#============================================================================== data_global #============================================================================== _audit_creation_date 21-01-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Ian P. Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Dr. W. Lafayette IN 47907-2084 USA ; _publ_contact_author_email 'rothwell@purdue.edu' _publ_contact_author_fax '1(765)494-0239' _publ_contact_author_phone '1(765)494-7012' _publ_requested_journal 'INORGANIC CHEMISTRY' _publ_requested_category ? _publ_requested_coeditor_name ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge ? _journal_name_full ? _journal_volume ? _journal_year ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Group 1 Metal 2,6-Diphenylphenoxide Complexes [M(OC6H3Ph2-2,6)] (M = Li, Na, K, Rb, Cs) and Structures of the Solvent-Free Complexes [Rb(OC6H3Ph2-2,6)]x and [Cs(OC6H3Ph2-2,6)]x: One Dimensional Extended Arrays of Metal Aryloxides . ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses and footnotes # of all authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Ian P. Rothwell' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'Charles S. Weinert' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'Phillip E. Fanwick' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _database_code_CSD 'SW2290' _publ_section_experimental ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G.L., Giacovazzo, C., Polidori, G., Spagna R. (2003). J. Appl. Cryst., in preperation Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of G\"ottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; data_SW2290 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C18 H13 O1 Rb1' _chemical_formula_moiety 'C18 H13 O1 Rb1' _chemical_formula_structural ? _chemical_formula_weight 330.77 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 5.7681(2) _cell_length_b 21.1759(8) _cell_length_c 11.4656(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.7636(13) _cell_angle_gamma 90.00 _cell_volume 1390.72(9) _cell_measurement_reflns_used 9828 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.455 _cell_measurement_temperature 150 _exptl_crystal_F_000 664 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.5830 _exptl_absorpt_correction_T_max 0.7718 _diffrn_reflns_number 9828 _diffrn_measured_fraction_theta_max 0.9976 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9976 _reflns_number_total 3176 _reflns_number_gt 2372 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_max 14 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.078 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 3169 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.8895P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.89 _refine_diff_density_min -0.58 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR2002,_Burla_et_al.,_2003) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb Rb 0.76404(6) 0.04671(2) 0.06469(3) 0.02497(14) Uani 1 1 d . . . O(1) O 0.2802(4) 0.03762(12) 0.1171(2) 0.0204(6) Uani 1 1 d . . . C(1) C 0.3467(6) 0.06119(18) 0.2213(3) 0.0179(9) Uani 1 1 d . . . C(2) C 0.5117(6) 0.03055(18) 0.3057(3) 0.0199(9) Uani 1 1 d . . . C(3) C 0.5799(7) 0.0584(2) 0.4150(4) 0.0266(10) Uani 1 1 d . . . C(4) C 0.4888(7) 0.1148(2) 0.4484(4) 0.0278(10) Uani 1 1 d . . . C(5) C 0.3250(7) 0.1450(2) 0.3689(4) 0.0270(10) Uani 1 1 d . . . C(6) C 0.2557(6) 0.12051(19) 0.2578(3) 0.0205(9) Uani 1 1 d . . . C(21) C 0.6065(6) -0.03341(19) 0.2841(3) 0.0212(9) Uani 1 1 d . . . C(22) C 0.4630(6) -0.08102(19) 0.2300(3) 0.0204(9) Uani 1 1 d . . . C(23) C 0.5444(7) -0.1428(2) 0.2240(4) 0.0279(10) Uani 1 1 d . . . C(24) C 0.7704(7) -0.1580(2) 0.2726(4) 0.0330(11) Uani 1 1 d . . . C(25) C 0.9147(7) -0.1111(2) 0.3231(4) 0.0340(12) Uani 1 1 d . . . C(26) C 0.8355(7) -0.0503(2) 0.3282(4) 0.0287(10) Uani 1 1 d . . . C(61) C 0.0826(6) 0.15712(18) 0.1779(3) 0.0182(9) Uani 1 1 d . . . C(62) C -0.1223(6) 0.17910(19) 0.2197(4) 0.0244(10) Uani 1 1 d . . . C(63) C -0.2839(7) 0.2148(2) 0.1481(4) 0.0295(11) Uani 1 1 d . . . C(64) C -0.2481(7) 0.2285(2) 0.0353(4) 0.0348(12) Uani 1 1 d . . . C(65) C -0.0470(7) 0.2061(2) -0.0084(4) 0.0302(11) Uani 1 1 d . . . C(66) C 0.1168(6) 0.17072(19) 0.0622(3) 0.0209(9) Uani 1 1 d . . . H(3) H 0.6935 0.0376 0.4683 0.032 Uiso 1 1 calc R . . H(4) H 0.5366 0.1325 0.5235 0.033 Uiso 1 1 calc R . . H(5) H 0.2582 0.1835 0.3912 0.032 Uiso 1 1 calc R . . H(22) H 0.3085 -0.0711 0.1970 0.024 Uiso 1 1 calc R . . H(23) H 0.4457 -0.1746 0.1868 0.034 Uiso 1 1 calc R . . H(24) H 0.8246 -0.2003 0.2709 0.040 Uiso 1 1 calc R . . H(25) H 1.0702 -0.1210 0.3546 0.041 Uiso 1 1 calc R . . H(26) H 0.9385 -0.0187 0.3626 0.034 Uiso 1 1 calc R . . H(62) H -0.1507 0.1694 0.2977 0.029 Uiso 1 1 calc R . . H(63) H -0.4205 0.2298 0.1780 0.035 Uiso 1 1 calc R . . H(64) H -0.3588 0.2531 -0.0132 0.042 Uiso 1 1 calc R . . H(65) H -0.0222 0.2152 -0.0871 0.036 Uiso 1 1 calc R . . H(66) H 0.2525 0.1557 0.0315 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rb 0.0190(2) 0.0298(2) 0.0266(2) -0.00522(19) 0.00496(14) -0.0083(2) O(1) 0.0190(13) 0.0244(17) 0.0169(15) 0.0014(12) -0.0016(10) 0.0001(13) C(1) 0.0123(18) 0.024(3) 0.018(2) -0.0043(16) 0.0038(15) 0.0000(18) C(2) 0.021(2) 0.019(2) 0.019(2) -0.0025(16) 0.0018(16) 0.0008(18) C(3) 0.027(2) 0.028(3) 0.022(3) -0.0021(19) -0.0026(17) 0.002(2) C(4) 0.039(2) 0.024(3) 0.020(2) -0.002(2) 0.0015(19) -0.005(2) C(5) 0.035(2) 0.022(3) 0.024(3) 0.0024(19) 0.0049(19) -0.002(2) C(6) 0.0185(19) 0.023(2) 0.020(2) -0.0005(17) 