#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003321.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_2003321 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 595 _journal_page_last 598 _publ_section_title ; Azidotetrakis(trimethylphosphine)nickel(II) Tetrafluoroborate ; _chemical_formula_moiety 'C12 H36 N3 Ni P4 1+, B F4 1-' _chemical_formula_sum 'C12 H36 B F4 N3 Ni P4' _chemical_formula_structural 'Ni N3 (P (C H3)3)4 B F4' _chemical_formula_weight 491.84 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _symmetry_space_group_name_H-M 'P b c a' _cell_length_a 13.778(2) _cell_length_b 13.2816(13) _cell_length_c 26.188(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4792.1(9) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 39 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.0 _exptl_absorpt_coefficient_mu 1.109 _cell_measurement_temperature 298(2) _exptl_crystal_description 'prism' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_colour 'dark violet' _diffrn_measurement_device 'Siemans P4' _diffrn_measurement_method 'Profile-fitted \w' _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.609 _diffrn_reflns_number 5242 _reflns_number_total 4220 _reflns_number_observed 2018 _reflns_observed_criterion 'I>2\s(I)' _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 1 _diffrn_standards_number 3 _diffrn_standards_interval_time 97 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef 'Fsqd' _refine_ls_R_factor_obs 0.0577 _refine_ls_wR_factor_obs 0.1337 _refine_ls_wR_factor_all 0.1529 _refine_ls_goodness_of_fit_obs 1.106 _refine_ls_goodness_of_fit_all 0.852 _refine_ls_number_reflns 4220 _refine_ls_number_parameters 232 _refine_ls_hydrogen_treatment 'H atoms refined as riding' _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0743P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.052 _refine_diff_density_max .657 _refine_diff_density_min -.633 _refine_ls_extinction_method none 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' .0033 .0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 'B' 'B' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0013 .0007 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033 'F' 'F' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0171 .0103 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1023 .0942 'Ni' 'Ni' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .3393 1.11 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 Ni1 1 0.0554(1) 0.1954(1) 0.1057(1) 0.045(1) P1 1 -0.0521(1) 0.0847(2) 0.1435(1) 0.064(1) P2 1 0.0447(1) 0.2476(1) 0.0221(1) 0.054(1) P3 1 0.2006(1) 0.2210(1) 0.1483(1) 0.053(1) P4 1 -0.0137(1) 0.3283(1) 0.1353(1) 0.061(1) N1 1 0.1045(4) 0.0742(4) 0.0744(2) 0.064(2) N2 1 0.1775(5) 0.0430(5) 0.0588(2) 0.066(2) N3 1 0.2459(5) 0.0070(6) 0.0414(3) 0.135(3) C1 1 -0.1307(6) 0.1079(7) 0.1977(3) 0.104(3) H1A 1 -0.1721(26) 0.0507(17) 0.2029(12) 0.125 H1B 1 -0.1696(26) 0.1664(23) 0.1912(8) 0.125 H1C 1 -0.0919(6) 0.1188(37) 0.2276(5) 0.125 C2 1 0.0090(6) -0.0275(6) 0.1652(4) 0.117(3) H2A 1 -0.0382(7) -0.0761(17) 0.1761(19) 0.140 H2B 1 0.0509(29) -0.0110(10) 0.1933(13) 0.140 H2C 1 0.0469(32) -0.0551(23) 0.1378(7) 0.140 C3 1 -0.1370(5) 0.0334(7) 0.0972(3) 0.105(3) H3A 1 -0.1659(28) -0.0267(22) 0.1107(9) 0.126 H3B 1 -0.1031(9) 0.0176(37) 0.0662(8) 0.126 H3C 1 -0.1867(21) 0.0821(16) 0.0902(15) 0.126 C4 