#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003321.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_2003321 loop_ _publ_author_name 'Carson, C. C.' 'Pike, R. D.' 'Carpenter, G. B.' _publ_section_title ; Azidotetrakis(trimethylphosphine)nickel(II) Tetrafluoroborate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 595 _journal_page_last 598 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C12 H36 N3 Ni P4 1+, B F4 1-' _chemical_formula_structural 'Ni N3 (P (C H3)3)4 B F4' _chemical_formula_sum 'C12 H36 B F4 N3 Ni P4' _chemical_formula_weight 491.84 _chemical_melting_point 408.15 _chemical_name_systematic ; azidotetrakis(trimethylphosphine)nickel(II) tetrafluoroborate ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.778(2) _cell_length_b 13.2816(13) _cell_length_c 26.188(3) _cell_measurement_reflns_used 39 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 2.15 _cell_volume 4792.2(10) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1993)' _computing_data_reduction XSCANS _computing_molecular_graphics SHELXTL/PC _computing_publication_material 'SHELXL93 ' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1994)' _computing_structure_solution 'SHELXTL/PC (Siemens, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measurement_device 'Siemans P4' _diffrn_measurement_method 'Profile-fitted \w' _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 0.0427 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 5242 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_T_max 0.609 _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_type empirical _exptl_crystal_colour 'dark violet' _exptl_crystal_density_diffrn 1.363 _exptl_crystal_description prism _exptl_crystal_F_000 2064 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _refine_diff_density_max .657 _refine_diff_density_min -.633 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.852 _refine_ls_goodness_of_fit_obs 1.106 _refine_ls_hydrogen_treatment 'H atoms refined as riding' _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 4220 _refine_ls_number_restraints 94 _refine_ls_restrained_S_all 0.894 _refine_ls_restrained_S_obs 1.166 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_obs 0.0577 _refine_ls_shift/esd_max -0.052 _refine_ls_shift/esd_mean 0.003 _refine_ls_structure_factor_coef Fsqd _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_wR_factor_all 0.1529 _refine_ls_wR_factor_obs 0.1337 _reflns_number_observed 2018 _reflns_number_total 4220 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file bk1077.cif _[local]_cod_data_source_block rp03 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '135 C' was changed to '408.15' - it was converted from degrees Celsius(C) to Kelvins(K). