#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:29:39 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180184 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/80/7108079.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_7108079
loop_
_publ_author_name
'Celedonio M. Alvarez'
'Romen Carrillo'
'Raul Garcia-Rodriguez'
'Daniel Miguel'
_publ_section_title
;
 Intramolecular carboboration of carbonyl ligands to form boroxycarbenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7705
_journal_paper_doi               10.1039/c2cc33443g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C14 H13 F3 N O8 Re S'
_chemical_formula_weight         598.51
_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                109.086(4)
_cell_angle_beta                 104.152(4)
_cell_angle_gamma                91.234(4)
_cell_formula_units_Z            2
_cell_length_a                   8.830(2)
_cell_length_b                   9.860(2)
_cell_length_c                   11.793(3)
_cell_measurement_reflns_used    903
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.88
_cell_volume                     935.1(4)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8209
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    6.681
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0229
_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)+(0.0295P)²+0.3712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                3491
_reflns_number_total             3803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33443g.txt
_cod_data_source_block           compound_7(re)_rg659am
_cod_original_cell_volume        935.0(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108079
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 0.249164(16) 0.766362(16) 0.859426(14) 0.03735(7) Uani 1 1 d .
N1 N 0.4654(4) 0.7284(3) 0.9727(3) 0.0363(7) Uani 1 1 d .
C1 C 0.0607(5) 0.7740(6) 0.7402(5) 0.0580(12) Uani 1 1 d .
O1 O -0.0538(4) 0.7710(5) 0.6679(4) 0.0896(13) Uani 1 1 d .
C2 C 0.2240(5) 0.9524(5) 0.9617(4) 0.0491(10) Uani 1 1 d .
O2 O 0.2102(5) 1.0640(4) 1.0284(4) 0.0716(10) Uani 1 1 d .
C3 C 0.1206(5) 0.6941(5) 0.9394(4) 0.0459(10) Uani 1 1 d .
O3 O 0.0460(4) 0.6530(4) 0.9901(3) 0.0683(9) Uani 1 1 d .
O4 O 0.3113(3) 0.5606(3) 0.7508(3) 0.0418(6) Uani 1 1 d .
O5 O 0.4086(3) 0.8450(3) 0.7732(3) 0.0425(6) Uani 1 1 d .
C11 C 0.5232(5) 0.7921(5) 1.0970(4) 0.0464(10) Uani 1 1 d .
H11 H 0.4667 0.8587 1.1407 0.056 Uiso 1 1 calc R
C12 C 0.6618(5) 0.7620(5) 1.1606(4) 0.0532(11) Uani 1 1 d .
H12 H 0.6988 0.8082 1.2462 0.064 Uiso 1 1 calc R
C13 C 0.7467(5) 0.6628(5) 1.0977(4) 0.0504(10) Uani 1 1 d .
H13 H 0.8420 0.6423 1.1399 0.061 Uiso 1 1 calc R
C14 C 0.6883(5) 0.5948(4) 0.9717(4) 0.0442(9) Uani 1 1 d .
H14 H 0.7425 0.5260 0.9276 0.053 Uiso 1 1 calc R
C15 C 0.5499(4) 0.6293(4) 0.9119(4) 0.0371(8) Uani 1 1 d .
C16 C 0.4814(4) 0.5616(4) 0.7728(3) 0.0395(8) Uani 1 1 d .
H16 H 0.5063 0.4616 0.7464 0.047 Uiso 1 1 calc R
C17 C 0.5445(5) 0.6398(4) 0.7000(4) 0.0430(9) Uani 1 1 d .
H17A H 0.6581 0.6419 0.7218 0.052 Uiso 1 1 calc R
H17B H 0.5058 0.5832 0.6122 0.052 Uiso 1 1 calc R
C18 C 0.5057(4) 0.7906(5) 0.7174(4) 0.0420(9) Uani 1 1 d .
C19 C 0.5889(6) 0.8768(5) 0.6643(4) 0.0557(11) Uani 1 1 d .
H19A H 0.5376 0.9617 0.6645 0.084 Uiso 1 1 calc R
H19B H 0.5869 0.8199 0.5804 0.084 Uiso 1 1 calc R
H19C H 0.6959 0.9045 0.7136 0.084 Uiso 1 1 calc R
C40 C 0.2201(6) 0.4631(5) 0.6288(4) 0.0610(12) Uani 1 1 d .
