#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/12/2101246.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_2101246 loop_ _publ_author_name 'Crano, J.' 'Knowles, D.' 'Kwiatkowski, P.' 'Flood, T.' 'Ross, R.' 'Chiang, L.' 'Lasch, J.' 'Chadha, R.' 'Siuzdak, G.' _publ_section_title ; Structure of three novel photochromic compounds; X-ray crystallographic and theoretical studies ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 772 _journal_page_last 779 _journal_paper_doi 10.1107/S0108768194005938 _journal_volume 50 _journal_year 1994 _chemical_formula_sum 'C21 H24 N2 O4' _chemical_formula_weight 368.4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 99.31(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.025(2) _cell_length_b 12.415(3) _cell_length_c 19.319(4) _cell_measurement_reflns_used 15 _cell_measurement_temperature 173 _cell_measurement_theta_max 30 _cell_measurement_theta_min 20 _cell_volume 1899.4(8) _diffrn_measurement_device 'Rigaku AFC-6R four-circle' _diffrn_measurement_method 2\q-\q _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.005 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 2401 _diffrn_reflns_theta_max 59.0 _diffrn_standards_decay_% 'not significant' _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.288 _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.30 _refine_diff_density_min -0.22 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.56 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 244 _refine_ls_number_reflns 1611 _refine_ls_R_factor_obs 0.0486 _refine_ls_shift/esd_max 0.010 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)+gF^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0749 _reflns_number_observed 1611 _reflns_number_total 1995 _reflns_observed_criterion F>4.0\s(F) _[local]_cod_data_source_file st1087.cif _[local]_cod_data_source_block st1087b _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F)+gF^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F)+gF^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2101246 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O(1) .7008(3) .0151(2) .4156(2) .0590(10) O(2) .1274(3) .3360(2) .34960(10) .0350(10) O(3) -.2018(3) .6524(2) .31360(10) .0430(10) O(4) -.2430(3) .3897(2) .13290(10) .0500(10) N(1) .3971(3) .4157(2) .39200(10) .0370(10) N(2) .0262(4) .5334(2) .4003(2) .0430(10) C(1) .8294(5) -.0140(3) .3767(2) .064(2) C(2) .6395(4) .1191(3) .4071(2) .0410(10) C(3) .4995(4) .1402(3) .4403(2) .0430(10) C(4) .4288(4) .2422(3) .4331(2) .0340(10) C(5) .4957(4) .3201(3) .3940(2) .0330(10) C(6) .6320(4) .2989(3) .3627(2) .0400(10) C(7) .7055(4) .1983(3) .3697(2) .0420(10) C(8) .2817(4) .2916(3) .4627(2) .0400(10) C(9) .1394(5) .2124(4) .4653(2) .069(2) C(10) .3479(6) .3337(4) .5363(2) .064(2) C(11) .2357(4) .3849(3) .4104(2) .0350(10) C(12) .4025(5) .4912(3) .3350(2) .0460(10) C(13) .1468(5) .4800(3) .4359(2) .0450(10) C(14) -.0346(4) .4970(3) .3318(2) .0330(10) C(15) .0146(4) .3991(3) .3073(2) .0320(10) C(16) -.0514(4) .3576(3) .2422(2) .0340(10) C(17) -.1710(4) .4188(3) .1993(2) .0360(10) C(18) -.2226(4) .5190(3) .2209(2) .0380(10) C(19) -.1567(4) .5573(3) .2868(2) .0370(10) C(20) -.3366(4) .7114(3) .2727(2) .0500(10) C(21) -.2007(5) .2866(3) .1088(2) .0530(10) H1A .8619 -.0875 .3867 ? H1B .9254 .0321 .3896 ? H1C .7878 -.0063 .3275 ? H3A .4543 .0855 .4671 ? H6A .6769 .3536 .3358 ? H7A .8031 .1834 .3484 ? H9A .0984 .1863 .4189 ? H9B .0493 .2476 .4836 ? H9C .1802 .1530 .4951 ? H10A .2566 .3653 .5558 ? H10B .4333 .3871 .5339 ? H10C .3953 .2752 .5655 ? H12A .3307 .5515 .3402 ? H12B .3642 .4562 .2911 ? H12C .5163 .5159 .3362 ? H13A .1842 .5028 .4833 ? H16A -.0158 .2888 .2272 ? H18A -.3033 .5611 .1902 ? H20A -.3567 .7765 .2968 ? H20B -.4372 .6682 .2659 ? H20C -.3062 .7289 .2280 ? H21A -.2587 .2756 .0618 ? H21B -.2339 .2319 .1390 ? H21C -.0811 .2827 .1093 ? 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 C(1) O(1) C(2) 116.8(3) yes C(19) O(3) C(20) 117.2(3) yes C(5) N(1) C(11) 106.8(3) yes C(11) N(1) C(12) 119.6(3) yes O(1) C(2) C(3) 114.5(3) yes C(3) C(2) C(7) 120.7(3) yes C(3) C(4) C(5) 120.2(3) yes C(5) C(4) C(8) 108.3(3) yes N(1) C(5) C(6) 129.4(3) yes C(5) C(6) C(7) 119.6(3) yes C(4) C(8) C(9) 112.7(3) yes C(9) C(8) C(10) 109.9(3) yes C(9) C(8) C(11) 114.1(3) yes O(2) C(11) N(1) 110.4(3) yes N(1) C(11) C(8) 103.3(2) yes N(1) C(11) C(13) 111.3(3) yes N(2) C(13) C(11) 126.1(3) yes N(2) C(14) C(19) 120.5(3) yes O(2) C(15) C(14) 119.9(3) yes C(14) C(15) C(16) 123.3(3) yes O(4) C(17) C(16) 124.2(3) yes C(16) C(17) C(18) 121.3(3) yes O(3) C(19) C(14) 115.2(3) yes C(14) C(19) C(18) 120.5(3) yes C(11) O(2) C(15) 119.2(2) yes C(17) O(4) C(21) 117.3(3) yes C(5) N(1) C(12) 118.3(3) yes C(13) N(2) C(14) 117.1(3) yes O(1) C(2) C(7) 124.8(3) yes C(2) C(3) C(4) 118.0(3) yes C(3) C(4) C(8) 131.4(3) yes N(1) C(5) C(4) 109.5(3) yes C(4) C(5) C(6) 121.1(3) yes C(2) C(7) C(6) 120.3(3) yes C(4) C(8) C(10) 108.3(3) yes C(4) C(8) C(11) 100.1(3) yes C(10) C(8) C(11) 111.3(3) yes O(2) C(11) C(8) 105.1(3) yes O(2) C(11) C(13) 109.6(2) yes C(8) C(11) C(13) 116.8(3) yes N(2) C(14) C(15) 121.9(3) yes C(15) C(14) C(19) 117.6(3) yes O(2) C(15) C(16) 116.7(3) yes C(15) C(16) C(17) 117.7(3) yes O(4) C(17) C(18) 114.5(3) yes C(17) C(18) C(19) 119.6(3) yes O(3) C(19) C(18) 124.3(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O(1) C(1) 1.418(5) yes O(2) C(11) 1.474(4) yes O(3) C(19) 1.361(4) yes O(4) C(17) 1.368(4) yes N(1) C(5) 1.423(4) yes N(1) C(12) 1.453(5) yes N(2) C(14) 1.409(4) yes C(2) C(7) 1.375(5) yes C(4) C(5) 1.388(5) yes C(5) C(6) 1.359(5) yes C(8) C(9) 1.515(6) yes C(8) C(11) 1.542(5) yes C(14) C(15) 1.384(5) yes C(15) C(16) 1.384(4) yes C(17) C(18) 1.396(5) yes O(1) C(2) 1.382(4) yes O(2) C(15) 1.364(4) yes O(3) C(20) 1.434(4) yes O(4) C(21) 1.422(5) yes N(1) C(11) 1.448(4) yes N(2) C(13) 1.278(4) yes C(2) C(3) 1.405(5) yes C(3) C(4) 1.385(5) yes C(4) C(8) 1.521(5) yes C(6) C(7) 1.379(5) yes C(8) C(10) 1.528(5) yes C(11) C(13) 1.508(5) yes C(14) C(19) 1.414(4) yes C(16) C(17) 1.388(4) yes C(18) C(19) 1.381(5) yes