136(7) 0.0119(7) 0.0114(7) 0.0005(6) 0.0023(5) 0.0017(5) C32 0.0140(7) 0.0121(7) 0.0139(7) -0.0001(6) 0.0036(6) -0.0005(5) C33 0.0124(7) 0.0157(8) 0.0153(7) -0.0007(6) 0.0022(6) 0.0028(5) C34 0.0147(7) 0.0146(8) 0.0117(7) -0.0005(6) 0.0025(6) 0.0035(6) C35 0.0155(7) 0.0121(7) 0.0120(7) -0.0012(6) 0.0037(6) -0.0005(6) C36 0.0133(7) 0.0131(7) 0.0126(7) -0.0006(6) 0.0020(5) 0.0005(6) C37 0.0113(7) 0.0234(9) 0.0289(10) 0.0002(8) 0.0018(7) -0.0011(6) C38 0.0175(8) 0.0142(8) 0.0221(8) 0.0003(7) 0.0032(7) 0.0045(6) C39 0.0155(8) 0.0163(8) 0.0229(9) -0.0020(7) 0.0035(6) -0.0014(6) _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 Sb1 Cl1 2.3524(5) . ? Sb1 Cl4 2.3665(5) . ? Sb1 Cl6 2.3687(5) . ? Sb1 Cl2 2.3716(6) . ? Sb1 Cl3 2.3745(5) . ? Sb1 Cl5 2.3754(5) . ? O12 C12 1.331(2) . ? O12 C17 1.449(2) . ? O15 C15 1.344(2) . ? O15 C19 1.444(2) . ? O32 C32 1.363(2) . ? O32 C37 1.432(2) . ? O35 C35 1.369(2) . ? O35 C39 1.435(2) . ? C11 C16 1.397(2) . ? C11 C12 1.440(2) . ? C11 C21 1.466(2) . ? C12 C13 1.411(2) . ? C13 C14 1.377(3) . ? C14 C15 1.436(2) . ? C14 C18 1.500(2) . ? C15 C16 1.387(2) . ? C21 C26 1.408(2) . ? C21 C22 1.409(2) . ? C22 C23 1.379(2) . ? C23 C24 1.406(2) . ? C24 C25 1.414(2) . ? C24 C31 1.474(2) . ? C25 C26 1.379(2) . ? C31 C36 1.409(2) . ? C31 C32 1.416(2) . ? C32 C33 1.399(2) . ? C33 C34 1.393(2) . ? C34 C35 1.410(2) . ? C34 C38 1.505(2) . ? C35 C36 1.383(2) . ? 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 Cl1 Sb1 Cl4 178.47(2) . . ? Cl1 Sb1 Cl6 90.25(2) . . ? Cl4 Sb1 Cl6 89.28(2) . . ? Cl1 Sb1 Cl2 91.05(3) . . ? Cl4 Sb1 Cl2 89.42(2) . . ? Cl6 Sb1 Cl2 178.70(2) . . ? Cl1 Sb1 Cl3 89.66(2) . . ? Cl4 Sb1 Cl3 88.88(2) . . ? Cl6 Sb1 Cl3 90.27(2) . . ? Cl2 Sb1 Cl3 89.80(2) . . ? Cl1 Sb1 Cl5 90.30(2) . . ? Cl4 Sb1 Cl5 91.16(2) . . ? Cl6 Sb1 Cl5 89.85(2) . . ? Cl2 Sb1 Cl5 90.09(2) . . ? Cl3 Sb1 Cl5 179.878(15) . . ? C12 O12 C17 119.99(14) . . ? C15 O15 C19 117.65(13) . . ? C32 O32 C37 118.37(14) . . ? C35 O35 C39 117.58(13) . . ? C16 C11 C12 117.45(15) . . ? C16 C11 C21 120.45(15) . . ? C12 C11 C21 122.02(15) . . ? O12 C12 C13 123.4(2) . . ? O12 C12 C11 115.94(15) . . ? C13 C12 C11 120.6(2) . . ? C14 C13 C12 121.0(2) . . ? C13 C14 C15 118.3(2) . . ? C13 C14 C18 121.9(2) . . ? C15 C14 C18 119.8(2) . . ? O15 C15 C16 124.4(2) . . ? O15 C15 C14 114.63(14) . . ? C16 C15 C14 121.0(2) . . ? C15 C16 C11 121.4(2) . . ? C26 C21 C22 117.68(15) . . ? C26 C21 C11 119.58(15) . . ? C22 C21 C11 122.71(15) . . ? C23 C22 C21 120.4(2) . . ? C22 C23 C24 122.2(2) . . ? C23 C24 C25 117.27(15) . . ? C23 C24 C31 118.99(15) . . ? C25 C24 C31 123.69(15) . . ? C26 C25 C24 120.6(2) . . ? C25 C26 C21 121.8(2) . . ? C36 C31 C32 117.67(15) . . ? C36 C31 C24 117.97(14) . . ? C32 C31 C24 124.35(15) . . ? O32 C32 C33 122.71(15) . . ? O32 C32 C31 117.09(14) . . ? C33 C32 C31 120.19(15) . . ? C34 C33 C32 121.7(2) . . ? C33 C34 C35 118.12(15) . . ? C33 C34 C38 121.5(2) . . ? C35 C34 C38 120.3(2) . . ? O35 C35 C36 123.72(15) . . ? O35 C35 C34 115.53(15) . . ? C36 C35 C34 120.7(2) . . ? C35 C36 C31 121.6(2) . . ? _refine_diff_density_max 0.703 _refine_diff_density_min -1.480 _refine_diff_density_rms 0.118 data_sunfsy _database_code_CSD 162402 _audit_creation_method SHELXL _chemical_name_systematic ; 2,2''',5,5'''-tetramethoxy-4,4'''-dimethylquaterphenyl hexachloroantimonate ; _chemical_name_common ? _chemical_formula_moiety '(C30 H30 O4)^+^, (Cl6 Sb)^-^' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H30 Cl6 O4 Sb' _chemical_formula_weight 788.99 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 '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' 'Sb' 'Sb' -0.5866 1.5461 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.21820(10) _cell_length_b 16.6646(3) _cell_length_c 13.43140(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.8840(10) _cell_angle_gamma 90.00 _cell_volume 1568.44(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6830 _cell_measurement_theta_min 2 _cell_measurement_theta_max 35 _exptl_crystal_description 'prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method ? _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 1.426 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.918 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23274 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 35.66 _reflns_number_total 13253 _reflns_number_observed 9677 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 5 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.0000P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 13248 _refine_ls_number_parameters 376 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_obs 0.0461 _refine_ls_wR_factor_all 0.0776 _refine_ls_wR_factor_obs 0.0675 _refine_ls_goodness_of_fit_all 1.008 _refine_ls_goodness_of_fit_obs 1.038 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.038 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sb1 Sb -0.24372(3) -0.141948(15) -0.731464(15) 0.01676(4) Uani 1 d . . Cl1 Cl -0.19044(12) -0.07690(5) -0.57054(6) 0.0259(2) Uani 1 d . . Cl2 Cl -0.28882(12) -0.21034(5) -0.89078(6) 0.0272(2) Uani 1 d . . Cl3 Cl 0.02036(11) -0.22684(5) -0.66397(7) 0.0271(2) Uani 1 d . . Cl4 Cl -0.45672(12) -0.23301(5) -0.68223(7) 0.0313(2) Uani 1 d . . Cl5 Cl -0.50781(12) -0.05691(5) -0.79970(7) 0.0288(2) Uani 1 d . . Cl6 Cl -0.04335(14) -0.04896(5) -0.78586(7) 0.0323(2) Uani 1 d . . O1 O -0.4509(3) -0.54642(13) -0.8232(2) 0.0202(5) Uani 1 d . . O2 O -0.3135(3) -0.84542(13) -0.6635(2) 0.0248(5) Uani 1 d . . O3 O -0.1253(3) 0.06556(13) -0.1993(2) 0.0283(5) Uani 1 d . . O4 O 0.0686(3) -0.23807(13) -0.0409(2) 0.0209(5) Uani 1 d . . C11 C -0.2517(4) -0.4258(2) -0.4684(2) 0.0149(5) Uani 1 d . . C12 C -0.3351(4) -0.4972(2) -0.4451(2) 0.0181(6) Uani 1 d . . H12A H -0.3702(4) -0.5020(2) -0.3816(2) 0.022 Uiso 1 calc R . C13 C -0.3669(4) -0.5608(2) -0.5132(2) 0.0177(6) Uani 1 d . . H13A H -0.4218(4) -0.6088(2) -0.4950(2) 0.021 Uiso 1 calc R . C14 C -0.3204(4) -0.5563(2) -0.6082(2) 0.0158(6) Uani 1 d . . C15 C -0.2383(4) -0.4845(2) -0.6326(2) 0.0178(6) Uani 1 d . . H15A H -0.2052(4) -0.4796(2) -0.6966(2) 0.021 Uiso 1 calc R . C16 C -0.2053(4) -0.4214(2) -0.5642(2) 0.0169(6) Uani 1 d . . H16A H -0.1496(4) -0.3736(2) -0.5822(2) 0.020 Uiso 1 calc R . C21 C -0.2121(4) -0.3578(2) -0.3949(2) 0.0159(6) Uani 1 d . . C22 C -0.1767(4) -0.2803(2) -0.4271(2) 0.0182(6) Uani 1 d . . H22A H -0.1819(4) -0.2710(2) -0.4975(2) 0.022 Uiso 1 calc R . C23 C -0.1345(4) -0.2175(2) -0.3584(2) 0.0191(6) Uani 1 d . . H23A H -0.1092(4) -0.1661(2) -0.3828(2) 0.023 Uiso 1 calc R . C24 C -0.1279(4) -0.2271(2) -0.2544(2) 0.0159(6) Uani 1 d . . C25 C -0.1670(4) -0.3039(2) -0.2214(2) 0.0168(6) Uani 1 d . . H25A H -0.1648(4) -0.3128(2) -0.1513(2) 0.020 Uiso 1 calc R . C26 C -0.2089(5) -0.3672(2) -0.2909(3) 0.0175(7) Uani 1 d . . H26A H -0.2364(5) -0.4184(2) -0.2670(3) 0.021 Uiso 1 calc R . C31 C -0.3484(4) -0.62648(15) -0.6763(2) 0.0155(6) Uani 1 d . . C32 C -0.4082(4) -0.6198(2) -0.7867(2) 0.0157(6) Uani 1 d . . C33 C -0.4243(4) -0.6885(2) -0.8495(2) 0.0197(6) Uani 1 d . . H33A H -0.4600(4) -0.6826(2) -0.9220(2) 0.024 Uiso 1 calc R . C34 C -0.3893(4) -0.7637(2) -0.8077(3) 0.0194(6) Uani 1 d . . C35 C -0.3412(4) -0.7709(2) -0.6981(3) 0.0199(6) Uani 1 d . . C36 C -0.3203(4) -0.7028(2) -0.6351(2) 0.0165(6) Uani 1 d . . H36A H -0.2862(4) -0.7092(2) -0.5628(2) 0.020 Uiso 1 calc R . C37 C -0.5340(5) -0.5351(2) -0.9321(2) 0.0242(7) Uani 1 d . . H37A H -0.5678(30) -0.4785(3) -0.9455(4) 0.036 Uiso 1 calc R . H37B H -0.6488(19) -0.5683(11) -0.9532(4) 0.036 Uiso 1 calc R . H37C H -0.4412(13) -0.5510(13) -0.9711(3) 0.036 Uiso 1 calc R . C38 C -0.2787(5) -0.8587(2) -0.5540(3) 0.0254(8) Uani 1 d . . H38A H -0.2719(33) -0.9164(2) -0.5400(3) 0.038 Uiso 1 calc R . H38B H -0.3829(17) -0.8351(12) -0.5285(4) 0.038 Uiso 1 calc R . H38C H -0.1578(17) -0.8334(12) -0.5194(3) 0.038 Uiso 1 calc R . C39 C -0.4004(5) -0.8378(2) -0.8718(3) 0.0261(7) Uani 1 d . . H39A H -0.4441(33) -0.8236(3) -0.9445(3) 0.039 Uiso 1 calc R . H39B H -0.4904(26) -0.8757(6) -0.8533(13) 0.039 Uiso 1 calc R . H39C H -0.2738(8) -0.8627(8) -0.8596(14) 0.039 Uiso 1 calc R . C41 C -0.0790(4) -0.15717(15) -0.1841(2) 0.0158(6) Uani 1 d . . C42 C 0.0213(4) -0.1630(2) -0.0805(2) 0.0161(6) Uani 1 d . . C43 C 0.0751(4) -0.0939(2) -0.0224(2) 0.0192(6) Uani 1 d . . H43A H 0.1459(4) -0.0991(2) 0.0467(2) 0.023 Uiso 1 calc R . C44 C 0.0284(5) -0.0174(2) -0.0624(3) 0.0202(6) Uani 1 d . . C45 C -0.0754(4) -0.0114(2) -0.1641(3) 0.0189(6) Uani 1 d . . C46 C -0.1281(4) -0.0797(2) -0.2239(3) 0.0164(6) Uani 1 d . . H46A H -0.1986(4) -0.0740(2) -0.2930(3) 0.020 Uiso 1 calc R . C47 C 0.1771(5) -0.2438(2) 0.0639(3) 0.0237(7) Uani 1 d . . H47A H 0.1985(28) -0.3005(2) 0.0828(6) 0.036 Uiso 1 calc R . H47B H 0.1063(15) -0.2182(12) 0.1090(3) 0.036 Uiso 1 calc R . H47C H 0.3002(14) -0.2168(12) 0.0711(5) 0.036 Uiso 1 calc R . C48 C -0.2368(5) 0.0749(2) -0.3011(3) 0.0257(8) Uani 1 d . . H48A H -0.2675(29) 0.1318(3) -0.3144(7) 0.039 Uiso 1 calc R . H48B H -0.3551(16) 0.0440(12) -0.3097(6) 0.039 Uiso 1 calc R . H48C H -0.1647(14) 0.0554(13) -0.3494(3) 0.039 Uiso 1 calc R . C49 C 0.0865(5) 0.0567(2) 0.0010(3) 0.0261(7) Uani 1 d . . H49A H 0.1436(30) 0.0953(6) -0.0380(7) 0.039 Uiso 1 calc R . H49B H 0.1799(25) 0.0425(3) 0.0644(8) 0.039 Uiso 1 calc R . H49C H -0.0260(7) 0.0808(8) 0.0178(15) 0.039 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 Sb1 0.01636(8) 0.01749(7) 0.01645(8) 0.00165(10) 0.00395(6) -0.00018(9) Cl1 0.0313(4) 0.0276(4) 0.0188(5) -0.0018(3) 0.0063(3) 0.0011(3) Cl2 0.0249(4) 0.0324(4) 0.0219(5) -0.0074(3) 0.0008(3) 0.0028(3) Cl3 0.0209(4) 0.0310(4) 0.0274(5) 0.0020(3) 0.0022(3) 0.0075(3) Cl4 0.0247(4) 0.0351(5) 0.0330(5) 0.0082(4) 0.0047(4) -0.0102(3) Cl5 0.0301(5) 0.0314(4) 0.0228(5) 0.0020(3) 0.0023(3) 0.0131(3) Cl6 0.0369(5) 0.0336(5) 0.0294(5) 0.0016(4) 0.0141(4) -0.0133(4) O1 0.0262(12) 0.0193(11) 0.0139(11) -0.0003(9) 0.0024(9) -0.0007(9) O2 0.0287(13) 0.0174(10) 0.0258(13) 0.0009(9) 0.0017(10) -0.0002(9) O3 0.0337(13) 0.0167(11) 0.0294(14) 0.0008(9) -0.0022(10) 0.0003(9) O4 0.0266(12) 0.0169(11) 0.0167(12) 