#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:42:27 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178820 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/74/4107461.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_4107461
loop_
_publ_author_name
'Daesung Chong'
'Derek R. Laws'
'Ayman Nafady'
'Paulo Jorge Costa'
'Arnold L. Rheingold'
'Maria José Calhorda'
'William E. Geiger'
_publ_section_title
;
 [Re(η5-C5H5)(CO)3]+ Family of 17-Electron Compounds: Monomer/Dimer
 Equilibria and Other Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2692
_journal_page_last               2703
_journal_paper_doi               10.1021/ja710513n
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C32 H8 B F20 N O4 Re'
_chemical_formula_weight         1047.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.2680(10)
_cell_angle_beta                 92.2090(10)
_cell_angle_gamma                118.2330(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9709(5)
_cell_length_b                   12.1176(5)
_cell_length_c                   12.3692(6)
_cell_measurement_reflns_used    5300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.40
_cell_volume                     1570.85(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13063
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    4.031
_exptl_absorpt_correction_T_max  0.6655
_exptl_absorpt_correction_T_min  0.3680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.214
_exptl_crystal_description       plate
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         6866
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          1.198
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0350P)²+0.6000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                6522
_reflns_number_total             6866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710513n-file001.cif
_cod_data_source_block           geiger4
_cod_database_code               4107461
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Re1 Re 0.977458(10) 0.368878(9) 1.029411(8) 0.01278(5) Uani 1 1 d .
F12 F 0.24892(17) 0.37467(16) 0.69100(15) 0.0205(4) Uani 1 1 d .
F13 F 0.3972(2) 0.58724(17) 0.61342(15) 0.0262(4) Uani 1 1 d .
F14 F 0.6520(2) 0.66248(17) 0.59781(16) 0.0309(5) Uani 1 1 d .
F15 F 0.74492(17) 0.50447(17) 0.65058(16) 0.0259(4) Uani 1 1 d .
F16 F 0.59167(16) 0.28069(16) 0.71386(14) 0.0183(4) Uani 1 1 d .
F22 F 0.41923(17) 0.16932(16) 0.51010(13) 0.0184(4) Uani 1 1 d .
F23 F 0.38587(17) -0.03525(17) 0.38648(13) 0.0210(4) Uani 1 1 d .
F24 F 0.28559(18) -0.26384(17) 0.46702(14) 0.0234(4) Uani 1 1 d .
F25 F 0.22065(18) -0.28193(16) 0.67500(15) 0.0242(4) Uani 1 1 d .
F26 F 0.24895(16) -0.08127(16) 0.80009(13) 0.0171(3) Uani 1 1 d .
F32 F 0.12671(16) 0.02766(16) 0.90074(13) 0.0181(4) Uani 1 1 d .
F33 F -0.12046(17) -0.08377(16) 0.85917(15) 0.0223(4) Uani 1 1 d .
F34 F -0.22802(16) -0.05404(18) 0.67335(16) 0.0259(4) Uani 1 1 d .
F35 F -0.07326(17) 0.08890(19) 0.52386(15) 0.0251(4) Uani 1 1 d .
F36 F 0.17586(16) 0.17690(16) 0.55135(13) 0.0192(4) Uani 1 1 d .
F42 F 0.27493(17) 0.30660(17) 0.91572(15) 0.0229(4) Uani 1 1 d .
F43 F 0.3578(2) 0.3488(2) 1.12401(15) 0.0314(5) Uani 1 1 d .
F44 F 0.5167(2) 0.2608(2) 1.19728(15) 0.0304(5) Uani 1 1 d .
F45 F 0.59314(17) 0.13495(17) 1.05298(14) 0.0215(4) Uani 1 1 d .
F46 F 0.50751(16) 0.08648(16) 0.84482(14) 0.0170(3) Uani 1 1 d .
O1 O 1.2632(2) 0.5479(2) 1.09394(18) 0.0221(5) Uani 1 1 d .
O2 O 1.0177(2) 0.2667(2) 1.24028(18) 0.0234(5) Uani 1 1 d .
O3 O 0.8016(2) 0.4334(2) 1.16734(18) 0.0232(5) Uani 1 1 d .
O4 O 1.0614(3) 0.4445(3) 0.5712(2) 0.0431(7) Uani 1 1 d D
C1 C 0.8115(3) 0.2355(3) 0.9015(2) 0.0171(6) Uani 1 1 d .
H1A H 0.7244 0.2278 0.8967 0.020 Uiso 1 1 calc R
C2 C 0.8513(3) 0.1663(3) 0.9665(2) 0.0168(6) Uani 1 1 d .
