#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200635.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_2200635 loop_ _publ_author_name 'Subha Nandhini, M.' 'Krishnakumar, R. V.' 'Natarajan, S.' _publ_section_title ; Dichlorobis(sarcosinato)zinc(II) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m435 _journal_page_last m437 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Zn Cl2 (C6 H14 N2 O4)]' _chemical_formula_moiety 'C6 H14 Cl2 N2 O4 Zn' _chemical_formula_sum 'C6 H14 Cl2 N2 O4 Zn' _chemical_formula_weight 314.46 _chemical_name_common Dichlorobis(sarcosinato)zinc(II) _chemical_name_systematic ; Dichlorobis(sarcosinato)zinc(II) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 14.191(2) _cell_length_b 10.6550(10) _cell_length_c 15.917(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27 _cell_measurement_theta_min 15 _cell_volume 2406.7(5) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 Software' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .881 _diffrn_measured_fraction_theta_max .881 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents .000 _diffrn_reflns_av_sigmaI/netI .0137 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2182 _diffrn_reflns_theta_full 67.89 _diffrn_reflns_theta_max 67.89 _diffrn_reflns_theta_min 5.56 _diffrn_standards_decay_% .1 _diffrn_standards_interval_count 200 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 6.941 _exptl_absorpt_correction_T_max .503 _exptl_absorpt_correction_T_min .400 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_meas 1.74 _exptl_crystal_density_method 'floatation in a mixture of carbon tetrachloride and bromoform' _exptl_crystal_description needle _exptl_crystal_F_000 1280 _exptl_crystal_size_max .16 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .10 _refine_diff_density_max .28 _refine_diff_density_min -.43 _refine_ls_extinction_coef .00071(4) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.18 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 2182 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.18 _refine_ls_R_factor_all .031 _refine_ls_R_factor_gt .028 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0299P)^2^+2.1069P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .075 _reflns_number_gt 2004 _reflns_number_total 2182 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ci6057.cif _[local]_cod_data_source_block I _cod_original_cell_volume 2406.5(4) _cod_database_code 2200635 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Zn1 .91616(2) .26684(3) .374714(18) .02767(13) Uani d . 1 Zn Cl1 .82235(4) .23686(7) .26065(4) .04149(18) Uani d . 1 Cl Cl2 .85109(5) .21851(6) .50017(4) .04106(18) Uani d . 1 Cl O1A .96149(12) .43918(17) .36814(12) .0407(5) Uani d . 1 O O1B 1.02354(12) .15641(18) .34808(11) .0386(4) Uani d . 1 O O2A .81985(13) .51561(19) .40136(14) .0474(5) Uani d . 1 O O2B 1.10244(14) .1897(2) .46595(12) .0502(5) Uani d . 1 O N1A .86855(15) .75410(19) .36977(12) .0324(5) Uani d . 1 N H1A1 .8531 .7594 .4245 .039 Uiso calc R 1 H H1A2 .8165 .7310 .3414 .039 Uiso calc R 1 H N1B 1.24257(13) .0311(2) .42703(13) .0322(5) Uani d . 1 N H1B1 1.2600 .1064 .4473 .039 Uiso calc R 1 H H1B2 1.2212 -.0151 .4704 .039 Uiso calc R 1 H C1A .90174(17) .5272(2) .37881(14) .0303(5) Uani d . 1 C C1B 1.09122(16) .1399(2) .39819(14) .0277(5) Uani d . 1 C C2A .94081(17) .6563(2) .35948(16) .0323(5) Uani d . 1 C H2A1 .9933 .6737 .3967 .039 Uiso calc R 1 H H2A2 .9642 .6578 .3022 .039 Uiso calc R 1 H C2B 1.16529(17) .0490(3) .36588(15) .0322(5) Uani d . 1 C H2B1 1.1359 -.0314 .3543 .039 Uiso calc R 1 H H2B2 1.1911 .0807 .3136 .039 Uiso calc R 1 H C3A .8985(2) .8799(3) .3400(2) .0554(8) Uani d . 1 C H3A1 .8482 .9389 .3486 .083 Uiso calc R 1 H H3A2 .9135 .8758 .2813 .083 Uiso calc R 1 H H3A3 .9530 .9065 .3709 .083 Uiso calc R 1 H C3B 1.32584(18) -.0316(3) .39022(18) .0448(7) Uani d . 