0.0027(9) 0.0000(9) 0.0024(9) C11 0.0138(13) 0.0161(12) 0.0146(14) -0.0019(10) 0.0031(10) 0.0009(10) C12 0.0224(15) 0.0191(13) 0.0132(15) -0.0028(11) 0.0052(11) -0.0023(11) C13 0.0184(15) 0.0165(13) 0.018(2) -0.0005(11) 0.0042(12) 0.0003(11) C14 0.0172(14) 0.0144(13) 0.0159(15) -0.0038(11) 0.0041(11) 0.0029(11) C15 0.0199(15) 0.0188(13) 0.0152(15) -0.0021(11) 0.0053(11) -0.0007(11) C16 0.0152(14) 0.0157(13) 0.020(2) -0.0014(11) 0.0046(12) -0.0011(11) C21 0.0131(13) 0.0175(13) 0.0174(15) -0.0021(11) 0.0046(11) 0.0017(10) C22 0.0200(15) 0.0179(13) 0.017(2) -0.0006(11) 0.0048(12) 0.0007(11) C23 0.023(2) 0.0170(13) 0.018(2) 0.0003(11) 0.0062(12) -0.0014(11) C24 0.0155(14) 0.0177(14) 0.0139(15) -0.0018(11) 0.0021(11) -0.0006(11) C25 0.0178(14) 0.0183(13) 0.0152(15) 0.0001(11) 0.0057(11) -0.0008(11) C26 0.020(2) 0.0153(14) 0.015(2) -0.0009(12) -0.0002(13) 0.0022(11) C31 0.0151(12) 0.014(2) 0.0169(14) -0.0025(10) 0.0026(10) -0.0017(9) C32 0.0127(13) 0.0145(12) 0.020(2) -0.0018(10) 0.0038(11) -0.0019(9) C33 0.0191(15) 0.0241(15) 0.015(2) -0.0054(12) 0.0030(11) -0.0008(11) C34 0.0177(15) 0.0207(15) 0.020(2) -0.0086(12) 0.0053(12) -0.0052(11) C35 0.0162(14) 0.0171(13) 0.026(2) -0.0007(12) 0.0048(12) -0.0018(11) C36 0.0172(14) 0.0189(14) 0.0134(15) -0.0012(12) 0.0037(11) -0.0002(11) C37 0.028(2) 0.028(2) 0.016(2) 0.0012(12) 0.0041(13) 0.0030(13) C38 0.029(2) 0.0197(15) 0.024(2) 0.0048(13) 0.0003(15) -0.0028(13) C39 0.035(2) 0.0214(15) 0.024(2) -0.0074(13) 0.0101(14) -0.0031(13) C41 0.0159(13) 0.013(2) 0.0188(14) -0.0014(10) 0.0050(10) 0.0007(9) C42 0.0150(13) 0.0160(13) 0.0181(15) 0.0003(10) 0.0053(11) 0.0017(9) C43 0.0198(15) 0.0191(14) 0.018(2) -0.0007(11) 0.0027(12) -0.0005(11) C44 0.020(2) 0.0205(15) 0.020(2) -0.0083(12) 0.0050(12) -0.0013(11) C45 0.0189(15) 0.0164(13) 0.022(2) 0.0002(11) 0.0053(12) -0.0007(11) C46 0.0152(14) 0.0186(15) 0.015(2) -0.0017(12) 0.0032(11) -0.0007(11) C47 0.024(2) 0.025(2) 0.019(2) 0.0066(12) 0.0006(13) 0.0008(12) C48 0.027(2) 0.019(2) 0.030(2) 0.0061(15) 0.006(2) 0.0035(13) C49 0.031(2) 0.0194(14) 0.025(2) -0.0065(13) 0.0010(13) -0.0018(12) _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 Sb1 Cl6 2.3524(9) . ? Sb1 Cl4 2.3647(8) . ? Sb1 Cl1 2.3656(8) . ? Sb1 Cl3 2.3722(8) . ? Sb1 Cl5 2.3757(8) . ? Sb1 Cl2 2.3769(8) . ? O1 C32 1.325(3) . ? O1 C37 1.454(4) . ? O2 C35 1.324(4) . ? O2 C38 1.448(4) . ? O3 C45 1.385(4) . ? O3 C48 1.419(4) . ? O4 C42 1.370(3) . ? O4 C47 1.440(4) . ? C11 C12 1.403(4) . ? C11 C16 1.407(4) . ? C11 C21 1.485(4) . ? C12 C13 1.383(4) . ? C13 C14 1.397(4) . ? C14 C15 1.407(4) . ? C14 C31 1.469(4) . ? C15 C16 1.380(4) . ? C21 C26 1.400(5) . ? C21 C22 1.404(4) . ? C22 C23 1.380(4) . ? C23 C24 1.396(4) . ? C24 C25 1.406(4) . ? C24 C41 1.488(4) . ? C25 C26 1.392(4) . ? C31 C36 1.383(4) . ? C31 C32 1.446(4) . ? C32 C33 1.411(4) . ? C33 C34 1.371(4) . ? C34 C35 1.435(5) . ? C34 C39 1.497(4) . ? C35 C36 1.401(4) . ? C41 C42 1.410(4) . ? C41 C46 1.410(4) . ? C42 C43 1.392(4) . ? C43 C44 1.393(4) . ? C44 C45 1.396(5) . ? C44 C49 1.501(4) . ? C45 C46 1.392(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 Cl6 Sb1 Cl4 177.46(4) . . ? Cl6 Sb1 Cl1 90.27(3) . . ? Cl4 Sb1 Cl1 90.72(3) . . ? Cl6 Sb1 Cl3 90.80(3) . . ? Cl4 Sb1 Cl3 91.56(3) . . ? Cl1 Sb1 Cl3 89.11(3) . . ? Cl6 Sb1 Cl5 89.05(3) . . ? Cl4 Sb1 Cl5 88.59(3) . . ? Cl1 Sb1 Cl5 91.07(3) . . ? Cl3 Sb1 Cl5 179.77(4) . . ? Cl6 Sb1 Cl2 89.88(3) . . ? Cl4 Sb1 Cl2 89.21(3) . . ? Cl1 Sb1 Cl2 178.08(3) . . ? Cl3 Sb1 Cl2 88.97(3) . . ? Cl5 Sb1 Cl2 90.85(3) . . ? C32 O1 C37 119.6(2) . . ? C35 O2 C38 118.3(2) . . ? C45 O3 C48 118.1(2) . . ? C42 O4 C47 117.8(2) . . ? C12 C11 C16 117.2(3) . . ? C12 C11 C21 121.6(3) . . ? C16 C11 C21 121.2(3) . . ? C13 C12 C11 121.0(3) . . ? C12 C13 C14 121.6(3) . . ? C13 C14 C15 117.8(3) . . ? C13 C14 C31 119.9(3) . . ? C15 C14 C31 122.3(3) . . ? C16 C15 C14 120.5(3) . . ? C15 C16 C11 121.9(3) . . ? C26 C21 C22 116.7(3) . . ? C26 C21 C11 122.1(3) . . ? C22 C21 C11 121.1(3) . . ? C23 C22 C21 121.3(3) . . ? C22 C23 C24 122.1(3) . . ? C23 C24 C25 117.3(3) . . ? C23 C24 C41 119.4(3) . . ? C25 C24 C41 123.3(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C21 122.2(3) . . ? C36 C31 C32 117.4(2) . . ? C36 C31 C14 119.9(3) . . ? C32 C31 C14 122.7(2) . . ? O1 C32 C33 123.4(3) . . ? O1 C32 C31 115.8(2) . . ? C33 C32 C31 120.8(2) . . ? C34 C33 C32 121.1(3) . . ? C33 C34 C35 118.2(3) . . ? C33 C34 C39 122.6(3) . . ? C35 C34 C39 119.2(3) . . ? O2 C35 C36 124.2(3) . . ? O2 C35 C34 114.7(3) . . ? C36 C35 C34 121.1(3) . . ? C31 C36 C35 121.3(3) . . ? C42 C41 C46 117.4(2) . . ? C42 C41 C24 124.1(2) . . ? C46 C41 C24 118.4(3) . . ? O4 C42 C43 121.8(3) . . ? O4 C42 C41 117.8(2) . . ? C43 C42 C41 120.3(2) . . ? C42 C43 C44 122.1(3) . . ? C43 C44 C45 117.8(3) . . ? C43 C44 C49 121.7(3) . . ? C45 C44 C49 120.5(3) . . ? O3 C45 C46 123.2(3) . . ? O3 C45 C44 115.8(3) . . ? C46 C45 C44 121.0(3) . . ? C45 C46 C41 121.4(3) . . ? _refine_diff_density_max 0.902 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.129 data_sunisx _database_code_CSD 162403 _audit_creation_method SHELXL _chemical_name_systematic ; 2,2",5,5"-tetramethoxy-4,2',3',5',6',4"-hexamethylterphenyl ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H34 O4' _chemical_formula_weight 434.55 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.0278(10) _cell_length_b 7.3676(3) _cell_length_c 14.2868(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.8830(10) _cell_angle_gamma 90.00 _cell_volume 2310.