#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/07/2200748.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_2200748 loop_ _publ_author_name 'Cotton, F. Albert' 'Daniels, Lee M.' 'Wilkinson, Chad C.' _publ_section_title ; A highly disordered cobaltocenium salt ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m529 _journal_page_last m530 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Co (C5 H5)2], B F4' _chemical_formula_moiety 'C10 H10 Co 1+, B F4 1-' _chemical_formula_sum 'C10 H10 B Co F4' _chemical_formula_weight 275.92 _chemical_name_systematic ; cobaltocenium tetrafluoroborate ; _space_group_IT_number 66 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2 2c' _symmetry_space_group_name_H-M 'C c c m' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.3586(7) _cell_length_b 11.9176(11) _cell_length_c 12.4369(13) _cell_measurement_reflns_used 1619 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 2.36 _cell_volume 1090.68(18) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Siemens, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 213(2) _diffrn_measured_fraction_theta_full .998 _diffrn_measured_fraction_theta_max .998 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0184 _diffrn_reflns_av_sigmaI/netI .0133 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3263 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.28 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.593 _exptl_absorpt_correction_T_max .727 _exptl_absorpt_correction_T_min .609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Blessing, 1995)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .20 _refine_diff_density_max .193 _refine_diff_density_min -.177 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 665 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all .0395 _refine_ls_R_factor_gt .0284 _refine_ls_shift/su_max .003 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.036P)^2^+0.60P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0840 _reflns_number_gt 485 _reflns_number_total 665 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file om6064.cif _[local]_cod_data_source_block I _cod_database_code 2200748 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co .2500 .2500 .4821(4) .0622(10) Uani d SP .50 . . Co C1 .3131(4) .4145(3) .4953(10) .0860(16) Uani d PG .50 A -1 C H1 .2311 .4730 .5050 .103 Uiso calc PR .50 A -1 H C2 .3970(13) .3527(7) .5769(8) .113(4) Uani d PG .50 A -1 C H2 .3806 .3629 .6504 .136 Uiso calc PR .50 A -1 H C3 .5098(10) .2730(6) .5287(5) .101(7) Uani d PG .50 A -1 C H3 .5817 .2208 .5645 .122 Uiso calc PR .50 A -1 H C4 .4956(9) .2854(4) .4173(5) .092(4) Uani d PG .50 A -1 C H4 .5563 .2429 .3659 .110 Uiso calc PR .50 A -1 H C5 .3740(14) .3729(7) .3967(6) .0721(18) Uani d PG .50 A -1 C H5 .3397 .3989 .3292 .087 Uiso calc PR .50 A -1 H F .1069(3) .4337(2) .18803(19) .1734(10) Uani d . 1 . . F B .0000 .5000 .2500 .124(3) Uani d S 1 . . B loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co .0360(3) .0488(3) .102(3) -.00996(18) .000 .000 C1 .065(2) .0539(17) .139(4) -.0181(18) -.030(9) .008(11) C2 .095(9) .140(11) .104(6) -.077(7) .000(4) -.025(5) C3 .040(2) .096(4) .17(2) -.023(2) -.018(5) .043(8) C4 .050(3) .061(3) .164(11) -.010(2) .025(5) .006(4) C5 .056(3) .051(2) .110(5) -.012(2) .013(3) .005(3) F .217(3) .1521(18) .1513(18) -.0482(15) .0620(17) -.0701(14) B .156(8) .119(6) .095(5) .000 .000 .000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co C1 . 2.021(4) ? Co C2 . 2.015(11) ? Co C3 . 2.016(7) ? Co C4 . 2.023(7) ? Co C5 . 2.027(10) ? C1 C2 . 1.397(4) ? C1 C5 . 1.397(4) ? C2 C3 . 1.397(4) ? C3 C4 . 1.397(4) ? C4 C5 . 1.397(4) ? B F . 1.355(2) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C1 C2 C3 . . 108.0 C2 C3 C4 . . 108.0 C3 C4 C5 . . 108.0 C4 C5 C1 . . 108.0 C2 C1 C5 . . 108.0 C2 C1 Co . . 69.5(4) C5 C1 Co . . 70.0(4) C1 C2 Co . . 70.0(3) C3 C2 Co . . 69.77(15) C2 C3 Co . . 69.7(3) C4 C3 Co . . 70.0(5) C5 C4 Co . . 69.9(3) C3 C4 Co . . 69.5(5) C1 C5 Co . . 69.6(3) C4 C5 Co . . 69.70(15) F B F 3 . 108.7(2) F B F 3 4_565 110.7(2) F B F . 4_565 109.05(19) _cod_database_fobs_code 2200748 _journal_paper_doi 10.1107/S1600536801017172