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 4792.1(9) _cod_database_code 2003321 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' 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 _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_type_symbol Ni1 1 0.0554(1) 0.1954(1) 0.1057(1) 0.045(1) Uani d . . Ni P1 1 -0.0521(1) 0.0847(2) 0.1435(1) 0.064(1) Uani d . . P P2 1 0.0447(1) 0.2476(1) 0.0221(1) 0.054(1) Uani d . . P P3 1 0.2006(1) 0.2210(1) 0.1483(1) 0.053(1) Uani d . . P P4 1 -0.0137(1) 0.3283(1) 0.1353(1) 0.061(1) Uani d . . P N1 1 0.1045(4) 0.0742(4) 0.0744(2) 0.064(2) Uani d . . N N2 1 0.1775(5) 0.0430(5) 0.0588(2) 0.066(2) Uani d . . N N3 1 0.2459(5) 0.0070(6) 0.0414(3) 0.135(3) Uani d . . N C1 1 -0.1307(6) 0.1079(7) 0.1977(3) 0.104(3) Uani d . . C H1A 1 -0.1721(26) 0.0507(17) 0.2029(12) 0.125 Uiso calc R . H H1B 1 -0.1696(26) 0.1664(23) 0.1912(8) 0.125 Uiso calc R . H H1C 1 -0.0919(6) 0.1188(37) 0.2276(5) 0.125 Uiso calc R . H C2 1 0.0090(6) -0.0275(6) 0.1652(4) 0.117(3) Uani d . . C H2A 1 -0.0382(7) -0.0761(17) 0.1761(19) 0.140 Uiso calc R . H H2B 1 0.0509(29) -0.0110(10) 0.1933(13) 0.140 Uiso calc R . H H2C 1 0.0469(32) -0.0551(23) 0.1378(7) 0.140 Uiso calc R . H C3 1 -0.1370(5) 0.0334(7) 0.0972(3) 0.105(3) Uani d . . C H3A 1 -0.1659(28) -0.0267(22) 0.1107(9) 0.126 Uiso calc R . H H3B 1 -0.1031(9) 0.0176(37) 0.0662(8) 0.126 Uiso calc R . H H3C 1 -0.1867(21) 0.0821(16) 0.0902(15) 0.126 Uiso calc R . H C4 1 0.1597(5) 0.2487(7) -0.0110(2) 0.104(3) Uani d . . C H4A 1 0.1487(5) 0.2572(39) -0.0469(3) 0.125 Uiso calc R . H H4B 1 0.1928(17) 0.1862(16) -0.0051(16) 0.125 Uiso calc R . H H4C 1 0.1986(15) 0.3033(23) 0.0015(14) 0.125 Uiso calc R . H C5 1 -0.0031(7) 0.3651(6) -0.0028(3) 0.127(4) Uani d . . C H5A 1 -0.0042(40) 0.3624(18) -0.0395(3) 0.152 Uiso calc R . H H5B 1 0.0376(25) 0.4198(8) 0.0080(19) 0.152 Uiso calc R . H H5C 1 -0.0677(17) 0.3753(22) 0.0098(18) 0.152 Uiso calc R . H C6 1 -0.0250(6) 0.1607(6) -0.0140(3) 0.094(3) Uani d . . C H6A 1 -0.0274(29) 0.1822(20) -0.0490(4) 0.113 Uiso calc R . H H6B 1 -0.0897(11) 0.1577(26) -0.0005(11) 0.113 Uiso calc R . H H6C 1 0.0043(19) 0.0953(10) -0.0121(15) 0.113 Uiso calc R . H C7 1 0.2418(5) 0.1089(5) 0.1797(3) 0.087(2) Uani d . . C H7A 1 0.3096(9) 0.1153(14) 0.1875(14) 0.105 Uiso calc R . H H7B 1 0.2321(29) 0.0520(7) 0.1577(7) 0.105 Uiso calc R . H H7C 1 0.2059(22) 0.0995(18) 0.2108(9) 0.105 Uiso calc R . H C8 1 0.2271(6) 0.3115(5) 0.1980(3) 0.085(2) Uani d . . C H8A 1 0.2939(10) 0.3053(22) 0.2080(12) 0.102 Uiso calc R . H H8B 1 0.1861(22) 0.2989(21) 0.2269(7) 0.102 Uiso calc R . H H8C 1 0.2154(30) 0.3783(6) 0.1854(6) 0.102 Uiso calc R . H C9 1 0.2988(5) 0.2474(7) 0.1035(3) 0.094(3) Uani d . . C H9A 1 0.3594(6) 0.2494(36) 0.1216(4) 0.113 Uiso calc R . H H9B 1 0.2875(18) 0.3112(17) 0.0873(13) 0.113 Uiso calc R . H H9C 1 0.3012(22) 0.1954(19) 0.0781(11) 0.113 Uiso calc R . H C10 1 0.0457(5) 0.4435(5) 0.1184(3) 0.078(2) Uani d . . C H10A 1 0.0245(23) 0.4963(8) 0.1408(10) 0.094 Uiso calc R . H H10B 1 0.0298(23) 0.4607(16) 0.0838(6) 0.094 Uiso calc R . H H10C 1 0.1147(5) 0.4352(10) 0.1215(15) 0.094 Uiso calc R . H C11 1 -0.1383(5) 0.3483(7) 0.1138(3) 0.097(3) Uani d . . C H11A 1 -0.1601(13) 0.4135(17) 0.1248(16) 0.116 Uiso calc R . H H11B 1 -0.1795(8) 0.2973(23) 0.1281(15) 0.116 Uiso calc R . H H11C 1 -0.1407(8) 0.3448(37) 0.0772(3) 0.116 Uiso calc R . H C12 1 -0.0239(6) 0.3390(7) 0.2042(3) 0.098(3) Uani d . . C H12A 1 -0.0390(34) 0.4074(10) 0.2132(3) 0.118 Uiso calc R . H H12B 1 0.0365(13) 0.3200(35) 0.2198(3) 0.118 Uiso calc R . H H12C 1 -0.0746(25) 0.2954(28) 0.2162(3) 0.118 Uiso calc R . H B1A 0.50 0.5877(13) 0.1762(14) 0.1749(7) 0.091(3) Uiso d PD 1 B F1A 0.50 0.6431(9) 0.2511(9) 0.1930(5) 0.125(5) Uiso d PD 1 F F2A 0.50 0.6170(9) 0.0885(9) 0.1978(5) 0.143(4) Uiso d PD 1 F F3A 0.50 0.5931(11) 0.1587(11) 0.1241(4) 0.164(5) Uiso d PD 1 F F4A 0.50 0.4943(7) 0.1954(8) 0.1857(4) 0.122(4) Uiso d PD 1 F B1B 0.50 0.5961(14) 0.1787(14) 0.1687(7) 0.091(3) Uiso d PD 2 B F1B 0.50 0.6541(8) 0.2595(8) 0.1723(4) 0.104(4) Uiso d PD 2 F F2B 0.50 0.6433(8) 0.1076(9) 0.1402(5) 0.134(4) Uiso d PD 2 F F3B 0.50 0.5189(9) 0.2053(9) 0.1390(5) 0.141(4) Uiso d PD 2 F F4B 0.50 0.5706(10) 0.1377(11) 0.2148(4) 0.161(5) Uiso d PD 2 F 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) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 Ni1 P4 173.6(2) yes N1 Ni1 P2 82.6(2) yes P4 Ni1 P2 93.89(7) yes N1 Ni1 P1 82.9(2) yes P4 Ni1 P1 94.80(8) yes P2 Ni1 P1 123.95(7) yes N1 Ni1 P3 91.4(2) yes P4 Ni1 P3 95.03(7) yes P2 Ni1 P3 118.02(7) yes P1 Ni1 P3 116.15(7) yes C2 P1 C1 99.9(4) ? C2 P1 C3 101.6(5) ? C1 P1 C3 101.7(4) ? C2 P1 Ni1 111.2(3) ? C1 P1 Ni1 127.7(3) ? C3 P1 Ni1 111.4(3) ? C6 P2 C4 