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7341 _cell_measurement_theta_min 2 _cell_measurement_theta_max 35 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method none _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.962 _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16277 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 35.59 _reflns_number_total 5036 _reflns_number_observed 3995 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 20 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+0.0000P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5016 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_obs 0.0399 _refine_ls_wR_factor_all 0.1393 _refine_ls_wR_factor_obs 0.1161 _refine_ls_goodness_of_fit_all 1.019 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.154 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/esd_max -0.095 _refine_ls_shift/esd_mean 0.008 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 O1 O 0.07383(2) 0.31521(8) 0.22258(4) 0.02148(12) Uani 1 d . . O2 O 0.28370(2) 0.49588(7) 0.05682(4) 0.01833(11) Uani 1 d . . C1 C 0.05787(3) 0.46663(9) 0.04495(4) 0.01459(11) Uani 1 d . . C2 C 0.02555(3) 0.62288(9) 0.06780(4) 0.01606(12) Uani 1 d . . C3 C 0.03243(3) 0.34343(9) -0.02255(5) 0.01640(12) Uani 1 d . . C4 C 0.05320(4) 0.75318(11) 0.14123(6) 0.0252(2) Uani 1 d . . C5 C 0.06719(3) 0.17569(11) -0.04776(7) 0.0269(2) Uani 1 d . . C11 C 0.11992(3) 0.43290(9) 0.09316(4) 0.01444(11) Uani 1 d . . C12 C 0.12672(3) 0.35698(9) 0.18342(4) 0.01474(11) Uani 1 d . . C13 C 0.18493(3) 0.32616(8) 0.22774(4) 0.01387(11) Uani 1 d . . C14 C 0.23730(3) 0.37015(8) 0.18391(4) 0.01251(11) Uani 1 d . . C15 C 0.23029(3) 0.44926(8) 0.09459(4) 0.01316(11) Uani 1 d . . C16 C 0.17244(3) 0.47847(9) 0.04979(4) 0.01494(12) Uani 1 d . . C17 C 0.07792(4) 0.27151(13) 0.31989(5) 0.0262(2) Uani 1 d . . C18 C 0.29982(3) 0.32872(9) 0.22961(5) 0.01580(12) Uani 1 d . . C19 C 0.28015(3) 0.53588(9) -0.04117(5) 0.01802(13) Uani 1 d . . H4A H 0.0454(13) 0.6888(33) 0.2074(19) 0.031(6) Uiso 0.50 d P . H4B H 0.0324(11) 0.8753(30) 0.1463(18) 0.020(5) Uiso 0.50 d P . H4C H 0.0994(13) 0.7649(39) 0.1334(20) 0.038(7) Uiso 0.50 d P . H4D H 0.0243(13) 0.8010(41) 0.1841(21) 0.040(7) Uiso 0.50 d P . H4E H 0.0571(15) 0.8819(40) 0.1142(22) 0.048(8) Uiso 0.50 d P . H4F H 0.0861(14) 0.6975(38) 0.1729(22) 0.043(7) Uiso 0.50 d P . H5A H 0.0453(6) 0.0694(18) -0.0341(9) 0.037(3) Uiso 1 d . . H5B H 0.0749(7) 0.1727(18) -0.1174(11) 0.051(4) Uiso 1 d . . H5C H 0.1060(7) 0.1709(18) -0.0158(11) 0.049(4) Uiso 1 d . . H13 H 0.1892(5) 0.2685(14) 0.2912(8) 0.021(2) Uiso 1 d . . H16 H 0.1664(5) 0.5329(14) -0.0171(8) 0.025(3) Uiso 1 d . . H17A H 0.0372(6) 0.2605(16) 0.3363(10) 0.038(3) Uiso 1 d . . H17B H 0.0976(6) 0.3721(18) 0.3531(10) 0.046(4) Uiso 1 d . . H17C H 0.1008(6) 0.1615(17) 0.3351(9) 0.042(3) Uiso 1 d . . H18A H 0.2963(5) 0.2547(15) 0.2857(8) 0.025(3) Uiso 1 d . . H18B H 0.3222(6) 0.4413(17) 0.2486(9) 0.036(3) Uiso 1 d . . H18C H 0.3251(6) 0.2662(17) 0.1859(9) 0.035(3) Uiso 1 d . . H19A H 0.2548(5) 0.6455(14) -0.0559(8) 0.024(2) Uiso 1 d . . H19B H 0.2617(6) 0.4338(16) -0.0780(9) 0.032(3) Uiso 1 d . . H19C H 0.3236(6) 0.5514(16) -0.0543(8) 0.029(3) Uiso 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 O1 0.0100(2) 0.0379(3) 0.0166(2) 0.0058(2) 0.0015(2) -0.0032(2) O2 0.0095(2) 0.0297(2) 0.0159(2) 0.0058(2) 0.0013(2) 0.0001(2) C1 0.0079(2) 0.0220(3) 0.0135(2) 0.0009(2) -0.0009(2) 0.0006(2) C2 0.0095(2) 0.0232(3) 0.0151(2) -0.0021(2) -0.0013(2) 0.0006(2) C3 0.0092(2) 0.0218(3) 0.0178(3) -0.0015(2) -0.0010(2) 0.0016(2) C4 0.0151(3) 0.0334(4) 0.0260(3) -0.0123(3) -0.0053(3) 0.0024(3) C5 0.0141(3) 0.0269(3) 0.0385(4) -0.0108(3) -0.0049(3) 0.0057(2) C11 0.0086(2) 0.0207(3) 0.0136(2) 0.0008(2) -0.0014(2) 0.0009(2) C12 0.0089(2) 0.0208(3) 0.0144(2) 0.0013(2) 0.0004(2) -0.0009(2) C13 0.0104(2) 0.0176(2) 0.0133(2) 0.0009(2) -0.0006(2) 0.0002(2) C14 0.0093(2) 0.0148(2) 0.0131(2) -0.0001(2) -0.0011(2) 0.0010(2) C15 0.0084(2) 0.0172(2) 0.0137(2) 0.0009(2) 0.0000(2) 0.0007(2) C16 0.0095(2) 0.0211(3) 0.0140(2) 0.0023(2) -0.0007(2) 0.0011(2) C17 0.0158(3) 0.0446(4) 0.0189(3) 0.0097(3) 0.0047(2) 0.0033(3) C18 0.0100(2) 0.0198(3) 0.0170(3) 0.0025(2) -0.0020(2) 0.0014(2) C19 0.0167(3) 0.0224(3) 0.0155(3) 0.0024(2) 0.0041(2) 0.0023(2) _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 O1 C12 1.3698(8) . ? O1 C17 1.4225(9) . ? O2 C15 1.3788(8) . ? O2 C19 1.4262(8) . ? C1 C3 1.4057(9) . ? C1 C2 1.4064(9) . ? C1 C11 1.4981(9) . ? C2 C3 1.4037(9) 5_565 ? C2 C4 1.5113(9) . ? C3 C2 1.4036(9) 5_565 ? C3 C5 1.5133(10) . ? C4 H4A 1.08(3) . ? C4 H4B 1.01(2) . ? C4 H4C 1.04(3) . ? C4 H4D 0.99(3) . ? C4 H4E 1.03(3) . ? C4 H4F 0.92(3) . ? C5 H5A 0.948(13) . ? C5 H5B 1.02(2) . ? C5 H5C 0.93(2) . ? C11 C16 1.3989(9) . ? C11 C12 1.4018(8) . ? C12 C13 1.3995(8) . ? C13 C14 1.3966(8) . ? C13 H13 0.998(11) . ? C14 C15 1.3996(8) . ? C14 C18 1.5044(8) . ? C15 C16 1.3933(8) . ? C16 H16 1.035(11) . ? C17 H17A 0.950(13) . ? C17 H17B 0.963(14) . ? C17 H17C 0.969(13) . ? C18 H18A 0.978(11) . ? C18 H18B 0.990(13) . ? C18 H18C 0.986(12) . ? C19 H19A 0.993(11) . ? C19 H19B 0.985(12) . ? C19 H19C 0.998(12) . ? 