#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:23:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179058 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/20/4302088.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_4302088
loop_
_publ_author_name
'Margarida Videira'
'Carolina Moura'
'Amitabha Datta'
'António Paulo'
'Isabel C. Santos'
'I. Santos'
_publ_section_title
;
Rhenium(I) Tricarbonyl Complexes with Poly(azolyl)borates Generated in Situ
from an Organometallic Precursor Containing the B-H...Re Coordination
Motif
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4251
_journal_page_last               4257
_journal_paper_doi               10.1021/ic802403u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C15 H20 B N5 O5 Re S'
_chemical_formula_sum            'C15 H20 B N5 O5 Re S'
_chemical_formula_weight         579.43
_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                106.6540(10)
_cell_angle_beta                 91.5020(10)
_cell_angle_gamma                95.9390(10)
_cell_formula_units_Z            2
_cell_length_a                   7.1432(3)
_cell_length_b                   11.8530(5)
_cell_length_c                   12.5983(6)
_cell_measurement_reflns_used    4987
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.81
_cell_volume                     1014.70(8)
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_molecular_graphics    SCHAKAL(Keller,1989),ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6485
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    6.127
_exptl_absorpt_correction_T_max  0.4051
_exptl_absorpt_correction_T_min  0.2608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0222
_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)+(0.0281P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                3579
_reflns_number_total             3822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802403u_si_001_4.cif
_cod_data_source_block           COMPLEX_6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4302088
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
Re1 Re 0.284607(19) 0.296186(11) 0.880540(10) 0.01419(6) Uani 1 1 d . . .
S1 S 0.36664(13) 0.08951(8) 0.85391(8) 0.01723(19) Uani 1 1 d . . .
O1 O 0.1616(4) 0.5468(2) 0.9197(2) 0.0284(7) Uani 1 1 d . . .
O2 O 0.6790(4) 0.3846(3) 0.8273(3) 0.0307(7) Uani 1 1 d . . .
O3 O 0.4211(4) 0.3576(2) 1.1262(2) 0.0255(6) Uani 1 1 d . . .
O4 O -0.3067(5) 0.2525(3) 0.4046(3) 0.0392(8) Uani 1 1 d . . .
O5 O -0.0140(4) 0.3285(2) 0.3822(2) 0.0276(6) Uani 1 1 d . . .
N1 N 0.1366(4) -0.1042(3) 0.8641(2) 0.0167(6) Uani 1 1 d . . .
N2 N -0.0194(4) 0.0419(3) 0.8512(2) 0.0146(6) Uani 1 1 d . . .
N3 N -0.0211(4) 0.1735(3) 0.7222(2) 0.0147(6) Uani 1 1 d . . .
N4 N 0.1509(4) 0.2311(3) 0.7155(2) 0.0170(6) Uani 1 1 d . . .
C1 N 0.2089(5) 0.4530(4) 0.9045(3) 0.0362(9) Uani 1 1 d . . .
C2 C 0.5313(6) 0.3513(3) 0.8471(3) 0.0207(8) Uani 1 1 d . . .
C3 C 0.3711(5) 0.3361(3) 1.0347(3) 0.0190(8) Uani 1 1 d . . .
C4 C 0.1549(5) 0.0084(3) 0.8556(3) 0.0144(7) Uani 1 1 d . . .
C5 C -0.0549(5) -0.1417(3) 0.8650(3) 0.0199(8) Uani 1 1 d . . .
H5 H -0.1080 -0.2167 0.8701 0.024 Uiso 1 1 calc R . .
C6 C -0.1508(5) -0.0515(3) 0.8572(3) 0.0198(8) Uani 1 1 d . . .
H6 H -0.2838 -0.0517 0.8560 0.024 Uiso 1 1 calc R . .
C7 C 0.2924(6) -0.1695(3) 0.8788(3) 0.0227(8) Uani 1 1 d . . .
H7C H 0.3645 -0.1857 0.8121 0.034 Uiso 1 1 calc R . .
H7A H 0.2426 -0.2446 0.8913 0.034 Uiso 1 1 calc R . .
H7B H 0.3747 -0.1222 0.9429 0.034 Uiso 1 1 calc R . .
C8 C -0.3068(5) 0.0681(4) 0.6035(3) 0.0244(9) Uani 1 1 d . . .
H8A H -0.3016 -0.0079 0.6192 0.037 Uiso 1 1 calc R . .
H8B H -0.3530 0.0537 0.5263 0.037 Uiso 1 1 calc R . .
H8C H -0.3922 0.1146 0.6533 0.037 Uiso 1 1 calc R . .
C9 C -0.1143(5) 0.1348(3) 0.6213(3) 0.0182(8) Uani 1 1 d . . .
C10 C 0.0018(5) 0.1686(3) 0.5466(3) 0.0177(8) Uani 1 1 d . . .
C11 C 0.1669(6) 0.2296(3) 0.6088(3) 0.0190(8) Uani 1 1 d . . .
C12 C 0.3367(6) 0.2894(4) 0.5718(3) 0.0265(9) Uani 1 1 d . . .
H12A H 0.3863 0.3605 0.6313 0.040 Uiso 1 1 calc R . .
H12B H 0.3018 0.3118 0.5055 0.040 Uiso 1 1 calc R . .
H12C H 0.4334 0.2350 0.5544 0.040 Uiso 1 1 calc R . .
C13 C -0.0439(6) 0.1465(3) 0.4243(3) 0.0231(8) Uani 1 1 d . . .
H13A H -0.1276 0.0711 0.3953 0.028 Uiso 1 1 calc R . .
H13B H 0.0737 0.1388 0.3843 0.028 Uiso 1 1 calc R . .
