#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006382.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2006382 loop_ _publ_author_name 'Meyers, C. Y.' 'Hou, Y.' 'Scott, D.' 'Robinson, P. D.' _publ_section_title ; Exclusive Formation of Crystalline sp-9-(o-Isopropylphenyl)fluorene from its ap Rotamer in Solution ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1149 _journal_page_last 1151 _journal_volume 53 _journal_year 1997 _chemical_formula_moiety 'C22 H20' _chemical_formula_sum 'C22 H20' _chemical_formula_weight 284.40 _chemical_name_systematic ; sp-9-(o-isopropylphenyl)fluorene ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90.00 _cell_angle_beta 95.182(14) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.7734(17) _cell_length_b 15.773(2) _cell_length_c 8.7960(16) _cell_measurement_reflns_used 22 _cell_measurement_temperature 296 _cell_measurement_theta_max 17.3 _cell_measurement_theta_min 10.3 _cell_volume 1626.8(4) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1996) ; _computing_data_reduction 'PROCESS TEXSAN (Molecular Structure Corporation, 1995)' _computing_molecular_graphics 'TEXSAN, ORTEP (Johnson, 1965)' _computing_publication_material 'TEXSAN, SHELXL93, and PLATON (Spek, 1990)' _computing_structure_refinement 'TEXSAN LS and SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'TEXSAN, SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 296 _diffrn_measurement_device 'Rigaku AFC-5S diffractometer' _diffrn_measurement_method '\w (rate 4\% min^-1^ in \w)' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0912 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3064 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 2.16 _diffrn_standards_decay_% -0.56 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.29 _refine_diff_density_max 0.188 _refine_diff_density_min -0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.016 _refine_ls_goodness_of_fit_obs 1.173 _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_matrix_type full _refine_ls_number_parameters 201 _refine_ls_number_reflns 2864 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.173 _refine_ls_R_factor_all 0.1830 _refine_ls_R_factor_obs 0.0459 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.3571P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1619 _refine_ls_wR_factor_obs 0.1090 _reflns_number_observed 1090 _reflns_number_total 2864 _reflns_observed_criterion >2\s(I) _[local]_cod_data_source_file fg1290.cif _[local]_cod_data_source_block default _cod_original_cell_volume 1626.7(4) _cod_database_code 2006382 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' 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 C1 0.065(2) 0.071(2) 0.069(3) 0.007(2) 0.013(2) 0.003(2) C2 0.063(2) 0.093(3) 0.093(3) 0.012(2) -0.004(2) -0.012(3) C3 0.054(2) 0.082(3) 0.115(4) -0.005(2) 0.007(3) -0.027(3) C4 0.057(2) 0.063(2) 0.095(3) 0.000(2) 0.025(2) -0.010(2) C4a 0.050(2) 0.050(2) 0.070(2) 0.005(2) 0.019(2) -0.005(2) C4b 0.063(2) 0.047(2) 0.061(2) 0.007(2) 0.019(2) 0.001(2) C5 0.090(3) 0.060(2) 0.080(3) 0.006(2) 0.031(2) 0.005(2) C6 0.126(4) 0.074(3) 0.065(3) 0.024(3) 0.027(3) 0.004(2) C7 0.110(3) 