#------------------------------------------------------------------------------ #$Date: 2017-01-30 16:01:18 +0200 (Mon, 30 Jan 2017) $ #$Revision: 191095 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/59/2005905.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_2005905 loop_ _publ_author_name 'Gerber, T. I. A.' 'Perils, J.' 'Du Preez, J. G. H.' 'Bandoli, G.' _publ_section_title ;Chelation of 2,6-Bis(hydroxymethyl)pyridine in cis-Dichloro(triphenylphosphine-P)[2-(oxymethylene-O)-6-(hydroxymethyl)pyridine-N]oxorhenium(V)--Water (2/1) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 217 _journal_page_last 219 _journal_paper_doi 10.1107/S0108270196013030 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '2[Re Cl2 O (C7 H8 N O2) (C18 H15 P)], H2 O' _chemical_formula_sum 'C50 H48 Cl4 N2 O7 P2 Re2' _chemical_formula_weight 1365.0 _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 16.331(6) _cell_length_b 29.61(1) _cell_length_c 10.854(5) _cell_measurement_reflns_used 40 _cell_measurement_temperature 296 _cell_measurement_theta_max 14 _cell_measurement_theta_min 8 _cell_volume 5249(4) _computing_cell_refinement SHELXTL-Plus _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1987)' _computing_data_reduction SHELXTL-Plus _computing_molecular_graphics SHELXTL-Plus _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution SHELXTL-Plus _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5162 _diffrn_reflns_theta_max 25.0 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 250 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 4.923 _exptl_absorpt_correction_T_max 0.48 _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_type 'empirical (four \y scans) (North, Phillips & Mathews, 1968)' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_meas ? _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.87 _refine_diff_density_min -1.67 _refine_ls_abs_structure_details 'Flack (1983) = -0.003(19)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.85 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 419 _refine_ls_number_reflns 3741 _refine_ls_R_factor_obs 0.0443 _refine_ls_shift/esd_max 0.48 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)+0.0049F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0597 _reflns_number_observed 3741 _reflns_number_total 4880 _reflns_observed_criterion F>4.0\s(F) _cod_data_source_file ab1373.cif _cod_data_source_block ab1373a _cod_depositor_comments ; Adding the _atom_site_type_symbol data item. Antanas Vaitkus, 2017-01-30 The following automatic conversions were performed: '_geom_bond_publ_flag' value 