0.0047(16) 0.0038(19) C(21) 0.021(2) 0.026(3) 0.017(2) -0.0002(18) 0.0049(16) 0.0053(19) C(22) 0.022(2) 0.021(2) 0.017(2) 0.0055(18) -0.0003(16) 0.0047(18) C(23) 0.041(3) 0.023(3) 0.019(2) 0.000(2) 0.0038(18) -0.001(2) C(24) 0.043(3) 0.028(3) 0.031(3) 0.017(2) 0.017(2) 0.003(2) C(25) 0.019(2) 0.039(3) 0.044(3) 0.009(2) 0.0062(19) 0.010(2) C(26) 0.020(2) 0.030(3) 0.035(3) -0.002(2) 0.0005(17) 0.004(2) C(61) 0.0185(19) 0.011(2) 0.024(2) -0.0021(16) -0.0009(16) -0.0042(18) C(62) 0.023(2) 0.021(2) 0.029(3) -0.0025(18) 0.0048(17) -0.005(2) C(63) 0.023(2) 0.025(3) 0.039(3) 0.0021(19) -0.0008(19) -0.016(2) C(64) 0.030(2) 0.029(3) 0.042(3) 0.005(2) -0.013(2) -0.005(2) C(65) 0.035(2) 0.024(3) 0.030(3) -0.001(2) -0.001(2) 0.006(2) C(66) 0.0163(19) 0.019(2) 0.027(3) -0.0007(17) -0.0003(16) 0.0001(19) # 10. MOLECULAR GEOMETRY _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_publ_flag Rb O(1) 2.734(3) YES Rb O(1) 2.930(2) YES Rb O(1) 2.973(2) YES Rb C(61) 3.157(4) YES Rb C(1) 3.183(3) YES Rb C(21) 3.251(4) YES Rb C(2) 3.290(4) YES Rb C(66) 3.324(4) YES Rb C(62) 3.343(4) YES Rb C(22) 3.552(4) YES Rb C(1) 3.632(3) YES Rb C(26) 3.637(4) YES O(1) C(1) 1.310(4) YES O(1) Rb 2.734(3) YES O(1) Rb 2.973(2) YES C(1) C(2) 1.431(5) YES C(1) C(6) 1.442(5) YES C(1) Rb 3.632(3) YES C(2) C(3) 1.399(5) YES C(2) C(21) 1.492(5) YES C(3) C(4) 1.376(6) YES C(4) C(5) 1.389(5) YES C(5) C(6) 1.390(5) YES C(6) C(61) 1.490(5) YES C(6) Rb 3.729(4) YES C(21) C(22) 1.402(5) YES C(21) C(26) 1.404(5) YES C(22) C(23) 1.395(6) YES C(22) Rb 3.552(4) YES C(23) C(24) 1.393(6) YES C(24) C(25) 1.378(6) YES C(25) C(26) 1.369(6) YES C(61) C(66) 1.395(5) YES C(61) C(62) 1.406(5) YES C(61) Rb 3.157(4) YES C(62) C(63) 1.391(6) YES C(62) Rb 3.343(4) YES C(63) C(64) 1.365(6) YES C(63) Rb 3.705(4) YES C(64) C(65) 1.400(6) YES C(65) C(66) 1.389(5) YES C(65) Rb 3.674(4) YES C(66) Rb 3.324(4) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Rb O(1) 96.20(7) YES O(1) Rb O(1) 96.50(7) YES O(1) Rb O(1) 155.46(10) YES O(1) Rb C(61) 142.64(8) YES O(1) Rb C(61) 119.12(8) YES O(1) Rb C(61) 56.24(8) YES O(1) Rb C(1) 118.96(8) YES O(1) Rb C(1) 24.29(8) YES O(1) Rb C(1) 134.26(9) YES C(61) Rb C(1) 97.98(9) YES O(1) Rb C(21) 103.87(9) YES O(1) Rb C(21) 56.44(8) YES O(1) Rb C(21) 100.03(8) YES C(61) Rb C(21) 105.69(10) YES C(1) Rb C(21) 46.76(10) YES O(1) Rb C(2) 124.18(8) YES O(1) Rb C(2) 45.11(8) YES O(1) Rb C(2) 110.79(8) YES C(61) Rb C(2) 91.45(10) YES C(1) Rb C(2) 25.47(9) YES C(21) Rb C(2) 26.37(9) YES O(1) Rb C(66) 120.77(9) YES O(1) Rb C(66) 130.73(8) YES O(1) Rb C(66) 56.88(8) YES C(61) Rb C(66) 24.68(9) YES C(1) Rb C(66) 115.67(10) YES C(21) Rb C(66) 130.24(10) YES C(2) Rb C(66) 114.92(10) YES O(1) Rb C(62) 161.46(9) YES O(1) Rb C(62) 94.47(8) YES O(1) Rb C(62) 79.50(8) YES