#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307804.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_4307804
loop_
_publ_author_name
'Michael Middleditch'
'James C. Anderson'
'Alexander J. Blake'
'Clare Wilson'
_publ_section_title
;
A Series of [3 + 2] Cycloaddition Products from the Reaction of Rhenium Oxo
Complexes with Diphenyl Ketene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2797
_journal_page_last               2804
_journal_paper_doi               10.1021/ic062290b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C33 H32 B N2 O5 Re'
_chemical_formula_weight         789.66
_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                72.523(1)
_cell_angle_beta                 78.082(1)
_cell_angle_gamma                72.196(1)
_cell_formula_units_Z            2
_cell_length_a                   8.4662(7)
_cell_length_b                   11.2918(10)
_cell_length_c                   17.789(2)
_cell_measurement_reflns_used    7209
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.4
_cell_volume                     1532.1(3)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'enCIFer (CCDC, 2003); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13216
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.019
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS v2.05'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.256
_refine_diff_density_min         -2.314
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0439P)²+1.9820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                6611
_reflns_number_total             6933
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic062290bsi20061201_094724_2.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1532.0(4)
_cod_database_code               4307804
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.693462(18) 0.039186(14) 0.173405(8) 0.01419(6) Uani 1 1 d . . .
O3 O 0.8874(4) 0.0424(3) 0.12624(17) 0.0220(6) Uani 1 1 d . . .
N5 N 0.4939(4) 0.3153(3) 0.15790(19) 0.0157(6) Uani 1 1 d . . .
C1P C 0.2353(5) 0.4231(4) 0.0843(2) 0.0181(8) Uani 1 1 d . . .
B1 B 0.3736(6) 0.2910(4) 0.1105(3) 0.0164(8) Uani 1 1 d . . .
O1 O 0.6783(4) -0.1390(3) 0.18321(16) 0.0174(6) Uani 1 1 d . . .
N1 N 0.6208(4) 0.2188(3) 0.19342(19) 0.0159(6) Uani 1 1 d . . .
C2P C 0.2659(5) 0.5173(4) 0.0150(3) 0.0229(9) Uani 1 1 d . . .
H2A H 0.3660 0.4984 -0.0200 0.027 Uiso 1 1 calc R . .
O2 O 0.7111(4) -0.0328(3) 0.28553(16) 0.0175(6) Uani 1 1 d . . .
N4 N 0.3031(4) 0.1780(3) 0.16698(19) 0.0165(6) Uani 1 1 d . . .
C3P C 0.1530(6) 0.6381(4) -0.0039(3) 0.0267(9) Uani 1 1 d . . .
H3A H 0.1761 0.6998 -0.0516 0.032 Uiso 1 1 calc R . .
O4 O 0.6816(4) -0.3310(3) 0.26674(18) 0.0223(6) Uani 1 1 d . . .
N3 N 0.4141(4) 0.0696(3) 0.20351(19) 0.0162(6) Uani 1 1 d . . .
C4P C 0.0071(6) 0.6682(4) 0.0468(3) 0.0275(9) Uani 1 1 d . . .
H4A H -0.0697 0.7504 0.0339 0.033 Uiso 1 1 calc R . .
N6 N 0.4826(4) 0.2322(3) 0.0414(2) 0.0178(7) Uani 1 1 d . . .
C5P C -0.0265(5) 0.5782(4) 0.1162(3) 0.0247(9) Uani 1 1 d . . .
H5A H -0.1267 0.5983 0.1510 0.030 Uiso 1 1 calc R . .
N2 N 0.6073(4) 0.1212(3) 0.0599(2) 0.0184(7) Uani 1 1 d . . .
C6P C 0.0874(5) 0.4580(4) 0.1349(2) 0.0219(8) Uani 1 1 d . . .
H6A H 0.0644 0.3978 0.1833 0.026 Uiso 1 1 calc R . .
C7 C 0.4823(5) 0.4226(4) 0.1791(2) 0.0209(8) Uani 1 1 d . . .
H7A H 0.4039 0.5031 0.1628 0.025 Uiso 1 1 calc R . .
C8 C 0.6017(6) 0.3980(4) 0.2281(3) 0.0248(9) Uani 1 1 d . . .