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 C12 O1 C17 117.69(5) . . ? C15 O2 C19 117.28(5) . . ? C3 C1 C2 120.51(6) . . ? C3 C1 C11 120.21(5) . . ? C2 C1 C11 119.28(5) . . ? C3 C2 C1 119.77(6) 5_565 . ? C3 C2 C4 120.29(6) 5_565 . ? C1 C2 C4 119.94(6) . . ? C2 C3 C1 119.72(6) 5_565 . ? C2 C3 C5 119.59(6) 5_565 . ? C1 C3 C5 120.69(6) . . ? C2 C4 H4A 104.0(13) . . ? C2 C4 H4B 117.1(13) . . ? H4A C4 H4B 102.6(19) . . ? C2 C4 H4C 108.6(14) . . ? H4A C4 H4C 111.2(20) . . ? H4B C4 H4C 112.8(21) . . ? C2 C4 H4D 114.5(16) . . ? H4A C4 H4D 57.0(19) . . ? H4B C4 H4D 47.1(17) . . ? H4C C4 H4D 136.9(21) . . ? C2 C4 H4E 111.5(17) . . ? H4A C4 H4E 138.9(21) . . ? H4B C4 H4E 42.6(17) . . ? H4C C4 H4E 76.6(23) . . ? H4D C4 H4E 89.0(22) . . ? C2 C4 H4F 108.3(17) . . ? H4A C4 H4F 63.4(20) . . ? H4B C4 H4F 134.6(21) . . ? H4C C4 H4F 49.4(19) . . ? H4D C4 H4F 112.2(25) . . ? H4E C4 H4F 120.5(25) . . ? C3 C5 H5A 110.5(8) . . ? C3 C5 H5B 112.2(8) . . ? H5A C5 H5B 108.1(11) . . ? C3 C5 H5C 112.0(8) . . ? H5A C5 H5C 109.1(11) . . ? H5B C5 H5C 104.7(12) . . ? C16 C11 C12 118.39(5) . . ? C16 C11 C1 120.87(5) . . ? C12 C11 C1 120.73(5) . . ? O1 C12 C13 123.86(6) . . ? O1 C12 C11 115.94(5) . . ? C13 C12 C11 120.20(6) . . ? C14 C13 C12 121.29(6) . . ? C14 C13 H13 119.2(6) . . ? C12 C13 H13 119.5(6) . . ? C13 C14 C15 118.32(5) . . ? C13 C14 C18 121.26(5) . . ? C15 C14 C18 120.40(5) . . ? O2 C15 C16 124.01(5) . . ? O2 C15 C14 115.41(5) . . ? C16 C15 C14 120.58(5) . . ? C15 C16 C11 121.20(6) . . ? C15 C16 H16 121.6(6) . . ? C11 C16 H16 117.2(6) . . ? O1 C17 H17A 106.1(8) . . ? O1 C17 H17B 107.2(8) . . ? H17A C17 H17B 109.9(11) . . ? O1 C17 H17C 113.4(8) . . ? H17A C17 H17C 111.0(11) . . ? H17B C17 H17C 109.2(11) . . ? C14 C18 H18A 109.6(7) . . ? C14 C18 H18B 111.3(8) . . ? H18A C18 H18B 108.3(10) . . ? C14 C18 H18C 111.5(7) . . ? H18A C18 H18C 110.3(10) . . ? H18B C18 H18C 105.7(11) . . ? O2 C19 H19A 111.0(6) . . ? O2 C19 H19B 110.6(7) . . ? H19A C19 H19B 108.0(10) . . ? O2 C19 H19C 103.6(7) . . ? H19A C19 H19C 113.4(9) . . ? H19B C19 H19C 110.2(10) . . ? _refine_diff_density_max 0.546 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.057 data_sungsy _database_code_CSD 162404 _audit_creation_method SHELXL _chemical_name_systematic ; 2,7-Bis(2',5'-dimethoxy-4'-methylphenyl)-9,9-dimethylfluorene hexachloroantimonate dichlormethane solvate ; _chemical_name_common ? _chemical_formula_moiety ; (C33 H34 O4)^+^, (Cl6 Sb)^-^, 1.76(C H2 Cl2) ; _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34.76 H37.53 Cl9.53 O4 Sb' _chemical_formula_weight 978.95 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' 'O' 'O' 0.0106 0.0060 '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' 'Sb' 'Sb' -0.5866 1.5461 '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 13.1454(2) _cell_length_b 13.4568(3) _cell_length_c 14.1244(3) _cell_angle_alpha 103.3750(10) _cell_angle_beta 101.8580(10) _cell_angle_gamma 116.0560(10) _cell_volume 2044.47(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5755 _cell_measurement_theta_min 2 _cell_measurement_theta_max 35 _exptl_crystal_description 'prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method none _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 1.334 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 0.863 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; \w-scan, frame range 0.3 deg, hemisphere ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32329 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 35.60 _reflns_number_total 16881 _reflns_number_observed 11957 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART V4.050 (Siemens, 1989-95)' _computing_cell_refinement 'SAINT V4.050 (Siemens, 1989-95)' _computing_data_reduction 'SAINT & SADABS V2.03 (Sheldrick, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP V5.06 (Siemens, 1996)' _computing_publication_material 'SHELXL-93 & XCIF V5.05 (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for all reflections except for 11 with very negative F^2^ or flagged by us for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+2.7409P] 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 ; riding and rotating model with Uiso=1.2Uiso/eq of an adjacent atom (1.5Uiso/eq for Me-hydrogens) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16870 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_obs 0.0435 _refine_ls_wR_factor_all 0.1029 _refine_ls_wR_factor_obs 0.0894 _refine_ls_goodness_of_fit_all 