#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/06/2200613.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_2200613 loop_ _publ_author_name 'Farrugia, Louis J.' 'Cross, Ronald J.' 'Barley, Helen R. L.' _publ_section_title ; cis-(2-Amino-1,1-dimethylethylamine)dichloropalladium(II) ethanol hemisolvate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m494 _journal_page_last m495 _journal_paper_doi 10.1107/S1600536801015884 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C4 H12 Cl2 N2 Pd, 0.5 C2 H6 O' _chemical_formula_moiety 'C4 H12 Cl2 N2 Pd, 0.5 C2 H6 O' _chemical_formula_sum 'C5 H15 Cl2 N2 O0.5 Pd' _chemical_formula_weight 288.49 _chemical_name_systematic ; cis-(2-amino-1,1-dimethylethylamine)-dichloro-palladium(II) ethanol solvate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _cell_angle_alpha 90 _cell_angle_beta 90.28(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.435(5) _cell_length_b 7.562(5) _cell_length_c 16.527(4) _cell_measurement_reflns_used 3005 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.034 _cell_measurement_theta_min 2 _cell_volume 2054.0(16) _computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1997-2000)' _computing_data_reduction 'HKL DENZO (Otwinowski & Minor, 1997) and WinGX (Farrugia, 1999)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full .997 _diffrn_measured_fraction_theta_max .997 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0451 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 15940 _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 30.02 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_theta_min 2.46 _exptl_absorpt_coefficient_mu 2.274 _exptl_absorpt_correction_T_max .834 _exptl_absorpt_correction_T_min .727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Blessing (1995) ; _exptl_crystal_colour yellow-green _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rectangular block' _exptl_crystal_F_000 1144 _exptl_crystal_size_max .2 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .08 _refine_diff_density_max .67 _refine_diff_density_min -.636 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 2993 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all .0352 _refine_ls_R_factor_gt .0258 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0222P)^2^+4.1385P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0583 _reflns_number_gt 2577 _reflns_number_total 2993 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cf6110.cif _cod_data_source_block I _cod_original_cell_volume 2053.9(16) _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 2200613 _cod_database_fobs_code 2200613 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pd .750252(10) .07626(2) .182124(9) .02253(6) Uani d . 1 . . Pd Cl2 .84550(4) -.06266(8) .26453(4) .03756(15) Uani d . 1 . . Cl Cl1 .84636(4) .17181(10) .09074(3) .03878(16) Uani d . 1 . . Cl N1 .66102(11) .1942(3) .11725(10) .0254(4) Uani d . 1 . . N H12 .6606 .3134 .1283 .054(10) Uiso calc R 1 . . H H11 .671 .1799 .0629 .043(8) Uiso calc R 1 . . H N2 .65645(12) .0038(3) .25503(12) .0313(4) Uani d . 1 . . N H21 .6488 -.1165 .252 .050(9) Uiso calc R 1 . . H H22 .6686 .0323 .3078 .054(9) Uiso calc R 1 . . H C1 .57971(13) .1159(3) .13749(13) .0277(5) Uani d . 1 . . C C10 .51213(15) .2408(4) .10985(16) .0384(6) Uani d . 1 . . C H10A .4592 .1913 .125 .045(8) Uiso calc R 1 . . H H10B .5144 .255 .051 .045(8) Uiso calc R 1 . . H H10C .5193 .3562 .1359 .046(8) Uiso calc R 1 . . H C11 .57229(16) -.0635(4) .09621(15) .0348(6) Uani d . 1 . . C H11A .6158 -.1415 .1156 .044(8) Uiso calc R 1 . . H H11B .5769 -.0484 .0375 .037(8) Uiso calc R 1 . . H H11C .5194 -.1159 .109 .045(8) Uiso calc R 1 . . H C2 .58073(14) .0965(4) .22943(14) .0314(5) Uani d . 