#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007293.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_2007293 loop_ _publ_author_name 'Thiele, G.' 'Wittenburg, G.' _publ_section_title ; Trimethylammonium Nickel(II) Chloride Dihydrate ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 764 _journal_page_last 766 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '(C3 H10 N)[Ni Cl2 (H2 O)2]Cl' _chemical_formula_moiety '[(CH~3~)~3~NH]NiCl~3~^.^2H~2~O' _chemical_formula_sum 'C3 H14 Cl3 N Ni O2' _chemical_formula_weight 261.21 _chemical_name_common Trimethylammoniumnickel(II)chloridedihydrate _chemical_name_systematic Trimethylammoniumdiaquodichloronickel(II)chloride _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m 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 4 _cell_length_a 16.675(3) _cell_length_b 7.1630(10) _cell_length_c 8.100(2) _cell_measurement_reflns_used 19 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.29 _cell_measurement_theta_min 10.19 _cell_volume 967.5(3) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CADFOR/CADSEX (Keller, 1981)' _computing_molecular_graphics 'ORTEPIII (Johnson & Burnett, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 2 _diffrn_measured_fraction_theta_full 0.912 _diffrn_measured_fraction_theta_max 0.912 _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1032 _diffrn_reflns_theta_full 24.97 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.44 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.783 _exptl_absorpt_correction_T_max 0.757 _exptl_absorpt_correction_T_min 0.528 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'XEMP (Siemens, 1989)' _exptl_crystal_colour yellow-green _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.578 _refine_diff_density_min -0.488 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 85 _refine_ls_number_reflns 925 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0271 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0764P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref 0.0789 _reflns_number_gt 622 _reflns_number_total 925 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ab1508.cif _[local]_cod_data_source_block 1 _[local]_cod_cif_authors_sg_H-M 'P n m a ' _[local]_cod_cif_authors_sg_Hall '-P 2ac 2n ' _cod_database_code 2007293 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, 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 Ni 0.0000 0.0000 0.0000 0.0199(2) Uani d S 1 Ni Cl1 0.09605(7) -0.2500 0.06739(16) 0.0247(3) Uani d S 1 Cl Cl2 0.09687(6) 0.2500 0.00711(14) 0.0234(3) Uani d S 1 Cl O 0.02440(17) -0.0374(4) -0.2465(3) 0.0262(5) Uani d S 1 O H3A 0.041(3) 0.070(7) -0.285(6) 0.058(15) Uiso d S 1 H H3B -0.009(2) -0.093(6) -0.290(6) 0.045(15) Uiso d S 1 H Cl3 0.08792(8) 0.2500 -0.50303(14) 0.0298(3) Uani d S 1 Cl N 0.1825(3) -0.2500 -0.3051(5) 0.0273(10) Uani d S 1 N H1 0.142(3) -0.2500 -0.265(6) 0.022(15) Uiso d S 1 H C1 0.2255(3) -0.0790(6) -0.2521(6) 0.0397(10) Uani d S 1 C H1A 0.276(3) -0.083(7) -0.309(6) 0.067(14) Uiso d S 1 H H1B 0.226(2) -0.078(6) -0.141(7) 0.056(14) Uiso d S 1 H H1C 0.196(3) 0.037(7) -0.291(6) 0.065(14) Uiso d S 1 H C2 0.1671(4) -0.2500 -0.4853(7) 0.0378(14) Uani d S 1 C H2A 0.140(3) -0.146(7) -0.506(5) 0.063(16) Uiso d S 1 H H2B 0.222(4) -0.2500 -0.541(7) 0.039(16) Uiso d S 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 Ni 0.0207(3) 0.0195(3) 0.0196(3) -0.0001(2) 0.0006(2) -0.0011(3) Cl1 0.0214(6) 0.0237(6) 0.0291(6) 0.000 -0.0026(5) 0.000 Cl2 0.0196(6) 0.0209(6) 0.0295(6) 0.000 -0.0022(6) 0.000 O 0.0311(13) 0.0236(13) 0.0239(13) -0.0046(13) 0.0009(11) 0.0001(12) Cl3 0.0359(7) 0.0293(7) 0.0242(6) 0.000 -0.0009(6) 0.000 N 0.021(2) 0.032(3) 0.029(2) 0.000 0.007(2) 0.000 C1 0.037(2) 0.036(2) 0.045(3) -0.002(2) 0.004(2) -0.009(2) C2 0.040(4) 0.041(4) 0.032(3) 0.000 0.000(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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 O Ni O . 5 180.0 no O Ni Cl2 . 5 90.72(9) yes O Ni Cl2 5 5 89.28(9) yes O Ni Cl2 . . 89.28(9) no O Ni Cl2 5 . 90.72(9) no Cl2 Ni Cl2 5 . 180.0 no O Ni Cl1 . . 89.53(8) yes O Ni Cl1 5 . 90.47(8) yes Cl2 Ni Cl1 5 . 84.32(3) yes Cl2 Ni Cl1 . . 95.68(3) yes O Ni Cl1 . 5 90.47(8) no O Ni Cl1 5 5 89.53(8) no Cl2 Ni Cl1 5 5 95.68(3) no Cl2 Ni Cl1 . 5 84.32(3) no Cl1 Ni Cl1 . 5 180.0 yes Ni Cl1 Ni 3_545 . 93.25(4) yes Ni Cl2 Ni . 3 95.86(4) yes C2 N C1 . . 111.7(3) yes C2 N C1 . 7 111.7(3) no C1 N C1 . 7 111.4(5) yes 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 Ni O . 2.055(3) yes Ni O 5 2.055(3) no Ni Cl2 5 2.4123(8) no Ni Cl2 . 2.4123(8) yes Ni Cl1 . 2.4637(8) yes Ni Cl1 5 2.4637(8) no Cl1 Ni 3_545 2.4637(8) no Cl2 Ni 3 2.4123(8) no N C2 . 1.482(8) yes N C1 . 1.483(5) yes N C1 7 1.483(5) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O H3A Cl3 0.87(5) 2.32(5) 3.111(3) 150(4) yes O H3B Cl3 0.77(4) 2.41(4) 3.153(3) 163(4) yes N H1 O 0.75(5) 2.49(4) 3.082(5) 138(4) yes N H1 Cl1 0.75(5) 2.80(5) 3.344(4) 132(5) yes