#------------------------------------------------------------------------------ #$Date: 2011-09-28 16:24:46 +0200 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003338.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_2003338 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 586 _journal_page_last 588 _publ_section_title ; Bis(isopropyldiphenylphosphine oxide)diiodocobalt(II) ; _chemical_formula_sum 'C30 H34 Co I2 O2 P2' _chemical_formula_weight 801.24 _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.497(2) _cell_length_b 17.505(6) _cell_length_c 9.903(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.46(5) _cell_angle_gamma 90.00 _cell_volume 1669.3(8) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas 1.567(2) _exptl_crystal_density_method 'neutral buoyancy in CCl~4~ and hexanes' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_absorpt_coefficient_mu 2.483 _cell_measurement_temperature 293(2) _exptl_crystal_description 'irregular blocks' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_colour 'dark green' _chemical_compound_source ; A solution of CoI~2~ in ethanol was prepared by mixing ethanolic CoCl~2~(H~2~O)~6~ and NaI in a 1:2 ratio, removing NaCl by filtration, and reducing volume by vacuum evaporation. A stoichiometric amount of (CH~3~)~2~CH(C~6~H~5~)~2~P was added and the solution stirred for 1 h. Evaporation gave a dark green product, recrystallized from ethanol. Analysis: Found; C 45.70, H 4.28, P 7.20%. Calculated for C~30~H~34~CoI~2~O~2~P~2~: C 44.96, H 4.25, P 7.73%. Data crystals were grown by diffusion using benzene with hexanes. ; _diffrn_measurement_device 'Enraf-Nonius CAD4F diffractometer' _diffrn_measurement_method '\q/2\q scans, moving backgrounds' _exptl_absorpt_correction_type 'empirical, \y scans' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.00 _diffrn_reflns_number 4327 _reflns_number_total 4042 _reflns_number_observed 3449 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0354 _refine_ls_wR_factor_obs 0.0865 _refine_ls_wR_factor_all 0.0965 _refine_ls_goodness_of_fit_obs 1.060 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_number_reflns 4039 _refine_ls_number_parameters 334 _refine_ls_hydrogen_treatment 'H atoms: riding' _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0579P)^2^+0.6939P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.028 _refine_diff_density_max 0.543 _refine_diff_density_min -0.785 _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 '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 'Co' 'Co' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3494 0.9 'I' 'I' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.4742 1.81 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.05(3) 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 