#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:14:00 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178554 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/62/4066206.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_4066206
loop_
_publ_author_name
'Dai, Wei'
'Kim, Sang Bok'
'Pike, Robert D.'
'Cahill, Christopher L.'
'Sweigart, Dwight A.'
_publ_section_title
;
 Electrochemical Study of Manganese and Rhenium Arene Complexes
 (C6R6)M(CO)3+(R = Me, Et)§
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5173
_journal_paper_doi               10.1021/om100350e
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C20 H20 B4 F4 Mn2 O4'
_chemical_formula_weight         553.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9357(18)
_cell_length_b                   14.007(3)
_cell_length_c                   17.480(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2187.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18886
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.215
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.157(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0491P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                4572
_reflns_number_total             5297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100350e_si_002.cif
_cod_data_source_block           kim9s
_cod_database_code               4066206
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
F1 F 0.6620(2) 0.57117(13) 0.75273(10) 0.0454(5) Uani 1 1 d .
Mn1 Mn 0.34792(4) 0.50943(3) 0.040278(18) 0.01572(10) Uani 1 1 d .
C1 C 0.1321(3) 0.46840(18) 0.09584(12) 0.0163(5) Uani 1 1 d .
O3 O 0.6585(2) 0.57771(14) 0.01623(10) 0.0274(4) Uani 1 1 d .
C2 C 0.2763(3) 0.58079(19) -0.03903(14) 0.0193(5) Uani 1 1 d .
C3 C 0.1420(3) 0.25675(18) 0.18103(14) 0.0220(6) Uani 1 1 d .
H3A H 0.2058 0.2678 0.2243 0.033 Uiso 1 1 calc R
H3B H 0.1254 0.1894 0.1752 0.033 Uiso 1 1 calc R
H3C H 0.0479 0.2884 0.1888 0.033 Uiso 1 1 calc R
C4 C 0.1565(3) 0.56811(17) 0.10573(12) 0.0153(5) Uani 1 1 d .
C5 C 0.2172(3) 0.29627(18) 0.10839(14) 0.0187(5) Uani 1 1 d .
H5A H 0.3113 0.2635 0.0996 0.022 Uiso 1 1 calc R
H5B H 0.1530 0.2854 0.0645 0.022 Uiso 1 1 calc R
O2 O 0.2260(2) 0.62574(15) -0.08710(11) 0.0297(5) Uani 1 1 d .
C6 C -0.0181(3) 0.4335(2) 0.06509(13) 0.0188(5) Uani 1 1 d .
H6A H -0.0954 0.4769 0.0826 0.023 Uiso 1 1 calc R
H6B H -0.0388 0.3714 0.0874 0.023 Uiso 1 1 calc R
C7 C 0.3805(3) 0.43550(18) 0.15174(13) 0.0166(5) Uani 1 1 d .
C8 C 0.5375(3) 0.5521(2) 0.02227(13) 0.0201(6) Uani 1 1 d .
C9 C 0.0350(3) 0.63842(19) 0.08284(14) 0.0177(5) Uani 1 1 d .
H9A H -0.0200 0.6136 0.0393 0.021 Uiso 1 1 calc R
H9B H 0.0802 0.6985 0.0679 0.021 Uiso 1 1 calc R
C10 C 0.4027(3) 0.53520(19) 0.16217(13) 0.0167(5) Uani 1 1 d .
O1 O 0.3884(2) 0.34399(15) -0.06326(11) 0.0304(5) Uani 1 1 d .
C11 C 0.5437(3) 0.5701(2) 0.20103(14) 0.0196(5) Uani 1 1 d .
H11A H 0.5687 0.6334 0.1824 0.024 Uiso 1 1 calc R
H11B H 0.6261 0.5277 0.1889 0.024 Uiso 1 1 calc R
C12 C 0.2451(3) 0.40277(18) 0.11801(13) 0.0166(5) Uani 1 1 d .
C13 C 0.3835(3) 0.7662(2) 0.09270(15) 0.0250(6) Uani 1 1 d .
