#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003783.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003783 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1995 _journal_volume 51 _journal_page_first 1621 _journal_page_last 1627 _publ_section_title ; 4-Substituted 1-Methyl-1H-2,3-benzodiazepine Compounds ; _chemical_formula_moiety 'C22 H24 N2 O2' _chemical_formula_sum 'C22 H24 N2 O2' _chemical_formula_weight 348.43 _symmetry_cell_setting Orthorhombic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z' 'x, y-1/2, -z-1/2' _symmetry_space_group_name_H-M 'P c a b' _cell_length_a 12.962(2) _cell_length_b 13.4604(8) _cell_length_c 22.2464(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3881.5(6) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 42 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 12.5 _exptl_absorpt_coefficient_mu 0.077 _cell_measurement_temperature 298(2) _exptl_crystal_description Block _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.42 _exptl_crystal_colour 'Pale yellow--green' _diffrn_measurement_device 'Stoe Stadi-4 four-circle diffractometer' _diffrn_measurement_method ; \w-2\q scans using on-line profile fitting (Clegg, 1981) ; _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2541 _reflns_number_total 2541 _reflns_number_observed 2139 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 22.52 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0345 _refine_ls_wR_factor_obs 0.0938 _refine_ls_wR_factor_all 0.0992 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_number_reflns 2538 _refine_ls_number_parameters 236 _refine_ls_weighting_scheme ;calc w = 1/[s^2^(Fo^2^) + (0.0485P)^2^ + 0.6225P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.113 _refine_diff_density_min -0.121 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0044(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.0060 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.13299(12) 0.33571(13) 0.58551(8) 0.0550(4) H1 1 0.11639(12) 0.32963(13) 0.62833(8) 0.066 C1m 1 0.04611(14) 0.3900(2) 0.55427(10) 0.0816(6) H1M1 1 -0.01757(14) 0.3554(2) 0.56106(10) 0.122 H1M2 1 0.05980(14) 0.3929(2) 0.51190(10) 0.122 H1M3 1 0.04091(14) 0.4562(2) 0.57002(10) 0.122 N2 1 0.14029(10) 0.23410(11) 0.55882(6) 0.0565(4) N3 1 0.18049(11) 0.16703(11) 0.59002(6) 0.0536(4) C4 1 0.22999(12) 0.18390(12) 0.64570(6) 0.0474(4) C5 1 0.29828(12) 0.25755(12) 0.65467(7) 0.0473(4) H5 1 0.33765(12) 0.25420(12) 0.68956(7) 0.057 C5a 1 0.31675(12) 0.34153(11) 0.61553(7) 0.0450(4) C6 1 0.41400(13) 0.38592(13) 0.61394(8) 0.0564(4) H6 1 0.46585(13) 0.36253(13) 0.63913(8) 0.068 C7 1 0.43416(14) 0.46333(14) 0.57589(8) 0.0667(5) H7 1 0.49948(14) 0.49189(14) 0.57510(8) 0.080 C8 1 0.35769(15) 0.49890(14) 0.53877(8) 0.0670(5) H8 1 0.37188(15) 0.55066(14) 0.51235(8) 0.080 C9 1 0.26072(14) 0.45843(13) 0.54055(7) 0.0586(5) H9 1 0.20948(14) 0.48351(13) 0.51553(7) 0.070 C9a 1 0.23793(12) 0.38034(11) 0.57929(7) 0.0473(4) C1' 1 0.21374(13) 0.09823(12) 0.68846(7) 0.0530(4) H1' 1 0.14690(13) 0.06820(12) 0.67878(7) 0.064 C2' 1 0.2944(2) 0.01413(13) 