#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003276.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003276 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 368 _journal_page_last 370 _publ_section_title ; [1,2-Bis(diphenylphosphino)ethane-P,P'](4-morpholinecarbodithioato- S,S')nickel(II) Perchlorate Dichloromethane Solvate ; _chemical_formula_moiety 'C31 H32 N Ni O P2 S2 , CH2 Cl2 , Cl O4' _chemical_formula_sum 'C32 H34 Cl3 N Ni O5 P2 S2' _chemical_formula_weight 803.72 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.456(2) _cell_length_b 22.745(4) _cell_length_c 16.707(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.16(2) _cell_angle_gamma 90.00 _cell_volume 3587.8(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_meas No _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 15 _exptl_absorpt_coefficient_mu 1.010 _cell_measurement_temperature 293(2) _exptl_crystal_description Needles _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_colour Orange _chemical_compound_source ; The preparation of the title compound was accomplished by established procedures (Ramalingam, Aravamudan, Seshasayee & Subramanyam, 1984; Ramalingam, Aravamudan & Seshasayee, 1987). The parent dithiocarbamato complex was prepared from morpholinium morpholine 4-carbodithioate and nickel chloride (Aravamudan, Brown & Venkappayya, 1971). Single crystals were obtained from dichloromethane solution by slow evaporation at room temperature. ; _diffrn_measurement_device 'Siemens P4 four-circle' _diffrn_measurement_method '\q-2\q scans' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 8522 _reflns_number_total 8245 _reflns_number_observed 3962 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_theta_max 27.57 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <3 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0510 _refine_ls_wR_factor_obs 0.1073 _refine_ls_wR_factor_all 0.1306 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_goodness_of_fit_all 0.869 _refine_ls_number_reflns 8245 _refine_ls_number_parameters 457 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^) + (0.0621P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.002 _refine_diff_density_max 0.447 _refine_diff_density_min -0.431 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.094 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.123 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1484 0.1 'Ni' 'Ni' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3393 1.1 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ni 1 0.34673(5) 0.52070(2) 0.69655(3) 0.04178(15) S1 1 0.41710(12) 0.44922(5) 0.61808(6) 0.0523(3) S2 1 0.49575(13) 0.47404(5) 0.77950(6) 0.0604(3) P1 1 0.24779(10) 0.58224(5) 0.61166(6) 0.0425(3) P2 1 0.26153(11) 0.57390(5) 0.78957(6) 0.0444(3) C1 1 0.1856(4) 0.6411(2) 0.7465(2) 0.0534(11) H1A 1 0.2586(4) 0.6699(2) 0.7411(2) 0.080 H1B 1 0.1164(4) 0.6569(2) 0.7806(2) 0.080 C2 1 0.1190(4) 0.6262(2) 0.6635(2) 0.0511(10) H2A 1 0.0339(4) 0.6040(2) 0.6694(2) 0.080 H2B 1 0.0956(4) 0.6612(2) 0.6335(2) 0.080 C3 1 