1.008 _refine_ls_goodness_of_fit_obs 1.054 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.054 _refine_ls_shift/esd_max 0.012 _refine_ls_shift/esd_mean 0.001 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 Sb1 Sb 0.5000 0.5000 0.0000 0.01691(5) Uani 1 d S . Sb2 Sb -0.5000 -0.5000 -0.5000 0.02312(5) Uani 1 d S . Cl1 Cl 0.40662(6) 0.53029(7) 0.12092(5) 0.03488(15) Uani 1 d . . Cl2 Cl 0.57186(8) 0.69933(7) 0.01167(9) 0.0415(3) Uani 0.869(2) d P . Cl2A Cl 0.5086(5) 0.6570(5) -0.0533(5) 0.0323(12) Uiso 0.131(2) d P . Cl3 Cl 0.67662(7) 0.56232(8) 0.13991(6) 0.0349(2) Uani 0.869(2) d P . Cl3A Cl 0.7031(5) 0.6264(5) 0.1160(4) 0.0339(13) Uiso 0.131(2) d P . Cl4 Cl -0.58355(6) -0.37730(5) -0.51913(6) 0.03416(15) Uani 1 d . . Cl5 Cl -0.69838(6) -0.66710(6) -0.57118(7) 0.0425(2) Uani 1 d . . Cl6 Cl -0.49003(9) -0.52726(8) -0.66801(6) 0.0487(2) Uani 1 d . . O32 O 0.29297(15) 0.97226(14) 0.35052(14) 0.0259(4) Uani 1 d . . O35 O 0.68737(15) 0.9167(2) 0.38036(14) 0.0269(4) Uani 1 d . . O42 O -0.2378(2) -0.0099(2) -0.0949(2) 0.0299(4) Uani 1 d . . O45 O -0.70779(15) -0.1044(2) -0.19117(14) 0.0266(4) Uani 1 d . . C11 C 0.0150(2) 0.5415(2) 0.1356(2) 0.0198(4) Uani 1 d . . C12 C 0.1053(2) 0.5259(2) 0.1936(2) 0.0201(4) Uani 1 d . . C13 C 0.2191(2) 0.6231(2) 0.2523(2) 0.0200(4) Uani 1 d . . H13A H 0.2799(2) 0.6130(2) 0.2907(2) 0.024 Uiso 1 calc R . C14 C 0.2452(2) 0.7389(2) 0.2551(2) 0.0195(4) Uani 1 d . . C15 C 0.1519(2) 0.7513(2) 0.1968(2) 0.0206(4) Uani 1 d . . H15A H 0.1684(2) 0.8280(2) 0.1987(2) 0.025 Uiso 1 calc R . C16 C 0.0389(2) 0.6546(2) 0.1381(2) 0.0209(4) Uani 1 d . . H16A H -0.0224(2) 0.6641(2) 0.0997(2) 0.025 Uiso 1 calc R . C17 C 0.0540(2) 0.3945(2) 0.1790(2) 0.0216(4) Uani 1 d . . C18 C 0.1299(2) 0.3446(2) 0.1424(2) 0.0279(5) Uani 1 d . . H18A H 0.1378(16) 0.3566(17) 0.0779(9) 0.042 Uiso 1 calc R . H18B H 0.0901(10) 0.2594(4) 0.1300(16) 0.042 Uiso 1 calc R . H18C H 0.2104(7) 0.3858(13) 0.1960(7) 0.042 Uiso 1 calc R . C19 C 0.0414(2) 0.3760(2) 0.2810(2) 0.0312(5) Uani 1 d . . H19A H -0.0085(17) 0.4066(18) 0.3033(9) 0.047 Uiso 1 calc R . H19B H 0.1216(3) 0.4186(16) 0.3351(5) 0.047 Uiso 1 calc R . H19C H 0.0029(18) 0.2910(3) 0.2692(5) 0.047 Uiso 1 calc R . C21 C -0.0924(2) 0.4278(2) 0.0779(2) 0.0190(4) Uani 1 d . . C22 C -0.0713(2) 0.3381(2) 0.0966(2) 0.0191(4) Uani 1 d . . C23 C -0.1591(2) 0.2195(2) 0.0442(2) 0.0201(4) Uani 1 d . . H23A H -0.1442(2) 0.1594(2) 0.0556(2) 0.024 Uiso 1 calc R . C24 C -0.2717(2) 0.1879(2) -0.0269(2) 0.0189(4) Uani 1 d . . C25 C -0.2916(2) 0.2805(2) -0.0405(2) 0.0194(4) Uani 1 d . . H25A H -0.3678(2) 0.2600(2) -0.0859(2) 0.023 Uiso 1 calc R . C26 C -0.2036(2) 0.3989(2) 0.0102(2) 0.0196(4) Uani 1 d . . H26A H -0.2181(2) 0.4593(2) -0.0007(2) 0.024 Uiso 1 calc R . C31 C 0.3674(2) 0.8419(2) 0.3110(2) 0.0183(4) Uani 1 d . . C32 C 0.3901(2) 0.9603(2) 0.3525(2) 0.0204(4) Uani 1 d . . C33 C 0.5088(2) 1.0570(2) 0.3973(2) 0.0218(4) Uani 1 d . . H33A H 0.5220(2) 1.1351(2) 0.4224(2) 0.026 Uiso 1 calc R . C34 C 0.6073(2) 1.0420(2) 0.4060(2) 0.0224(4) Uani 1 d . . C35 C 0.5854(2) 0.9239(2) 0.3680(2) 0.0215(4) Uani 1 d . . C36 C 0.4687(2) 0.8275(2) 0.3221(2) 0.0204(4) Uani 1 d . . H36A H 0.4565(2) 0.7497(2) 0.2974(2) 0.025 Uiso 1 calc R . C37 C 0.3115(2) 1.0902(2) 0.3824(2) 0.0273(5) Uani 1 d . . H37A H 0.2333(3) 1.0855(2) 0.3725(15) 0.041 Uiso 1 calc R . H37B H 0.3511(16) 1.1319(6) 0.3405(11) 0.041 Uiso 1 calc R . H37C H 0.3629(15) 1.1336(6) 0.4559(5) 0.041 Uiso 1 calc R . C38 C 0.7344(2) 1.1460(2) 0.4548(2) 0.0304(5) Uani 1 d . . H38A H 0.7329(2) 1.2194(3) 0.4805(15) 0.046 Uiso 1 calc R . H38B H 0.7740(7) 1.1505(11) 0.4029(5) 0.046 Uiso 1 calc R . H38C H 0.7794(6) 1.1361(9) 0.5129(10) 0.046 Uiso 1 calc R . C39 C 0.6714(3) 0.8004(3) 0.3427(2) 0.0347(6) Uani 1 d . . H39A H 0.7505(3) 0.8064(3) 0.3613(15) 0.052 Uiso 1 calc R . H39B H 0.6319(18) 0.7653(8) 0.2669(3) 0.052 Uiso 1 calc R . H39C H 0.6209(17) 0.7500(6) 0.3740(13) 0.052 Uiso 1 calc R . C41 C -0.3711(2) 0.0643(2) -0.0847(2) 0.0201(4) Uani 1 d . . C42 C -0.3539(2) -0.0342(2) -0.1159(2) 0.0223(4) Uani 1 d . . C43 C -0.4533(2) -0.1498(2) -0.1679(2) 0.0249(5) Uani 1 d . . H43A H -0.4400(2) -0.2143(2) -0.1873(2) 0.030 Uiso 1 calc R . C44 C -0.5713(2) -0.1723(2) -0.1920(2) 0.0239(4) Uani 1 d . . C45 C -0.5894(2) -0.0751(2) -0.1640(2) 0.0219(4) Uani 1 d . . C46 C -0.4917(2) 0.0398(2) -0.1109(2) 0.0207(4) Uani 1 d . . H46A H -0.5061(2) 0.1036(2) -0.0916(2) 0.025 Uiso 1 calc R . C47 C -0.2173(3) -0.1080(2) -0.1145(2) 0.0331(6) Uani 1 d . . H47A H -0.1301(3) -0.0777(2) -0.0913(16) 0.050 Uiso 1 calc R . H47B H -0.2539(17) -0.1554(11) -0.1891(3) 0.050 Uiso 1 calc R . H47C H -0.2539(17) -0.1578(11) -0.0764(14) 0.050 Uiso 1 calc R . C48 C -0.6776(2) -0.2972(2) -0.2457(2) 0.0341(6) Uani 1 d . . H48A H -0.6486(3) -0.3527(3) -0.2609(16) 0.051 Uiso 1 calc R . H48B H -0.7287(11) -0.3037(6) -0.3108(9) 0.051 Uiso 1 calc R . H48C H -0.7249(12) -0.3166(7) -0.2005(7) 0.051 Uiso 1 calc R . C49 C -0.7315(2) -0.0091(2) -0.1680(2) 0.0299(5) Uani 1 d . . H49A H -0.8190(2) -0.0414(3) -0.1928(15) 0.045 Uiso 1 calc R . H49B H -0.6940(16) 0.0450(10) -0.2025(13) 0.045 Uiso 1 calc R . H49C H -0.6977(17) 0.0343(12) -0.0926(3) 0.045 Uiso 1 calc R . Cl1X Cl 1.04927(15) 1.11900(14) 0.86716(13) 0.0728(5) Uani 0.797(3) d P . Cl2X Cl 1.01678(12) 0.99952(14) 0.65436(14) 0.0769(5) Uani 0.797(3) d P . C1X C 1.0530(7) 1.1321(6) 0.7485(6) 0.092(2) Uani 0.797(3) d P . H1XA H 1.1349(7) 1.1953(6) 0.7584(6) 0.110 Uiso 0.797(3) calc PR . H1XB H 0.9951(7) 1.1566(6) 0.7231(6) 0.110 Uiso 0.797(3) calc PR . Cl3X Cl 1.0618(2) 1.3936(2) 0.6583(2) 0.0606(7) Uani 0.481(4) d P 1 Cl4X Cl 1.0501(2) 1.2090(3) 0.4984(4) 0.0903(11) Uani 0.481(4) d P 1 C2X C 1.1280(9) 1.3762(8) 0.5703(8) 0.057(2) Uiso 0.481(4) d P 1 H2XA H 1.2157(9) 1.4105(8) 0.6054(8) 0.069 Uiso 0.481(4) calc PR 1 H2XB H 1.1168(9) 1.4158(8) 0.5215(8) 0.069 Uiso 0.481(4) calc PR 1 Cl3Y Cl 1.0463(3) 1.4346(3) 0.5417(3) 0.123(2) Uani 0.490(4) d P 2 Cl4Y Cl 1.0504(3) 1.2339(3) 0.5828(6) 0.180(3) Uani 0.490(4) d P 2 C2Y C 1.1243(18) 1.3845(17) 0.6177(15) 0.136(7) Uiso 0.490(4) d P 2 H2YA H 1.2050(18) 1.4120(17) 0.6113(15) 0.163 Uiso 0.490(4) calc PR 2 H2YB H 1.1368(18) 1.4211(17) 0.6916(15) 0.163 Uiso 0.490(4) calc PR 2 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 Sb1 0.01559(9) 0.01659(9) 0.01740(10) 0.00640(8) 0.00406(7) 0.00797(8) Sb2 0.02816(11) 0.01581(9) 0.01896(11) 0.00398(8) -0.00227(8) 0.01179(9) Cl1 0.0366(3) 0.0607(4) 0.0264(3) 0.0210(3) 0.0166(3) 0.0353(3) Cl2 0.0429(5) 0.0232(3) 0.0679(7) 0.0237(4) 0.0278(5) 0.0173(4) Cl3 0.0260(3) 0.0522(5) 0.0222(3) 0.0051(3) 0.0010(3) 0.0239(4) Cl4 0.0327(3) 0.0198(3) 0.0401(4) 0.0064(2) -0.0045(3) 0.0151(2) Cl5 0.0295(3) 0.0200(3) 0.0622(5) 0.0088(3) -0.0024(3) 0.0110(2) Cl6 0.0735(6) 0.0588(5) 0.0259(3) 0.0183(3) 0.0160(4) 0.0428(5) O32 0.0201(7) 0.0156(7) 0.0330(10) 0.0002(7) 0.0053(7) 0.0080(6) O35 0.0187(7) 0.0296(9) 0.0302(9) 0.0090(7) 0.0076(7) 0.0118(7) O42 0.0236(8) 0.0203(8) 0.0396(11) 0.0048(7) 0.0063(8) 0.0113(7) O45 0.0187(7) 0.0194(8) 0.0311(10) 0.0064(7) 0.0068(7) 0.0035(6) C11 0.0185(9) 0.0154(9) 0.0206(10) 0.0058(8) 0.0009(8) 0.0077(8) C12 0.0196(9) 0.0153(9) 0.0191(10) 0.0050(8) 0.0003(8) 0.0073(8) C13 0.0181(9) 0.0162(9) 0.0186(10) 0.0045(8) 0.0003(8) 0.0066(8) C14 0.0183(9) 0.0144(9) 0.0194(10) 0.0036(8) 0.0019(8) 0.0065(8) C15 0.0203(9) 0.0139(9) 0.0223(11) 0.0042(8) 0.0033(8) 0.0074(8) C16 0.0190(9) 0.0152(9) 0.0231(11) 0.0053(8) 0.0007(8) 0.0082(8) C17 0.0197(9) 0.0160(9) 0.0224(11) 0.0075(8) -0.0017(8) 0.0075(8) C18 0.0216(10) 0.0186(10) 0.0354(14) 0.0079(10) 0.0002(10) 0.0089(9) C19 0.0307(12) 0.0279(12) 0.0263(13) 0.0141(10) 0.0013(10) 0.0098(10) C21 0.0176(9) 0.0146(8) 0.0200(10) 0.0058(8) 0.0014(8) 0.0067(8) C22 0.0184(9) 0.0157(9) 0.0193(10) 0.0072(8) 0.0022(8) 0.0070(8) C23 0.0203(9) 0.0155(9) 0.0217(10) 0.0088(8) 0.0039(8) 0.0075(8) C24 0.0176(9) 0.0142(9) 0.0191(10) 0.0051(8) 0.0041(8) 0.0051(8) C25 0.0154(9) 0.0162(9) 0.0205(10) 0.0051(8) 0.0023(8) 0.0056(8) C26 0.0183(9) 0.0158(9) 0.0218(10) 0.0068(8) 0.0036(8) 0.0079(8) C31 0.0177(9) 0.0149(9) 0.0168(9) 0.0040(7) 0.0022(7) 0.0064(8) C32 0.0185(9) 0.0165(9) 0.0202(10) 0.0038(8) 0.0039(8) 0.0067(8) C33 0.0213(10) 0.0152(9) 0.0208(11) 0.0035(8) 0.0038(8) 0.0059(8) C34 0.0192(10) 0.0209(10) 0.0186(10) 0.0059(8) 0.0038(8) 0.0052(9) C35 0.0185(9) 0.0240(11) 0.0192(10) 0.0077(9) 0.0047(8) 0.0095(9) C36 0.0194(10) 0.0177(9) 0.0181(10) 0.0036(8) 0.0024(8) 0.0079(8) C37 0.0269(11) 0.0176(10) 0.0316(13) 0.0024(9) 0.0062(10) 0.0117(9) C38 0.0201(11) 0.0253(12) 0.0311(14) 0.0059(10) 0.0042(10) 0.0040(10) C39 0.0292(13) 0.0368(14) 0.039(2) 0.0075(12) 0.0100(11) 0.0213(12) C41 0.0196(9) 0.0149(9) 0.0213(11) 0.0061(8) 0.0053(8) 0.0063(8) C42 0.0208(10) 0.0175(9) 0.0254(11) 0.0081(9) 0.0072(9) 0.0074(8) C43 0.0279(11) 0.0138(9) 0.0270(12) 0.0059(9) 0.0087(9) 0.0070(9) C44 0.0233(10) 0.0165(9) 0.0231(11) 0.0057(8) 0.0075(9) 0.0042(9) C45 0.0192(9) 0.0178(10) 0.0209(11) 0.0061(8) 0.0056(8) 0.0042(8) C46 0.0195(10) 0.0174(9) 0.0194(11) 0.0065(8) 0.0055(8) 0.0054(8) C47 0.0326(13) 0.0260(12) 0.042(2) 0.0106(11) 0.0092(12) 0.0184(11) C48 0.0284(12) 0.0162(10) 0.042(2) 0.0035(10) 0.0091(11) 0.0038(10) C49 0.0232(11) 0.0269(12) 0.0370(15) 0.0119(11) 0.0103(10) 0.0106(10) Cl1X 0.0864(10) 0.0676(9) 0.0941(12) 0.0474(8) 0.0438(9) 0.0491(8) Cl2X 0.0420(6) 0.0723(10) 0.1007(12) 0.0131(8) 0.0208(7) 0.0275(7) C1X 0.136(6) 0.069(4) 0.121(6) 0.052(4) 0.098(5) 0.061(4) Cl3X 0.0437(10) 0.0730(15) 0.0548(13) 0.0217(10) 0.0250(9) 0.0192(10) Cl4X 0.0440(13) 0.074(2) 0.143(3) 0.030(2) 0.036(2) 0.0256(13) Cl3Y 0.093(2) 0.114(3) 0.081(2) -0.030(2) 0.012(2) 0.027(2) Cl4Y 0.054(2) 0.086(2) 0.277(7) -0.059(3) -0.048(3) 0.045(2) _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 Sb1 Cl1 2.3599(6) . ? Sb1 Cl1 2.3599(6) 2_665 ? Sb1 Cl2A 2.367(5) . ? Sb1 Cl2A 2.367(5) 2_665 ? Sb1 Cl2 2.3706(7) . ? Sb1 Cl2 2.3707(7) 2_665 ? Sb1 Cl3A 2.372(5) 2_665 ? Sb1 Cl3A 2.372(5) . ? Sb1 Cl3 2.3740(7) 2_665 ? Sb1 Cl3 2.3741(7) . ? Sb2 Cl6 2.3559(8) 2_444 ? Sb2 Cl6 2.3560(8) . ? Sb2 Cl5 2.3649(7) . ? Sb2 