0.68940(8) 0.0656(5) C21' 1 0.3033(2) -0.0281(2) 0.62569(9) 0.0859(7) H2A' 1 0.2368(2) -0.0506(2) 0.61246(9) 0.129 H2B' 1 0.3508(2) -0.0829(2) 0.62567(9) 0.129 H2C' 1 0.3279(2) 0.0227(2) 0.59899(9) 0.129 C22' 1 0.3998(2) 0.0500(2) 0.71081(10) 0.0874(7) H2D' 1 0.4244(2) 0.1011(2) 0.68435(10) 0.131 H2E' 1 0.4475(2) -0.0046(2) 0.71072(10) 0.131 H2F' 1 0.3938(2) 0.0761(2) 0.75082(10) 0.131 C23' 1 0.2550(2) -0.0674(2) 0.73148(10) 0.1019(8) H2G' 1 0.1887(2) -0.0899(2) 0.71793(10) 0.153 H2H' 1 0.2490(2) -0.0414(2) 0.77151(10) 0.153 H2I' 1 0.3026(2) -0.1220(2) 0.73140(10) 0.153 O1' 1 0.20741(8) 0.13609(8) 0.74953(5) 0.0542(3) C3' 1 0.11859(14) 0.17934(13) 0.76603(8) 0.0556(4) O3' 1 0.04901(10) 0.19375(12) 0.73132(6) 0.0838(4) C1p 1 0.11671(12) 0.20635(12) 0.83028(7) 0.0525(4) C2p 1 0.19944(15) 0.19121(15) 0.86803(8) 0.0650(5) H2P 1 0.25925(15) 0.16165(15) 0.85342(8) 0.078 C3p 1 0.1938(2) 0.2198(2) 0.92749(9) 0.0769(6) H3P 1 0.2502(2) 0.2106(2) 0.95269(9) 0.092 C4p 1 0.1059(2) 0.2614(2) 0.94931(9) 0.0792(6) H4P 1 0.1025(2) 0.2806(2) 0.98942(9) 0.095 C5p 1 0.0224(2) 0.2751(2) 0.91264(11) 0.0865(7) H5P 1 -0.0380(2) 0.3026(2) 0.92797(11) 0.104 C6p 1 0.0279(2) 0.2483(2) 0.85303(9) 0.0733(6) H6P 1 -0.0285(2) 0.2585(2) 0.82799(9) 0.088 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0587(10) 0.0066(8) -0.0034(7) 0.0598(11) 0.0001(9) 0.0464(9) C1m 0.0669(12) 0.0130(10) -0.0144(10) 0.090(2) 0.0078(12) 0.0880(15) N2 0.0634(9) -0.0057(7) -0.0075(6) 0.0611(10) 0.0007(7) 0.0448(8) N3 0.0686(9) -0.0086(7) -0.0047(6) 0.0525(9) -0.0019(7) 0.0398(8) C4 0.0644(10) -0.0009(7) -0.0029(7) 0.0433(9) -0.0033(7) 0.0345(8) C5 0.0629(9) 0.0021(7) -0.0067(7) 0.0437(9) -0.0013(7) 0.0352(8) C5a 0.0588(9) 0.0016(7) -0.0008(7) 0.0392(9) -0.0020(7) 0.0371(8) C6 0.0615(10) -0.0016(8) -0.0067(8) 0.0523(11) 0.0031(9) 0.0554(10) C7 0.0705(11) -0.0102(9) 0.0041(9) 0.0585(12) 0.0076(10) 0.0711(13) C8 0.0874(13) -0.0017(10) 0.0087(10) 0.0520(11) 0.0145(9) 0.0614(12) C9 0.0751(12) 0.0095(9) -0.0031(8) 0.0520(11) 0.0059(8) 0.0487(10) C9a 0.0605(10) 0.0059(7) -0.0005(7) 0.0442(9) -0.0024(7) 0.0371(8) C1' 0.0761(11) -0.0098(8) -0.0021(7) 0.0462(10) -0.0013(7) 0.0368(9) C2' 0.1011(14) 0.0035(9) -0.0054(9) 0.0438(10) 0.0016(8) 0.0520(11) C21' 0.131(2) 0.0152(12) -0.0001(11) 0.0577(13) -0.0123(11) 0.0687(13) C22' 0.102(2) 0.0258(12) -0.0166(12) 0.0722(15) -0.0050(12) 0.088(2) C23' 0.175(2) 0.0018(14) 0.0024(14) 0.0531(13) 0.0187(12) 0.0779(15) O1' 0.0703(8) -0.0043(5) -0.0010(5) 0.0549(7) 0.0007(5) 0.0375(6) C3' 0.0625(11) -0.0077(8) -0.0027(8) 0.0543(11) 0.0020(8) 0.0499(10) O3' 0.0792(9) 0.0097(8) -0.0200(7) 0.1080(12) -0.0124(8) 0.0642(9) C1p 0.0653(10) -0.0081(8) 0.0009(8) 0.0460(10) 0.0012(8) 0.0462(10) C2p 0.0766(12) 0.0036(9) -0.0019(9) 0.0698(13) -0.0029(9) 0.0485(11) C3p 0.103(2) 0.0001(12) -0.0063(10) 0.0811(15) -0.0063(10) 0.0466(12) C4p 0.118(2) -0.0134(12) 0.0144(12) 0.0675(14) -0.0126(10) 0.0520(11) C5p 0.095(2) 0.0020(12) 0.0240(13) 0.083(2) -0.0210(12) 0.082(2) C6p 0.0724(13) 0.0015(10) 0.0009(10) 0.0752(13) -0.0085(11) 0.0723(13) _cod_database_code 2003783