#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/11/4331135.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_4331135
loop_
_publ_author_name
'Shengwen Liang'
'Haoshuang Wang'
'Tapash Deb'
'Jeffrey L. Petersen'
'Gordon T. Yee'
'Michael P. Jensen'
_publ_section_title
;
 Structural and Spectroscopic Trends in a Series of Half-Sandwich
 Scorpionate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12707
_journal_page_last               12719
_journal_paper_doi               10.1021/ic301409s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C22 H32.5 B2 Co F4 N9.5'
_chemical_formula_weight         586.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.6161(9)
_cell_length_b                   11.6161(9)
_cell_length_c                   37.839(4)
_cell_measurement_reflns_used    4117
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.29
_cell_volume                     4421.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            10468
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0829P)²+1.3382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                1721
_reflns_number_total             2260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301409s_si_002_4.cif
_cod_data_source_block           3Co
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C22 H32.50 B2 Co F4 N9.50'
_cod_database_code               4331135
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 1.0000 0.0000 0.086284(13) 0.0467(2) Uani 1 3 d S
N1 N 0.84348(18) -0.02243(19) 0.11949(5) 0.0488(4) Uani 1 1 d .
N2 N 0.87072(18) -0.00913(18) 0.15502(5) 0.0466(4) Uani 1 1 d .
N3 N 0.9802(2) 0.1394(2) 0.05171(6) 0.0644(6) Uani 1 1 d .
C1 C 0.7235(2) -0.0322(2) 0.11574(7) 0.0544(6) Uani 1 1 d .
C2 C 0.6751(2) -0.0250(2) 0.14860(8) 0.0590(6) Uani 1 1 d .
H2 H 0.5943 -0.0295 0.1532 0.071 Uiso 1 1 calc R
C3 C 0.7690(2) -0.0100(2) 0.17301(6) 0.0506(5) Uani 1 1 d .
C4 C 0.7670(3) 0.0032(3) 0.21197(7) 0.0696(7) Uani 1 1 d .
H4A H 0.6878 0.0039 0.2188 0.104 Uiso 1 1 calc R
H4B H 0.8436 0.0847 0.2193 0.104 Uiso 1 1 calc R
H4C H 0.7685 -0.0704 0.2230 0.104 Uiso 1 1 calc R
C5 C 0.6610(3) -0.0450(4) 0.08054(8) 0.0781(8) Uani 1 1 d .
H5A H 0.7231 -0.0343 0.0623 0.117 Uiso 1 1 calc R
H5B H 0.6365 0.0222 0.0781 0.117 Uiso 1 1 calc R
H5C H 0.5832 -0.1313 0.0785 0.117 Uiso 1 1 calc R
C6 C 0.9848(3) 0.2290(3) 0.03825(7) 0.0635(7) Uani 1 1 d .
C7 C 0.9948(4) 0.3470(4) 0.02237(10) 0.0970(12) Uani 1 1 d .
H7A H 0.9251 0.3605 0.0313 0.146 Uiso 1 1 calc R
H7B H 0.9865 0.3363 -0.0028 0.146 Uiso 1 1 calc R
H7C H 1.0795 0.4227 0.0281 0.146 Uiso 1 1 calc R
B1 B 1.0000 0.0000 0.16875(12) 0.0463(9) Uani 1 3 d S
H1 H 1.0000 0.0000 0.1946 0.056 Uiso 1 3 calc SR
B2 B 0.6667 0.3333 0.0237(3) 0.098(2) Uani 1 3 d S
F1 F 0.6667 0.3333 -0.0093(2) 0.276(5) Uani 1 3 d S
F2 F 0.7727(3) 0.4481(3) 0.03491(10) 0.1576(12) Uani 1 1 d .
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
N1 Co1 N1 88.35(7) 3_765 .
N1 Co1 N1 88.35(7) 3_765 2_645
N1 Co1 N1 88.35(7) . 2_645
N1 Co1 N3 179.05(8) 3_765 2_645
N1 Co1 N3 91.37(8) . 2_645
N1 Co1 N3 92.55(8) 2_645 2_645
N1 Co1 N3 92.54(8) 3_765 3_765
N1 Co1 N3 179.05(8) . 3_765
N1 Co1 N3 91.37(8) 2_645 3_765
N3 Co1 N3 87.75(9) 2_645 3_765
N1 Co1 N3 91.37(8) 3_765 .
N1 Co1 N3 92.55(8) . .
N1 Co1 N3 179.05(8) 2_645 .
N3 Co1 N3 87.75(9) 2_645 .
N3 Co1 N3 87.75(9) 3_765 .
C1 N1 N2 106.46(18) . .
C1 N1 Co1 137.40(16) . .
N2 N1 Co1 115.62(13) . .
C3 N2 N1 109.82(18) . .
C3 N2 B1 130.2(2) . .
N1 N2 B1 120.0(2) . .
C6 N3 Co1 167.2(2) . .
N1 C1 C2 109.5(2) . .
N1 C1 C5 122.3(2) . .
C2 C1 C5 128.1(2) . .
C3 C2 C1 106.9(2) . .
N2 C3 C2 107.2(2) . .
N2 C3 C4 123.7(2) . .
C2 C3 C4 129.1(2) . .
N3 C6 C7 177.3(4) . .
N2 B1 N2 109.25(17) 2_645 .
N2 B1 N2 109.25(17) 2_645 3_765
N2 B1 N2 109.25(17) . 3_765
F1 B2 F2 108.3(5) . 3_665
F1 B2 F2 108.3(5) . .
F2 B2 F2 110.7(4) 3_665 .
F1 B2 F2 108.3(5) . 2_655
F2 B2 F2 110.7(4) 3_665 2_655
F2 B2 F2 110.7(4) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.1163(19) 3_765
Co1 N1 2.1163(19) .
Co1 N1 2.1163(19) 2_645
Co1 N3 2.182(2) 2_645
Co1 N3 2.182(2) 3_765
Co1 N3 2.182(2) .
N1 C1 1.348(3) .
N1 N2 1.372(3) .
N2 C3 1.360(3) .
N2 B1 1.542(2) .
N3 C6 1.135(3) .
C1 C2 1.384(4) .
C1 C5 1.488(4) .
C2 C3 1.372(4) .
C3 C4 1.483(4) .
C6 C7 1.448(4) .
B1 N2 1.542(2) 2_645
B1 N2 1.542(2) 3_765
B2 F1 1.249(11) .
B2 F2 1.354(4) 3_665
B2 F2 1.354(4) .
B2 F2 1.354(4) 2_655