Cl5 2.3649(7) 2_444 ? Sb2 Cl4 2.3839(6) . ? Sb2 Cl4 2.3840(6) 2_444 ? Cl2 Cl2A 0.942(6) . ? Cl3 Cl3A 0.948(6) . ? O32 C32 1.351(3) . ? O32 C37 1.437(3) . ? O35 C35 1.365(3) . ? O35 C39 1.435(3) . ? O42 C42 1.362(3) . ? O42 C47 1.438(3) . ? O45 C45 1.368(3) . ? O45 C49 1.431(3) . ? C11 C16 1.402(3) . ? C11 C12 1.422(3) . ? C11 C21 1.432(3) . ? C12 C13 1.380(3) . ? C12 C17 1.534(3) . ? C13 C14 1.429(3) . ? C14 C15 1.428(3) . ? C14 C31 1.464(3) . ? C15 C16 1.373(3) . ? C17 C22 1.533(3) . ? C17 C18 1.534(3) . ? C17 C19 1.546(3) . ? C21 C26 1.400(3) . ? C21 C22 1.420(3) . ? C22 C23 1.382(3) . ? C23 C24 1.422(3) . ? C24 C25 1.425(3) . ? C24 C41 1.471(3) . ? C25 C26 1.379(3) . ? C31 C36 1.411(3) . ? C31 C32 1.431(3) . ? C32 C33 1.399(3) . ? C33 C34 1.382(3) . ? C34 C35 1.427(3) . ? C34 C38 1.500(3) . ? C35 C36 1.382(3) . ? C41 C46 1.415(3) . ? C41 C42 1.427(3) . ? C42 C43 1.399(3) . ? C43 C44 1.391(3) . ? C44 C45 1.413(3) . ? C44 C48 1.505(3) . ? C45 C46 1.388(3) . ? Cl1X C1X 1.733(7) . ? Cl2X C1X 1.754(7) . ? Cl3X C2X 1.687(10) . ? Cl4X C2X 1.906(10) . ? Cl3Y C2Y 1.77(2) . ? Cl4Y C2Y 1.70(2) . ? 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 Cl1 Sb1 Cl1 180.0 . 2_665 ? Cl1 Sb1 Cl2A 94.50(13) . . ? Cl1 Sb1 Cl2A 85.51(13) 2_665 . ? Cl1 Sb1 Cl2A 85.51(13) . 2_665 ? Cl1 Sb1 Cl2A 94.49(13) 2_665 2_665 ? Cl2A Sb1 Cl2A 179.997(1) . 2_665 ? Cl1 Sb1 Cl2 88.70(3) . . ? Cl1 Sb1 Cl2 91.30(3) 2_665 . ? Cl2A Sb1 Cl2 22.92(14) . . ? Cl2A Sb1 Cl2 157.08(14) 2_665 . ? Cl1 Sb1 Cl2 91.30(3) . 2_665 ? Cl1 Sb1 Cl2 88.70(3) 2_665 2_665 ? Cl2A Sb1 Cl2 157.08(14) . 2_665 ? Cl2A Sb1 Cl2 22.92(14) 2_665 2_665 ? Cl2 Sb1 Cl2 180.0 . 2_665 ? Cl1 Sb1 Cl3A 82.85(13) . 2_665 ? Cl1 Sb1 Cl3A 97.15(13) 2_665 2_665 ? Cl2A Sb1 Cl3A 89.7(2) . 2_665 ? Cl2A Sb1 Cl3A 90.3(2) 2_665 2_665 ? Cl2 Sb1 Cl3A 110.99(14) . 2_665 ? Cl2 Sb1 Cl3A 69.01(14) 2_665 2_665 ? Cl1 Sb1 Cl3A 97.15(13) . . ? Cl1 Sb1 Cl3A 82.85(13) 2_665 . ? Cl2A Sb1 Cl3A 90.3(2) . . ? Cl2A Sb1 Cl3A 89.7(2) 2_665 . ? Cl2 Sb1 Cl3A 69.01(14) . . ? Cl2 Sb1 Cl3A 110.99(14) 2_665 . ? Cl3A Sb1 Cl3A 180.0 2_665 . ? Cl1 Sb1 Cl3 90.71(2) . 2_665 ? Cl1 Sb1 Cl3 89.29(2) 2_665 2_665 ? Cl2A Sb1 Cl3 67.44(14) . 2_665 ? Cl2A Sb1 Cl3 112.56(15) 2_665 2_665 ? Cl2 Sb1 Cl3 89.64(3) . 2_665 ? Cl2 Sb1 Cl3 90.36(3) 2_665 2_665 ? Cl3A Sb1 Cl3 23.05(13) 2_665 2_665 ? Cl3A Sb1 Cl3 156.95(13) . 2_665 ? Cl1 Sb1 Cl3 89.29(2) . . ? Cl1 Sb1 Cl3 90.71(2) 2_665 . ? Cl2A Sb1 Cl3 112.56(14) . . ? Cl2A Sb1 Cl3 67.44(15) 2_665 . ? Cl2 Sb1 Cl3 90.36(3) . . ? Cl2 Sb1 Cl3 89.64(3) 2_665 . ? Cl3A Sb1 Cl3 156.95(13) 2_665 . ? Cl3A Sb1 Cl3 23.05(13) . . ? Cl3 Sb1 Cl3 180.0 2_665 . ? Cl6 Sb2 Cl6 180.0 2_444 . ? Cl6 Sb2 Cl5 90.14(3) 2_444 . ? Cl6 Sb2 Cl5 89.86(3) . . ? Cl6 Sb2 Cl5 89.86(3) 2_444 2_444 ? Cl6 Sb2 Cl5 90.14(3) . 2_444 ? Cl5 Sb2 Cl5 180.0 . 2_444 ? Cl6 Sb2 Cl4 89.74(3) 2_444 . ? Cl6 Sb2 Cl4 90.26(3) . . ? Cl5 Sb2 Cl4 88.97(2) . . ? Cl5 Sb2 Cl4 91.03(2) 2_444 . ? Cl6 Sb2 Cl4 90.26(3) 2_444 2_444 ? Cl6 Sb2 Cl4 89.74(3) . 2_444 ? Cl5 Sb2 Cl4 91.03(2) . 2_444 ? Cl5 Sb2 Cl4 88.97(2) 2_444 2_444 ? Cl4 Sb2 Cl4 180.0 . 2_444 ? Cl2A Cl2 Sb1 78.3(3) . . ? Cl2 Cl2A Sb1 78.7(3) . . ? Cl3A Cl3 Sb1 78.4(3) . . ? Cl3 Cl3A Sb1 78.6(3) . . ? C32 O32 C37 118.2(2) . . ? C35 O35 C39 117.2(2) . . ? C42 O42 C47 118.2(2) . . ? C45 O45 C49 117.4(2) . . ? C16 C11 C12 121.1(2) . . ? C16 C11 C21 129.7(2) . . ? C12 C11 C21 109.1(2) . . ? C13 C12 C11 119.8(2) . . ? C13 C12 C17 130.1(2) . . ? C11 C12 C17 110.2(2) . . ? C12 C13 C14 119.8(2) . . ? C15 C14 C13 118.8(2) . . ? C15 C14 C31 120.3(2) . . ? C13 C14 C31 120.7(2) . . ? C16 C15 C14 121.3(2) . . ? C15 C16 C11 119.1(2) . . ? C22 C17 C18 112.3(2) . . ? C22 C17 C12 100.9(2) . . ? C18 C17 C12 113.1(2) . . ? C22 C17 C19 110.1(2) . . ? C18 C17 C19 109.8(2) . . ? C12 C17 C19 110.3(2) . . ? C26 C21 C22 121.1(2) . . ? C26 C21 C11 129.7(2) . . ? C22 C21 C11 109.2(2) . . ? C23 C22 C21 120.2(2) . . ? C23 C22 C17 129.5(2) . . ? C21 C22 C17 110.2(2) . . ? C22 C23 C24 119.6(2) . . ? C23 C24 C25 118.6(2) . . ? C23 C24 C41 123.4(2) . . ? C25 C24 C41 118.0(2) . . ? C26 C25 C24 122.1(2) . . ? C25 C26 C21 118.3(2) . . ? C36 C31 C32 117.4(2) . . ? C36 C31 C14 120.1(2) . . ? C32 C31 C14 122.5(2) . . ? O32 C32 C33 122.7(2) . . ? O32 C32 C31 116.9(2) . . ? C33 C32 C31 120.3(2) . . ? C34 C33 C32 121.8(2) . . ? C33 C34 C35 118.1(2) . . ? C33 C34 C38 121.5(2) . . ? C35 C34 C38 120.3(2) . . ? O35 C35 C36 124.7(2) . . ? O35 C35 C34 114.5(2) . . ? C36 C35 C34 120.9(2) . . ? C35 C36 C31 121.5(2) . . ? C46 C41 C42 117.2(2) . . ? C46 C41 C24 118.8(2) . . ? C42 C41 C24 124.0(2) . . ? O42 C42 C43 122.3(2) . . ? O42 C42 C41 117.1(2) . . ? C43 C42 C41 120.6(2) . . ? C44 C43 C42 121.4(2) . . ? C43 C44 C45 118.5(2) . . ? C43 C44 C48 121.0(2) . . ? C45 C44 C48 120.5(2) . . ? O45 C45 C46 124.3(2) . . ? O45 C45 C44 114.9(2) . . ? C46 C45 C44 120.7(2) . . ? C45 C46 C41 121.6(2) . . ? Cl1X C1X Cl2X 112.8(3) . . ? Cl3X C2X Cl4X 105.7(5) . . ? Cl4Y C2Y Cl3Y 113.6(11) . . ? _refine_diff_density_max 1.613 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.104