C(61) Rb C(62) 24.77(9) YES C(1) Rb C(62) 74.53(9) YES C(21) Rb C(62) 94.67(10) YES C(2) Rb C(62) 73.68(10) YES C(66) Rb C(62) 42.28(10) YES O(1) Rb C(22) 54.37(8) YES O(1) Rb C(22) 87.44(8) YES O(1) Rb C(22) 116.99(8) YES C(61) Rb C(22) 111.79(10) YES C(1) Rb C(22) 107.36(9) YES C(21) Rb C(22) 137.51(9) YES C(2) Rb C(22) 132.10(9) YES C(66) Rb C(22) 89.29(9) YES C(62) Rb C(22) 111.19(10) YES O(1) Rb C(1) 115.46(8) YES O(1) Rb C(1) 138.80(8) YES O(1) Rb C(1) 19.83(7) YES C(61) Rb C(1) 43.47(9) YES C(1) Rb C(1) 115.48(11) YES C(21) Rb C(1) 89.32(9) YES C(2) Rb C(1) 93.93(9) YES C(66) Rb C(1) 53.56(9) YES C(62) Rb C(1) 63.52(9) YES C(22) Rb C(1) 131.99(8) YES O(1) Rb C(26) 104.81(9) YES O(1) Rb C(26) 79.04(8) YES O(1) Rb C(26) 77.44(8) YES C(61) Rb C(26) 94.20(10) YES C(1) Rb C(26) 66.74(9) YES C(21) Rb C(26) 22.64(8) YES C(2) Rb C(26) 42.39(9) YES C(66) Rb C(26) 116.36(10) YES C(62) Rb C(26) 92.08(10) YES C(22) Rb C(26) 154.00(10) YES C(1) Rb C(26) 68.24(8) YES C(1) O(1) Rb 159.3(2) YES C(1) O(1) Rb 88.76(18) YES Rb O(1) Rb 83.80(7) YES C(1) O(1) Rb 109.78(19) YES Rb O(1) Rb 83.50(7) YES Rb O(1) Rb 155.45(10) YES O(1) C(1) C(2) 123.0(3) YES O(1) C(1) C(6) 121.3(3) YES C(2) C(1) C(6) 115.8(3) YES O(1) C(1) Rb 66.95(17) YES C(2) C(1) Rb 81.4(2) YES C(6) C(1) Rb 124.9(2) YES O(1) C(1) Rb 50.38(15) YES C(2) C(1) Rb 143.1(2) YES C(6) C(1) Rb 82.5(2) YES Rb C(1) Rb 115.48(11) YES C(3) C(2) C(1) 120.6(4) YES C(3) C(2) C(21) 117.5(3) YES C(1) C(2) C(21) 121.8(3) YES C(3) C(2) Rb 127.1(2) YES C(1) C(2) Rb 73.1(2) YES C(21) C(2) Rb 75.4(2) YES C(4) C(3) C(2) 122.6(4) YES C(3) C(4) C(5) 118.0(4) YES C(4) C(5) C(6) 122.0(4) YES C(5) C(6) C(1) 121.0(4) YES C(5) C(6) C(61) 118.0(4) YES C(1) C(6) C(61) 121.0(3) YES C(5) C(6) Rb 144.8(2) YES C(1) C(6) Rb 74.9(2) YES C(61) C(6) Rb 56.34(19) YES C(22) C(21) C(26) 117.2(4) YES C(22) C(21) C(2) 121.1(3) YES C(26) C(21) C(2) 121.3(4) YES C(22) C(21) Rb 103.7(2) YES C(26) C(21) Rb 94.3(2) YES C(2) C(21) Rb 78.2(2) YES C(23) C(22) C(21) 120.8(4) YES C(23) C(22) Rb 103.5(3) YES C(21) C(22) Rb 114.0(2) YES C(24) C(23) C(22) 120.1(4) YES C(25) C(24) C(23) 119.5(4) YES C(26) C(25) C(24) 120.4(4) YES C(25) C(26) C(21) 122.0(4) YES C(25) C(26) Rb 120.1(3) YES C(21) C(26) Rb 63.1(2) YES C(66) C(61) C(62) 118.3(4) YES C(66) C(61) C(6) 122.2(3) YES C(62) C(61) C(6) 119.5(4) YES C(66) C(61) Rb 84.4(2) YES C(62) C(61) Rb 85.0(2) YES C(6) C(61) Rb 100.5(2) YES C(63) C(62) C(61) 120.7(4) YES C(63) C(62) Rb 93.8(2) YES C(61) C(62) Rb 70.2(2) YES C(64) C(63) C(62) 120.6(4) YES C(64) C(63) Rb 86.3(3) YES C(62) C(63) Rb 64.2(2) YES C(63) C(64) C(65) 119.4(4) YES C(66) C(65) C(64) 120.7(4) YES C(66) C(65) Rb 64.6(2) YES C(64) C(65) Rb 87.1(3) YES C(65) C(66) C(61) 120.2(4) YES C(65) C(66) Rb 93.2(2) YES C(61) C(66) Rb 70.9(2) YES #===END #============================================================================== data_global #============================================================================== _audit_creation_date 14-01-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Ian P. Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Dr. W. Lafayette IN 47907-2084 USA ; _publ_contact_author_email 'rothwell@purdue.edu' _publ_contact_author_fax '1(765)494-0239' _publ_contact_author_phone '1(765)494-7012' _publ_requested_journal 'INORGANIC CHEMISTRY' _publ_requested_category ? _publ_requested_coeditor_name ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge ? _journal_name_full ? _journal_volume ? _journal_year ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Group 1 Metal 2,6-Diphenylphenoxide Complexes [M(OC6H3Ph2-2,6)] (M = Li, Na, K, Rb, Cs) and Structures of the Solvent-Free Complexes [Rb(OC6H3Ph2-2,6)]x and [Cs(OC6H3Ph2-2,6)]x: One Dimensional Extended Arrays of Metal Aryloxides . ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses and footnotes # of all authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Ian P. Rothwell' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'Charles S. Weinert' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'Phillip E. Fanwick' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _database_code_CSD 'SW3336' _publ_section_experimental ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G.L., Giacovazzo, C., Polidori, G., Spagna R. (2003). J. Appl. Cryst., in preperation Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of G\"ottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; data_SW3336 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C18 H13 Cs1 O1' _chemical_formula_moiety 'C18 H13 Cs1 O1' _chemical_formula_structural ? _chemical_formula_weight 378.21 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 11.7492(6) _cell_length_b 7.3061(3) _cell_length_c 16.9160(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.989(2) _cell_angle_gamma 90.00 _cell_volume 1425.46(12) _cell_measurement_reflns_used 10697 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.76 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.569 _cell_measurement_temperature 150 _exptl_crystal_F_000 736 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.4353 _exptl_absorpt_correction_T_max 0.7735 _diffrn_reflns_number 10697 _diffrn_measured_fraction_theta_max 0.9964 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9964 _reflns_number_total 3392 _reflns_number_gt 2935 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_max 21 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.068 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 3382 