I1 1 0.28917(7) 0.32379(4) 0.22220(8) 0.0688(2) I2 1 0.58368(6) 0.25003(4) 0.65936(6) 0.0542(2) Co 1 0.35880(11) 0.22413(6) 0.42800(11) 0.0346(3) P1 1 0.0895(2) 0.22514(15) 0.5343(2) 0.0449(6) P2 1 0.3711(3) 0.04880(14) 0.2845(3) 0.0433(6) O1 1 0.2007(6) 0.2066(3) 0.4817(6) 0.048(2) O2 1 0.3733(7) 0.1278(4) 0.3370(7) 0.060(2) C1 1 0.1327(12) 0.3034(7) 0.6628(11) 0.065(3) H1 1 0.0553(12) 0.3121(7) 0.6876(11) 0.071 C2 1 0.1557(19) 0.3756(7) 0.5896(17) 0.113(5) H2A 1 0.0710(19) 0.3902(7) 0.5120(17) 0.124 H2B 1 0.2237(19) 0.3661(7) 0.5509(17) 0.124 H2C 1 0.1868(19) 0.4156(7) 0.6602(17) 0.124 C3 1 0.2553(13) 0.2823(8) 0.8030(12) 0.094(4) H3A 1 0.2319(13) 0.2393(8) 0.8470(12) 0.103 H3B 1 0.2779(13) 0.3242(8) 0.8694(12) 0.103 H3C 1 0.3329(13) 0.2702(8) 0.7804(12) 0.103 C4 1 0.4757(11) -0.0136(7) 0.4297(11) 0.065(3) H4 1 0.4786(11) -0.0622(7) 0.3883(11) 0.071 C5 1 0.6224(12) 0.0161(7) 0.5025(14) 0.084(4) H5A 1 0.6206(12) 0.0681(7) 0.5294(14) 0.092 H5B 1 0.6669(12) 0.0122(7) 0.4359(14) 0.092 H5C 1 0.6721(12) -0.0132(7) 0.5881(14) 0.092 C6 1 0.4095(15) -0.0230(9) 0.5381(13) 0.091(4) H6A 1 0.3209(15) -0.0461(9) 0.4905(13) 0.100 H6B 1 0.3991(15) 0.0257(9) 0.5750(13) 0.100 H6C 1 0.4666(15) -0.0544(9) 0.6172(13) 0.100 C11 1 -0.0685(8) 0.2516(7) 0.3817(9) 0.050(2) C12 1 -0.0689(9) 0.2558(7) 0.2425(9) 0.061(3) H12 1 0.0090(9) 0.2450(7) 0.2291(9) 0.067 C13 1 -0.1863(11) 0.2761(7) 0.1253(11) 0.080(4) H13 1 -0.1837(11) 0.2812(7) 0.0360(11) 0.088 C14 1 -0.3079(12) 0.2889(8) 0.1411(15) 0.096(4) H14 1 -0.3865(12) 0.2986(8) 0.0619(15) 0.106 C15 1 -0.3090(11) 0.2870(10) 0.2757(16) 0.113(6) H15 1 -0.3869(11) 0.2995(10) 0.2879(16) 0.124 C16 1 -0.1898(10) 0.2657(9) 0.3975(12) 0.092(4) H16 1 -0.1931(10) 0.2612(9) 0.4866(12) 0.101 C21 1 0.0590(9) 0.1420(6) 0.6266(10) 0.059(3) C22 1 -0.0262(13) 0.1422(8) 0.7017(14) 0.099(5) H22 1 -0.0689(13) 0.1857(8) 0.7087(14) 0.109 C23 1 -0.0470(15) 0.0760(10) 0.7669(16) 0.112(6) H23 1 -0.1074(15) 0.0763(10) 0.8107(16) 0.123 C24 1 0.0210(18) 0.0121(9) 0.7657(16) 0.113(6) H24 1 0.0082(18) -0.0306(9) 0.8095(16) 0.124 C25 1 0.1083(19) 0.0126(8) 0.698(2) 0.131(6) H25 1 0.1576(19) -0.0298(8) 0.7009(20) 0.144 C26 1 0.1260(13) 0.0762(6) 0.6245(15) 0.085(4) H26 1 0.1818(13) 0.0738(6) 0.5753(15) 0.094 C31 1 0.1939(9) 0.0136(5) 0.2106(9) 0.044(2) C32 1 0.1630(9) -0.0621(6) 0.1680(11) 0.060(3) H32 1 0.2313(9) -0.0954(6) 0.1778(11) 0.065 C33 1 0.0273(12) -0.0853(6) 0.1111(12) 0.073(3) H33 1 0.0069(12) -0.1340(6) 0.0814(12) 0.080 C34 1 -0.0766(12) -0.0365(8) 0.0985(14) 0.085(4) H34 1 -0.1655(12) -0.0523(8) 0.0592(14) 0.094 C35 1 -0.0458(11) 0.0360(7) 0.1453(14) 0.079(4) H35 1 -0.1142(11) 0.0678(7) 0.1429(14) 0.086 C36 1 0.0878(10) 0.0623(6) 0.1964(12) 0.066(3) H36 1 0.1058(10) 0.1118(6) 0.2209(12) 0.073 C41 1 0.4377(9) 0.0455(5) 0.1427(9) 0.047(2) C42 