#------------------------------------------------------------------------------ #$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/57/2005758.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_2005758 loop_ _publ_author_name 'Wang, A.' 'Lee, T.-J.' 'Chen, B.-H.' 'Yuan, Y.-Z.' 'Chung, C.-S.' _publ_section_title ;\b-meso-(5,7,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) Diperchlorate Monohydrate ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 3033 _journal_page_last 3035 _journal_paper_doi 10.1107/S0108270196010608 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Ni (C16 H36 N4)] (Cl O4)2 , H2 O' _chemical_formula_moiety 'C16 H36 N4 Ni,2(Cl O4),H2 O' _chemical_formula_sum 'C16 H38 Cl2 N4 Ni O9' _chemical_formula_weight 560.1 _chemical_name_systematic ; \b-meso (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazzcyclo- tetradecane) Nickel(II) Diperchlorate Monohydrate ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source 'SHELXTL-Plus (Sheldrick, 1990)' _cell_angle_alpha 90 _cell_angle_beta 116.7(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.494(3) _cell_length_b 9.172(2) _cell_length_c 17.388(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 18 _cell_measurement_theta_min 7 _cell_volume 2492(2) _computing_cell_refinement 'CAD4-Software (Enraf-Nonius, 1989)' _computing_data_collection 'CAD4-Software (Enraf-Nonius, 1989)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1990)' _computing_publication_material 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4520 _diffrn_reflns_theta_max 22.5 _diffrn_standards_decay_% 0.08 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_type 'empirical \y scan (North, Phillips & Mathews, 1968)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.49 _exptl_crystal_description 'Rectangular parallepiped' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.59 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.81 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 311 _refine_ls_number_reflns 3025 _refine_ls_R_factor_obs 0.0596 _refine_ls_shift/esd_max 0.042 _refine_ls_structure_factor_coef F _refine_ls_weighting_details w^-1^=\s^2^(F) _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0581 _reflns_number_observed 3025 _reflns_number_total 4371 _reflns_observed_criterion 'F> 4\s(F)' _[local]_cod_data_source_file de1023.cif _[local]_cod_data_source_block NITETD _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_cell_measurement_temperature' value '298K' was changed to '298' - the value should be numeric and without a unit designator. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_cell_measurement_temperature' value '298K' was changed to '298' - the value should be numeric and without a unit designator. '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w^-1^=\s^2^(F)' 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)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2492.1(13) _cod_database_code 2005758 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni .0440(10) .0470(10) .0410(10) .0020(10) .0150(10) -.0050(10) N(1) .053(3) .058(4) .073(4) .010(3) .023(3) .010(3) N(2) .063(3) .061(4) .051(3) -.016(3) -.001(3) .003(3) N(3) .052(3) .057(3) .046(3) -.003(2) .024(2) .001(2) N(4) .042(2) .071(4) .059(3) .003(3) .014(2) -.011(3) C(1) .064(5) .085(6) .185(10) -.013(4) .022(6) .058(7) C(2) .102(7) .153(10) .193(12) -.083(7) -.062(7) .005(9) C(3) .057(3) .089(5) .039(3) -.014(4) .015(3) -.010(3) C(4) .058(4) .131(8) .078(5) -.021(5) .022(3) .006(5) C(5) .053(3) .063(4) .048(3) .003(3) .014(3) -.004(3) C(6) .058(3) .053(4) .048(3) .001(3) .018(3) -.001(3) C(7) .092(5) .066(5) .071(5) .008(4) .032(4) .016(4) C(8) .066(4) .063(4) .063(4) -.006(3) .027(3) -.015(3) C(9) .063(4) .079(5) .073(4) -.008(4) .035(3) .006(4) C(10) .047(3) .080(5) .090(5) -.011(3) .027(3) -.003(4) C(11) .055(3) .096(6) .059(4) .010(4) .013(3) -.005(4) C(12) .083(5) .104(6) .070(5) .012(5) .022(4) -.018(4) C(13) .057(4) .126(7) .071(4) .007(5) .000(3) -.009(5) C(14) .066(4) .092(6) .052(4) .027(4) .012(3) .009(4) C(15) .072(4) .085(5) .065(4) .029(4) .036(4) .019(4) C(16) .092(6) .145(9) .101(6) .037(6) .050(5) .059(6) Cl(1) .0860(10) .0800(10) .106(2) -.0150(10) .0560(10) -.0190(10) Cl(2) .0790(10) .0850(10) .0600(10) .0190(10) .0390(10) .0210(10) O(1) .105(6) .314(15) .231(11) .054(8) .035(6) .042(10) O(2) .263(10) .196(9) .153(7) -.072(8) .145(7) -.061(7) O(3) .357(14) .092(5) .389(15) -.081(7) .317(14) -.078(8) O(4) .119(5) .103(5) .179(6) -.025(4) .103(5) -.023(4) O(5) .121(5) .146(6) .107(5) -.029(5) .028(4) .021(4) O(6) .164(6) .157(6) .106(5) .096(5) .080(4) .067(4) O(7) .126(5) .129(5) .123(5) -.024(4) .072(4) .016(4) O(8) .139(5) .143(5) .083(4) .064(4) .067(4) .029(4) O(9) .270(14) .349(17) .148(8) .142(12) .068(8) -.043(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_attached_atom Ni .2436(1) .2230(1) .7447(1) .045(1) Uani ? N(1) .2508(3) .0484(6) .8099(3) .063(2) Uani ? N(2) .1252(3) .1768(6) .6743(3) .068(2) Uani ? N(3) .2335(3) .3839(5) .6705(3) .051(2) Uani ? N(4) .3624(3) .2738(6) .8144(3) .061(2) Uani ? C(1) .1633(5) -.0098(10) .7751(7) .124(6) Uani ? C(2) .1111(6) .0377(12) .7044(7) .198(7) Uani ? C(3) .0681(4) .2985(8) .6736(3) .064(3) Uani ? C(4) -.0264(4) .2531(10) .6294(5) .092(4) Uani ? C(5) .0816(4) .4256(7) .6268(4) .058(3) Uani ? C(6) .1692(4) .4990(7) .6636(4) .055(3) Uani ? C(7) .1665(5) .6191(8) .6018(4) .078(4) Uani ? C(8) .1921(4) .5647(7) .7523(4) .065(3) Uani ? C(9) .3217(4) .4316(8) .6892(4) .070(3) Uani ? C(10) .3793(4) .4168(8) .7852(4) .074(3) Uani ? C(11) .3993(4) .2627(9) .9115(4) .075(3) Uani ? C(12) .3556(5) .3747(9) .9434(5) .090(4) Uani ? C(13) .4960(4) .2897(10) .9505(4) .095(4) Uani ? C(14) .3848(4) .1088(8) .9346(4) .075(3) Uani ? C(15) .2953(4) .0589(8) .9063(4) .072(3) Uani ? C(16) .2921(5) -.0870(10) .9465(5) .110(5) Uani ? Cl(1) .4292(1) -.1653(2) .7732(2) .085(1) Uani ? Cl(2) .0940(1) .3024(2) .9296(1) .072(1) Uani ? O(1) .5032(5) -.2438(14) .8255(7) .232(7) Uani ? O(2) .4134(7) -.2147(10) .6943(6) .185(6) Uani ? O(3) .4514(8) -.0242(8) .7872(8) .223(10) Uani ? O(4) .3655(4) -.2002(7) .7966(4) .120(4) Uani ? O(5) .0230(4) .2453(8) .8483(4) .133(4) Uani ? O(6) .1460(4) .1810(8) .9725(4) .135(4) Uani ? O(7) .1337(4) .3990(7) .9003(4) .120(4) Uani ? O(8) .0570(4) .3622(7) .9772(3) .115(3) Uani ? O(9) .2662(9) .0672(16) .6146(7) .265(9) Uani ? H(1) .2790(37) -.0037(61) .7868(40) .080 Uiso N1 H(2) .1317(43) .1661(76) .6261(25) .080 Uiso N2 H(3) .2108(37) .3369(63) .6197(21) .080 Uiso N3 H(4) .3921(36) .2125(57) .7974(40) .080 Uiso N4 H(5) .3009(32) -.0042(46) .6306(34) .080 Uiso O9 H(6) .2323(31) .0456(63) .5628(16) .080 Uiso O9 H(1A) .1419 .0118 .8159 .080 Uiso C1 H(1B) .1664 -.1135 .7697 .080 Uiso C1 H(2A) .1066 -.0338 .6623 .080 Uiso C2 H(2B) .0573 .0452 .7066 .080 Uiso C2 H(3A) .0824 .3242 .7320 .080 