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.12 _refine_diff_density_min -0.96 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR2002,_Burla_et_al.,_2003) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cs Cs 0.137727(17) 0.06329(3) 0.436974(11) 0.02994(8) Uani 1 1 d . . . O O 0.07001(17) 0.1716(3) 0.58923(11) 0.0256(4) Uani 1 1 d . . . C(1) C 0.1164(2) 0.3003(4) 0.63741(15) 0.0206(6) Uani 1 1 d . . . C(2) C 0.2390(2) 0.3102(4) 0.66838(16) 0.0210(6) Uani 1 1 d . . . C(3) C 0.2857(3) 0.4470(4) 0.72203(18) 0.0246(6) Uani 1 1 d . . . C(4) C 0.2177(3) 0.5807(4) 0.74840(18) 0.0264(7) Uani 1 1 d . . . C(5) C 0.0986(3) 0.5782(4) 0.71775(17) 0.0239(6) Uani 1 1 d . . . C(6) C 0.0475(3) 0.4452(4) 0.66303(16) 0.0209(6) Uani 1 1 d . . . C(21) C 0.3208(2) 0.1758(4) 0.64338(16) 0.0225(6) Uani 1 1 d . . . C(22) C 0.3030(3) -0.0125(4) 0.64465(19) 0.0282(7) Uani 1 1 d . . . C(23) C 0.3866(3) -0.1342(5) 0.62662(19) 0.0323(7) Uani 1 1 d . . . C(24) C 0.4860(3) -0.0694(4) 0.6037(2) 0.0331(7) Uani 1 1 d . . . C(25) C 0.5044(3) 0.1185(5) 0.60121(19) 0.0322(7) Uani 1 1 d . . . C(26) C 0.4233(3) 0.2386(4) 0.62119(18) 0.0270(7) Uani 1 1 d . . . C(61) C -0.0788(3) 0.4618(4) 0.63009(17) 0.0217(6) Uani 1 1 d . . . C(62) C -0.1566(3) 0.5189(4) 0.67810(18) 0.0239(6) Uani 1 1 d . . . C(63) C -0.2733(3) 0.5467(4) 0.64668(19) 0.0257(6) Uani 1 1 d . . . C(64) C -0.3153(3) 0.5185(4) 0.56522(19) 0.0267(7) Uani 1 1 d . . . C(65) C -0.2399(3) 0.4626(4) 0.51629(19) 0.0267(7) Uani 1 1 d . . . C(66) C -0.1237(3) 0.4318(4) 0.54741(18) 0.0244(6) Uani 1 1 d . . . H(3) H 0.3671 0.4490 0.7413 0.030 Uiso 1 1 calc R . . H(4) H 0.2512 0.6711 0.7861 0.032 Uiso 1 1 calc R . . H(5) H 0.0510 0.6697 0.7346 0.029 Uiso 1 1 calc R . . H(22) H 0.2334 -0.0589 0.6579 0.034 Uiso 1 1 calc R . . H(23) H 0.3748 -0.2624 0.6301 0.039 Uiso 1 1 calc R . . H(24) H 0.5413 -0.1523 0.5899 0.040 Uiso 1 1 calc R . . H(25) H 0.5726 0.1643 0.5858 0.039 Uiso 1 1 calc R . . H(26) H 0.4372 0.3665 0.6199 0.032 Uiso 1 1 calc R . . H(62) H -0.1288 0.5392 0.7339 0.029 Uiso 1 1 calc R . . H(63) H -0.3243 0.5850 0.6808 0.031 Uiso 1 1 calc R . . H(64) H -0.3951 0.5373 0.5432 0.032 Uiso 1 1 calc R . . H(65) H -0.2683 0.4451 0.4604 0.032 Uiso 1 1 calc R . . H(66) H -0.0738 0.3903 0.5131 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cs 0.03670(13) 0.02640(12) 0.02922(12) -0.00732(9) 0.01262(8) -0.00459(8) O 0.0250(10) 0.0236(11) 0.0284(10) -0.0024(9) 0.0059(9) -0.0070(9) C(1) 0.0252(14) 0.0212(14) 0.0157(12) -0.0027(12) 0.0045(11) 0.0001(11) C(2) 0.0246(15) 0.0195(14) 0.0190(13) -0.0008(12) 0.0046(11) 0.0037(12) C(3) 0.0247(15) 0.0239(15) 0.0241(14) -0.0029(12) 0.0017(12) 0.0014(12) C(4) 0.0320(17) 0.0236(16) 0.0230(14) -0.0031(13) 0.0042(12) -0.0038(12) C(5) 0.0292(15) 0.0220(15) 0.0214(14) 0.0025(12) 