H8A H 0.6225 0.4566 0.2512 0.030 Uiso 1 1 calc R . .
C9 C 0.6845(5) 0.2694(4) 0.2363(2) 0.0199(8) Uani 1 1 d . . .
H9A H 0.7733 0.2235 0.2675 0.024 Uiso 1 1 calc R . .
C10 C 0.1514(5) 0.1556(4) 0.1785(2) 0.0204(8) Uani 1 1 d . . .
H10A H 0.0546 0.2146 0.1572 0.024 Uiso 1 1 calc R . .
C11 C 0.1595(5) 0.0328(4) 0.2265(3) 0.0223(8) Uani 1 1 d . . .
H11A H 0.0711 -0.0082 0.2458 0.027 Uiso 1 1 calc R . .
C12 C 0.3254(5) -0.0173(4) 0.2403(2) 0.0194(8) Uani 1 1 d . . .
H12A H 0.3704 -0.1015 0.2713 0.023 Uiso 1 1 calc R . .
C13 C 0.4586(6) 0.2533(4) -0.0348(2) 0.0230(9) Uani 1 1 d . . .
H13A H 0.3759 0.3219 -0.0616 0.028 Uiso 1 1 calc R . .
C14 C 0.5725(6) 0.1598(5) -0.0675(3) 0.0274(10) Uani 1 1 d . . .
H14A H 0.5864 0.1526 -0.1205 0.033 Uiso 1 1 calc R . .
C15 C 0.6624(6) 0.0785(4) -0.0063(2) 0.0232(9) Uani 1 1 d . . .
H15A H 0.7500 0.0036 -0.0105 0.028 Uiso 1 1 calc R . .
C1 C 0.6964(5) -0.2231(4) 0.2532(2) 0.0177(8) Uani 1 1 d . . .
C2 C 0.7384(5) -0.1702(4) 0.3156(2) 0.0168(8) Uani 1 1 d . . .
C18 C 0.9254(5) -0.2271(4) 0.3245(2) 0.0177(8) Uani 1 1 d . . .
C19 C 1.0401(6) -0.2664(4) 0.2632(3) 0.0254(9) Uani 1 1 d . . .
H19A H 1.0021 -0.2634 0.2158 0.030 Uiso 1 1 calc R . .
C20 C 1.2101(6) -0.3101(4) 0.2701(3) 0.0298(10) Uani 1 1 d . . .
H20A H 1.2874 -0.3363 0.2275 0.036 Uiso 1 1 calc R . .
C21 C 1.2670(6) -0.3154(4) 0.3387(3) 0.0320(11) Uani 1 1 d . . .
H21A H 1.3830 -0.3462 0.3437 0.038 Uiso 1 1 calc R . .
C22 C 1.1539(6) -0.2756(6) 0.3999(3) 0.0380(12) Uani 1 1 d . . .
H22A H 1.1922 -0.2789 0.4473 0.046 Uiso 1 1 calc R . .
C23 C 0.9847(6) -0.2308(5) 0.3925(3) 0.0287(10) Uani 1 1 d . . .
H23A H 0.9081 -0.2023 0.4347 0.034 Uiso 1 1 calc R . .
C24 C 0.6257(5) -0.1989(4) 0.3937(2) 0.0192(8) Uani 1 1 d . . .
C25 C 0.6422(6) -0.3246(4) 0.4400(3) 0.0237(9) Uani 1 1 d . . .
H25A H 0.7239 -0.3930 0.4224 0.028 Uiso 1 1 calc R . .
C26 C 0.5400(6) -0.3513(5) 0.5120(3) 0.0287(10) Uani 1 1 d . . .
H26A H 0.5526 -0.4374 0.5433 0.034 Uiso 1 1 calc R . .
C27 C 0.4192(6) -0.2510(5) 0.5377(3) 0.0304(10) Uani 1 1 d . . .
H27A H 0.3487 -0.2689 0.5864 0.036 Uiso 1 1 calc R . .
C28 C 0.4021(6) -0.1261(5) 0.4926(3) 0.0287(10) Uani 1 1 d . . .
H28A H 0.3208 -0.0577 0.5104 0.034 Uiso 1 1 calc R . .
