#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/04/2000490.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_2000490 loop_ _publ_author_name 'Schaefer, W. P.' 'Krotz, A. H.' 'Kuo, L. Y.' 'Shields, T. P.' 'Barton, J. K.' _publ_section_title ; Metallointercalators: structure of rac-bis(ethylenediamine)(9,10-phenanthrenequinone diimine)rhodium(III) tribromide trihydrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2071 _journal_page_last 2073 _journal_paper_doi 10.1107/S0108270192006917 _journal_volume 48 _journal_year 1992 _chemical_formula_moiety 'C18 H26 Br3 N6 Rh1,3(H2 O1)' _chemical_formula_sum 'C18 H32 Br3 N6 O3 Rh' _chemical_formula_weight 723.11 _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 103.59(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.975(7) _cell_length_b 8.377(3) _cell_length_c 16.234(6) _cell_measurement_reflns_used 24 _cell_measurement_temperature 294 _cell_measurement_theta_max 8.4 _cell_measurement_theta_min 3.1 _cell_volume 2640.4(17) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents '0.080 for 1511 duplicates' _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 5284 _diffrn_reflns_theta_max 20 _diffrn_standards_decay_% 'within counting statistics' _diffrn_standards_interval_time 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.16 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_type empirical _exptl_crystal_colour Orange-red _exptl_crystal_density_diffrn 1.82 _exptl_crystal_description Lath _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.44 _refine_diff_density_min -1.64 _refine_ls_goodness_of_fit_obs 1.16 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 200 _refine_ls_number_reflns 2451 _refine_ls_R_factor_obs ; 0.116 for 2059 reflections with F~o~^2^>0, 0.052 for 1077 reflections with F~o~^2^>3\s(F~o~)^2^ ; _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(F~o~^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs '0.015 ' _reflns_number_observed 2451 _reflns_number_total 2451 _cod_data_source_file hh1011.cif _cod_data_source_block hh1011a _cod_depositor_comments ; Marking attached hydrogen atoms. Antanas Vaitkus, 2017-01-19 Adding the _atom_site_type_symbol data item. Antanas Vaitkus, 2017-01-19 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F~o~^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~o~^2^)]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2640(2) _cod_original_formula_sum 'C18 H32 Br3 N6 O3 Rh1' _cod_database_code 2000490 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_attached_hydrogens Rh Rh .17280(10) -.0080(2) .26140(10) .0284(4) 0 N1 N .2483(8) -.1607(16) .2560(9) 2.5(3) 0 C1 C .3108(9) -.119(2) .2921(10) 1.9(4) 0 C2 C .3724(10) -.217(2) .2982(12) 2.4(4) 0 C3 C .3672(11) -.371(2) .2633(13) 3.8(5) 0 C4 C .4257(11) -.463(2) .2717(12) 4.0(5) 0 C5 C .4887(11) -.395(2) .3096(13) 4.1(5) 0 C6 C .4948(11) -.247(3) .3407(13) 4.1(5) 0 C7 C .4367(10) -.146(2) .3350(11) 2.1(4) 0 C8 C .4418(9) .014(3) .3700(10) 2.9(4) 0 C9 C .5061(10) .083(2) .4081(12) 3.3(5) 0 C10 C .5094(11) .233(3) .4430(13) 3.9(5) 0 C11 C .4513(12) .316(2) .4473(13) 4.3(5) 0 C12 C .38770(10) .254(2) .4097(13) 3.5(5) 0 C13 C .3827(10) .108(2) .3708(11) 2.7(4) 0 C14 C .3157(9) .0406(18) .3278(10) 1.8(4) 0 N2 N .2577(8) .1106(15) .3209(9) 2.2(3) 0 N3 N .1624(8) -.0998(18) .3759(10) .040(6) 0 C15 C .1335(12) .026(3) .4193(13) .066(8) 0 C16 C .0792(12) .110(3) .3621(16) .069(8) 0 N4 N .1033(9) .1587(17) .2833(10) .045(6) 0 N5 N .0936(8) -.1423(17) .1895(10) .041(5) 0 C17 C .0958(12) -.135(2) .0970(14) .055(10) 0 C18 C .1145(12) .037(2) .0819(12) .054(8) 0 N6 N .1759(8) .0854(18) .1470(10) .040(5) 0 Br1 Br .94520(10) .0854(3) .1552(2) .0592(7) 0 Br2 Br .17640(10) .0171(3) .6748(2) .0657(8) 0 Br3 Br .32050(10) -.0022(3) .08070(10) .0625(7) 0 O1 O .6990(8) .1547(16) .5224(9) .073(5) 2 O2 O .2205(8) .0961(17) .8964(9) .074(5) 2 O3 O .3095(9) .1075(18) .5829(10) .096(6) 2 HN1 H .2387 -.2598 .2289 ? 0 H3 H .3226 -.4104 .2375 ? 0 H4 H .4196 -.5683 .2478 ? 0 H5 H .5280 -.4646 .3152 ? 0 H6 H .5395 -.2081 .3646 ? 0 H9 H .5474 .0272 .4099 ? 0 H10 H .5538 .2856 .4651 ? 0 H11 H .4521 .4102 .4771 ? 0 H12 H .3473 .3116 .4083 ? 0 HN2 H .2545 .2123 .3431 ? 0 HN3A H .2054 -.1343 .4098 ? 0 HN3B H .1319 -.1924 .3663 ? 0 H15A H .1674 .1022 .4408 ? 0 H15B H .1142 -.0164 .4621 ? 0 H16A H .0650 .2000 .3866 ? 0 H16B H .0399 .0387 .3432 ? 0 HN4A H .0658 .1643 .2348 ? 0 HN4B H .1253 .2597 .2926 ? 0 HN5A H .0509 -.1000 .1961 ? 0 HN5B H .0982 -.2493 .2091 ? 0 H17A H .0530 -.1651 .0625 ? 0 H17B H .1310 -.2050 .0874 ? 0 H18A H .0758 .1047 .0873 ? 0 H18B H .1211 .0488 .0272 ? 0 HN6A H .1779 .1993 .1501 ? 0 HN6B H .2154 .0476 .1297 ? 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Rh N2 77.1(6) N1 Rh N3 92.2(6) N1 Rh N4 172.0(6) N1 Rh N5 96.5(6) N1 Rh N6 91.2(6) N2 Rh N3 90.2(6) N2 Rh N4 96.3(6) N2 Rh N5 172.1(6) N2 Rh N6 92.6(6) N3 Rh N4 83.3(6) N3 Rh N5 94.6(6) N3 Rh N6 176.0(6) N4 Rh N5 90.5(6) N4 Rh N6 93.6(6) N5 Rh N6 82.9(6) Rh N1 C1 117.8(12) Rh N2 C14 117.4(12) Rh N3 C15 107.5(13) Rh N4 C16 108.8(13) Rh N5 C17 110.0(12) Rh N6 C18 110.5(12) C2 C1 N1 125.8(16) C14 C1 N1 113.3(15) C14 C1 C2 120.9(15) C3 C2 C1 120.5(17) C7 C2 C1 117.3(16) C7 C2 C3 122.0(17) C4 C3 C2 119.5(19) C5 C4 C3 118.4(19) C6 C5 C4 123.(2) C7 C6 C5 122.(2) C6 C7 C2 115.3(17) C8 C7 C2 121.8(17) C8 C7 C6 122.8(17) C9 C8 C7 121.6(17) C13 C8 C7 122.3(17) C13 C8 C9 116.1(17) C10 C9 C8 120.4(18) C11 C10 C9 122.(2) C12 C11 C10 120.(2) C13 C12 C11 119.9(19) C12 C13 C8 122.0(18) C14 C13 C8 116.6(16) C14 C13 C12 121.4(17) C13 C14 C1 120.8(15) N2 C14 C1 114.4(15) N2 C14 C13 124.8(15) C16 C15 N3 111.4(19) N4 C16 C15 109.5(19) C18 C17 N5 105.1(16) N6 C18 C17 109.8(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Rh N1 1.996(15) Rh N2 2.007(14) Rh N3 2.066(15) Rh N4 2.058(16) Rh N5 2.065(16) Rh N6 2.029(16) N1 C1 1.29(2) N1 HN1 0.938 C1 C2 1.46(3) C1 C14 1.45(2) C2 C3 1.40(3) C2 C7 1.41(3) C3 C4 1.38(3) C3 H3 0.951 C4 C5 1.39(3) C4 H4 0.964 C5 C6 1.33(3) C5 H5 0.966 C6 C7 1.42(3) C6 H6 0.945 C7 C8 1.45(3) C8 C9 1.41(3) C8 C13 1.42(3) C9 C10 1.38(3) C9 H9 0.943 C10 C11 1.37(3) C10 H10 0.980 C11 C12 1.37(3) C11 H11 0.925 C12 C13 1.37(3) C12 H12 0.935 C13 C14 1.47(3) C14 N2 1.28(2) N2 HN2 0.934 N3 C15 1.46(3) N3 HN3A 0.951 N3 HN3B 0.976 C15 C16 1.44(3) C15 H15A 0.936 C15 H15B 0.940 C16 N4 1.52(3) C16 H16A 0.928 C16 H16B 0.976 N4 HN4A 952 N4 HN4B 0.948 N5 C17 1.51(3) N5 HN5A 0.952 N5 HN5B 0.948 C17 C18 1.52(3) C17 H17A 0.939 C17 H17B 0.953 C18 N6 1.48(3) C18 H18A 0.981 C18 H18B 0.933 N6 HN6A 0.956 N6 HN6B 0.953 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139053357