#------------------------------------------------------------------------------ #$Date: 2013-01-18 12:43:08 +0200 (Fri, 18 Jan 2013) $ #$Revision: 71116 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/87/2018704.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_2018704 loop_ _publ_author_name 'Vranec, Peter' 'Poto\catena-Poly[dimethylammonium [[dichloridopalladate(II)]-\m-chlorido]] ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.359(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.7896(7) _cell_length_b 13.2070(11) _cell_length_c 7.1410(6) _cell_measurement_reflns_used 545 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.8506 _cell_measurement_theta_min 3.0786 _cell_volume 734.44(11) _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2007)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2007)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2007)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8.3438 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur (Sapphire2, large Be window)' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 1387 _diffrn_reflns_theta_full 26.49 _diffrn_reflns_theta_max 26.49 _diffrn_reflns_theta_min 3.08 _exptl_absorpt_coefficient_mu 3.508 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; [CrysAlis PRO (Oxford Diffraction, 2007), based on expressions derived by Clark & Reid (1995)] ; _exptl_crystal_colour red-brown _exptl_crystal_density_diffrn 2.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.9712 _exptl_crystal_size_mid 0.1924 _exptl_crystal_size_min 0.1834 _refine_diff_density_max 0.667 _refine_diff_density_min -0.678 _refine_ls_extinction_coef 0.0188(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 40 _refine_ls_number_reflns 762 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0272 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.0643 _reflns_number_gt 629 _reflns_number_total 762 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL II CELL 0.71073 7.7896 13.2070 7.1410 90.000 91.359 90.000 ZERR 4.00 0.0007 0.0011 0.0006 0.000 0.007 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N CL PD UNIT 8 32 4 12 4 MERG 2 OMIT -2.00 53.00 FMAP 2 PLAN 10 ACTA BOND $H EQIV $1 x, -y+1, z-1/2 HTAB N1 Cl2 HTAB N1 Cl2_$1 L.S. 15 WGHT 0.029100 EXTI 0.018796 FVAR 5.22269 PD1 5 0.500000 0.500000 0.500000 10.50000 0.02412 0.02538 = 0.01850 0.00164 0.00107 0.00037 CL1 4 0.500000 0.610903 0.750000 10.50000 0.04712 0.02936 = 0.02237 0.00000 0.00107 0.00000 CL2 4 0.749366 0.427232 0.614924 11.00000 0.03238 0.04407 = 0.03654 -0.00050 -0.00512 0.01028 C1 1 0.919268 0.312040 0.100930 11.00000 0.03844 0.04433 = 0.04322 -0.00635 -0.00710 -0.00580 AFIX 33 H1A 2 0.869167 0.355720 0.007107 11.00000 -1.50000 H1B 2 0.831435 0.270354 0.153012 11.00000 -1.50000 H1C 2 1.004436 0.269828 0.045237 11.00000 -1.50000 AFIX 0 N1 3 1.000000 0.373569 0.250000 10.50000 0.03504 0.03238 = 0.03703 0.00000 -0.00504 0.00000 H1N1 2 0.918864 0.406327 0.303477 11.00000 0.08952 HKLF 4 REM exp_341 in C2/c REM R1 = 0.0272 for 629 Fo > 4sig(Fo) and 0.0389 for all 762 data REM 40 parameters refined using 0 restraints END WGHT 0.0288 0.0000 REM Highest difference peak 0.667, deepest hole -0.678, 1-sigma level 0.132 Q1 1 0.5000 0.3927 0.7500 10.50000 0.05 0.67 Q2 1 0.5961 0.4965 0.7803 11.00000 0.05 0.65 Q3 1 0.7468 0.4299 0.1249 11.00000 0.05 0.60 Q4 1 0.5479 0.5513 0.3747 11.00000 0.05 0.47 Q5 1 0.6412 0.4461 0.6752 11.00000 0.05 0.42 Q6 1 0.6842 0.4190 0.7108 11.00000 0.05 0.41 Q7 1 0.6525 0.5169 0.4063 11.00000 0.05 0.38 Q8 1 0.4432 0.6654 0.8995 11.00000 0.05 0.37 Q9 1 0.8776 0.2328 0.1590 11.00000 0.05 0.37 Q10 1 0.7965 0.5029 0.5119 11.00000 0.05 0.37 ; _[local]_cod_data_source_file fg3281.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2018704 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _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_symmetry_multiplicity Pd Pd1 0.5000 0.5000 0.5000 0.0227(2) Uani d S 1 2 Cl Cl1 0.5000 0.61090(11) 0.7500 0.0329(4) Uani d S 1 2 Cl Cl2 0.74937(14) 0.42723(9) 0.61492(15) 0.0378(3) Uani d . 1 1 C C1 0.9193(6) 0.3120(4) 0.1009(6) 0.0421(11) Uani d . 1 1 H H1A 0.8692 0.3557 0.0071 0.063 Uiso calc R 1 1 H H1B 0.8314 0.2704 0.1530 0.063 Uiso calc R 1 1 H H1C 1.0044 0.2698 0.0452 0.063 Uiso calc R 1 1 N N1 1.0000 0.3736(4) 0.2500 0.0349(13) Uani d S 1 2 H H1N1 0.919(8) 0.406(4) 0.303(9) 0.09(2) Uiso d . 1 1 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 Pd1 0.0241(3) 0.0254(3) 0.0185(3) 0.0004(2) 0.00107(17) 0.00164(16) Cl1 0.0471(10) 0.0294(8) 0.0224(7) 0.000 0.0011(6) 0.000 Cl2 0.0324(6) 0.0441(7) 0.0365(6) 0.0103(6) -0.0051(4) -0.0005(5) C1 0.038(3) 0.044(3) 0.043(3) -0.006(2) -0.007(2) -0.006(2) N1 0.035(3) 0.032(3) 0.037(3) 0.000 -0.005(3) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 Pd1 Cl2 5_666 . 180.0 yes Cl2 Pd1 Cl1 5_666 . 89.73(3) yes Cl2 Pd1 Cl1 . . 90.27(3) yes Cl2 Pd1 Cl1 5_666 5_666 90.27(3) yes Cl2 Pd1 Cl1 . 5_666 89.73(3) yes Cl1 Pd1 Cl1 . 5_666 180.0 yes Pd1 Cl1 Pd1 . 2_656 101.27(6) yes N1 C1 H1A . . 109.5 ? N1 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? N1 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? C1 N1 C1 . 2_755 112.8(5) ? C1 N1 H1N1 . . 107(5) ? C1 N1 H1N1 2_755 . 105(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 Pd1 Cl2 5_666 2.3010(10) yes Pd1 Cl2 . 2.3010(10) yes Pd1 Cl1 . 2.3092(9) yes Pd1 Cl1 5_666 2.3092(9) yes Cl1 Pd1 2_656 2.3092(9) yes C1 N1 . 1.469(5) ? C1 H1A . 0.9600 ? C1 H1B . 0.9600 ? C1 H1C . 0.9600 ? N1 C1 2_755 1.469(5) ? N1 H1N1 . 0.86(5) ? 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 H1N1 Cl2 . 0.86(5) 2.63(6) 3.3684(16) 145(6) N1 H1N1 Cl2 6_565 0.86(5) 2.88(6) 3.402(5) 121(5)