C29 C 0.5047(5) -0.1004(4) 0.4206(3) 0.0236(9) Uani 1 1 d . . .
H29A H 0.4916 -0.0142 0.3895 0.028 Uiso 1 1 calc R . .
O1S O -0.0449(4) 0.2652(4) 0.3423(2) 0.0341(8) Uani 1 1 d . . .
C2S C 0.0721(7) 0.1702(5) 0.3912(3) 0.0322(11) Uani 1 1 d . . .
H2SA H 0.1119 0.0902 0.3729 0.039 Uiso 1 1 calc R . .
H2SB H 0.0206 0.1498 0.4472 0.039 Uiso 1 1 calc R . .
C3S C 0.2146(6) 0.2294(5) 0.3829(3) 0.0370(12) Uani 1 1 d . . .
H3SA H 0.2986 0.2120 0.3371 0.044 Uiso 1 1 calc R . .
H3SB H 0.2700 0.1965 0.4317 0.044 Uiso 1 1 calc R . .
C4S C 0.1273(8) 0.3729(5) 0.3694(4) 0.0480(15) Uani 1 1 d . . .
H4SA H 0.1269 0.4036 0.4161 0.058 Uiso 1 1 calc R . .
H4SB H 0.1837 0.4237 0.3219 0.058 Uiso 1 1 calc R . .
C5S C -0.0499(7) 0.3841(5) 0.3574(3) 0.0356(11) Uani 1 1 d . . .
H5SA H -0.1286 0.3975 0.4055 0.043 Uiso 1 1 calc R . .
H5SB H -0.0861 0.4573 0.3118 0.043 Uiso 1 1 calc R . .
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'
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'
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
_geom_angle_publ_flag
O3 Re O2 107.60(13) . . ?
O3 Re O1 104.55(13) . . ?
O2 Re O1 80.98(11) . . ?
O3 Re N1 98.37(14) . . ?
O2 Re N1 88.54(12) . . ?
O1 Re N1 156.76(12) . . ?
O3 Re N2 87.24(13) . . ?
O2 Re N2 165.16(12) . . ?
O1 Re N2 95.56(12) . . ?
N1 Re N2 89.28(13) . . ?
O3 Re N3 164.12(13) . . ?
O2 Re N3 87.95(12) . . ?
O1 Re N3 80.55(12) . . ?
N1 Re N3 78.39(13) . . ?
N2 Re N3 77.24(12) . . ?
C7 N5 N1 108.3(3) . . ?
C7 N5 B1 128.5(3) . . ?
N1 N5 B1 122.8(3) . . ?
C2P C1P C6P 116.6(4) . . ?
C2P C1P B1 121.4(4) . . ?
C6P C1P B1 121.4(4) . . ?
N6 B1 N4 103.3(3) . . ?
N6 B1 N5 108.3(3) . . ?
N4 B1 N5 106.3(3) . . ?
N6 B1 C1P 115.8(3) . . ?
N4 B1 C1P 114.8(3) . . ?
N5 B1 C1P 107.8(3) . . ?
C1 O1 Re 117.3(2) . . ?
C9 N1 N5 107.1(3) . . ?
C9 N1 Re 130.5(3) . . ?
N5 N1 Re 122.3(2) . . ?
C3P C2P C1P 121.7(4) . . ?
C2 O2 Re 117.5(2) . . ?
C10 N4 N3 109.4(3) . . ?
C10 N4 B1 131.5(3) . . ?
N3 N4 B1 118.1(3) . . ?
C4P C3P C2P 120.0(4) . . ?
C12 N3 N4 106.2(3) . . ?
C12 N3 Re 129.3(3) . . ?
N4 N3 Re 122.4(2) . . ?
C5P C4P C3P 119.9(4) . . ?
C13 N6 N2 108.3(3) . . ?
C13 N6 B1 131.6(3) . . ?
N2 N6 B1 118.5(3) . . ?
C4P C5P C6P 119.6(4) . . ?
C15 N2 N6 107.1(3) . . ?
C15 N2 Re 128.3(3) . . ?
N6 N2 Re 124.6(2) . . ?