H40A H 0.2304 0.5018 0.5658 0.091 Uiso 1 1 calc R
H40B H 0.1114 0.4533 0.6281 0.091 Uiso 1 1 calc R
H40C H 0.2585 0.3701 0.6122 0.091 Uiso 1 1 calc R
S1 S 0.76313(15) 0.30349(13) 0.64141(11) 0.0559(3) Uani 1 1 d .
O11 O 0.8827(5) 0.4100(4) 0.7307(4) 0.0845(12) Uani 1 1 d .
O12 O 0.6423(7) 0.2580(5) 0.6862(6) 0.125(2) Uani 1 1 d .
O13 O 0.7081(8) 0.3291(5) 0.5293(5) 0.133(2) Uani 1 1 d .
C51 C 0.8585(7) 0.1430(6) 0.5977(6) 0.0728(15) Uani 1 1 d .
F1 F 0.7650(5) 0.0324(4) 0.5168(4) 0.1029(12) Uani 1 1 d .
F2 F 0.9799(6) 0.1659(5) 0.5614(7) 0.174(3) Uani 1 1 d .
F3 F 0.9157(6) 0.1016(5) 0.6940(6) 0.148(2) 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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
C2 Re1 C3 86.41(19)
C2 Re1 C1 88.3(2)
C3 Re1 C1 88.0(2)
C2 Re1 N1 100.15(16)
C3 Re1 N1 93.66(16)
C1 Re1 N1 171.44(17)
C2 Re1 O4 172.46(14)
C3 Re1 O4 98.07(15)
C1 Re1 O4 97.85(17)
N1 Re1 O4 73.61(11)
C2 Re1 O5 94.63(15)
C3 Re1 O5 176.72(14)
C1 Re1 O5 95.16(17)
N1 Re1 O5 83.09(11)
O4 Re1 O5 80.57(11)
C11 N1 C15 117.3(3)
C11 N1 Re1 126.3(3)
C15 N1 Re1 116.3(2)
O1 C1 Re1 176.4(5)
O2 C2 Re1 177.1(4)
O3 C3 Re1 178.3(4)
C16 O4 C40 114.8(3)
C16 O4 Re1 111.2(2)
C40 O4 Re1 126.8(3)
C18 O5 Re1 134.5(3)
N1 C11 C12 122.2(4)
C11 C12 C13 119.8(4)
C14 C13 C12 118.9(4)
C15 C14 C13 119.2(4)
C14 C15 N1 122.6(4)
C14 C15 C16 121.9(3)
N1 C15 C16 115.5(3)
O4 C16 C15 106.2(3)
O4 C16 C17 111.7(3)
C15 C16 C17 113.1(3)
C18 C17 C16 117.2(3)
O5 C18 C19 119.5(4)
O5 C18 C17 122.9(4)
C19 C18 C17 117.6(4)
O13 S1 O11 113.8(3)
O13 S1 O12 114.1(4)
O11 S1 O12 116.3(3)
O13 S1 C51 103.3(4)
O11 S1 C51 105.0(3)
O12 S1 C51 102.1(3)
F2 C51 F1 111.5(6)
F2 C51 F3 104.1(6)
F1 C51 F3 104.4(5)
F2 C51 S1 111.3(4)
F1 C51 S1 113.6(4)
F3 C51 S1 111.3(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C2 1.890(5)
Re1 C3 1.900(4)
Re1 C1 1.919(5)
Re1 N1 2.164(3)
Re1 O4 2.180(3)
Re1 O5 2.187(3)
N1 C11 1.350(5)
N1 C15 1.364(5)
C1 O1 1.145(6)
C2 O2 1.153(5)
C3 O3 1.138(5)
O4 C16 1.459(5)
O4 C40 1.462(5)
O5 C18 1.234(5)
C11 C12 1.364(6)
C12 C13 1.378(7)
C13 C14 1.371(6)
C14 C15 1.364(5)
C15 C16 1.512(5)
C16 C17 1.513(5)
C17 C18 1.493(6)
C18 C19 1.483(6)
S1 O13 1.399(5)
S1 O11 1.418(4)
S1 O12 1.424(5)
S1 C51 1.793(6)
C51 F2 1.289(7)
C51 F1 1.295(7)
C51 F3 1.320(8)
