#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010356.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_2010356 loop_ _publ_author_name 'Boys, D.' 'Araya-Maturana, R.' 'Gonzalez, O.' 'Manriquez, V.' _publ_section_title ; [1-(Ethoxycarbonyl)-1-cyclopentyl]triphenylphosphonium Bromide, [(C~6~H~5~)~3~PC(C~4~H~8~)(COOC~2~H~5~)]Br ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 105 _journal_page_last 107 _journal_paper_doi 10.1107/S0108270194005433 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C26 H28 Br O2 P' _chemical_formula_weight 483.4 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_type_scat_source IntTabC _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.875(2) _cell_length_b 9.826(2) _cell_length_c 26.468(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 15 _cell_measurement_theta_min 2 _cell_volume 2308.2(8) _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 3051 _diffrn_reflns_theta_max 25.0 _diffrn_standards_decay_% <2 _diffrn_standards_interval_count 98 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.391 _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.26 _refine_diff_density_min -0.36 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.006 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 272 _refine_ls_number_reflns 1271 _refine_ls_R_factor_obs 0.032 _refine_ls_shift/esd_max 0.012 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0002F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.031 _reflns_number_observed 1271 _reflns_number_total 2325 _reflns_observed_criterion F>4.0\s(F) _cod_data_source_file bk1011.cif _cod_data_source_block bk1011a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F) + 0.0002F^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) + 0.0002F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_formula_sum 'C26 H28 O2 P Br' _cod_database_code 2010356 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-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 Br .67860(10) 1.02620(10) .13810(10) .0470(10) P .3540(2) .5374(2) .13450(10) .0280(10) O(1) .6081(6) .4206(5) .0869(2) .043(2) O(2) .7822(7) .5594(8) .1191(2) .068(3) C(1) .5446(8) .5301(8) .1634(3) .028(3) C(2) .5833(10) .6640(7) .1927(3) .037(3) C(3) .6293(12) .6169(9) .2450(3) .065(4) C(4) .6673(13) .4748(9) .2429(3) .068(4) C(5) .5645(10) .4122(7) .2027(3) .037(3) C(6) .6598(11) .5061(9) .1208(3) .040(4) C(7) .6998(11) .3922(9) .0424(3) .060(4) C(8) .6349(14) .2728(10) .0168(3) .090(6) C(11) .2269(9) .6331(8) .1740(3) .027(3) C(12) .1319(10) .7308(8) .1520(3) .037(3) C(13) .0202(11) .7948(9) .1817(3) .044(4) C(14) .0102(12) .7627(9) .2318(3) .053(4) C(15) .1050(11) .6669(9) .2540(4) .047(4) C(16) .2123(10) .6018(8) .2246(3) .036(3) C(21) .2651(10) .3742(8) .1267(3) .029(3) C(22) .1068(11) .3712(10) .1264(3) .039(4) C(23) .0285(11) .2507(10) .1209(3) .047(4) C(24) .1098(14) .1303(11) .1165(3) .050(4) C(25) .2638(13) .1310(10) .1174(3) .046(4) C(26) .3428(10) .2517(8) .1221(3) .037(3) C(31) .3689(8) .6253(8) .0750(3) .028(3) C(32) .4350(10) .7541(8) .0733(3) .037(3) C(33) .4525(11) .8217(9) .0282(3) .047(4) C(34) .4034(11) .7603(11) -.0154(3) .054(4) C(35) .3360(13) .6324(10) -.0150(3) .056(4) C(36) .3226(10) .5652(8) .0302(3) .039(3) H(2A) .4967 .7222 .1948 .040 H(2B) .6633 .7130 .1764 .040 H(3A) .5493 .6318 .2688 .070 H(3B) .7156 .6680 .2559 .070 H(4A) .6497 .4325 .2750 .070 H(4B) .7713 .4626 .2340 .070 H(5A) .6116 .3346 .1874 .040 H(5B) .4696 .3848 .2169 .040 H(7A) .8014 .3708 .0520 .060 H(7B) .7012 .4692 .0201 .060 H(8A) .6901 .2484 -.0131 .090 H(8B) .6340 .1973 .0398 .090 H(8C) .5334 .2960 .0078 .090 H(12A) .1419 .7543 .1169 .040 H(13A) -.0468 .8610 .1674 .050 H(14A) -.0617 .8099 .2525 .060 H(15A) .0930 .6448 .2891 .050 H(16A) .2776 .5354 .2397 .040 H(22A) .0515 .4545 .1302 .040 H(23A) -.0796 .2493 .1201 .050 H(24A) .0563 .0460 .1128 .060 H(25A) .3168 .0462 .1145 .050 H(26A) .4509 .2510 .1224 .040 H(32A) .4685 .7958 .1041 .040 H(33A) .4971 .9107 .0270 .050 H(34A) .4177 .8061 -.0470 .060 H(35A) .3015 .5917 -.0459 .060 H(36A) .2776 .4765 .0320 .040 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) P C(11) 110.6(3) yes C(1) P C(21) 114.4(4) yes C(11) P C(21) 104.9(4) yes C(1) P C(31) 108.1(3) yes C(11) P C(31) 107.6(4) yes C(21) P C(31) 111.0(4) yes P C(1) C(6) 108.1(5) yes C(2) C(1) C(6) 110.2(7) yes C(5) C(1) C(6) 107.3(6) yes O(1) C(6) C(1) 111.5(7) yes O(1) C(7) C(8) 107.8(8) yes C(2) C(1) C(5) 105.5(6) yes C(1) C(2) C(3) 104.8(6) yes C(2) C(3) C(4) 108.8(7) yes C(3) C(4) C(5) 106.1(8) yes C(1) C(5) C(4) 103.4(6) yes P C(1) C(2) 111.8(5) yes P C(1) C(5) 113.8(5) yes C(6) O(1) C(7) 118.7(7) yes O(1) C(6) O(2) 124.5(8) yes O(2) C(6) C(1) 124.0(7) yes P C(11) C(16) 120.3(6) no C(11) C(12) C(13) 119.6(7) no C(13) C(14) C(15) 121.7(9) no C(11) C(16) C(15) 120.4(8) no P C(21) C(26) 124.3(7) no C(21) C(22) C(23) 121.5(9) no C(23) C(24) C(25) 120.9(10) no C(21) C(26) C(25) 119.9(10) no P C(31) C(36) 121.4(6) no C(31) C(32) C(33) 120.9(8) no C(33) C(34) C(35) 121.9(9) no C(31) C(36) C(35) 121.0(8) no P C(11) C(12) 119.5(6) no C(12) C(11) C(16) 119.9(7) no C(12) C(13) C(14) 119.0(8) no C(14) C(15) C(16) 119.4(8) no P C(21) C(22) 117.3(6) no C(22) C(21) C(26) 118.5(8) no C(22) C(23) C(24) 118.5(9) no C(24) C(25) C(26) 120.8(10) no P C(31) C(32) 119.6(6) no C(32) C(31) C(36) 118.9(7) no C(32) C(33) C(34) 118.7(9) no C(34) C(35) C(36) 118.4(8) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag P C(1) 1.857(8) yes P C(11) 1.803(8) yes P C(21) 1.800(9) yes P C(31) 1.802(8) yes O(1) C(6) 1.313(10) yes O(1) C(7) 1.458(10) yes O(2) C(6) 1.206(11) yes C(1) C(2) 1.565(11) yes C(1) C(5) 1.569(11) yes C(2) C(3) 1.517(12) yes C(3) C(4) 1.438(13) yes C(4) C(5) 1.529(13) yes C(1) C(6) 1.539(11) yes C(7) C(8) 1.472(13) yes C(11) C(12) 1.404(11) no C(12) C(13) 1.414(12) no C(14) C(15) 1.392(13) no C(21) C(22) 1.405(13) no C(22) C(23) 1.380(13) no C(24) C(25) 1.367(17) no C(31) C(32) 1.396(11) no C(32) C(33) 1.374(12) no C(34) C(35) 1.392(15) no C(11) C(16) 1.381(11) no C(13) C(14) 1.366(13) no C(15) C(16) 1.386(12) no C(21) C(26) 1.393(12) no C(23) C(24) 1.390(15) no C(25) C(26) 1.383(13) no C(31) C(36) 1.385(11) no C(33) C(34) 1.373(13) no C(35) C(36) 1.373(12) no