C14 C -0.1398(6) 0.2465(3) 0.4032(3) 0.0230(9) Uani 1 1 d . . .
C15 C -0.0868(7) 0.4305(4) 0.3601(3) 0.0289(9) Uani 1 1 d . . .
H15A H -0.1405 0.4792 0.4273 0.035 Uiso 1 1 calc R . .
H15B H -0.1871 0.4040 0.2995 0.035 Uiso 1 1 calc R . .
C16 C 0.0758(8) 0.5012(4) 0.3269(4) 0.0389(12) Uani 1 1 d . . .
H16A H 0.1763 0.5238 0.3861 0.058 Uiso 1 1 calc R . .
H16B H 0.0336 0.5728 0.3145 0.058 Uiso 1 1 calc R . .
H16C H 0.1238 0.4532 0.2584 0.058 Uiso 1 1 calc R . .
B1 B -0.0651(6) 0.1608(4) 0.8382(3) 0.0158(8) Uani 1 1 d . . .
H1B H -0.205(6) 0.178(3) 0.860(3) 0.019 Uiso 1 1 d . . .
H1A H 0.032(6) 0.249(4) 0.908(4) 0.029(12) Uiso 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'
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'
S S 0.1246 0.1234 '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'
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
C2 Re1 C3 89.04(16) . . ?
C2 Re1 C1 90.30(16) . . ?
C3 Re1 C1 90.18(15) . . ?
C2 Re1 N4 100.08(14) . . ?
C3 Re1 N4 170.14(13) . . ?
C1 Re1 N4 93.47(14) . . ?
C2 Re1 S1 92.76(11) . . ?
C3 Re1 S1 89.26(11) . . ?
C1 Re1 S1 176.88(11) . . ?
N4 Re1 S1 86.60(8) . . ?
C2 Re1 H1A 175.4(12) . . ?
C3 Re1 H1A 93.7(13) . . ?
C1 Re1 H1A 86.1(13) . . ?
N4 Re1 H1A 77.4(13) . . ?
S1 Re1 H1A 90.9(13) . . ?
C4 S1 Re1 104.10(13) . . ?
C14 O5 C15 117.2(3) . . ?
C4 N1 C5 108.4(3) . . ?
C4 N1 C7 125.2(3) . . ?
C5 N1 C7 126.3(3) . . ?
C4 N2 C6 108.4(3) . . ?
C4 N2 B1 125.6(3) . . ?
C6 N2 B1 125.9(3) . . ?
C9 N3 N4 110.4(3) . . ?
C9 N3 B1 134.0(3) . . ?
N4 N3 B1 115.6(3) . . ?
C11 N4 N3 107.2(3) . . ?
C11 N4 Re1 144.7(3) . . ?
N3 N4 Re1 108.0(2) . . ?
O1 C1 Re1 179.1(3) . . ?
O2 C2 Re1 179.8(5) . . ?
O3 C3 Re1 178.6(3) . . ?
N2 C4 N1 108.0(3) . . ?
N2 C4 S1 128.0(3) . . ?
N1 C4 S1 124.0(3) . . ?
C6 C5 N1 107.3(3) . . ?
C6 C5 H5 126.3 . . ?
N1 C5 H5 126.3 . . ?
C5 C6 N2 107.8(3) . . ?
C5 C6 H6 126.1 . . ?
N2 C6 H6 126.1 . . ?
N1 C7 H7C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
H7C C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7C C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 107.4(3) . . ?
N3 C9 C8 122.2(3) . . ?
C10 C9 C8 130.4(3) . . ?
C9 C10 C11 106.0(3) . . ?
C9 C10 C13 126.4(3) . . ?
C11 C10 C13 127.6(3) . . ?
N4 C11 C10 109.0(3) . . ?
N4 C11 C12 121.8(3) . . ?
C10 C11 C12 129.2(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 C14 111.0(3) . . ?
C10 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C10 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
O4 C14 O5 123.9(4) . . ?
O4 C14 C13 124.9(4) . . ?
O5 C14 C13 111.1(3) . . ?
O5 C15 C16 107.0(4) . . ?
O5 C15 H15A 110.3 . . ?
C16 C15 H15A 110.3 . . ?
O5 C15 H15B 110.3 . . ?
C16 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 B1 N3 112.2(3) . . ?
N2 B1 H1B 112(2) . . ?
N3 B1 H1B 113(2) . . ?
N2 B1 H1A 112.5(19) . . ?
N3 B1 H1A 105.5(19) . . ?
H1B B1 H1A 101(3) . . ?
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
Re1 C2 1.916(4) . ?
Re1 C3 1.931(4) . ?
Re1 C1 1.932(4) . ?
Re1 N4 2.158(3) . ?
Re1 S1 2.5086(9) . ?
Re1 H1A 1.90(4) . ?
S1 C4 1.710(4) . ?
O1 C1 1.160(5) . ?
O2 C2 1.146(5) . ?
O3 C3 1.145(5) . ?
O4 C14 1.203(5) . ?
O5 C14 1.342(5) . ?
O5 C15 1.458(4) . ?
N1 C4 1.363(4) . ?
N1 C5 1.395(5) . ?
N1 C7 1.457(5) . ?
N2 C4 1.350(5) . ?
N2 C6 1.396(4) . ?
N2 B1 1.531(5) . ?
N3 C9 1.352(5) . ?
N3 N4 1.360(4) . ?
N3 B1 1.548(4) . ?
N4 C11 1.347(4) . ?
C5 C6 1.352(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 C9 1.491(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.386(5) . ?
C10 C11 1.406(5) . ?
C10 C13 1.508(5) . ?
C11 C12 1.494(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.511(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C15 C16 1.501(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
B1 H1B 1.07(4) . ?
B1 H1A 1.28(4) . ?