1 C H3B1 1.3737 -.0405 .4324 .067 Uiso calc R 1 H H3B2 1.3498 .0180 .3446 .067 Uiso calc R 1 H H3B3 1.3081 -.1130 .3697 .067 Uiso calc R 1 H 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 Zn1 .01822(19) .0360(2) .0288(2) .00084(12) .00124(11) -.00157(13) Cl1 .0290(3) .0618(4) .0337(3) .0001(3) -.0053(2) -.0061(3) Cl2 .0417(3) .0462(4) .0353(3) -.0046(3) .0121(3) .0024(3) O1A .0235(9) .0372(10) .0614(12) -.0007(8) .0015(8) -.0009(9) O1B .0285(9) .0559(11) .0314(9) .0152(9) -.0047(7) -.0046(8) O2A .0295(9) .0469(11) .0658(13) -.0015(8) .0147(9) .0044(10) O2B .0392(10) .0691(14) .0423(11) .0155(10) -.0106(9) -.0204(10) N1A .0285(11) .0370(11) .0318(11) -.0016(9) -.0017(8) -.0007(9) N1B .0213(9) .0401(11) .0352(11) .0056(9) .0004(8) .0007(9) C1A .0257(12) .0403(14) .0249(12) -.0039(10) -.0008(9) -.0016(10) C1B .0213(11) .0359(12) .0259(11) -.0018(10) .0014(9) .0021(10) C2A .0254(12) .0374(13) .0340(12) -.0033(11) .0011(10) -.0012(11) C2B .0242(12) .0431(14) .0294(12) .0057(11) -.0012(9) -.0012(10) C3A .0547(18) .0411(16) .070(2) -.0005(14) .0015(17) .0141(15) C3B .0243(13) .0592(18) .0509(16) .0142(12) .0065(12) .0070(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .3639 .7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 .6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1A Zn1 O1B 107.20(8) y O1A Zn1 Cl2 113.40(6) y O1B Zn1 Cl2 111.71(6) y O1A Zn1 Cl1 106.43(6) y O1B Zn1 Cl1 101.36(5) y Cl2 Zn1 Cl1 115.74(3) y C1A O1A Zn1 117.80(16) ? C1B O1B Zn1 122.43(16) ? C2A N1A C3A 113.9(2) y C2A N1A H1A1 108.8 ? C3A N1A H1A1 108.8 ? C2A N1A H1A2 108.8 ? C3A N1A H1A2 108.8 ? H1A1 N1A H1A2 107.7 ? C3B N1B C2B 112.97(19) y C3B N1B H1B1 109.0 ? C2B N1B H1B1 109.0 ? C3B N1B H1B2 109.0 ? C2B N1B H1B2 109.0 ? H1B1 N1B H1B2 107.8 ? O2A C1A O1A 126.6(2) y O2A C1A C2A 120.0(2) y O1A C1A C2A 113.4(2) y O2B C1B O1B 127.0(2) y O2B C1B C2B 119.3(2) y O1B C1B C2B 113.7(2) y N1A C2A C1A 111.4(2) y N1A C2A H2A1 109.3 ? C1A C2A H2A1 109.3 ? N1A C2A H2A2 109.3 ? C1A C2A H2A2 109.3 ? H2A1 C2A H2A2 108.0 ? N1B C2B C1B 111.88(19) y N1B C2B H2B1 109.2 ? C1B C2B H2B1 109.2 ? N1B C2B H2B2 109.2 ? C1B C2B H2B2 109.2 ? H2B1 C2B H2B2 107.9 ? N1A C3A H3A1 109.5 ? N1A C3A H3A2 109.5 ? H3A1 C3A H3A2 109.5 ? N1A C3A H3A3 109.5 ? H3A1 C3A H3A3 109.5 ? H3A2 C3A H3A3 109.5 ? N1B C3B H3B1 109.5 ? N1B C3B H3B2 109.5 ? H3B1 C3B H3B2 109.5 ? N1B C3B H3B3 109.5 ? H3B1 C3B H3B3 109.5 ? H3B2 C3B H3B3 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Zn1 O1A 1.9484(19) y Zn1 O1B 1.9713(17) y Zn1 Cl2 2.2595(7) y Zn1 Cl1 2.2739(7) y O1A C1A 1.276(3) y O1B C1B 1.261(3) y O2A C1A 1.223(3) y O2B C1B 1.213(3) y N1A C2A 1.471(3) y N1A C3A 1.484(3) y N1A H1A1 .90 ? N1A H1A2 .90 ? N1B C3B 1.478(3) y N1B C2B 1.479(3) y N1B H1B1 .90 ? N1B H1B2 .90 ? C1A C2A 1.514(3) y C1B C2B 1.519(3) y C2A H2A1 .97 ? C2A H2A2 .97 ? C2B H2B1 .97 ? C2B H2B2 .97 ? C3A H3A1 .96 ? C3A H3A2 .96 ? C3A H3A3 .96 ? C3B H3B1 .96 ? C3B H3B2 .96 ? C3B H3B3 .96 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1A H1A1 O2B 5_766 .90 1.93 2.714(3) 144.3 N1A H1A2 Cl1 7_765 .90 2.35 3.223(2) 162.5 N1B H1B1 Cl2 3_556 .90 2.42 3.291(2) 163.5 N1B H1B2 Cl2 5_756 .90 2.44 3.191(2) 140.7 N1B H1B2 O2A 3_556 .90 2.48 2.985(3) 116.3 C2A H2A2 O1B 4_755 .97 2.40 3.342(3) 164.1 C2B H2B2 Cl1 6_656 .97 2.76 3.610(3) 146.2 C3A H3A1 O2A 7_765 .96 2.66 3.555(4) 155.9 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag O1B Zn1 O1A C1A 176.31(17) ? Cl2 Zn1 O1A C1A -59.92(18) ? Cl1 Zn1 O1A C1A 68.47(18) ? O1A Zn1 O1B C1B 72.3(2) ? Cl2 Zn1 O1B C1B -52.5(2) ? Cl1 Zn1 O1B C1B -176.30(18) ? Zn1 O1A C1A O2A 8.0(3) ? Zn1 O1A C1A C2A -171.24(15) ? Zn1 O1B C1B O2B -2.6(4) ? Zn1 O1B C1B C2B 178.76(16) ? C3A N1A C2A C1A -171.6(2) y O2A C1A C2A N1A -1.3(3) y O1A C1A C2A N1A 178.0(2) y C3B N1B C2B C1B -166.3(2) y O2B C1B C2B N1B 2.1(3) y O1B C1B C2B N1B -179.2(2) y