1 0.4613(13) 0.1114(6) 0.0827(12) 0.080(4) H42 1 0.4407(13) 0.1565(6) 0.1129(12) 0.088 C43 1 0.5156(14) 0.1105(8) -0.0221(13) 0.094(4) H43 1 0.5314(14) 0.1549(8) -0.0586(13) 0.104 C44 1 0.5452(13) 0.0448(8) -0.0707(13) 0.080(4) H44 1 0.5826(13) 0.0446(8) -0.1382(13) 0.088 C45 1 0.5188(12) -0.0215(8) -0.0178(13) 0.081(4) H45 1 0.5343(12) -0.0659(8) -0.0545(13) 0.089 C46 1 0.4685(12) -0.0229(6) 0.0910(12) 0.069(3) H46 1 0.4556(12) -0.0677(6) 0.1284(12) 0.076 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 I1 0.0696(5) 0.0039(4) 0.0243(4) 0.0752(5) 0.0194(4) 0.0600(4) I2 0.0476(3) -0.0067(3) 0.0098(2) 0.0635(4) -0.0049(3) 0.0437(3) Co 0.0348(6) 0.0014(5) 0.0156(5) 0.0368(6) -0.0030(5) 0.0341(5) P1 0.0413(12) 0.0014(12) 0.0234(10) 0.057(2) 0.0002(12) 0.0426(12) P2 0.0466(14) 0.0048(11) 0.0136(10) 0.0375(14) -0.0082(11) 0.0418(12) O1 0.038(3) 0.000(3) 0.021(3) 0.058(4) -0.001(3) 0.052(4) O2 0.060(4) 0.011(3) 0.015(3) 0.051(4) -0.020(3) 0.060(4) C1 0.067(7) 0.006(6) 0.036(6) 0.083(9) -0.008(6) 0.055(6) C2 0.185(16) -0.023(9) 0.082(12) 0.067(10) -0.039(8) 0.108(11) C3 0.102(10) -0.004(8) 0.027(7) 0.126(12) -0.023(7) 0.051(7) C4 0.068(7) 0.025(6) 0.013(5) 0.067(7) -0.006(5) 0.050(6) C5 0.062(7) 0.013(6) 0.003(7) 0.070(8) -0.010(7) 0.093(9) C6 0.105(10) 0.043(8) 0.024(7) 0.109(10) 0.007(7) 0.053(7) C11 0.044(5) 0.014(5) 0.030(4) 0.055(6) 0.010(6) 0.061(5) C12 0.044(5) 0.006(6) 0.025(5) 0.081(7) 0.022(6) 0.061(6) C13 0.063(7) 0.004(6) 0.014(6) 0.106(11) 0.017(6) 0.060(7) C14 0.064(9) 0.005(7) -0.001(7) 0.096(10) 0.029(8) 0.098(11) C15 0.041(7) 0.032(8) 0.025(8) 0.177(17) 0.012(11) 0.115(12) C16 0.063(7) 0.019(8) 0.046(7) 0.140(13) 0.011(9) 0.088(8) C21 0.039(5) -0.011(5) 0.015(4) 0.091(9) 0.018(5) 0.046(6) C22 0.093(10) 0.014(9) 0.067(9) 0.128(12) 0.039(9) 0.103(10) C23 0.095(11) -0.028(11) 0.058(9) 0.164(17) 0.040(11) 0.094(11) C24 0.117(14) -0.012(12) 0.029(9) 0.140(17) 0.047(10) 0.073(10) C25 0.173(19) 0.009(11) 0.064(15) 0.076(12) 0.021(11) 0.145(15) C26 0.101(10) 0.019(7) 0.053(9) 0.058(8) 0.015(7) 0.108(11) C31 0.054(6) 0.004(5) 0.021(4) 0.048(6) 0.001(4) 0.034(5) C32 0.050(6) -0.006(5) 0.027(5) 0.057(7) -0.001(6) 0.074(7) C33 0.089(9) -0.029(7) 0.040(7) 0.061(8) -0.010(6) 0.075(8) C34 0.057(8) -0.020(8) 0.034(7) 0.119(13) -0.009(9) 0.085(9) C35 0.059(7) 0.013(7) 0.023(6) 0.091(10) -0.017(7) 0.081(9) C36 0.058(7) -0.005(6) 0.023(6) 0.064(8) -0.024(6) 0.072(7) C41 0.045(5) 0.003(4) 0.015(4) 0.046(6) -0.008(4) 0.048(5) C42 0.123(11) 0.009(7) 0.051(8) 0.060(8) 0.003(6) 0.068(8) C43 0.137(13) -0.002(9) 0.066(9) 0.082(10) 0.017(8) 0.084(9) C44 0.073(8) -0.013(8) 0.043(6) 0.118(12) -0.011(8) 0.064(8) C45 0.084(9) -0.005(7) 0.052(7) 0.089(10) -0.033(8) 0.087(9) C46 0.086(8) 0.001(6) 0.054(7) 0.057(7) -0.010(6) 0.083(8) _cod_database_code 2003338