#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003312.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_2003312 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 602 _journal_page_last 604 _publ_section_title ; Dibromo[bis(\o-N,N-dimethylaminomethylphenyl)methylsilanol]cobalt(II) ; _chemical_formula_moiety 'Co Br~2~ (C19 H28 N2 O Si)' _chemical_formula_sum 'C19 H28 Br2 Co N2 O Si' _chemical_formula_weight 547.3 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z 1/2-X,-Y,1/2+Z -X,1/2+Y,1/2-Z 1/2+X,1/2-Y,-Z _symmetry_space_group_name_H-M 'P 21 21 21 ' _cell_length_a 11.8440(10) _cell_length_b 12.8710(10) _cell_length_c 15.237(2) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 2322.7(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 12.5 _exptl_absorpt_coefficient_mu 4.241 _cell_measurement_temperature 293 _exptl_crystal_description Prismatic _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_size_rad ? _exptl_crystal_colour 'deep blue' _chemical_compound_source ;Tris(o-N,N-dimethylaminomethylphenyl)methylsilane was prepared by the reaction of (\o-N,N-dimethylaminomethyl)phenyl lithium with methyltrichlorosilane, 1:1 molar ratio, in ether--tetrahydrofuran. The reacting mixture was stirred for 24 h, filtered, and the solution was evaporated until an oily residue was obtained. This residue was dissolved in acetonitrile and a crystalline product was obtained from this solution. The ligand was characterized by ^1^H NMR spectroscopy using a CCl~4~ solution with an internal standard of tetramethylsilane (TMS). Characteristic peaks were obtained at 7.0-7.6 (multiplet, corresponding to 12H of the phenyl rings), 3.25 (singlet, corresponding to 6H of methylene groups bonded to the phenyl rings), 2.0 (singlet, corresponding to 18H of methyl groups bonded to N atoms) and 0.93 p.p.m. (singlet, corresponding to 3H of methyl group bonded to the Si atom). Anhydrous CoBr~2~ was added to a freshly prepared solution of the ligand in acetonitrile. This solution gave blue crystals of the title complex on standing. ; _diffrn_measurement_device 'Siemens R3m difractometer' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'Semi-mpirical (\y scans)' _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_T_max 0.495 _diffrn_reflns_number 2329 _reflns_number_total 2231 _reflns_number_observed 1784 _reflns_observed_criterion 4.0 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.039 _refine_ls_wR_factor_obs 0.049 _refine_ls_wR_factor_all 0.055 _refine_ls_goodness_of_fit_obs 0.83 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1784 _refine_ls_number_parameters 235 _refine_ls_hydrogen_treatment ;Idealized H-atom positions riding on host atom ; _refine_ls_weighting_scheme '1/[\s^2^(F) + 0.0021F^2^]' _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.49 _refine_diff_density_min -0.56 _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 ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? H ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? Br ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? Co ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? N ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? O ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? Si ? ;International Tables for X-ray Crystallography (1991, Vol C, Tables 6.1.1.4 and 6.1.1.5) ; ? ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_flack ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Co1 .0278(1) .0560(1) .5630(1) .0035(1) Br1 .1071(1) -.0715(1) .4654(1) .0068(1) Br2 .1679(1) .1423(1) .6486(1) .0057(1) Si1 -.1622(2) .0314(2) .7067(2) .0037(1) N1 -.1699(7) -.1909(6) .5850(5) .0044(3) N2 -.0694(6) .1608(6) .4892(5) .0042(3) O1 -.0831(5) -.0170(5) .6300(4) .0041(2) C1 -.0931(10) .1145(9) .4018(7) .0066(5) C2 -.0108(10) .2606(8) .4772(8) .0064(4) C3 -.1850(8) .1777(8) .5319(7) .0045(4) C4 -.1799(8) .2322(7) .6178(6) .0037(3) C5 -.1951(9) .3406(8) .6208(8) .0053(4) C6 -.1924(9) .3932(9) .6968(9) .0059(4) C7 -.1732(10) .3444(9) .7761(9) .0063(5) C8 -.1616(9) .2362(8) .7752(7) .0049(4) C9 -.1668(8) .1785(7) .6983(7) .0043(3) C10 -.3120(8) -.0160(8) .6881(7) .0041(3) C11 -.4029(9) .0520(9) .6995(7) .0054(4) C12 -.5150(9) .0195(12) .6878(9) .0078(6) C13 -.5378(10) -.0779(12) .6642(10) .0085(6) C14 -.4502(9) -.1498(11) .6515(9) .0068(5) C15 -.3384(8) -.1213(8) .6662(7) .0047(4) C16 -.2529(9) -.2049(8) .6591(7) .0048(4) C17 -.0906(10) -.2809(8) .5838(9) .0070(5) C18 -.2241(10) -.1801(9) .4981(7) .0061(4) C19 -.1138(9) -.0099(8) .8172(6) .0053(4) H1d -.0925 -.0892 .6169 .080 H1a -.1378 .1613 .3672 .080 H1b -.0234 .1002 .3719 .080 H1c -.1338 .0509 .4104 .080 H2a -.0578 .3059 .4431 .080 H2b .0046 .2921 .5330 .080 H2c .0590 .2488 .4467 .080 H3a -.2218 .1119 .5395 .080 H3b -.2304 .2186 .4927 .080 H5a -.2066 .3786 .5673 .080 H6a -.2053 .4668 .6968 .080 H7a -.1653 .3834 .8295 .080 H8a -.1503 .2000 .8296 .080 H11a -.3876 .1215 .7189 .080 H12a -.5785 .0691 .6897 .080 H13a -.6144 -.1001 .6559 .080 H14a -.4672 -.2193 .6330 .080 H16a -.2909 -.2703 .6521 .080 H16b -.2111 -.2075 .7131 .080 H17a -.0380 -.2729 .5363 .080 H17b -.0504 -.2816 .6385 .080 H17c -.1310 -.3451 .5769 .080 H18a -.2759 -.1228 .4997 .080 H18b -.1671 -.1672 .4547 .080 H18c -.2642 -.2426 .4835 .080 H19a -.0378 .0136 .8267 .080 H19b -.1626 .0199 .8608 .080 H19c -.1164 -.0843 .8214 .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 Co1 .033(1) .001(1) .003(1) .034(1) -.001(1) .039(1) Br1 .082(1) .017(1) .021(1) .054(1) -.011(1) .068(1) Br2 .055(1) -.017(1) -.013(1) .060(1) .003(1) .056(1) Si1 .035(1) .000(1) .001(1) .042(2) .001(1) .035(2) N1 .050(5) .005(4) -.011(5) .043(5) .000(4) .040(5) N2 .047(5) .004(4) .004(4) .043(5) .003(4) .035(5) O1 .037(3) -.006(3) .004(4) .034(3) .001(3) .052(5) C1 .072(8) .023(7) .001(7) .085(9) .000(7) .041(7) C2 .067(8) .018(7) .023(7) .068(7) .022(7) .056(8) C3 .032(5) .013(5) -.006(5) .053(6) .014(6) .049(7) C4 .028(5) -.005(5) -.001(5) .046(6) -.004(5) .038(6) C5 .055(7) .015(5) .009(6) .038(6) .001(6) .065(8) C6 .058(8) .003(6) .013(7) .044(6) -.019(7) .074(9) C7 .059(7) -.007(7) .003(7) .070(8) -.034(7) .060(8) C8 .047(6) .000(6) .001(6) .052(7) -.007(6) .047(7) C9 .023(5) -.014(5) .003(5) .052(6) -.007(6) .054(7) C10 .032(5) .003(5) .008(5) .051(6) .008(5) .040(6) C11 .039(6) -.001(6) .005(6) .072(7) .011(6) .050(7) C12 .034(7) .006(8) .002(7) .107(11) .015(10) .094(11) C13 .041(7) -.035(8) -.006(8) .116(12) -.007(10) .097(12) C14 .054(7) -.028(7) -.005(7) .080(9) -.010(8) .071(9) C15 .042(6) -.019(6) -0.02(6) .066(7) .009(6) .034(6) C16 .057(7) -.021(6) -.007(6) .044(6) .009(6) .042(7) C17 .067(8) .004(6) -.004(8) .054(7) -.012(7) .088(10) C18 .064(7) -.022(7) .001(6) .074(8) -.003(6) .046(7) C19 .048(6) .010(6) -.011(6) .066(7) -.005(6) .046(7)