C5P C6P C1P 122.1(4) . . ?
N5 C7 C8 109.6(4) . . ?
C7 C8 C9 105.0(4) . . ?
N1 C9 C8 110.0(4) . . ?
N4 C10 C11 108.9(4) . . ?
C10 C11 C12 104.7(4) . . ?
N3 C12 C11 110.7(4) . . ?
N6 C13 C14 109.4(4) . . ?
C13 C14 C15 105.0(4) . . ?
N2 C15 C14 110.1(4) . . ?
O4 C1 O1 122.8(4) . . ?
O4 C1 C2 123.5(4) . . ?
O1 C1 C2 113.7(3) . . ?
O2 C2 C24 109.1(3) . . ?
O2 C2 C18 107.2(3) . . ?
C24 C2 C18 113.0(3) . . ?
O2 C2 C1 108.4(3) . . ?
C24 C2 C1 110.4(3) . . ?
C18 C2 C1 108.7(3) . . ?
C19 C18 C23 118.4(4) . . ?
C19 C18 C2 121.3(4) . . ?
C23 C18 C2 120.1(4) . . ?
C18 C19 C20 120.8(4) . . ?
C21 C20 C19 120.2(4) . . ?
C20 C21 C22 119.5(4) . . ?
C23 C22 C21 120.1(5) . . ?
C22 C23 C18 121.0(4) . . ?
C29 C24 C25 118.5(4) . . ?
C29 C24 C2 120.9(4) . . ?
C25 C24 C2 120.5(4) . . ?
C24 C25 C26 120.7(4) . . ?
C27 C26 C25 119.7(4) . . ?
C28 C27 C26 120.1(4) . . ?
C27 C28 C29 119.7(4) . . ?
C24 C29 C28 121.2(4) . . ?
C2S O1S C5S 104.7(4) . . ?
O1S C2S C3S 105.2(4) . . ?
C2S C3S C4S 103.0(4) . . ?
C5S C4S C3S 104.6(4) . . ?
O1S C5S C4S 105.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re O3 1.688(3) . ?
Re O2 1.933(3) . ?
Re O1 2.008(3) . ?
Re N1 2.050(3) . ?
Re N2 2.130(3) . ?
Re N3 2.256(3) . ?
N5 C7 1.344(5) . ?
N5 N1 1.376(4) . ?
N5 B1 1.578(5) . ?
C1P C2P 1.403(6) . ?
C1P C6P 1.407(6) . ?
C1P B1 1.598(6) . ?
B1 N6 1.566(5) . ?
B1 N4 1.562(5) . ?
O1 C1 1.325(5) . ?
N1 C9 1.349(5) . ?
C2P C3P 1.395(6) . ?
O2 C2 1.442(5) . ?
N4 C10 1.346(5) . ?
N4 N3 1.369(5) . ?
C3P C4P 1.386(7) . ?
O4 C1 1.209(5) . ?
N3 C12 1.348(5) . ?
C4P C5P 1.385(6) . ?
N6 C13 1.351(5) . ?
N6 N2 1.371(5) . ?
C5P C6P 1.394(6) . ?
N2 C15 1.348(5) . ?
C7 C8 1.381(6) . ?
C8 C9 1.383(6) . ?
C10 C11 1.383(6) . ?
C11 C12 1.388(6) . ?
C13 C14 1.377(6) . ?
C14 C15 1.386(6) . ?
C1 C2 1.551(5) . ?
C2 C24 1.522(5) . ?
C2 C18 1.538(5) . ?
C18 C19 1.386(6) . ?
C18 C23 1.387(6) . ?
C19 C20 1.391(6) . ?
C20 C21 1.380(7) . ?
C21 C22 1.381(8) . ?
C22 C23 1.386(7) . ?
C24 C29 1.391(6) . ?
C24 C25 1.392(6) . ?
C25 C26 1.397(6) . ?
C26 C27 1.396(7) . ?
C27 C28 1.377(7) . ?
C28 C29 1.397(6) . ?
O1S C2S 1.425(6) . ?
O1S C5S 1.434(6) . ?
C2S C3S 1.512(7) . ?
C3S C4S 1.528(8) . ?
C4S C5S 1.521(8) . ?
