#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010397.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_2010397 loop_ _publ_author_name 'Henderson, W.' 'Nicholson, B.K.' _publ_section_title ; Hexaaquanickel(II) D-Camphor-10-sulfonate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 37 _journal_page_last 40 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C20 H42 Ni1 O14 S2' _chemical_formula_sum 'C20 H42 Ni O14 S2' _chemical_formula_weight 629.37 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source 'SHELXL93 (Sheldrick, 1993)' _cell_angle_alpha 90. _cell_angle_beta 94.22(2) _cell_angle_gamma 90. _cell_formula_units_Z 2 _cell_length_a 11.677(2) _cell_length_b 7.064(2) _cell_length_c 17.078(2) _cell_measurement_reflns_used 37 _cell_measurement_temperature 143 _cell_measurement_theta_max 28 _cell_measurement_theta_min 10 _cell_volume 1404.9(5) _diffrn_measurement_device 'Nicolet R3' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 2834 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0.993-1.006 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.90 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_type empirical _exptl_crystal_colour 'pale blue-green' _exptl_crystal_density_diffrn 1.488 _exptl_crystal_description tablet _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.55 _refine_diff_density_min -0.54 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.038 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 375 _refine_ls_number_reflns 2694 _refine_ls_R_factor_obs 0.0491 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; w = [\s^2^(F~o~^2^) + (0.0440P)^2^ + 0.15P] where P = [max(F~o~^2^,0) + 2F~c~^2^]/3 ; _refine_ls_wR_factor_obs 0.0721 _reflns_number_observed 2222 _reflns_number_total 2694 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file oh1067.cif _[local]_cod_data_source_block oh1067_structure_1_of_1 _[local]_cod_cif_authors_sg_H-M 'P 21' _[local]_cod_cif_authors_sg_Hall 'P 2y1' _[local]_cod_chemical_formula_sum_orig 'C20 H42 Ni1 O14 S2' _cod_database_code 2010397 loop_ _symmetry_equiv_pos_as_xyz x,y,z -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 Ni(1) .75870(10) .0000 .00590(10) .012(1) O(1) .6674(4) .2152(7) .0523(3) .016(1) O(2) .6504(2) -.0004(9) -.0926(2) .018(1) O(3) .8517(4) -.2151(7) -.0422(3) .016(1) O(4) .8647(2) -.0025(8) .1064(2) .018(1) O(5) .6669(4) -.2197(7) .0494(3) .016(1) O(6) .8496(4) .2213(7) -.0374(3) .016(1) S(1) .08220(10) .0022(3) .83550(10) .012(1) O(11) .2013(2) .0001(8) .8695(2) .016(1) O(12) .0188(4) .1686(6) .8600(3) .016(1) O(13) .0212(4) -.1745(6) .8488(3) .015(1) O(14) .1232(3) .0704(6) .5729(2) .029(1) C(11) -.0063(3) -.0138(11) .6744(2) .013(1) C(12) .0268(4) .0431(7) .5926(3) .020(1) C(13) -.0845(4) .0554(8) .5396(3) .023(1) C(14) -.1734(3) .0000(12) .5968(2) .017(1) C(15) -.1578(4) -.2155(8) .6122(3) .020(1) C(16) -.0415(4) -.2242(8) .6627(3) .016