0.086(3) 0.069(3) 0.019(3) -0.008(3) -0.015(2) C8 0.077(3) 0.078(3) 0.076(3) 0.003(2) 0.006(2) -0.012(2) C8a 0.054(2) 0.051(2) 0.063(2) 0.003(2) 0.013(2) -0.008(2) C9 0.052(2) 0.046(2) 0.065(2) 0.001(2) 0.017(2) -0.002(2) C9a 0.050(2) 0.053(2) 0.057(2) 0.008(2) 0.015(2) -0.004(2) C1' 0.051(2) 0.055(2) 0.059(2) 0.000(2) 0.013(2) -0.006(2) C2' 0.047(2) 0.065(2) 0.057(2) -0.006(2) 0.005(2) -0.003(2) C3' 0.046(2) 0.094(3) 0.070(2) -0.005(2) 0.012(2) 0.000(2) C4' 0.057(2) 0.098(3) 0.082(3) 0.016(2) 0.018(2) -0.012(3) C5' 0.075(2) 0.073(3) 0.109(3) 0.009(2) 0.027(2) -0.013(2) C6' 0.065(2) 0.057(2) 0.108(3) 0.001(2) 0.030(2) -0.010(2) C7' 0.056(2) 0.070(2) 0.083(3) -0.013(2) 0.023(2) 0.004(2) C8' 0.131(4) 0.080(3) 0.089(3) -0.008(3) 0.002(3) -0.012(3) C9' 0.113(3) 0.105(3) 0.103(4) -0.014(3) 0.013(3) 0.031(3) loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol C1 0.9869(3) 0.0725(2) 0.2997(4) 0.0677(10) Uani d . 1 C C2 1.0919(3) 0.1091(2) 0.3409(5) 0.0838(13) Uani d . 1 C C3 1.1487(3) 0.1536(3) 0.2364(6) 0.0837(12) Uani d . 1 C C4 1.1023(3) 0.1629(2) 0.0876(5) 0.0705(11) Uani d . 1 C C4a 0.9963(3) 0.1263(2) 0.0443(4) 0.0556(9) Uani d . 1 C C4b 0.9264(3) 0.1252(2) -0.1017(4) 0.0561(9) Uani d . 1 C C5 0.9452(3) 0.1603(2) -0.2427(5) 0.0752(11) Uani d . 1 C C6 0.8645(4) 0.1483(3) -0.3639(5) 0.0872(13) Uani d . 1 C C7 0.7660(4) 0.1023(3) -0.3470(5) 0.0894(13) Uani d . 1 C C8 0.7466(3) 0.0675(2) -0.2059(4) 0.0771(11) Uani d . 1 C C8a 0.8278(3) 0.0788(2) -0.0840(4) 0.0557(9) Uani d . 1 C C9 0.8279(2) 0.0460(2) 0.0782(3) 0.0539(9) Uani d . 1 C C9a 0.9399(2) 0.0809(2) 0.1513(4) 0.0529(8) Uani d . 1 C C1' 0.7244(2) 0.0727(2) 0.1601(3) 0.0546(8) Uani d . 1 C C2' 0.6527(3) 0.0159(2) 0.2266(4) 0.0563(9) Uani d . 1 C C3' 0.5601(3) 0.0497(3) 0.2955(4) 0.0697(10) Uani d . 1 C C4' 0.5408(3) 0.1357(3) 0.3029(4) 0.0782(11) Uani d . 1 C C5' 0.6127(3) 0.1906(3) 0.2395(5) 0.0847(12) Uani d . 1 C C6' 0.7031(3) 0.1594(2) 0.1692(4) 0.0752(11) Uani d . 1 C C7' 0.6719(3) -0.0796(2) 0.2232(4) 0.0687(10) Uani d . 1 C C8' 0.6119(4) -0.1183(2) 0.0808(5) 0.1004(14) Uani d . 1 C C9' 0.6354(3) -0.1261(3) 0.3640(5) 0.1066(15) Uani d . 1 C H1 0.9487(3) 0.0427(2) 0.3709(4) 0.081 Uiso calc R 1 H H2 1.1246(3) 0.1037(2) 0.4407(5) 0.101 Uiso calc R 1 H H3 1.2192(3) 0.1777(3) 0.2665(6) 0.100 Uiso calc R 1 H H4 1.1410(3) 0.1929(2) 0.0173(5) 0.085 Uiso calc R 1 H H5 1.0111(3) 0.1912(2) -0.2546(5) 0.090 Uiso calc R 1 H H6 0.8761(4) 0.1714(3) -0.4585(5) 0.105 Uiso calc R 1 H H7 0.7126(4) 0.0946(3) -0.4303(5) 0.107 Uiso calc R 1 H H8 0.6802(3) 0.0373(2) -0.1940(4) 0.092 Uiso calc R 1 H H9 0.8322(2) -0.0161(2) 0.0768(3) 0.065 Uiso calc R 1 H H3' 0.5099(3) 0.0129(3) 0.3377(4) 0.084 Uiso calc R 1 H H4' 0.4792(3) 0.1562(3) 0.3508(4) 0.094 Uiso calc R 1 H H5' 0.6005(3) 0.2488(3) 0.2441(5) 0.102 Uiso calc R 1 H H6' 0.7517(3) 0.1972(2) 0.1262(4) 0.090 Uiso calc R 1 H H7' 0.7539(3) -0.0892(2) 0.2198(4) 0.082 Uiso calc R 1 H H8'a 0.5312(4) -0.1102(16) 0.0811(16) 0.151 Uiso calc R 1 H H8'b 0.628(2) -0.1779(4) 0.0784(16) 0.151 Uiso calc R 1 H H8'c 0.6381(18) -0.0914(13) -0.0075(5) 0.151 Uiso calc R 1 H H9'a 0.668(2) -0.0984(12) 0.4548(5) 0.160 Uiso calc R 1 H H9'b 