#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060272.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_4060272 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C20 H37 Br Ni P2' _chemical_formula_moiety 'C20 H37 Br Ni P2' _chemical_formula_weight 478.06 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' _cell_length_a 10.58(2) _cell_length_b 15.87(2) _cell_length_c 14.26(3) _cell_angle_alpha 90 _cell_angle_beta 110.33(6) _cell_angle_gamma 90 _cell_volume 2244.1(71) _cell_formula_units_Z 4 _cell_measurement_reflns_used 73 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 173.1 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000.00 _exptl_absorpt_coefficient_mu 2.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.390 _exptl_absorpt_correction_T_max 0.572 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 30142 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 27.88 _diffrn_measured_fraction_theta_max 0.9931 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.9802 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _reflns_number_total 5500 _reflns_number_gt 3900 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1460 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 5308 _refine_ls_number_parameters 365 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0516P)^2^+2.7603P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.3420 _refine_diff_density_max 0.65 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Ni' 'Ni' 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.60335(7) 0.13303(4) 0.67876(5) 0.0356(2) Uani 1.00 1 d . . . Ni(1) Ni 0.78081(7) 0.23314(4) 0.73614(5) 0.0169(2) Uani 1.00 1 d . . . P(1) P 0.9106(1) 0.34014(8) 0.77990(9) 0.0166(3) Uani 1.00 1 d . . . P(2) P 0.7157(1) 0.29721(8) 0.85302(10) 0.0192(3) Uani 1.00 1 d . . . C(1) C 0.8809(6) 0.1853(4) 0.6520(4) 0.0237(13) Uani 1.00 1 d . . . C(2) C 1.0030(6) 0.1386(3) 0.7129(4) 0.0197(12) Uani 1.00 1 d . . . C(3) C 1.1284(7) 0.1537(4) 0.7069(5) 0.030(1) Uani 1.00 1 d . . . C(4) C 1.2403(7) 0.1092(5) 0.7652(6) 0.045(2) Uani 1.00 1 d . . . C(5) C 1.2295(9) 0.0504(5) 0.8322(6) 0.051(2) Uani 1.00 1 d . . . C(6) C 1.1065(8) 0.0328(4) 0.8396(5) 0.043(2) Uani 1.00 1 d . . . C(7) C 0.9935(7) 0.0764(3) 0.7805(4) 0.030(1) Uani 1.00 1 d . . . C(8) C 1.0951(6) 0.3384(3) 0.8331(4) 0.0228(12) Uani 1.00 1 d . . . C(9) C 1.1461(7) 0.2716(4) 0.9149(4) 0.0266(13) Uani 1.00 1 d . . . C(10) C 1.1538(8) 0.4243(4) 0.8731(6) 0.038(2) Uani 1.00 1 d . . . C(11) C 0.8679(6) 0.4242(3) 0.6840(4) 0.0226(12) Uani 1.00 1 d . . . C(12) C 0.9458(8) 0.4163(5) 0.6127(5) 0.035(2) Uani 1.00 1 d . . . C(13) C 0.7187(7) 0.4266(5) 0.6271(5) 0.036(2) Uani 1.00 1 d . . . C(14) C 0.8511(6) 0.3762(4) 0.8800(4) 0.0201(12) Uani 1.00 