#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/50/2005018.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_2005018 loop_ _publ_author_name 'Lorenzo Luis, P. A.' 'Martin-Zarza, P.' 'Gili, P.' 'Ruiz-P\'erez, C.' 'Hern\'andez-Molina, M.' 'Solans, X.' _publ_section_title ; Five New Chlorochromates of Organic Bases ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1441 _journal_page_last 1448 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '(C10 H9 Cl N3) [Cr O3 Cl]' _chemical_formula_sum 'C10 H9 Cl2 Cr N3 O3' _chemical_formula_weight 342.10 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 92.83(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.396(2) _cell_length_b 10.915(5) _cell_length_c 19.192(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 18 _cell_measurement_theta_min 6 _cell_volume 1338.2(8) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 4009 _diffrn_reflns_theta_max 30 _diffrn_standards_decay_% <10 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.26 _exptl_absorpt_correction_type none _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 1.050 _refine_diff_density_min -0.518 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.164 _refine_ls_hydrogen_treatment 'H atoms see text' _refine_ls_number_parameters 195 _refine_ls_number_reflns 1981 _refine_ls_R_factor_obs 0.056 _refine_ls_shift/esd_max 0.023 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 1/[\s^2^(F)+0.00242F^2^] _refine_ls_wR_factor_obs 0.073 _reflns_number_observed 2472 _reflns_number_total 3874 _reflns_observed_criterion I>3\s(I) _[local]_cod_data_source_file ka1153.cif _[local]_cod_data_source_block 5 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2005018 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Cr(1) 0.12061(2) 0.21256(2) 0.15440(7) .0516(5) Cl(1) 0.25239(6) 0.39451(4) 0.15331(2) .0893(13) O(1) -0.1233(4) 0.2258(3) 0.1696(3) .0824(30) O(2) 0.1549(3) 0.1488(3) 0.0810(3) .0654(25) O(3) 0.2440(3) 0.14045(3) 0.21514(4) .1100(47) Cl(2) 0.8154(4) 0.5498(2) 0.1033(1) .0534(7) C(1) 0.3385(4) 0.7274(3) 0.0051(3) .0533(28) C(2) 0.5177(4) 0.6602(2) 0.0162(2) .0601(33) C(3) 0.5876(2) 0.6352(2) 0.0851(2) .0616(36) C(4) 0.4695(3) 0.6770(2) 0.1397(4) .0549(33) N(5) 0.2901(2) 0.7415(3) 0.1286(3) .0502(22) C(6) 0.2251(3) 0.7676(3) 0.0631(3) .0434(25) N(7) 0.0438(3) 0.8339(2) 0.0522(3) .0509(24) C(8) -0.0842(2) 0.8794(2) 0.1001(2) .0430(23) N(9) -0.0414(2) 0.8567(2) 0.1683(2) .0488(23) C(10) -0.1715(2) 0.8982(3) 0.2187(2) .0489(26) C(11) -0.3440(2) 0.9627(3) 0.2003(3) .0528(29) C(12) -0.3924(3) 0.9863(3) 0.1297(3) .0572(31) C(13) -0.2612(3) 0.9450(2) 0.0797(2) .0524(28) H1 0.28959(67) 0.74561(94) -0.03953(102) ? H2 0.59133(74) 0.63563(94) -0.02074(108) ? H4 0.51251(81) 0.65920(93) 0.18498(114) ? H10 -0.13553(95) 0.88382(100) 0.26521(104) ? H11 -0.43518(79) 0.98743(98) 0.23393(101) ? H12 -0.50882(87) 1.03239(94) 0.11618(102) ? H13 -0.29311(100) 0.96099(86) 0.03319(105) ? 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) Cr(1) O(2) 112.1(2) yes O(1) Cr(1) O(3) 111.4(2) yes O(2) Cr(1) O(3) 110.3(2) yes Cl(1) Cr(1) O(1) 107.60(10) yes Cl(1) Cr(1) O(2) 108.80(10) yes Cl(1) Cr(1) O(3) 106.50(10) yes C(2) C(1) C(6) 119.8(3) yes C(1) C(2) C(3) 118.5(3) yes Cl(2) C(3) C(2) 121.1(2) yes C(2) C(3) C(4) 119.0(2) yes Cl(2) C(3) C(4) 119.9(3) yes C(3) C(4) N(5) 122.4(6) yes C(4) N(5) C(6) 118.8(4) yes C(1) C(6) N(5) 121.5(2) yes N(5) C(6) N(7) 118.5(3) yes C(1) C(6) N(7) 120.0(3) yes C(6) N(7) C(8) 128.5(3) yes N(7) C(8) C(13) 120.7(3) yes N(7) C(8) N(9) 119.5(2) yes N(9) C(8) C(13) 119.8(3) yes C(8) N(9) C(10) 121.3(2) yes N(9) C(10) C(11) 120.2(4) yes C(10) C(11) C(12) 119.4(2) yes C(11) C(12) C(13) 120.0(4) yes C(8) C(13) C(12) 119.2(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cr(1) Cl(1) 2.1580(10) yes Cr(1) O(1) 1.608(3) yes Cr(1) O(2) 1.596(6) yes Cr(1) O(3) 1.583(6) yes Cl(2) C(3) 1.750(3) yes C(1) C(2) 1.369(3) yes C(1) C(6) 1.427(5) yes C(2) C(3) 1.400(5) yes C(3) C(4) 1.400(8) yes C(4) N(5) 1.354(3) yes N(5) C(6) 1.335(7) yes C(6) N(7) 1.374(3) yes N(7) C(8) 1.356(6) yes C(8) N(9) 1.345(6) yes C(8) C(13) 1.381(3) yes N(9) C(10) 1.383(5) yes C(10) C(11) 1.341(3) yes C(11) C(12) 1.398(7) yes C(12) C(13) 1.382(5) yes _journal_paper_doi 10.1107/S0108270196000637