'NO' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (12 times). '_geom_angle_publ_flag' value 'NO' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (30 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.0049F^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)+0.0049F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2005905 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2+x,1/2-y,z 1/2-x,1/2+y,1/2+z 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 Re(1) Re .1750(1) .8734(1) .7302 .039(1) Cl(1A) Cl .0859(3) .9386(2) .7335(9) .061(2) Cl(2A) Cl .1424(3) .8650(2) .5201(7) .060(2) P(1A) P .2647(2) .8065(1) .7183(7) .034(1) O(1A) O .1096(7) .8371(4) .7967(15) .050(5) O(2A) O .2711(8) .9074(5) .6869(13) .047(5) O(3A) O .0712(10) .8908(7) 1.1470(18) .075(7) N(1A) N .2264(10) .8964(5) .9072(18) .045(6) C(1A) C .1925(12) .8956(6) 1.016(2) .044(7) C(2A) C .2381(15) .9063(8) 1.121(2) .060(9) C(3A) C .3192(16) .9204(9) 1.108(2) .065(10) C(4A) C .3493(14) .9231(7) .997(3) .052(8) C(5A) C .3064(10) .9130(6) .896(2) .040(6) C(6A) C .3342(11) .9181(6) .766(2) .042(6) C(7A) C .1013(13) .8874(10) 1.030(2) .077(10) C(8A) C .2070(10) .7543(10) .721(2) .040(4) C(9A) C .2275(10) .7184(5) .7975(16) .030(4) C(10A) C .1876(13) .6782(7) .788(2) .051(5) C(11A) C .1219(12) .6718(6) .707(2) .044(5) C(12A) C .1008(13) .7096(7) .637(2) .049(5) C(13A) C .1409(12) .7489(7) .641(2) .042(5) C(14A) C .3310(14) .8038(7) .8486(18) .034(5) C(15A) C .3008(11) .8001(6) .9699(17) .035(4) C(16A) C .3493(13) .8039(7) 1.066(2) .049(6) C(17A) C .4300(13) .8099(8) 1.057(2) .044(5) C(18A) C .4643(15) .8142(8) .938(2) .052(6) C(19A) C .4146(13) .8105(7) .838(2) .046(5) C(20A) C .3316(3) .8001(7) .5850(17) .031(5) C(21A) C .3653(13) .7551(8) .563(2) .053(6) C(22A) C .4205(14) .7484(8) .467(2) .055(6) C(23A) C .4376(15) .7850(9) .388(2) .057(6) C(24A) C .4053(16) .8274(9) .410(2) .061(6) C(25A) C .3508(12) .8351(7) .5115(19) .043(5) Re(2) Re .6286(1) .9172(1) .2141(1) .040(1) Cl(1B) Cl .5233(3) .9752(2) .2146(10) .070(2) Cl(2B) Cl .5990(3) .9056(2) .0051(7) .060(2) P(1B) P .7395(2) .8610(2) .2095(6) .031(1) O(1B) O .5741(7) .8768(4) .2769(12) .045(4) O(2B) O .7104(9) .9588(5) .1769(16) .065(6) O(3B) O .5155(13) .9214(7) .628(2) .097(8) N(1B) N .6690(10) .9449(5) .3928(18) .041(6) C(1B) C .6353(14) .9400(7) .501(2) .051(8) C(2B) C .6738(16) .9531(8) .609(3) .073(10) C(3B) C .7458(19) .9751(9) .600(3) .077(11) C(4B) C .7794(16) .9818(8) .483(3) .080(12) C(5B) C .7390(13) .9677(7) .383(3) .058(8) C(6B) C .7691(12) .9746(6) .2510(17) .045(7) C(7B) C .5471(16) .9160(11) .509(3) .100(14) C(8B) C .6997(9) .8043(5) .227(3) .034(3) C(9B) C .7200(12) .7719(7) .308(2) .041(5) C(10B) C .6869(14) .7314(9) .310(2) .064(6) C(11B) C .6312(11) .7170(6) .226(3) .050(4) C(12B) C .6129(13) .7477(7) .1270(19) .043(5) C(13B) C .6462(12) .7891(8) .129(2) .049(6) C(14B) C .8048(13) .8605(7) .0721(19) .038(5) C(15B) C .8520(13) .8222(7) .053(2) .048(5) C(16B) C .9095(15) .8206(8) -.044(2) .061(6) C(17B) C .9169(16) .8563(9) -.113(2) .060(7) C(18B) C .8701(16) .8933(9) -.099(2) .061(6) C(19B) C .8153(13) .8961(7) .000(2) .047(5) C(20B) C .8101(13) .8656(7) .3391(19) .036(5) C(21B) C .7833(13) .8605(7) .455(2) .045(5) C(22B) C .8330(15) .8673(8) .552(2) .055(6) C(23B) C .9124(17) .8809(9) .539(2) .057(6) C(24B) C .9445(16) .8850(8) .416(2) .060(6) C(25B) C .8921(14) .8783(7) .319(2) .051(6) OW O .0596(16) .9793(9) .208(3) .063(7) H(2AA) H .2144 .9039 1.2019 ? H(3AA) H .3531 .9259 1.1791 ? H(4AA) H .4015 .9373 .9841 ? H(6AA) H .3794 .8981 .7513 ? H(6AB) H .3531 .9486 .7545 ? H(7AA) H .0975 .8555 1.0155 ? H(7AB) H .0691 .9026 .9682 ? H(9AA) H .2707 .7222 .8565 ? H(10A) H .2023 .6537 .8412 ? H(11A) H .0933 .6435 .7018 ? H(12A) H .0576 .7058 .5782 ? H(13A) H .1262 .7734 .5876 ? H(15A) H .2431 .7951 .9793 ? H(16A) H .3260 .8012 1.1465 ? H(17A) H .4644 .8121 1.1289 ? H(18A) H .5221 .8191 .9291 ? H(19A) H .4380 .8131 .7570 ? H(21A) H .3512 .7306 .6172 ? H(22A) H .4436 .7190 .4536 ? H(23A) H .4748 .7800 .3212 ? H(24A) H .4194 .8519 .3561 ? H(25A) H .3277 .8645 .5247 ? H(2BA) H .6504 .9479 .6891 ? H(3BA) H .7754 .9851 .6717 ? H(4BA) H .8303 .9974 .4697 ? H(6BA) H .8199 .9589 .2390 ? H(6BB) H .7789 1.0063 .2393 ? H(7BA) H .5540 .8843 .4932 ? H(7BB) H .5115 .9282 .4475 ? H(9BA) H .7570 .7810 .3717 ? H(10B) H .7005 .7107 .3756 ? H(11B) H .6077 .6873 .2266 ? H(12B) H .5759 .7386 .0629 ? H(13B) H .6327 .8098 .0640 ? H(15B) H .8453 .7966 .1067 ? H(16B) H .9417 .7939 -.0568 ? H(17B) H .9558 .8552 -.1797 ? H(18B) H .8767 .9189 -.1526 ? H(19B) H .7831 .9228 .0131 ? H(21B) H .7275 .8516 .4683 ? H(22B) H .8130 .8633 .6340 ? H(23B) H .9481 .8859 .6080 ? H(24B) H 1.0003 .8939 .4031 ? H(25B) H .9121 .8823 .2371 ? 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 Cl(1A) Re(1) Cl(2A) 87.8(3) no Cl(1A) Re(1) P(1A) 177.8(3) no Cl(1A) Re(1) O(1A) 97.1(4) no Cl(1A) Re(1) O(2A) 94.4(4) no Cl(1A) Re(1) N(1A) 88.2(5) no Cl(2A) Re(1) P(1A) 89.9(2) no Cl(2A) Re(1) O(1A) 101.8(6) no Cl(2A) Re(1) O(2A) 90.2(4) no Cl(2A) Re(1) N(1A) 164.3(5) no P(1A) Re(1) O(1A) 83.4(4) no P(1A) Re(1) O(2A) 85.6(4) no P(1A) Re(1) N(1A) 93.9(4) no O(1A) Re(1) O(2A) 163.7(6) no O(1A) Re(1) N(1A) 93.8(7) no O(2A) Re(1) N(1A) 75.0(6) no Cl(1B) Re(2) Cl(2B) 87.7(3) no