1 0.1597(5) 0.2487(7) -0.0110(2) 0.104(3) H4A 1 0.1487(5) 0.2572(39) -0.0469(3) 0.125 H4B 1 0.1928(17) 0.1862(16) -0.0051(16) 0.125 H4C 1 0.1986(15) 0.3033(23) 0.0015(14) 0.125 C5 1 -0.0031(7) 0.3651(6) -0.0028(3) 0.127(4) H5A 1 -0.0042(40) 0.3624(18) -0.0395(3) 0.152 H5B 1 0.0376(25) 0.4198(8) 0.0080(19) 0.152 H5C 1 -0.0677(17) 0.3753(22) 0.0098(18) 0.152 C6 1 -0.0250(6) 0.1607(6) -0.0140(3) 0.094(3) H6A 1 -0.0274(29) 0.1822(20) -0.0490(4) 0.113 H6B 1 -0.0897(11) 0.1577(26) -0.0005(11) 0.113 H6C 1 0.0043(19) 0.0953(10) -0.0121(15) 0.113 C7 1 0.2418(5) 0.1089(5) 0.1797(3) 0.087(2) H7A 1 0.3096(9) 0.1153(14) 0.1875(14) 0.105 H7B 1 0.2321(29) 0.0520(7) 0.1577(7) 0.105 H7C 1 0.2059(22) 0.0995(18) 0.2108(9) 0.105 C8 1 0.2271(6) 0.3115(5) 0.1980(3) 0.085(2) H8A 1 0.2939(10) 0.3053(22) 0.2080(12) 0.102 H8B 1 0.1861(22) 0.2989(21) 0.2269(7) 0.102 H8C 1 0.2154(30) 0.3783(6) 0.1854(6) 0.102 C9 1 0.2988(5) 0.2474(7) 0.1035(3) 0.094(3) H9A 1 0.3594(6) 0.2494(36) 0.1216(4) 0.113 H9B 1 0.2875(18) 0.3112(17) 0.0873(13) 0.113 H9C 1 0.3012(22) 0.1954(19) 0.0781(11) 0.113 C10 1 0.0457(5) 0.4435(5) 0.1184(3) 0.078(2) H10A 1 0.0245(23) 0.4963(8) 0.1408(10) 0.094 H10B 1 0.0298(23) 0.4607(16) 0.0838(6) 0.094 H10C 1 0.1147(5) 0.4352(10) 0.1215(15) 0.094 C11 1 -0.1383(5) 0.3483(7) 0.1138(3) 0.097(3) H11A 1 -0.1601(13) 0.4135(17) 0.1248(16) 0.116 H11B 1 -0.1795(8) 0.2973(23) 0.1281(15) 0.116 H11C 1 -0.1407(8) 0.3448(37) 0.0772(3) 0.116 C12 1 -0.0239(6) 0.3390(7) 0.2042(3) 0.098(3) H12A 1 -0.0390(34) 0.4074(10) 0.2132(3) 0.118 H12B 1 0.0365(13) 0.3200(35) 0.2198(3) 0.118 H12C 1 -0.0746(25) 0.2954(28) 0.2162(3) 0.118 B1A 0.50 0.5877(13) 0.1762(14) 0.1749(7) 0.091(3) F1A 0.50 0.6431(9) 0.2511(9) 0.1930(5) 0.125(5) F2A 0.50 0.6170(9) 0.0885(9) 0.1978(5) 0.143(4) F3A 0.50 0.5931(11) 0.1587(11) 0.1241(4) 0.164(5) F4A 0.50 0.4943(7) 0.1954(8) 0.1857(4) 0.122(4) B1B 0.50 0.5961(14) 0.1787(14) 0.1687(7) 0.091(3) F1B 0.50 0.6541(8) 0.2595(8) 0.1723(4) 0.104(4) F2B 0.50 0.6433(8) 0.1076(9) 0.1402(5) 0.134(4) F3B 0.50 0.5189(9) 0.2053(9) 0.1390(5) 0.141(4) F4B 0.50 0.5706(10) 0.1377(11) 0.2148(4) 0.161(5) 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 Ni1 0.039(1) 0.003(1) 0.001(1) 0.048(1) -0.001(1) 0.047(1) P1 0.053(1) -0.014(1) 0.009(1) 0.076(1) 0.001(1) 0.064(1) P2 0.062(1) 0.005(1) -0.010(1) 0.053(1) 0.004(1) 0.047(1) P3 0.044(1) -0.004(1) -0.006(1) 0.068(1) 0.005(1) 0.048(1) P4 0.054(1) 0.011(1) 0.006(1) 0.063(1) -0.010(1) 0.066(1) N1 0.065(4) 0.011(3) 0.017(3) 0.058(4) -0.010(3) 0.070(4) N2 0.069(4) 0.009(4) -0.011(3) 0.068(4) -0.007(3) 0.061(4) N3 0.083(5) 0.040(5) 0.010(6) 0.139(7) -0.063(7) 0.183(8) C1 0.095(6) -0.028(6) 0.040(5) 0.130(8) -0.002(6) 0.088(5) C2 0.117(7) -0.015(6) 0.040(6) 0.090(7) 0.054(6) 0.143(8) C3 0.088(6) -0.053(6) 0.006(5) 0.135(8) -0.006(6) 0.092(6) C4 0.085(6) -0.003(6) 0.009(4) 0.173(9) 0.033(6) 0.053(4) C5 0.222(11) 0.053(8) -0.030(6) 0.089(6) 0.021(5) 0.069(5) C6 0.120(7) -0.018(5) -0.039(5) 0.096(6) -0.004(5) 0.066(5) C7 0.085(5) 0.018(5) -0.040(5) 0.093(6) 0.001(5) 0.084(5) C8 0.084(5) -0.018(5) -0.024(4) 0.089(6) 0.003(5) 0.082(5) C9 0.045(4) -0.015(5) -0.004(4) 0.156(8) 0.021(6) 0.081(5) C10 0.089(5) 0.008(4) -0.003(5) 0.056(4) -0.008(4) 0.090(5) C11 0.060(5) 0.031(5) 0.006(5) 0.112(7) -0.014(6) 0.119(7) C12 0.089(6) 0.014(6) 0.021(5) 0.128(7) -0.028(6) 0.077(5) _cod_database_code 2003321