(1) C(17) -.1259(4) .0878(8) .6764(3) .015(1) C(18) -.1996(4) .0326(9) .7434(2) .019(1) C(19) -.1154(5) .3045(8) .6734(3) .024(1) C(110) .0955(4) .0270(10) .7331(2) .014(1) S(2) .40800(10) -.0002(3) .14770(10) .012(1) O(21) .2853(2) .0007(9) .1221(2) .016(1) O(22) .4665(4) -.1723(6) .1247(3) .017(1) O(23) .4678(4) .1702(6) .1241(3) .015(1) O(24) .4618(4) -.2454(7) .3836(2) .024(1) C(21) .5300(3) .0043(12) .2984(2) .015(1) C(22) .5293(5) -.1224(8) .3721(3) .019(1) C(23) .6301(5) -.0570(8) .4274(3) .023(1) C(24) .6815(4) .1042(8) .3803(3) .017(1) C(25) .7412(3) .0085(13) .3130(2) .021(1) C(26) .6388(4) -.0655(7) .2583(3) .015(1) C(27) .5714(4) .1936(8) .3370(3) .016(1) C(28) .5994(4) .3517(8) .2798(3) .019(1) C(29) .4910(5) .2765(10) .3941(4) .024(2) C(210) .4126(3) -.0007(12) .2519(2) .015(1) H(11) .708(5) .296(7) .081(3) .025(4) H(12) .600(3) .209(10) .070(3) .025(4) H(21) .609(5) -.097(7) -.111(3) .025((4) H(22) .595(4) .083(7) -.096(3) .025(4) H(31) .810(5) -.299(8) -.067(4) .025(4) H(32) .898(4) -.178(9) -.077(3) .025(4) H(41) .917(4) .083(7) .106(3) .025(4) H(42) .899(5) -.104(6) .124(3) .025(4) H(51) .700(5) -.312(7) .076(3) .025(4) H(52) .616(4) -.178(9) .078(3) .025(4) H(61) .802(4) .304(8) -.057(4) .025(4) H(62) .903(4) .223(10) -.069(3) .025(4) H(13A) -.0978(4) .1851(8) .5190(3) .028 H(13B) -.0842(4) -.0346(8) .4951(3) .028 H(14) -.2538(3) .0385(12) .5798(2) .021 H(15A) -.1538(4) -.2863(8) .5625(3) .024 H(15B) -.2211(4) -.2670(8) .6413(3) .024 H(16A) -.0510(4) -.2864(8) .7138(3) .019 H(16B) .0167(4) -.2945(8) .6350(3) .019 H(18A) -.177(2) .109(4) .7899(7) .029 H(18B) -.188(2) -.1019(15) .7557(13) .029 H(18C) -.2807(5) .056(5) .7273(8) .029 H(19A) -.066(2) .3401(8) .6320(14) .036 H(19B) -.082(3) .3514(9) .7241(7) .036 H(19C) -.1917(6) .3602(8) .662(2) .036 H(11A) .1201(4) .1587(10) .7239(2) .017 H(11B) .1592(4) -.0564(10) .7194(2) .017 H(23A) .6864(5) -.1603(8) .4382(3) .028 H(23B) .6038(5) -.0101(8) .4776(3) .028 H(24) .7307(4) .1953(8) .4125(3) .021 H(25A) .7911(3) -.0969(13) .3329(3) .026 H(25B) .7878(3) .1006(13) .2854(2) .026 H(26A) .6401(4) -.2054(7) .2549(3) .018 H(26B) .6407(4) -.0120(7) .2049(3) .018 H(28A) .648(2) .3009(13) .2401(11) .029 H(28B) .641(2) .454(2) .3088(4) .029 H(28C) .5279(4) .402(3) .2540(14) .029 H(29A) .5329(9) .368(4) .4284(14) .035 H(29B) .461(2) .1746(12) .4260(15) .035 H(29C) .4268(17) .340(5) .3647(4) .035 H(21A) .3681(3) .1099(12) .2683(2) .018 H(21B) .3718(3) -.1154(12) .2682(2) .018 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni(1) O(1) . . 2.050(5) yes Ni(1) O(3) . . 2.073(5) yes Ni(1) O(5) . . 2.056(5) yes Ni(1) O(2) . . 2.029(3) yes Ni(1) O(4) . . 2.041(3) yes Ni(1) O(6) . . 2.058(5) yes S(1) O(11) . . 1.467(3) yes S(1) O(13) . . 1.463(5) yes O(14) C(12) . . 1.214(6) yes S(2) O(22) . . 1.462(5) yes S(2) C(210) . . 1.776(4) yes S(1) O(12) . . 1.466(5) yes S(1) C(110) . . 1.776(4) yes S(2) O(21) . . 