1 . . C H2A .5783 .2147 .255 .026(6) Uiso calc R 1 . . H H2B .5326 .028 .2471 .037(7) Uiso calc R 1 . . H C100 .7223(7) .8271(17) .4655(6) .045(2) Uani d P .5 . . C H10D .727 .7098 .4394 .054 Uiso calc PR .5 . . H H10E .6693 .8335 .4936 .054 Uiso calc PR .5 . . H C101 .7912(10) .855(3) .5246(12) .125(9) Uani d P .5 . . C H10F .7901 .7622 .5658 .188 Uiso calc PR .5 . . H H10G .7851 .9709 .5507 .188 Uiso calc PR .5 . . H H10H .8431 .8512 .4958 .188 Uiso calc PR .5 . . H O100 .7278(6) .9516(12) .4123(4) .129(3) Uani d P .5 . . O H100 .6911 .9389 .3773 .194 Uiso calc PR .5 . . 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 Pd .02233(9) .02410(10) .02112(9) -.00189(7) -.00549(6) .00008(7) Cl2 .0318(3) .0346(3) .0461(4) -.0044(2) -.0164(3) .0124(3) Cl1 .0278(3) .0636(5) .0249(3) -.0062(3) -.0020(2) .0043(3) N1 .0251(9) .0325(11) .0186(8) .0025(8) -.0039(7) -.0004(8) N2 .0284(10) .0413(13) .0240(9) -.0087(9) -.0066(7) .0051(9) C1 .0222(10) .0391(14) .0218(10) .0005(9) -.0032(8) -.0030(9) C10 .0298(12) .0522(18) .0330(13) .0123(12) -.0062(10) -.0060(12) C11 .0310(12) .0465(16) .0270(12) -.0036(11) -.0070(9) -.0069(11) C2 .0262(11) .0461(15) .0219(10) -.0039(10) -.0010(8) -.0038(10) C100 .042(4) .054(5) .038(4) -.011(3) -.022(3) .010(3) C101 .126(13) .115(14) .135(14) .010(9) .056(10) -.059(11) O100 .172(8) .166(8) .049(3) -.033(6) -.035(4) .033(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .006 '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 N1 Pd N2 83.28(8) yes N1 Pd Cl1 90.69(6) yes N2 Pd Cl1 173.96(6) yes N1 Pd Cl2 175.58(5) yes N2 Pd Cl2 92.38(6) yes Cl1 Pd Cl2 93.66(3) yes C1 N1 Pd 110.66(14) ? C1 N1 H12 109.5 ? Pd N1 H12 109.5 ? C1 N1 H11 109.5 ? Pd N1 H11 109.5 ? H12 N1 H11 108.1 ? C2 N2 Pd 109.86(15) ? C2 N2 H21 109.7 ? Pd N2 H21 109.7 ? C2 N2 H22 109.7 ? Pd N2 H22 109.7 ? H21 N2 H22 108.2 ? N1 C1 C11 108.71(19) ? N1 C1 C10 109.7(2) ? C11 C1 C10 111.1(2) ? N1 C1 C2 104.73(17) ? C11 C1 C2 111.1(2) ? C10 C1 C2 111.2(2) ? C1 C10 H10A 109.5 ? C1 C10 H10B 109.5 ? H10A C10 H10B 109.5 ? C1 C10 H10C 109.5 ? H10A C10 H10C 109.5 ? H10B C10 H10C 109.5 ? C1 C11 H11A 109.5 ? C1 C11 H11B 109.5 ? H11A C11 H11B 109.5 ? C1 C11 H11C 109.5 ? H11A C11 H11C 109.5 ? H11B C11 H11C 109.5 ? N2 C2 C1 109.49(19) ? N2 C2 H2A 109.8 ? C1 C2 H2A 109.8 ? N2 C2 H2B 109.8 ? C1 C2 H2B 109.8 ? H2A C2 H2B 108.2 ? O100 C100 C101 106.5(13) ? O100 C100 H10D 110.4 ? C101 C100 H10D 110.4 ? O100 C100 H10E 110.4 ? C101 C100 H10E 110.4 ? H10D C100 H10E 108.6 ? C100 C101 H10F 109.5 ? C100 C101 H10G 109.5 ? H10F C101 H10G 109.5 ? C100 C101 H10H 109.5 ? H10F C101 H10H 109.5 ? H10G C101 H10H 109.5 ? C100 O100 H100 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd N1 . 2.0197(19) yes Pd N2 . 2.036(2) yes Pd Cl1 . 2.3068(8) yes Pd Cl2 . 2.3213(9) yes N1 C1 . 1.501(3) yes N1 H12 . .92 ? N1 H11 . .92 ? N2 C2 . 1.488(3) yes N2 H21 . .92 ? N2 H22 . .92 ? C1 C11 . 1.523(4) yes C1 C10 . 1.526(3) yes C1 C2 . 1.527(3) yes C10 H10A . .98 ? C10 H10B . .98 ? C10 H10C . .98 ? C11 H11A . .98 ? C11 H11B . .98 ? C11 H11C . .98 ? C2 H2A . .99 ? C2 H2B . .99 ? C100 O100 . 1.292(14) ? C100 C101 . 1.506(14) ? C100 H10D . .99 ? C100 H10E . .99 ? C101 H10F . .98 ? C101 H10G . .98 ? C101 H10H . .98 ? O100 H100 . .84 ? 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 N1 H12 Cl2 7_655 .92 2.59 3.405(3) 148.2 N1 H12 O100 7_665 .92 2.64 3.280(9) 127.0 N1 H11 Cl1 2_655 .92 2.55 3.443(2) 162.5 N2 H21 Cl2 7_645 .92 2.44 3.352(3) 169.5 N2 H22 O100 1_545 .92 2.07 2.873(6) 145.2 N2 H22 Cl1 7_655 .92 2.81 3.538(3) 137.2 O100 H100 N2 1_565 .84 2.15 2.873(6) 143.7