0.0069(12) -0.0007(12) C(6) 0.0251(14) 0.0212(14) 0.0168(13) -0.0014(12) 0.0055(11) 0.0021(11) C(21) 0.0260(15) 0.0248(15) 0.0155(13) 0.0020(13) 0.0008(11) 0.0003(12) C(22) 0.0325(17) 0.0272(16) 0.0246(15) -0.0016(14) 0.0046(13) -0.0018(13) C(23) 0.043(2) 0.0230(16) 0.0287(16) 0.0026(14) 0.0017(14) -0.0039(13) C(24) 0.0317(17) 0.0349(19) 0.0312(17) 0.0115(15) 0.0025(14) -0.0044(14) C(25) 0.0253(16) 0.0377(18) 0.0341(17) 0.0052(14) 0.0073(14) 0.0046(14) C(26) 0.0266(16) 0.0263(16) 0.0276(15) 0.0030(13) 0.0038(13) 0.0035(13) C(61) 0.0289(15) 0.0161(15) 0.0198(13) -0.0016(12) 0.0042(12) 0.0019(11) C(62) 0.0297(16) 0.0220(15) 0.0210(14) -0.0003(12) 0.0072(12) 0.0023(12) C(63) 0.0251(15) 0.0237(16) 0.0296(16) -0.0003(12) 0.0083(12) 0.0027(13) C(64) 0.0242(15) 0.0225(15) 0.0315(16) -0.0001(12) 0.0009(13) 0.0039(13) C(65) 0.0308(16) 0.0232(16) 0.0237(15) -0.0035(13) -0.0010(12) 0.0001(12) C(66) 0.0311(16) 0.0196(15) 0.0230(14) -0.0018(12) 0.0065(12) -0.0009(12) # 10. MOLECULAR GEOMETRY _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_publ_flag Cs O 2.9451(19) YES Cs O 2.947(2) YES Cs C(66) 3.633(3) YES Cs C(4) 3.648(3) YES Cs C(62) 3.650(3) YES Cs C(61) 3.675(3) YES Cs C(63) 3.677(3) YES Cs C(65) 3.702(3) YES Cs C(66) 3.704(3) YES Cs C(64) 3.705(3) YES Cs C(22) 3.717(3) YES Cs C(5) 3.792(3) YES O C(1) 1.294(3) YES O Cs 2.947(2) YES C(1) C(2) 1.437(4) YES C(1) C(6) 1.449(4) YES C(2) C(3) 1.391(4) YES C(2) C(21) 1.490(4) YES C(3) C(4) 1.388(4) YES C(4) C(5) 1.396(4) YES C(4) Cs 3.648(3) YES C(5) C(6) 1.397(4) YES C(5) Cs 3.792(3) YES C(6) C(61) 1.487(4) YES C(21) C(22) 1.392(4) YES C(21) C(26) 1.404(4) YES C(22) C(23) 1.401(5) YES C(23) C(24) 1.382(5) YES C(24) C(25) 1.391(5) YES C(25) C(26) 1.384(4) YES C(61) C(62) 1.397(4) YES C(61) C(66) 1.414(4) YES C(61) Cs 3.675(3) YES C(62) C(63) 1.388(4) YES C(62) Cs 3.650(3) YES C(63) C(64) 1.388(4) YES C(63) Cs 3.677(3) YES C(64) C(65) 1.385(5) YES C(64) Cs 3.705(3) YES C(65) C(66) 1.384(4) YES C(65) Cs 3.702(3) YES C(66) Cs 3.633(3) YES C(66) Cs 3.704(3) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O Cs O 86.22(5) YES O Cs C(66) 100.39(6) YES O Cs C(66) 51.93(6) YES O Cs C(4) 178.67(6) YES O Cs C(4) 92.56(6) YES C(66) Cs C(4) 78.42(7) YES O Cs C(62) 107.20(6) YES O Cs C(62) 122.66(6) YES C(66) Cs C(62) 151.61(7) YES C(4) Cs C(62) 73.91(7) YES O Cs C(61) 87.13(6) YES O Cs C(61) 113.67(6) YES C(66) Cs C(61) 162.56(7) YES C(4) Cs C(61) 93.85(7) YES C(62) Cs C(61) 21.99(7) YES O Cs C(63) 109.72(6) YES O Cs C(63) 143.18(6) YES C(66) Cs C(63) 145.96(7) YES C(4) Cs C(63) 71.59(7) YES C(62) Cs C(63) 21.83(7) YES C(61) Cs C(63) 38.68(7) YES O Cs C(65) 72.08(6) YES O Cs C(65) 143.36(6) YES C(66) Cs C(65) 159.00(7) YES C(4) Cs C(65) 109.24(7) YES C(62) Cs C(65) 44.03(7) YES C(61) Cs C(65) 