H13A H 0.4829 0.7426 0.0838 0.037 Uiso 1 1 calc R
H13B H 0.3884 0.8321 0.1075 0.037 Uiso 1 1 calc R
H13C H 0.3256 0.7602 0.0467 0.037 Uiso 1 1 calc R
C14 C 0.6142(3) 0.3338(2) 0.11956(16) 0.0248(6) Uani 1 1 d .
H14A H 0.5643 0.3057 0.0764 0.037 Uiso 1 1 calc R
H14B H 0.6814 0.2880 0.1417 0.037 Uiso 1 1 calc R
H14C H 0.6697 0.3887 0.1031 0.037 Uiso 1 1 calc R
C15 C 0.5208(3) 0.5735(2) 0.28811(14) 0.0276(6) Uani 1 1 d .
H15A H 0.4455 0.6199 0.3003 0.041 Uiso 1 1 calc R
H15B H 0.6132 0.5908 0.3125 0.041 Uiso 1 1 calc R
H15C H 0.4895 0.5118 0.3060 0.041 Uiso 1 1 calc R
C16 C 0.3754(3) 0.4095(2) -0.02514(14) 0.0224(6) Uani 1 1 d .
C17 C -0.0303(3) 0.4246(2) -0.02189(14) 0.0245(6) Uani 1 1 d .
H17A H -0.0125 0.4858 -0.0449 0.037 Uiso 1 1 calc R
H17B H -0.1287 0.4029 -0.0353 0.037 Uiso 1 1 calc R
H17C H 0.0427 0.3797 -0.0401 0.037 Uiso 1 1 calc R
C18 C 0.4979(3) 0.36385(19) 0.17932(14) 0.0206(6) Uani 1 1 d .
H18A H 0.4467 0.3071 0.1973 0.025 Uiso 1 1 calc R
H18B H 0.5502 0.3914 0.2227 0.025 Uiso 1 1 calc R
C19 C -0.0726(3) 0.6550(2) 0.14975(14) 0.0223(6) Uani 1 1 d .
H19A H -0.1102 0.5948 0.1675 0.033 Uiso 1 1 calc R
H19B H -0.1545 0.6942 0.1331 0.033 Uiso 1 1 calc R
H19C H -0.0204 0.6865 0.1906 0.033 Uiso 1 1 calc R
C20 C 0.2906(3) 0.60188(19) 0.14028(13) 0.0173(5) Uani 1 1 d .
C21 C 0.3100(3) 0.70844(18) 0.15638(14) 0.0194(5) Uani 1 1 d .
H21A H 0.2122 0.7356 0.1667 0.023 Uiso 1 1 calc R
H21B H 0.3695 0.7155 0.2024 0.023 Uiso 1 1 calc R
F3 F 0.6323(2) 0.47961(12) 0.85916(9) 0.0380(4) Uani 1 1 d .
F2 F 0.53948(19) 0.63042(11) 0.85663(9) 0.0292(4) Uani 1 1 d .
F4 F 0.4323(2) 0.51411(16) 0.78390(11) 0.0513(5) Uani 1 1 d .