H2A H 0.7958 0.0980 1.0106 0.020 Uiso 1 1 calc R
C3 C 0.9804(3) 0.2008(3) 0.9469(2) 0.0163(6) Uani 1 1 d .
H3A H 1.0299 0.1598 0.9743 0.020 Uiso 1 1 calc R
C4 C 1.0189(3) 0.2905(3) 0.8686(2) 0.0158(6) Uani 1 1 d .
H4A H 1.1026 0.3272 0.8361 0.019 Uiso 1 1 calc R
C5 C 0.9071(3) 0.2961(3) 0.8277(2) 0.0160(6) Uani 1 1 d .
C6 C 1.1560(3) 0.4884(3) 1.0719(2) 0.0167(6) Uani 1 1 d .
C7 C 1.0009(3) 0.3030(3) 1.1629(3) 0.0186(6) Uani 1 1 d .
C8 C 0.8714(3) 0.4165(3) 1.1184(2) 0.0177(6) Uani 1 1 d .
N1 N 0.8946(3) 0.3479(3) 0.7403(2) 0.0204(5) Uani 1 1 d .
C11 C 0.4093(3) 0.3101(3) 0.7000(2) 0.0155(6) Uani 1 1 d .
C12 C 0.3705(3) 0.3980(3) 0.6778(2) 0.0168(6) Uani 1 1 d .
C13 C 0.4478(3) 0.5133(3) 0.6407(2) 0.0199(6) Uani 1 1 d .
C14 C 0.5741(3) 0.5505(3) 0.6310(2) 0.0219(7) Uani 1 1 d .
C15 C 0.6202(3) 0.4700(3) 0.6569(2) 0.0192(6) Uani 1 1 d .
C16 C 0.5390(3) 0.3549(3) 0.6899(2) 0.0165(6) Uani 1 1 d .
C21 C 0.3361(3) 0.0565(3) 0.6633(2) 0.0137(5) Uani 1 1 d .
C22 C 0.3691(3) 0.0599(3) 0.5565(2) 0.0156(6) Uani 1 1 d .
C23 C 0.3539(3) -0.0447(3) 0.4900(2) 0.0167(6) Uani 1 1 d .
C24 C 0.3040(3) -0.1599(3) 0.5289(2) 0.0188(6) Uani 1 1 d .
C25 C 0.2705(3) -0.1692(3) 0.6346(2) 0.0179(6) Uani 1 1 d .
C26 C 0.2869(3) -0.0633(3) 0.6979(2) 0.0149(6) Uani 1 1 d .
C31 C 0.1689(3) 0.1139(3) 0.7292(2) 0.0141(6) Uani 1 1 d .
C32 C 0.0847(3) 0.0431(3) 0.8018(2) 0.0154(6) Uani 1 1 d .
C33 C -0.0463(3) -0.0153(3) 0.7839(2) 0.0180(6) Uani 1 1 d .
C34 C -0.1015(3) -0.0007(3) 0.6902(3) 0.0193(6) Uani 1 1 d .
C35 C -0.0232(3) 0.0704(3) 0.6157(2) 0.0186(6) Uani 1 1 d .
C36 C 0.1072(3) 0.1205(3) 0.6338(2) 0.0162(6) Uani 1 1 d .
C41 C 0.3816(3) 0.1896(3) 0.8687(2) 0.0144(5) Uani 1 1 d .
C42 C 0.3525(3) 0.2593(3) 0.9460(2) 0.0181(6) Uani 1 1 d .
C43 C 0.3943(3) 0.2833(3) 1.0548(3) 0.0215(6) Uani 1 1 d .
C44 C 0.4738(3) 0.2390(3) 1.0923(2) 0.0210(6) Uani 1 1 d .
C45 C 0.5109(3) 0.1737(3) 1.0188(2) 0.0178(6) Uani 1 1 d .
C46 C 0.4647(3) 0.1504(3) 0.9102(2) 0.0147(6) Uani 1 1 d .
B1 B 0.3248(3) 0.1691(3) 0.7403(3) 0.0128(6) Uani 1 1 d .
H5 H 0.959(4) 0.379(4) 0.693(3) 0.040 Uiso 1 1 d .
H6 H 0.829(4) 0.344(4) 0.721(4) 0.040 Uiso 1 1 d .
H4B H 1.048(4) 0.3859(19) 0.5091(16) 0.040 Uiso 1 1 d D
H4C H 1.124(3) 0.5278(10) 0.558(2) 0.040 Uiso 1 1 d 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'
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'
Re Re -1.0185 7.2310 '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'
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_3
C7 Re1 C6 80.36(12) .