0.3888(4) 0.6332(2) 0.5889(2) 0.0451(9) C4 1 0.3598(5) 0.6914(2) 0.5684(3) 0.0602(12) H4 1 0.2636(5) 0.7051(2) 0.5673(3) 0.080 C5 1 0.4669(6) 0.7283(2) 0.5492(3) 0.0729(14) H5 1 0.4458(6) 0.7687(2) 0.5368(3) 0.080 C6 1 0.6041(6) 0.7083(3) 0.5480(3) 0.082(2) H6 1 0.6787(6) 0.7343(3) 0.5338(3) 0.080 C7 1 0.6323(5) 0.6518(3) 0.5670(3) 0.081(2) H7 1 0.7278(5) 0.6378(3) 0.5651(3) 0.080 C8 1 0.5265(4) 0.6133(2) 0.5876(3) 0.0625(12) H8 1 0.5482(4) 0.5732(2) 0.6016(3) 0.080 C9 1 0.1658(4) 0.5631(2) 0.5137(2) 0.0446(9) C10 1 0.0389(4) 0.5863(2) 0.4862(3) 0.0631(12) H10 1 -0.0120(4) 0.6118(2) 0.5203(3) 0.080 C11 1 -0.0162(5) 0.5737(3) 0.4100(3) 0.081(2) H11 1 -0.1063(5) 0.5894(3) 0.3911(3) 0.080 C12 1 0.0576(6) 0.5377(3) 0.3611(3) 0.077(2) H12 1 0.0204(6) 0.5296(3) 0.3076(3) 0.080 C13 1 0.1828(6) 0.5141(2) 0.3882(3) 0.0740(14) H13 1 0.2336(6) 0.4886(2) 0.3541(3) 0.080 C14 1 0.2376(5) 0.5265(2) 0.4646(2) 0.0594(11) H14 1 0.3268(5) 0.5102(2) 0.4838(2) 0.080 C15 1 0.3866(4) 0.5944(2) 0.8703(2) 0.0480(10) C16 1 0.3808(5) 0.5719(3) 0.9458(3) 0.083(2) H16 1 0.3026(5) 0.5472(3) 0.9583(3) 0.080 C17 1 0.4851(7) 0.5853(3) 1.0036(3) 0.098(2) H17 1 0.4833(7) 0.5675(3) 1.0556(3) 0.080 C18 1 0.5920(6) 0.6221(3) 0.9887(3) 0.079(2) H18 1 0.6619(6) 0.6326(3) 1.0300(3) 0.080 C19 1 0.5973(5) 0.6450(2) 0.9145(4) 0.085(2) H19 1 0.6740(5) 0.6706(2) 0.9025(4) 0.080 C20 1 0.4969(5) 0.6318(2) 0.8553(3) 0.0735(14) H20 1 0.5024(5) 0.6487(2) 0.8029(3) 0.080 C21 1 0.1191(4) 0.5341(2) 0.8334(2) 0.0494(10) C22 1 0.1336(5) 0.4752(2) 0.8470(3) 0.0704(13) H22 1 0.2177(5) 0.4558(2) 0.8309(3) 0.080 C23 1 0.0302(7) 0.4435(3) 0.8822(3) 0.085(2) H23 1 0.0446(7) 0.4025(3) 0.8937(3) 0.080 C24 1 -0.0909(7) 0.4700(3) 0.9015(3) 0.098(2) H24 1 -0.1637(7) 0.4475(3) 0.9251(3) 0.080 C25 1 -0.1072(6) 0.5280(3) 0.8886(4) 0.114(2) H25 1 -0.1941(6) 0.5463(3) 0.9022(4) 0.080 C26 1 -0.0029(6) 0.5606(2) 0.8549(3) 0.089(2) H26 1 -0.0151(6) 0.6020(2) 0.8462(3) 0.080 C27 1 0.5140(5) 0.4263(2) 0.7019(2) 0.0583(12) N28A 0.50 0.6226(11) 0.3877(5) 0.7003(7) 0.053(2) C29A 0.50 0.6445(13) 0.3467(5) 0.6322(6) 0.067(2) H29A 0.50 0.7400(13) 0.3516(5) 0.6167(6) 0.080 H29B 0.50 0.5816(13) 0.3564(5) 0.5871(6) 0.080 C30A 0.50 0.6248(15) 0.2839(5) 0.6588(7) 0.086(2) H30A 0.50 0.6481(15) 0.2578(5) 0.6163(7) 0.080 H30B 0.50 0.5271(15) 0.2780(5) 0.6695(7) 0.080 O31A 0.50 0.720(5) 0.2714(19) 0.7301(26) 0.102(7) C32A 0.50 0.6869(15) 0.3075(5) 0.7916(8) 0.086(2) H32A 0.50 0.7487(15) 0.2959(5) 0.8364(8) 0.080 H32B 0.50 0.5910(15) 0.3025(5) 0.8064(8) 0.080 C33A 0.50 0.7088(12) 0.3713(5) 0.7738(6) 0.067(2) H33A 0.50 0.6837(12) 0.3957(5) 0.8177(6) 0.080 H33B 0.50 0.8069(12) 0.3777(5) 0.7645(6) 0.080 N28B 0.50 0.5647(11) 0.3712(5) 0.7115(7) 0.053(2) C29B 0.50 0.6286(11) 0.3497(5) 0.7882(6) 0.067(2) H29C 0.50 0.5720(11) 0.3197(5) 0.8109(6) 0.080 H29D 0.50 0.6358(11) 0.3821(5) 0.8250(6) 0.080 C30B 0.50 0.7746(14) 0.3265(6) 0.7765(8) 0.086(2) H30C 0.50 0.8339(14) 0.3579(6) 0.7596(8) 0.080 H30D 0.50 0.8158(14) 0.3110(6) 0.8259(8) 0.080 O31B 0.50 0.763(5) 0.2820(19) 0.7149(26) 0.102(7) C32B 0.50 0.7127(13) 