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#$Date: 2016-08-05 06:33:27 +0300 (Fri, 05 Aug 2016) $
#$Revision: 184942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/65/4086542.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_4086542
loop_
_publ_author_name
'Vanicek, Stefan'
'Kopacka, Holger'
'Wurst, Klaus'
'Müller, Thomas'
'Hassenrück, Christopher'
'Winter, Rainer F.'
'Bildstein, Benno'
_publ_section_title
;
 Monofunctionalized Cobaltocenium Compounds by Dediazoniation Reactions of
 Cobaltoceniumdiazonium Bis(hexafluorophosphate)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2101
_journal_paper_doi               10.1021/acs.organomet.6b00329
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C10 H9 Co I2'
_chemical_formula_weight         441.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4449(8)
_cell_length_b                   8.9340(6)
_cell_length_c                   11.4723(8)
_cell_measurement_reflns_used    8022
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.5
_cell_volume                     1173.03(14)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11289
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         2.514
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    6.680
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2014/5)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0221P)²+1.2289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1110
_reflns_number_total             1223
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00329_si_002.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 4086540--4086543.cif.'
_cod_database_code               4086542
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.415
_shelx_estimated_absorpt_t_max   0.690
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.75334(5) 0.2500 0.53875(4) 0.01814(12) Uani 1 2 d S T P
I1 I 0.44881(2) 0.2500 0.43078(2) 0.02724(9) Uani 1 2 d S T P
I2 I 0.14794(2) 0.2500 0.46868(3) 0.03305(10) Uani 1 2 d S T P
C1 C 0.6711(5) 0.2500 0.6944(4) 0.062(2) Uani 1 2 d S T P
H1 H 0.5891 0.2500 0.7070 0.074 Uiso 1 2 calc R U P
C2 C 0.7439(4) 0.3771(4) 0.6833(3) 0.0514(10) Uani 1 1 d . . .
H2 H 0.7193 0.4786 0.6862 0.062 Uiso 1 1 calc R U .
C3 C 0.8580(3) 0.3275(4) 0.6672(3) 0.0443(9) Uani 1 1 d . . .
H3 H 0.9247 0.3896 0.6578 0.053 Uiso 1 1 calc R U .
C4 C 0.8211(2) 0.3291(4) 0.3873(2) 0.0267(6) Uani 1 1 d . . .
H4 H 0.8879 0.3913 0.3792 0.032 Uiso 1 1 calc R U .
C5 C 0.7036(2) 0.3794(3) 0.4017(2) 0.0232(6) Uani 1 1 d . . .
H5 H 0.6784 0.4805 0.4057 0.028 Uiso 1 1 calc R U .
C6 C 0.6311(3) 0.2500 0.4089(3) 0.0219(8) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 Co1 C2 68.7(2) . 7_565
C2 Co1 C1 41.08(14) . .
C2 Co1 C1 41.08(14) 7_565 .
C2 Co1 C3 40.32(15) . .
C2 Co1 C3 67.92(14) 7_565 .
C1 Co1 C3 68.34(17) . .
C2 Co1 C3 67.92(14) . 7_565
C2 Co1 C3 40.32(15) 7_565 7_565
C1 Co1 C3 68.34(17) . 7_565
C3 Co1 C3 40.1(2) . 7_565
C2 Co1 C4 121.95(15) . .
C2 Co1 C4 157.22(16) 7_565 .
C1 Co1 C4 159.31(9) . .
C3 Co1 C4 106.17(13) . .
C3 Co1 C4 121.13(13) 7_565 .
C2 Co1 C4 157.22(16) . 7_565
C2 Co1 C4 121.95(15) 7_565 7_565
C1 Co1 C4 159.31(9) . 7_565
C3 Co1 C4 121.13(13) . 7_565
C3 Co1 C4 106.17(13) 7_565 7_565
C4 Co1 C4 40.74(18) . 7_565
C2 Co1 C5 107.55(13) . .
C2 Co1 C5 160.59(15) 7_565 .
C1 Co1 C5 123.64(13) . .
C3 Co1 C5 122.35(13) . .
C3 Co1 C5 157.61(14) 7_565 .
C4 Co1 C5 41.15(11) . .
C4 Co1 C5 69.07(12) 7_565 .