C7 Re1 C8 82.37(12) .
C6 Re1 C8 108.53(12) .
C7 Re1 C3 84.29(12) .
C6 Re1 C3 104.70(12) .
C8 Re1 C3 141.35(12) .
C7 Re1 C2 85.21(12) .
C6 Re1 C2 140.94(11) .
C8 Re1 C2 105.21(12) .
C3 Re1 C2 37.41(10) .
C7 Re1 C4 117.52(11) .
C6 Re1 C4 94.25(11) .
C8 Re1 C4 152.44(12) .
C3 Re1 C4 36.74(10) .
C2 Re1 C4 61.08(10) .
C7 Re1 C1 118.53(12) .
C6 Re1 C1 152.32(11) .
C8 Re1 C1 94.68(12) .
C3 Re1 C1 60.96(11) .
C2 Re1 C1 36.26(11) .
C4 Re1 C1 59.72(10) .
C7 Re1 C5 139.87(11) .
C6 Re1 C5 118.68(11) .
C8 Re1 C5 118.50(11) .
C3 Re1 C5 57.64(10) .
C2 Re1 C5 57.31(10) .
C4 Re1 C5 34.10(10) .
C1 Re1 C5 33.90(9) .
C7 Re1 Re1 134.58(9) 2_767
C6 Re1 Re1 72.83(8) 2_767
C8 Re1 Re1 72.67(8) 2_767
C3 Re1 Re1 137.37(7) 2_767
C2 Re1 Re1 137.33(8) 2_767
C4 Re1 Re1 100.67(7) 2_767
C1 Re1 Re1 101.12(7) 2_767
C5 Re1 Re1 85.53(7) 2_767
H4B O4 H4C 109.7(2) .
C2 C1 C5 108.1(3) .
C2 C1 Re1 68.74(17) .
C5 C1 Re1 81.84(17) .
C2 C1 H1A 125.3 .
C5 C1 H1A 125.3 .
Re1 C1 H1A 125.3 .
C1 C2 C3 107.9(3) .
C1 C2 Re1 75.00(17) .
C3 C2 Re1 70.65(16) .
C1 C2 H2A 125.8 .
C3 C2 H2A 125.8 .
Re1 C2 H2A 125.8 .
C4 C3 C2 107.8(3) .
C4 C3 Re1 74.91(16) .
C2 C3 Re1 71.94(16) .
C4 C3 H3A 125.8 .
C2 C3 H3A 125.8 .
Re1 C3 H3A 125.8 .
C3 C4 C5 107.6(3) .
C3 C4 Re1 68.35(16) .
C5 C4 Re1 82.17(16) .
C3 C4 H4A 125.5 .
C5 C4 H4A 125.5 .
Re1 C4 H4A 125.5 .
N1 C5 C1 126.4(3) .
N1 C5 C4 127.3(3) .
C1 C5 C4 106.3(3) .
N1 C5 Re1 136.3(2) .
C1 C5 Re1 64.26(15) .
C4 C5 Re1 63.73(15) .
O1 C6 Re1 172.6(3) .
O2 C7 Re1 178.3(3) .
O3 C8 Re1 173.9(3) .
C5 N1 H5 121(3) .
C5 N1 H6 121(3) .
H5 N1 H6 117(4) .
C12 C11 C16 112.4(3) .
C12 C11 B1 128.6(3) .
C16 C11 B1 119.0(3) .
F12 C12 C13 114.7(3) .
F12 C12 C11 120.8(3) .
C13 C12 C11 124.5(3) .
F13 C13 C14 120.7(3) .
F13 C13 C12 119.4(3) .
C14 C13 C12 119.9(3) .
F14 C14 C13 121.4(3) .
F14 C14 C15 120.2(3) .
C13 C14 C15 118.4(3) .
F15 C15 C16 120.2(3) .
F15 C15 C14 120.2(3) .
C16 C15 C14 119.7(3) .
F16 C16 C15 116.1(3) .
F16 C16 C11 118.9(3) .
C15 C16 C11 125.0(3) .
C22 C21 C26 112.9(3) .
C22 C21 B1 127.1(3) .
C26 C21 B1 119.0(2) .
F22 C22 C23 115.2(2) .
F22 C22 C21 120.6(3) .
C23 C22 C21 124.1(3) .
F23 C23 C24 118.9(3) .
F23 C23 C22 121.1(3) .
C24 C23 C22 120.0(3) .
F24 C24 C23 122.0(3) .
F24 C24 C25 119.3(3) .
C23 C24 C25 118.7(3) .
F25 C25 C26 120.5(3) .
F25 C25 C24 119.9(3) .