B1 B 0.5654(4) 0.5487(2) 0.81301(18) 0.0275(7) 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'
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 '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
C8 Mn1 C16 91.05(12)
C8 Mn1 C2 90.89(11)
C16 Mn1 C2 89.51(12)
C8 Mn1 C10 84.68(10)
C16 Mn1 C10 134.27(11)
C2 Mn1 C10 135.94(11)
C8 Mn1 C4 133.21(11)
C16 Mn1 C4 135.40(11)
C2 Mn1 C4 85.31(10)
C10 Mn1 C4 67.28(9)
C8 Mn1 C12 135.32(11)
C16 Mn1 C12 85.57(10)
C2 Mn1 C12 133.52(11)
C10 Mn1 C12 67.20(9)
C4 Mn1 C12 67.28(9)
C8 Mn1 C7 100.49(10)
C16 Mn1 C7 100.02(10)
C2 Mn1 C7 164.94(10)
C10 Mn1 C7 37.36(9)
C4 Mn1 C7 79.71(9)
C12 Mn1 C7 37.32(9)
C8 Mn1 C1 163.95(9)
C16 Mn1 C1 101.02(10)
C2 Mn1 C1 99.68(10)
C10 Mn1 C1 79.33(9)
C4 Mn1 C1 37.32(9)
C12 Mn1 C1 37.17(9)
C7 Mn1 C1 67.21(9)
C8 Mn1 C20 99.10(10)
C16 Mn1 C20 164.96(10)
C2 Mn1 C20 101.32(10)
C10 Mn1 C20 37.27(9)
C4 Mn1 C20 37.28(9)
C12 Mn1 C20 79.41(9)
C7 Mn1 C20 67.35(9)
C1 Mn1 C20 67.12(9)
C12 C1 C4 119.6(2)
C12 C1 C6 120.9(2)
C4 C1 C6 119.5(2)
C12 C1 Mn1 70.81(14)
C4 C1 Mn1 70.64(15)
C6 C1 Mn1 133.49(15)
O2 C2 Mn1 177.2(2)
C20 C4 C1 120.4(2)
C20 C4 C9 119.9(2)
C1 C4 C9 119.6(2)
C20 C4 Mn1 72.08(15)
C1 C4 Mn1 72.04(15)
C9 C4 Mn1 131.00(15)
C12 C5 C3 109.4(2)
C1 C6 C17 116.0(2)
C12 C7 C10 119.3(2)
C12 C7 C18 120.2(2)
C10 C7 C18 120.5(2)
C12 C7 Mn1 71.08(14)
C10 C7 Mn1 70.95(14)
C18 C7 Mn1 132.11(17)
O3 C8 Mn1 175.2(2)
C4 C9 C19 110.2(2)
C20 C10 C7 120.8(2)
C20 C10 C11 119.7(2)
C7 C10 C11 119.5(2)
C20 C10 Mn1 72.09(14)
C7 C10 Mn1 71.69(14)
C11 C10 Mn1 131.97(17)
C10 C11 C15 110.1(2)
C1 C12 C7 120.6(2)
C1 C12 C5 119.2(2)
C7 C12 C5 120.1(2)
C1 C12 Mn1 72.02(14)
C7 C12 Mn1 71.60(14)
C5 C12 Mn1 131.32(17)
O1 C16 Mn1 176.3(2)
C7 C18 C14 115.5(2)
C10 C20 C4 119.3(2)
C10 C20 C21 120.8(2)
C4 C20 C21 119.9(2)
C10 C20 Mn1 70.63(14)
C4 C20 Mn1 70.64(14)
C21 C20 Mn1 133.13(17)
C13 C21 C20 115.6(2)
F4 B1 F3 109.8(3)
F4 B1 F2 110.2(3)
F3 B1 F2 108.9(2)
F4 B1 F1 109.4(2)
F3 B1 F1 109.2(3)
F2 B1 F1 109.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
F1 B1 1.398(4)
Mn1 C8 1.824(3)
Mn1 C16 1.824(3)
Mn1 C2 1.825(3)
Mn1 C10 2.216(2)
Mn1 C4 2.216(3)
Mn1 C12 2.219(3)
Mn1 C7 2.225(2)
Mn1 C1 2.235(2)
Mn1 C20 2.235(3)
C1 C12 1.419(3)
C1 C4 1.424(3)
C1 C6 1.526(3)
O3 C8 1.144(3)
C2 O2 1.142(3)
C3 C5 1.539(3)
C4 C20 1.423(4)
C4 C9 1.519(3)
C5 C12 1.522(3)
C6 C17 1.529(3)
C7 C12 1.422(4)
C7 C10 1.422(4)
C7 C18 1.530(3)
C9 C19 1.531(3)
C10 C20 1.422(4)
C10 C11 1.512(4)
O1 C16 1.139(3)
C11 C15 1.537(3)
C13 C21 1.525(3)
C14 C18 1.532(4)
C20 C21 1.529(4)
F3 B1 1.394(4)
F2 B1 1.395(4)
F4 B1 1.382(4)