1.467(3) yes S(2) O(23) . . 1.464(5) yes O(24) C(22) . . 1.199(7) yes O(1) H(11) . . 0.87(2) no O(2) H(22) . . 0.87(2) no O(4) H(41) . . 0.86(2) no O(5) H(52) . . 0.85(2) no C(11) C(12) . . 1.530(6) no C(12) C(13) . . 1.530(6) no C(14) C(17) . . 1.559(7) no C(17) C(19) . . 1.537(7) no C(21) C(210) . . 1.534(5) no C(21) C(26) . . 1.566(6) no C(24) C(25) . . 1.543(7) no C(27) C(29) . . 1.521(8) no O(1) H(12) . . 0.86(2) no O(3) H(31) . . 0.87(2) no O(4) H(42) . . 0.86(2) no O(6) H(61) . . 0.86(2) no C(11) C(16) . . 1.551(9) no C(13) C(14) . . 1.529(6) no C(15) C(16) . . 1.554(6) no C(21) C(27) . . 1.552(8) no C(22) C(23) . . 1.525(7) no C(24) C(27) . . 1.568(6) no C(27) C(28) . . 1.534(7) no O(2) H(21) . . 0.88(2) no O(3) H(32) . . 0.87(2) no O(5) H(51) . . 0.86(2) no O(6) H(62) . . 0.86(2) no C(11) C(110) . . 1.525(5) no C(11) C(17) . . 1.573(6) no C(14) C(15) . . 1.554(9) no C(17) C(18) . . 1.531(6) no C(21) C(22) . . 1.545(8) no C(23) C(24) . . 1.541(7) no C(25) C(26) . . 1.553(6) no 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(2) Ni(1) O(4) 178.7(2) yes O(4) Ni(1) O(1) 88.9(2) yes O(4) Ni(1) O(5) 89.4(2) yes O(2) Ni(1) O(6) 90.5(2) yes O(1) Ni(1) O(6) 82.7(2) yes O(2) Ni(1) O(3) 89.0(2) yes O(1) Ni(1) O(3) 179.2(2) yes O(6) Ni(1) O(3) 96.6(2) yes O(2) Ni(1) O(1) 90.7(2) yes O(2) Ni(1) O(5) 89.4(2) yes O(1) Ni(1) O(5) 96.9(2) yes O(4) Ni(1) O(6) 90.7(2) yes O(5) Ni(1) O(6) 179.6(2) yes O(4) Ni(1) O(3) 91.4(2) yes O(5) Ni(1) O(3) 83.8(2) yes O(13) S(1) O(12) 112.2(2) yes O(12) S(1) O(11) 112.3(3) yes O(12) S(1) C(110) 106.5(3) yes C(110) C(11) C(12) 108.3(4) yes C(110) C(11) C(17) 123.3(5) yes O(14) C(12) C(13) 126.2(4) yes C(11) C(110) S(1) 120.6(3) yes O(22) S(2) O(21) 112.9(3) yes O(22) S(2) C(210) 106.7(3) yes O(21) S(2) C(210) 104.9(2) yes C(210) C(21) C(22) 110.5(4) yes O(24) C(22) C(23) 127.2(5) yes C(21) C(27) C(24) 94.1(4) yes O(13) S(1) O(11) 112.9(3) yes O(13) S(1) C(110) 108.4(3) yes O(11) S(1) C(110) 103.9(2) yes C(110) C(11) C(16) 116.9(5) yes O(14) C(12) C(11) 126.6(4) yes C(14) C(17) C(11) 93.4(4) yes O(22) S(2) O(23) 111.6(2) yes O(23) S(2) O(21) 112.9(3) yes O(23) S(2) C(210) 107.3(3) yes C(210) C(21) C(27) 118.6(6) yes C(210) C(21) C(26) 119.3(4) yes O(24) C(22) C(21) 126.6(5) yes C(21) C(210) S(2) 118.6(3) yes C(14) C(13) C(12) 101.2(3) no C(15) C(14) C(17) 102.2(4) no C(18) C(17) C(19) 109.2(5) no C(18) C(17) C(11) 116.7(4) no C(27) C(21) C(22) 100.0(4) no C(22) C(21) C(26) 103.1(5) no C(23) C(22) C(21) 106.2(4) no C(23) C(24) C(27) 101.9(4) no C(25) C(26) C(21) 104.2(4) no C(28) C(27) C(21) 115.6(4) no C(12) C(11) C(16) 102.5(4) no C(16) C(11) C(17) 102.3(4) no C(11) C(12) C(13) 107.1(4) no C(13) C(14) C(17) 103.9(4) no C(11) C(16) C(15) 104.2(4) no C(19) C(17) C(14) 113.0(5) no C(27) C(21) C(26) 102.7(4) no C(23) C(24) C(25) 106.2(5) no C(24) C(25) C(26) 103.0(3) no C(29) C(27) C(21) 114.6(4) no C(28) C(27) C(24) 112.8(4) no