C2 Co1 C5 160.59(15) . 7_565
C2 Co1 C5 107.55(13) 7_565 7_565
C1 Co1 C5 123.64(13) . 7_565
C3 Co1 C5 157.61(14) . 7_565
C3 Co1 C5 122.35(13) 7_565 7_565
C4 Co1 C5 69.07(12) . 7_565
C4 Co1 C5 41.15(11) 7_565 7_565
C5 Co1 C5 69.30(17) . 7_565
C2 Co1 C6 124.34(14) . .
C2 Co1 C6 124.34(14) 7_565 .
C1 Co1 C6 109.03(18) . .
C3 Co1 C6 159.57(11) . .
C3 Co1 C6 159.57(11) 7_565 .
C4 Co1 C6 68.76(12) . .
C4 Co1 C6 68.76(12) 7_565 .
C5 Co1 C6 40.93(9) . .
C5 Co1 C6 40.93(9) 7_565 .
C2 C1 C2 106.8(5) . 7_565
C2 C1 Co1 69.2(2) . .
C2 C1 Co1 69.2(2) 7_565 .
C2 C1 H1 126.6 . .
C2 C1 H1 126.6 7_565 .
Co1 C1 H1 126.5 . .
C3 C2 C1 108.0(3) . .
C3 C2 Co1 70.18(18) . .
C1 C2 Co1 69.7(2) . .
C3 C2 H2 126.0 . .
C1 C2 H2 126.0 . .
Co1 C2 H2 125.7 . .
C3 C3 C2 108.6(2) 7_565 .
C3 C3 Co1 69.97(11) 7_565 .
C2 C3 Co1 69.50(18) . .
C3 C3 H3 125.7 7_565 .
C2 C3 H3 125.7 . .
Co1 C3 H3 126.4 . .
C4 C4 C5 108.35(18) 7_565 .
C4 C4 Co1 69.63(9) 7_565 .
C5 C4 Co1 69.55(15) . .
C4 C4 H4 125.8 7_565 .
C5 C4 H4 125.8 . .
Co1 C4 H4 126.6 . .
C6 C5 C4 107.5(3) . .
C6 C5 Co1 69.96(18) . .
C4 C5 Co1 69.30(16) . .
C6 C5 H5 126.3 . .
C4 C5 H5 126.3 . .
Co1 C5 H5 126.0 . .
C5 C6 C5 108.4(3) . 7_565
C5 C6 Co1 69.11(17) . .
C5 C6 Co1 69.11(17) 7_565 .
C5 C6 I1 125.81(16) . .
C5 C6 I1 125.81(16) 7_565 .
Co1 C6 I1 126.33(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C2 2.013(3) .
Co1 C2 2.013(3) 7_565
Co1 C1 2.019(4) .
Co1 C3 2.021(3) .
Co1 C3 2.021(3) 7_565
Co1 C4 2.029(3) .
Co1 C4 2.030(3) 7_565
Co1 C5 2.033(3) .
Co1 C5 2.033(3) 7_565
Co1 C6 2.044(4) .
I1 C6 2.101(4) .
C1 C2 1.414(5) .
C1 C2 1.414(5) 7_565
C1 H1 0.9500 .
C2 C3 1.390(5) .
C2 H2 0.9500 .
C3 C3 1.385(8) 7_565
C3 H3 0.9500 .
C4 C4 1.413(6) 7_565
C4 C5 1.427(4) .
C4 H4 0.9500 .
C5 C6 1.425(3) .
C5 H5 0.9500 .
C6 C5 1.425(3) 7_565
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 C1 C2 C3 -0.7(5) 7_565 .
Co1 C1 C2 C3 -60.0(2) . .
C2 C1 C2 Co1 59.3(3) 7_565 .
C1 C2 C3 C3 0.4(3) . 7_565
Co1 C2 C3 C3 -59.23(10) . 7_565
C1 C2 C3 Co1 59.7(3) . .
C4 C4 C5 C6 -0.8(3) 7_565 .
Co1 C4 C5 C6 -59.8(2) . .
C4 C4 C5 Co1 59.00(8) 7_565 .
C4 C5 C6 C5 1.3(4) . 7_565
Co1 C5 C6 C5 -58.1(3) . 7_565
C4 C5 C6 Co1 59.39(19) . .
C4 C5 C6 I1 179.8(2) . .
Co1 C5 C6 I1 120.4(3) . .