0.662(2) -0.1838(6) 0.3631(18) 0.160 Uiso calc R 1 H H9'c 0.5537(4) -0.1253(17) 0.3621(18) 0.160 Uiso calc R 1 H 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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -3 -1 2 -4 -1 0 -2 0 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 C9a C1 C2 118.7(3) no C6' C1' C2' 119.1(3) no C2' C1' C9 124.0(3) yes C6' C1' C9 116.9(3) yes C3 C2 C1 121.0(4) no C1' C2' C3' 117.5(3) no C1' C2' C7' 122.0(3) yes C3' C2' C7' 120.5(3) yes C2 C3 C4 120.9(4) no C4' C3' C2' 122.3(3) no C3 C4 C4a 118.8(3) no C4 C4a C9a 119.7(3) no C4 C4a C4b 131.5(3) no C9a C4a C4b 108.8(3) no C5 C4b C8a 120.6(3) no C5 C4b C4a 130.9(3) no C8a C4b C4a 108.4(3) no C5' C4' C3' 119.7(3) no C6 C5 C4b 118.7(4) no C4' C5' C6' 119.4(4) no C5 C6 C7 120.9(4) no C5' C6' C1' 122.0(3) no C6 C7 C8 120.5(4) no C8' C7' C2' 110.9(3) no C8' C7' C9' 109.4(3) no C2' C7' C9' 113.8(3) no C8 C8a C4b 120.4(3) no C8 C8a C9 128.9(3) no C4b C8a C9 110.8(3) no C8a C8 C7 118.9(4) no C9a C9 C8a 101.6(2) no C9a C9 C1' 113.5(2) no C8a C9 C1' 114.5(3) no C1 C9a C4a 120.9(3) no C1 C9a C9 128.7(3) no C4a C9a C9 110.4(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C9a 1.377(4) no C1 C2 1.383(5) no C1' C6' 1.394(4) no C1' C2' 1.395(4) no C1' C9 1.529(4) yes C2 C3 1.377(5) no C2' C3' 1.400(4) no C2' C7' 1.524(5) yes C3 C4 1.380(5) no C3' C4' 1.377(5) no C4 C4a 1.396(4) no C4a C9a 1.398(4) no C4a C4b 1.461(4) no C4b C5 1.393(4) no C4b C8a 1.393(4) no C4' C5' 1.365(5) no C5 C6 1.376(5) no C5' C6' 1.370(4) no C6 C7 1.387(5) no C7 C8 1.394(5) no C7' C8' 1.510(5) no C7' C9' 1.533(4) no C8a C8 1.382(4) no C8a C9 1.518(4) no C9 C9a 1.517(4) no C2' C9 2.583(4) yes C6' C9 2.492(4) yes C1' C7' 2.554(4) yes C3' C7' 2.539(5) yes 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_publ_flag C9a C1 C2 C3 0.2(5) no C6' C1' C2' C3' 1.9(5) no C9 C1' C2' C3' -179.0(3) no C6' C1' C2' C7' -179.0(3) no C9 C1' C2' C7' 0.1(5) no C1 C2 C3 C4 0.0(6) no C1' C2' C3' C4' -1.9(5) no C7' C2' C3' C4' 179.0(3) no C2 C3 C4 C4a 0.1(5) no C3 C4 C4a C9a -0.4(5) no C3 C4 C4a C4b 179.9(3) no C4 C4a C4b C5 0.4(6) no C9a C4a C4b C5 -179.4(3) no C4 C4a C4b C8a 179.4(3) no C9a C4a C4b C8a -0.3(3) no C2' C3' C4' C5' 0.9(6) no C8a C4b C5 C6 0.1(5) no C4a C4b C5 C6 179.0(3) no C3' C4' C5' C6' 0.1(6) no C4b C5 C6 C7 0.0(6) no C4' C5' C6' C1' -0.1(6) no C2' C1' C6' C5' -1.0(6) no C9 C1' C6' C5' 179.9(3) no C5 C6 C7 C8 0.4(6) no C1' C2' C7' C8' -88.4(4) no C3' C2' C7' C8' 90.6(4) no C1' C2' C7' C9' 147.7(3) no C3' C2' C7' C9' -33.3(5) no C5 C4b C8a C8 -0.6(5) no C4a C4b C8a C8 -179.7(3) no C5 C4b C8a C9 178.9(3) no C4a C4b C8a C9 -0.2(3) no C4b C8a C8 C7 0.9(5) no C9 C8a C8 C7 -178.5(3) no C6 C7 C8 C8a -0.9(6) no C8 C8a C9 C9a -179.9(3) no C4b C8a C9 C9a 0.6(3) no C8 C8a C9 C1' -57.1(4) no C4b C8a C9 C1' 123.4(3) no C6' C1' C9 C9a 60.1(4) no C2' C1' C9 C9a -119.0(3) no C6' C1' C9 C8a -56.0(4) no C2' C1' C9 C8a 124.9(3) no C2 C1 C9a C4a -0.6(5) no C2 C1 C9a C9 179.1(3) no C4 C4a C9a C1 0.7(5) no C4b C4a C9a C1 -179.5(3) no C4 C4a C9a C9 -179.0(3) no C4b C4a C9a C9 0.7(3) no C8a C9 C9a C1 179.5(3) no C1' C9 C9a C1 56.0(4) no C8a C9 C9a C4a -0.8(3) no C1' C9 C9a C4a -124.3(3) no