Uiso C3 H(4A) -.0348 .1716 .6594 .080 Uiso C4 H(4B) -.0424 .2261 .5708 .080 Uiso C4 H(4C) -.0611 .3334 .6305 .080 Uiso C4 H(5A) .0409 .4991 .6230 .080 Uiso C5 H(5B) .0693 .3925 .5700 .080 Uiso C5 H(7A) .2213 .6665 .6241 .080 Uiso C7 H(7B) .1235 .6891 .5959 .080 Uiso C7 H(7C) .1533 .5776 .5465 .080 Uiso C7 H(8A) .1507 .6377 .7468 .080 Uiso C8 H(8B) .2480 .6082 .7753 .080 Uiso C8 H(8C) .1918 .4892 .7904 .080 Uiso C8 H(9A) .3430 .3713 .6579 .080 Uiso C9 H(9B) .3208 .5314 .6722 .080 Uiso C9 H(10A) .3673 .4939 .8155 .080 Uiso C10 H(10B) .4382 .4221 .7962 .080 Uiso C10 H(12A) .3790 .3679 1.0049 .080 Uiso C12 H(12B) .2953 .3548 .9179 .080 Uiso C12 H(12C) .3647 .4712 .9278 .080 Uiso C12 H(13A) .5204 .2833 1.0121 .080 Uiso C13 H(13B) .5062 .3851 .9344 .080 Uiso C13 H(13C) .5219 .2179 .9295 .080 Uiso C13 H(14A) .4140 .1009 .9962 .080 Uiso C14 H(14B) .4104 .0434 .9098 .080 Uiso C14 H(15A) .2661 .1285 .9249 .080 Uiso C15 H(16A) .3207 -.0778 1.0081 .080 Uiso C16 H(16B) .3203 -.1598 .9288 .080 Uiso C16 H(16C) .2337 -.1151 .9284 .080 Uiso C16 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 N(4) Ni N(3) 89.1(2) yes N(4) Ni N(1) 93.6(2) yes N(3) Ni N(1) 174.4(2) yes N(4) Ni N(2) 178.7(2) yes N(3) Ni N(2) 89.6(2) yes N(1) Ni N(2) 87.6(2) yes O(8) Cl(2) O(7) 115.1(5) yes O(8) Cl(2) O(6) 111.2(4) yes O(7) Cl(2) O(6) 113.2(5) yes O(8) Cl(2) O(5) 107.1(4) yes O(7) Cl(2) O(5) 102.7(4) yes O(6) Cl(2) O(5) 106.6(4) yes O(4) Cl(1) O(3) 112.0(8) yes O(4) Cl(1) O(2) 113.4(6) yes O(3) Cl(1) O(2) 114.7(8) yes O(4) Cl(1) O(1) 108.8(6) yes O(3) Cl(1) O(1) 105.6(7) yes O(2) Cl(1) O(1) 101.2(7) yes Ni N(4) C(11) 118.8(5) yes Ni N(4) C(10) 108.8(3) yes C(11) N(4) C(10) 113.0(5) yes Ni N(3) C(6) 115.7(4) yes Ni N(3) C(9) 107.8(3) yes C(6) N(3) C(9) 118.2(5) yes Ni N(1) C(15) 117.8(4) yes Ni N(1) C(1) 106.1(5) yes C(15) N(1) C(1) 113.9(7) yes Ni N(2) C(3) 111.4(4) yes Ni N(2) C(2) 106.0(4) yes C(3) N(2) C(2) 116.2(7) yes N(3) C(6) C(8) 110.3(4) yes N(3) C(6) C(5) 107.3(5) yes C(8) C(6) C(5) 110.8(6) yes N(3) C(6) C(7) 110.3(6) yes C(8) C(6) C(7) 109.7(5) yes C(5) C(6) C(7) 108.4(4) yes C(6) C(5) C(3) 119.2(4) yes N(2) C(3) C(5) 108.6(6) yes N(2) C(3) C(4) 111.5(6) yes C(5) C(3) C(4) 109.7(5) yes N(2) C(2) C(1) 120.2(8) yes N(1) C(15) C(14) 109.3(7) yes N(1) C(15) C(16) 110.5(6) yes C(14) C(15) C(16) 111.6(6) yes N(3) C(9) C(10) 108.8(6) yes N(4) C(11) C(14) 108.6(5) yes N(4) C(11) C(12) 109.1(5) yes C(14) C(11) C(12) 111.0(7) yes N(4) C(11) C(13) 108.4(6) yes C(14) C(11) C(13) 108.4(6) yes C(12) C(11) C(13) 111.4(6) yes N(1) C(1) C(2) 116.7(10) yes C(15) C(14) C(11) 118.4(6) yes N(4) C(10) C(9) 108.6(5) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni N(4) 1.935(4) yes Ni N(3) 1.915(5) yes Ni N(1) 1.933(6) yes Ni N(2) 1.921(5) yes Cl(2) O(8) 1.374(8) yes Cl(2) O(7) 1.359(8) yes Cl(2) O(6) 1.419(7) yes Cl(2) O(5) 1.496(6) yes Cl(1) O(4) 1.384(9) yes Cl(1) O(3) 1.342(8) yes Cl(1) O(2) 1.350(10) yes Cl(1) O(1) 1.401(9) yes N(4) C(11) 1.516(8) yes N(4) C(10) 1.484(10) yes N(3) C(6) 1.506(8) yes N(3) C(9) 1.494(9) yes N(1) C(15) 1.500(9) yes N(1) C(1) 1.471(10) yes N(2) C(3) 1.494(9) yes N(2) C(2) 1.442(13) yes C(6) C(8) 1.532(9) yes C(6) C(5) 1.527(8) yes C(6) C(7) 1.526(10) yes C(5) C(3) 1.499(10) yes C(3) C(4) 1.535(9) yes C(2) C(1) 1.235(13) yes C(15) C(14) 1.487(10) yes C(15) C(16) 1.522(12) yes C(9) C(10) 1.519(8) yes C(11) C(14) 1.520(11) yes C(11) C(12) 1.527(12) yes C(11) C(13) 1.533(9) yes