C26 C25 C24 119.6(3) .
F26 C26 C25 115.8(2) .
F26 C26 C21 119.5(2) .
C25 C26 C21 124.7(3) .
C32 C31 C36 112.6(3) .
C32 C31 B1 126.1(3) .
C36 C31 B1 120.7(2) .
F32 C32 C33 113.7(2) .
F32 C32 C31 121.5(3) .
C33 C32 C31 124.9(3) .
F33 C33 C34 119.8(3) .
F33 C33 C32 120.4(3) .
C34 C33 C32 119.7(3) .
F34 C34 C35 121.4(3) .
F34 C34 C33 120.3(3) .
C35 C34 C33 118.3(3) .
F35 C35 C34 120.2(3) .
F35 C35 C36 119.8(3) .
C34 C35 C36 120.0(3) .
F36 C36 C35 116.0(3) .
F36 C36 C31 119.7(3) .
C35 C36 C31 124.3(3) .
C42 C41 C46 113.3(3) .
C42 C41 B1 119.7(3) .
C46 C41 B1 126.9(3) .
F42 C42 C43 115.4(3) .
F42 C42 C41 119.5(3) .
C43 C42 C41 125.1(3) .
F43 C43 C44 120.1(3) .
F43 C43 C42 120.7(3) .
C44 C43 C42 119.2(3) .
F44 C44 C43 121.0(3) .
F44 C44 C45 120.4(3) .
C43 C44 C45 118.6(3) .
F45 C45 C44 119.5(3) .
F45 C45 C46 120.6(3) .
C44 C45 C46 119.9(3) .
F46 C46 C45 115.3(3) .
F46 C46 C41 120.9(3) .
C45 C46 C41 123.8(3) .
C11 B1 C31 115.5(2) .
C11 B1 C41 102.4(2) .
C31 B1 C41 111.8(2) .
C11 B1 C21 112.8(2) .
C31 B1 C21 100.5(2) .
C41 B1 C21 114.4(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C7 1.953(3) .
Re1 C6 1.953(3) .
Re1 C8 1.966(3) .
Re1 C3 2.225(3) .
Re1 C2 2.242(3) .
Re1 C4 2.312(3) .
Re1 C1 2.324(3) .
Re1 C5 2.554(3) .
Re1 Re1 3.1097(2) 2_767
F12 C12 1.363(3) .
F13 C13 1.352(4) .
F14 C14 1.340(3) .
F15 C15 1.354(3) .
F16 C16 1.361(3) .
F22 C22 1.354(3) .
F23 C23 1.348(3) .
F24 C24 1.342(3) .
F25 C25 1.351(3) .
F26 C26 1.357(3) .
F32 C32 1.365(3) .
F33 C33 1.351(3) .
F34 C34 1.336(3) .
F35 C35 1.346(3) .
F36 C36 1.349(3) .
F42 C42 1.356(3) .
F43 C43 1.345(4) .
F44 C44 1.337(3) .
F45 C45 1.343(3) .
F46 C46 1.353(3) .
O1 C6 1.144(4) .
O2 C7 1.132(4) .
O3 C8 1.135(4) .
O4 H4B 0.9602(10) .
O4 H4C 0.962(3) .
C1 C2 1.423(4) .
C1 C5 1.439(4) .
C1 H1A 1.0000 .
C2 C3 1.433(4) .
C2 H2A 1.0000 .
C3 C4 1.432(4) .
C3 H3A 1.0000 .
C4 C5 1.445(4) .
C4 H4A 1.0000 .
C5 N1 1.327(4) .
N1 H5 0.93(4) .
N1 H6 0.79(5) .
C11 C12 1.389(4) .
C11 C16 1.396(4) .
C11 B1 1.650(4) .
C12 C13 1.387(4) .
C13 C14 1.371(5) .
C14 C15 1.379(5) .
C15 C16 1.375(4) .
C21 C22 1.392(4) .
C21 C26 1.394(4) .
C21 B1 1.666(4) .
C22 C23 1.389(4) .
C23 C24 1.368(4) .
C24 C25 1.380(4) .
C25 C26 1.377(4) .
C31 C32 1.387(4) .
C31 C36 1.396(4) .
C31 B1 1.653(4) .
C32 C33 1.382(4) .
C33 C34 1.376(4) .
C34 C35 1.375(4) .
C35 C36 1.383(4) .
C41 C42 1.389(4) .
C41 C46 1.388(4) .
C41 B1 1.657(4) .
C42 C43 1.378(4) .
C43 C44 1.377(5) .
C44 C45 1.382(4) .
C45 C46 1.388(4) .