Cl(1B) Re(2) P(1B) 177.4(2) no Cl(1B) Re(2) O(1B) 97.5(5) no Cl(1B) Re(2) O(2B) 92.3(5) no Cl(1B) Re(2) N(1B) 87.0(5) no Cl(2B) Re(2) P(1B) 91.9(2) no Cl(2B) Re(2) O(1B) 100.6(5) no Cl(2B) Re(2) O(2B) 92.0(6) no Cl(2B) Re(2) N(1B) 165.2(5) no P(1B) Re(2) O(1B) 85.1(4) no P(1B) Re(2) O(2B) 85.1(5) no P(1B) Re(2) N(1B) 92.8(4) no O(1B) Re(2) O(2B) 164.3(7) no O(1B) Re(2) N(1B) 93.9(6) no O(2B) Re(2) N(1B) 74.4(7) no Re(1) P(1A) C(8A) 112.1(5) no Re(1) P(1A) C(20A) 118.7(7) no Re(1) O(2A) C(6A) 125.0(10) no C(1A) N(1A) C(5A) 119(2) no C(2A) C(1A) C(7A) 118(2) no C(3A) C(4A) C(5A) 123(2) no C(4A) C(5A) C(6A) 126(2) no P(1A) C(8A) C(9A) 122(2) no C(8A) C(9A) C(10A) 120(2) no C(11A) C(12A) C(13A) 124(2) no P(1A) C(14A) C(19A) 122(2) no C(15A) C(16A) C(17A) 124(2) no C(14A) C(19A) C(18A) 122(2) no C(21A) C(20A) C(25A) 121(2) no C(22A) C(23A) C(24A) 121(2) no Re(2) P(1B) C(8B) 111.1(5) no Re(2) P(1B) C(20B) 113.5(7) no Re(2) O(2B) C(6B) 128.0(10) no C(1B) N(1B) C(5B) 119(2) no C(2B) C(1B) C(7B) 119(2) no C(3B) C(4B) C(5B) 120(2) no C(4B) C(5B) C(6B) 124(2) no P(1B) C(8B) C(9B) 130(2) no C(8B) C(9B) C(10B) 125(2) no C(11B) C(12B) C(13B) 119(2) no P(1B) C(14B) C(19B) 123(2) no C(15B) C(16B) C(17B) 118(2) no C(14B) C(19B) C(18B) 119(2) no C(21B) C(20B) C(25B) 119(2) no C(22B) C(23B) C(24B) 118(2) no Re(1) P(1A) C(14A) 110.8(7) no C(8A) P(1A) C(20A) 104.0(10) no Re(1) N(1A) C(1A) 128.0(10) no N(1A) C(1A) C(2A) 121(2) no C(1A) C(2A) C(3A) 119(2) no N(1A) C(5A) C(4A) 120(2) no O(2A) C(6A) C(5A) 110.0(10) no P(1A) C(8A) C(13A) 120(2) no C(9A) C(10A) C(11A) 122(2) no C(8A) C(13A) C(12A) 120(2) no C(15A) C(14A) C(19A) 116(2) no C(16A) C(17A) C(18A) 118(2) no P(1A) C(20A) C(21A) 117(2) no C(20A) C(21A) C(22A) 120(2) no C(23A) C(24A) C(25A) 121(2) no Re(2) P(1B) C(14B) 116.8(7) no C(8B) P(1B) C(20B) 102.0(10) no Re(2) N(1B) C(1B) 129.0(10) no N(1B) C(1B) C(2B) 123(2) no C(1B) C(2B) C(3B) 118(3) no N(1B) C(5B) C(4B) 121(2) no O(2B) C(6B) C(5B) 107(2) no P(1B) C(8B) C(13B) 115(2) no C(9B) C(10B) C(11B) 123(2) no C(8B) C(13B) C(12B) 123(2) no C(15B) C(14B) C(19B) 120(2) no C(16B) C(17B) C(18B) 123(2) no P(1B) C(20B) C(21B) 121(2) no C(20B) C(21B) C(22B) 121(2) no C(23B) C(24B) C(25B) 118(2) no C(8A) P(1A) C(14A) 105.0(10) no C(14A) P(1A) C(20A) 105.0(10) no Re(1) N(1A) C(5A) 113.0(10) no N(1A) C(1A) C(7A) 121(2) no C(2A) C(3A) C(4A) 118(2) no N(1A) C(5A) C(6A) 114(2) no O(3A) C(7A) C(1A) 116(2) no C(9A) C(8A) C(13A) 118(2) no C(10A) C(11A) C(12A) 115(2) no P(1A) C(14A) C(15A) 122(2) no C(14A) C(15A) C(16A) 122(2) no C(17A) C(18A) C(19A) 119(2) no P(1A) C(20A) C(25A) 122(2) no C(21A) C(22A) C(23A) 