0.3038(6) 0.6428(7) 0.086(2) H32C 0.50 0.7725(13) 0.3357(6) 0.6280(7) 0.080 H32D 0.50 0.7168(13) 0.2737(6) 0.6028(7) 0.080 C33B 0.50 0.5674(11) 0.3282(5) 0.6467(6) 0.067(2) H33C 0.50 0.5364(11) 0.3468(5) 0.5973(6) 0.080 H33D 0.50 0.5054(11) 0.2958(5) 0.6560(6) 0.080 H34A 1 0.0647(7) 0.2281(3) 0.1962(5) 0.080 H34B 1 0.0509(7) 0.2279(3) 0.2884(5) 0.080 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ni 0.0492(3) 0.0075(2) 0.0006(2) 0.0424(3) 0.0006(2) 0.0336(3) S1 0.0660(7) 0.0185(5) -0.0064(5) 0.0533(6) -0.0053(5) 0.0366(5) S2 0.0787(8) 0.0273(6) -0.0086(5) 0.0650(7) -0.0055(5) 0.0360(5) P1 0.0443(6) 0.0046(5) 0.0014(4) 0.0444(6) 0.0045(5) 0.0388(5) P2 0.0524(6) 0.0028(5) 0.0046(5) 0.0425(6) -0.0025(5) 0.0386(5) C1 0.065(3) 0.008(2) 0.011(2) 0.041(2) -0.003(2) 0.054(3) C2 0.050(2) 0.012(2) 0.009(2) 0.049(3) 0.008(2) 0.055(3) C3 0.051(2) 0.000(2) -0.002(2) 0.050(3) -0.001(2) 0.035(2) C4 0.065(3) 0.000(2) 0.007(2) 0.051(3) 0.004(2) 0.065(3) C5 0.094(4) -0.017(3) 0.007(3) 0.056(3) 0.003(3) 0.069(3) C6 0.084(4) -0.038(3) 0.006(3) 0.087(4) 0.002(3) 0.075(4) C7 0.050(3) -0.011(3) 0.007(3) 0.103(5) 0.003(3) 0.092(4) C8 0.054(3) -0.002(2) 0.005(2) 0.062(3) 0.006(2) 0.073(3) C9 0.043(2) -0.004(2) -0.001(2) 0.047(2) 0.010(2) 0.043(2) C10 0.046(2) 0.002(2) 0.000(2) 0.084(4) 0.015(3) 0.059(3) C11 0.050(3) -0.008(3) -0.022(3) 0.113(5) 0.021(4) 0.076(4) C12 0.082(4) -0.029(3) -0.021(3) 0.095(4) 0.012(3) 0.052(3) C13 0.094(4) -0.004(3) -0.008(3) 0.080(4) -0.004(3) 0.047(3) C14 0.068(3) 0.008(2) -0.008(2) 0.067(3) 0.003(2) 0.042(2) C15 0.056(2) 0.002(2) 0.005(2) 0.050(3) -0.010(2) 0.039(2) C16 0.079(4) -0.025(3) 0.001(2) 0.124(5) 0.001(3) 0.045(3) C17 0.114(5) -0.014(4) -0.003(3) 0.138(6) 0.000(3) 0.040(3) C18 0.075(4) 0.002(3) -0.014(3) 0.089(4) -0.027(3) 0.070(4) C19 0.073(4) -0.023(3) -0.012(3) 0.085(4) -0.008(4) 0.097(4) C20 0.081(3) -0.019(3) -0.011(3) 0.077(4) 0.006(3) 0.061(3) C21 0.053(2) -0.002(2) 0.006(2) 0.053(3) -0.005(2) 0.042(2) C22 0.066(3) -0.005(3) 0.014(3) 0.071(3) 0.010(3) 0.076(3) C23 0.103(4) -0.025(3) 0.007(3) 0.077(4) 0.010(3) 0.077(4) C24 0.088(4) -0.046(4) 0.029(3) 0.126(6) -0.012(4) 0.083(4) C25 0.086(4) 0.003(4) 0.066(4) 0.118(6) -0.014(5) 0.143(6) C26 0.083(4) 0.007(3) 0.041(4) 0.072(4) -0.004(3) 0.116(5) C27 0.080(3) 0.026(2) -0.003(2) 0.056(3) 0.001(2) 0.038(2) N28A 0.071(8) 0.010(4) -0.002(5) 0.045(6) 0.008(4) 0.042(4) C29A 0.091(6) 0.026(4) -0.002(4) 0.061(5) 0.004(3) 0.048(3) C30A 0.117(8) 0.030(5) -0.005(5) 0.062(5) 0.009(4) 0.077(4) O31A 0.165(24) 0.049(12) 0.004(10) 0.063(13) 0.017(7) 0.077(13) C32A 0.117(8) 0.030(5) -0.005(5) 0.062(5) 0.009(4) 0.077(4) C33A 0.091(6) 0.026(4) -0.002(4) 0.061(5) 0.004(3) 0.048(3) N28B 0.071(8) 0.010(4) -0.002(5) 0.045(6) 0.008(4) 0.042(4) C29B 0.091(6) 0.026(4) -0.002(4) 0.061(5) 0.004(3) 0.048(3) C30B 0.117(8) 0.030(5) -0.005(5) 0.062(5) 0.009(4) 0.077(4) O31B 0.165(24) 0.049(12) 0.004(10) 0.063(13) 0.017(7) 0.077(13) C32B 0.117(8) 0.030(5) -0.005(5) 0.062(5) 0.009(4) 0.077(4) C33B 0.091(6) 0.026(4) -0.002(4) 0.061(5) 0.004(3) 0.048(3) _cod_database_code 2003276