103.0(4) ? C6 P2 C5 99.9(4) ? C4 P2 C5 98.0(4) ? C6 P2 Ni1 110.2(3) ? C4 P2 Ni1 113.7(2) ? C5 P2 Ni1 128.7(3) ? C7 P3 C8 99.1(3) ? C7 P3 C9 102.7(4) ? C8 P3 C9 100.6(4) ? C7 P3 Ni1 111.9(2) ? C8 P3 Ni1 128.2(3) ? C9 P3 Ni1 111.1(2) ? C10 P4 C12 102.4(4) ? C10 P4 C11 103.2(4) ? C12 P4 C11 102.9(4) ? C10 P4 Ni1 114.1(2) ? C12 P4 Ni1 117.2(3) ? C11 P4 Ni1 115.1(3) ? N2 N1 Ni1 138.6(5) yes N3 N2 N1 174.9(8) yes F1A B1A F4A 109.2(14) ? F1A B1A F3A 116.4(2) ? F4A B1A F3A 107.1(14) ? F1A B1A F2A 107.9(14) ? F4A B1A F2A 110.5(14) ? F3A B1A F2A 105.6(14) ? F1B B1B F3B 107.2(13) ? F1B B1B F4B 114.2(14) ? F3B B1B F4B 114(2) ? F1B B1B F2B 107.9(14) ? F3B B1B F2B 103.8(13) ? F4B B1B F2B 109.2(14) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ni1 N1 1.929(6) yes Ni1 P4 2.152(2) yes Ni1 P2 2.301(2) yes Ni1 P1 2.309(2) yes Ni1 P3 2.316(2) yes P1 C2 1.804(8) yes P1 C1 1.812(7) yes P1 C3 1.817(7) yes P2 C6 1.773(7) yes P2 C4 1.806(7) yes P2 C5 1.815(7) yes P3 C7 1.793(7) yes P3 C8 1.809(7) yes P3 C9 1.825(6) yes P4 C10 1.791(7) yes P4 C12 1.815(7) yes P4 C11 1.826(7) yes N1 N2 1.162(7) yes N2 N3 1.150(8) yes B1A F1A 1.34(2) ? B1A F4A 1.34(2) ? B1A F3A 1.35(2) ? B1A F2A 1.37(2) ? B1B F1B 1.34(2) ? B1B F3B 1.36(2) ? B1B F4B 1.37(2) ? B1B F2B 1.37(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion N1 Ni1 P1 C2 43.2(4) P4 Ni1 P1 C2 -142.9(4) P2 Ni1 P1 C2 119.2(3) P3 Ni1 P1 C2 -44.9(4) N1 Ni1 P1 C1 165.4(4) P4 Ni1 P1 C1 -20.7(4) P2 Ni1 P1 C1 -118.6(4) P3 Ni1 P1 C1 77.3(4) N1 Ni1 P1 C3 -69.4(4) P4 Ni1 P1 C3 104.6(3) P2 Ni1 P1 C3 6.6(3) P3 Ni1 P1 C3 -157.4(3) N1 Ni1 P2 C6 55.0(4) P4 Ni1 P2 C6 -119.7(3) P1 Ni1 P2 C6 -21.2(3) P3 Ni1 P2 C6 142.5(3) N1 Ni1 P2 C4 -60.1(4) P4 Ni1 P2 C4 125.3(4) P1 Ni1 P2 C4 -136.3(3) P3 Ni1 P2 C4 27.5(4) N1 Ni1 P2 C5 176.9(5) P4 Ni1 P2 C5 2.3(4) P1 Ni1 P2 C5 100.7(4) P3 Ni1 P2 C5 -95.5(4) N1 Ni1 P3 C7 -48.2(3) P4 Ni1 P3 C7 132.4(3) P2 Ni1 P3 C7 -130.5(3) P1 Ni1 P3 C7 34.5(3) N1 Ni1 P3 C8 -170.4(3) P4 Ni1 P3 C8 10.2(3) P2 Ni1 P3 C8 107.3(3) P1 Ni1 P3 C8 -87.7(3) N1 Ni1 P3 C9 65.9(4) P4 Ni1 P3 C9 -113.5(3) P2 Ni1 P3 C9 -16.4(3) P1 Ni1 P3 C9 148.6(3) N1 Ni1 P4 C10 -113.4(16) P2 Ni1 P4 C10 -57.3(3) P1 Ni1 P4 C10 178.1(3) P3 Ni1 P4 C10 61.3(3) N1 Ni1 P4 C12 126.9(16) P2 Ni1 P4 C12 -177.0(3) P1 Ni1 P4 C12 58.4(3) P3 Ni1 P4 C12 -58.4(3) N1 Ni1 P4 C11 5.7(17) P2 Ni1 P4 C11 61.8(3) P1 Ni1 P4 C11 -62.8(3) P3 Ni1 P4 C11 -179.6(3) P4 Ni1 N1 N2 140.1(13) P2 Ni1 N1 N2 83.5(8) P1 Ni1 N1 N2 -150.8(8) P3 Ni1 N1 N2 -34.6(8) Ni1 N1 N2 N3 -161.(9)