1 d . . . C(15) C 0.5624(6) 0.3621(4) 0.8301(4) 0.0263(13) Uani 1.00 1 d . . . C(16) C 0.4307(7) 0.3152(5) 0.7792(5) 0.037(2) Uani 1.00 1 d . . . C(17) C 0.5631(8) 0.4122(5) 0.9223(6) 0.037(2) Uani 1.00 1 d . . . C(18) C 0.7454(6) 0.2381(4) 0.9706(4) 0.028(1) Uani 1.00 1 d . . . C(19) C 0.6267(9) 0.1799(6) 0.9616(6) 0.051(2) Uani 1.00 1 d . . . C(20) C 0.8760(8) 0.1887(4) 0.9971(5) 0.035(2) Uani 1.00 1 d . . . H(1) H 0.827(5) 0.424(3) 0.874(3) 0.007(13) Uiso 1.00 1 c . . . H(2) H 0.911(6) 0.369(3) 0.943(4) 0.03(2) Uiso 1.00 1 c . . . H(3) H 0.542(6) 0.379(4) 0.972(4) 0.03(2) Uiso 1.00 1 c . . . H(4) H 0.647(6) 0.438(3) 0.953(4) 0.02(2) Uiso 1.00 1 c . . . H(5) H 0.412(6) 0.284(4) 0.831(5) 0.04(2) Uiso 1.00 1 c . . . H(6) H 0.438(5) 0.284(3) 0.721(4) 0.02(2) Uiso 1.00 1 c . . . H(7) H 0.577(6) 0.404(3) 0.785(4) 0.03(2) Uiso 1.00 1 c . . . H(8) H 0.620(7) 0.145(4) 0.908(5) 0.04(2) Uiso 1.00 1 c . . . H(9) H 0.648(6) 0.149(3) 1.021(4) 0.03(2) Uiso 1.00 1 c . . . H(10) H 0.757(5) 0.276(3) 1.020(3) 0.004(12) Uiso 1.00 1 c . . . H(11) H 0.874(7) 0.145(4) 0.948(5) 0.06(2) Uiso 1.00 1 c . . . H(12) H 0.908(6) 0.062(3) 0.778(4) 0.02(2) Uiso 1.00 1 c . . . H(13) H 1.320(6) 0.122(3) 0.762(4) 0.02(2) Uiso 1.00 1 c . . . H(14) H 0.906(6) 0.231(3) 0.609(4) 0.03(2) Uiso 1.00 1 c . . . H(15) H 1.129(5) 0.323(3) 0.784(3) 0.004(11) Uiso 1.00 1 c . . . H(16) H 1.132(5) 0.291(3) 0.971(4) 0.011(13) Uiso 1.00 1 c . . . H(17) H 0.919(7) 0.369(4) 0.578(5) 0.04(2) Uiso 1.00 1 c . . . H(18) H 0.900(5) 0.466(3) 0.721(3) 0.000(11) Uiso 1.00 1 c . . . H(19) H 0.677(6) 0.433(3) 0.667(4) 0.03(2) Uiso 1.00 1 c . . . H(20) H 1.124(6) 0.444(4) 0.917(4) 0.03(2) Uiso 1.00 1 c . . . H(21) H 0.815(6) 0.146(3) 0.616(4) 0.02(1) Uiso 1.00 1 c . . . H(22) H 1.145(6) 0.191(3) 0.666(4) 0.02(2) Uiso 1.00 1 c . . . H(23) H 1.292(7) 0.026(4) 0.870(5) 0.05(2) Uiso 1.00 1 c . . . H(24) H 1.090(6) -0.011(4) 0.890(4) 0.04(2) Uiso 1.00 1 c . . . H(25) H 0.702(7) 0.471(4) 0.576(5) 0.05(2) Uiso 1.00 1 c . . . H(26) H 0.696(9) 0.380(5) 0.576(6) 0.09(3) Uiso 1.00 1 c . . . H(27) H 0.930(5) 0.463(3) 0.563(4) 0.02(1) Uiso 1.00 1 c . . . H(28) H 1.041(8) 0.412(4) 0.643(5) 0.05(2) Uiso 1.00 1 c . . . H(29) H 0.360(7) 0.356(4) 0.752(5) 0.04(2) Uiso 1.00 1 c . . . H(30) H 0.508(7) 0.455(4) 0.899(5) 0.04(2) Uiso 1.00 1 c . . . H(31) H 0.940(7) 0.217(4) 1.001(5) 0.04(2) Uiso 1.00 1 c . . . H(32) H 0.883(7) 0.143(4) 1.054(6) 0.07(2) Uiso 1.00 1 c . . . H(33) H 1.123(6) 0.218(4) 0.892(4) 0.03(2) Uiso 1.00 1 c . . . H(34) H 1.229(7) 0.265(4) 0.928(4) 0.03(2) Uiso 1.00 1 c . . . H(35) H 1.250(9) 0.423(5) 0.907(6) 0.08(3) Uiso 1.00 1 c . . . H(36) H 1.134(6) 0.467(4) 0.829(5) 0.04(2) Uiso 1.00 1 c . . . H(37) H 0.553(8) 0.216(5) 0.965(5) 0.06(2) Uiso 1.00 1 c . . .