118(2) no C(20A) C(25A) C(24A) 119(2) no C(8B) P(1B) C(14B) 107.0(10) no C(14B) P(1B) C(20B) 105.1(9) no Re(2) N(1B) C(5B) 112(2) no N(1B) C(1B) C(7B) 119(2) no C(2B) C(3B) C(4B) 118(3) no N(1B) C(5B) C(6B) 115(2) no O(3B) C(7B) C(1B) 110(2) no C(9B) C(8B) C(13B) 114(2) no C(10B) C(11B) C(12B) 116(2) no P(1B) C(14B) C(15B) 117(2) no C(14B) C(15B) C(16B) 120(2) no C(17B) C(18B) C(19B) 120(2) no P(1B) C(20B) C(25B) 120(2) no C(21B) C(22B) C(23B) 123(2) no C(20B) C(25B) C(24B) 121(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re(1) . Cl(1A) . 2.418(5) no Re(1) . Cl(2A) . 2.355(7) no Re(1) . P(1A) . 2.468(4) no Re(1) . O(1A) . 1.680(13) no Re(1) . O(2A) . 1.923(13) no Re(1) . N(1A) . 2.205(18) no Re(2) . Cl(1B) . 2.428(5) no Re(2) . Cl(2B) . 2.345(7) no Re(2) . P(1B) . 2.461(4) no Re(2) . O(1B) . 1.639(13) no Re(2) . O(2B) . 1.862(14) no Re(2) . N(1B) . 2.206(18) no P(1A) . C(8A) . 1.81(2) no P(1A) . C(20A) . 1.82(2) no O(3A) . C(7A) . 1.37(3) no N(1A) . C(5A) . 1.40(2) no C(1A) . C(7A) . 1.52(3) no C(3A) . C(4A) . 1.31(4) no C(5A) . C(6A) . 1.50(3) no C(8A) . C(13A) . 1.39(3) no C(10A) . C(11A) . 1.40(3) no C(12A) . C(13A) . 1.34(3) no C(14A) . C(19A) . 1.38(3) no C(16A) . C(17A) . 1.33(3) no C(18A) . C(19A) . 1.36(3) no C(20A) . C(25A) . 1.34(3) no C(22A) . C(23A) . 1.41(4) no C(24A) . C(25A) . 1.43(3) no P(1B) . C(8B) . 1.81(2) no P(1B) . C(20B) . 1.82(2) no O(3B) . C(7B) . 1.39(4) no N(1B) . C(5B) . 1.33(3) no C(1B) . C(7B) . 1.61(4) no C(3B) . C(4B) . 1.40(4) no C(5B) . C(6B) . 1.53(3) no C(8B) . C(13B) . 1.45(3) no C(10B) . C(11B) . 1.36(4) no C(12B) . C(13B) . 1.34(3) no C(14B) . C(19B) . 1.32(3) no C(16B) . C(17B) . 1.30(4) no C(18B) . C(19B) . 1.40(3) no C(20B) . C(25B) . 1.41(3) no C(22B) . C(23B) . 1.36(4) no C(24B) . C(25B) . 1.37(3) no P(1A) . C(14A) . 1.78(2) no O(2A) . C(6A) . 1.38(2) no N(1A) . C(1A) . 1.30(3) no C(1A) . C(2A) . 1.40(4) no C(2A) . C(3A) . 1.40(4) no C(4A) . C(5A) . 1.33(3) no C(8A) . C(9A) . 1.39(3) no C(9A) . C(10A) . 1.36(3) no C(11A) . C(12A) . 1.40(3) no C(14A) . C(15A) . 1.41(3) no C(15A) . C(16A) . 1.31(3) no C(17A) . C(18A) . 1.41(3) no C(20A) . C(21A) . 1.46(3) no C(21A) . C(22A) . 1.40(3) no C(23A) . C(24A) . 1.38(4) no P(1B) . C(14B) . 1.83(2) no O(2B) . C(6B) . 1.34(2) no N(1B) . C(1B) . 1.30(3) no C(1B) . C(2B) . 1.39(4) no C(2B) . C(3B) . 1.35(4) no C(4B) . C(5B) . 1.34(4) no C(8B) . C(9B) . 1.34(3) no C(9B) . C(10B) . 1.32(3) no C(11B) . C(12B) . 1.44(3) no C(14B) . C(15B) . 1.38(3) no C(15B) . C(16B) . 1.41(3) no C(17B) . C(18B) . 1.35(4) no C(20B) . C(21B) . 1.34(3) no C(21B) . C(22B) . 1.34(3) no C(23B) . C(24B) . 1.43(4) no