38.44(7) YES C(63) Cs C(65) 37.85(7) YES O Cs C(66) 69.32(6) YES O Cs C(66) 122.94(6) YES C(66) Cs C(66) 169.45(10) YES C(4) Cs C(66) 111.83(7) YES C(62) Cs C(66) 38.11(7) YES C(61) Cs C(66) 22.10(6) YES C(63) Cs C(66) 44.29(7) YES C(65) Cs C(66) 21.55(7) YES O Cs C(64) 91.93(7) YES O Cs C(64) 158.55(6) YES C(66) Cs C(64) 148.82(7) YES C(4) Cs C(64) 89.40(7) YES C(62) Cs C(64) 38.11(7) YES C(61) Cs C(64) 44.88(7) YES C(63) Cs C(64) 21.67(7) YES C(65) Cs C(64) 21.56(7) YES C(66) Cs C(64) 38.01(7) YES O Cs C(22) 52.63(6) YES O Cs C(22) 108.90(6) YES C(66) Cs C(22) 78.80(7) YES C(4) Cs C(22) 127.46(7) YES C(62) Cs C(22) 123.69(7) YES C(61) Cs C(22) 117.78(7) YES C(63) Cs C(22) 107.01(7) YES C(65) Cs C(22) 81.25(7) YES C(66) Cs C(22) 95.93(7) YES C(64) Cs C(22) 86.48(7) YES O Cs C(5) 157.79(6) YES O Cs C(5) 75.63(6) YES C(66) Cs C(5) 78.52(6) YES C(4) Cs C(5) 21.52(7) YES C(62) Cs C(5) 73.43(6) YES C(61) Cs C(5) 88.56(6) YES C(63) Cs C(5) 79.36(6) YES C(65) Cs C(5) 115.96(7) YES C(66) Cs C(5) 110.02(6) YES C(64) Cs C(5) 100.28(7) YES C(22) Cs C(5) 145.86(7) YES C(1) O Cs 126.46(17) YES C(1) O Cs 139.01(17) YES Cs O Cs 93.79(5) YES O C(1) C(2) 122.6(3) YES O C(1) C(6) 121.8(2) YES C(2) C(1) C(6) 115.6(2) YES O C(1) Cs 37.89(13) YES C(2) C(1) Cs 96.58(16) YES C(6) C(1) Cs 136.44(17) YES C(3) C(2) C(1) 121.2(3) YES C(3) C(2) C(21) 117.6(3) YES C(1) C(2) C(21) 121.3(3) YES C(4) C(3) C(2) 122.4(3) YES C(3) C(4) C(5) 117.9(3) YES C(3) C(4) Cs 109.76(19) YES C(5) C(4) Cs 85.06(18) YES C(6) C(5) C(4) 122.0(3) YES C(6) C(5) Cs 114.52(18) YES C(4) C(5) Cs 73.42(17) YES C(5) C(6) C(1) 120.8(3) YES C(5) C(6) C(61) 117.7(3) YES C(1) C(6) C(61) 121.5(2) YES C(22) C(21) C(26) 117.7(3) YES C(22) C(21) C(2) 122.6(3) YES C(26) C(21) C(2) 119.5(3) YES C(22) C(21) Cs 75.03(16) YES C(26) C(21) Cs 100.82(17) YES C(2) C(21) Cs 96.88(15) YES C(21) C(22) C(23) 120.7(3) YES C(21) C(22) Cs 83.75(16) YES C(23) C(22) Cs 98.64(19) YES C(24) C(23) C(22) 120.5(3) YES C(23) C(24) C(25) 119.4(3) YES C(26) C(25) C(24) 120.0(3) YES C(25) C(26) C(21) 121.6(3) YES C(62) C(61) C(66) 117.3(3) YES C(62) C(61) C(6) 121.5(3) YES C(66) C(61) C(6) 121.0(3) YES C(62) C(61) Cs 78.00(16) YES C(66) C(61) Cs 80.11(16) YES C(6) C(61) Cs 107.97(17) YES C(63) C(62) C(61) 122.0(3) YES C(63) C(62) Cs 80.17(17) YES C(61) C(62) Cs 80.01(16) YES C(62) C(63) C(64) 119.8(3) YES C(62) C(63) Cs 78.00(17) YES C(64) C(63) Cs 80.29(18) YES C(65) C(64) C(63) 119.3(3) YES C(65) C(64) Cs 79.10(17) YES C(63) C(64) Cs 78.04(17) YES C(66) C(65) C(64) 121.2(3) YES C(66) C(65) Cs 79.33(17) YES C(64) C(65) Cs 79.34(17) YES C(65) C(66) C(61) 120.4(3) YES C(65) C(66) Cs 97.71(18) YES C(61) C(66) Cs 95.50(17) YES C(65) C(66) Cs 79.12(17) YES C(61) C(66) Cs 77.79(16) YES Cs C(66) Cs 169.45(10) YES