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#$Date: 2017-07-19 06:37:55 +0300 (Wed, 19 Jul 2017) $
#$Revision: 198800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/36/7043692.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_7043692
loop_
_publ_author_name
'Alberto, Roger'
'Meola, Giuseppe'
'Braband, Henrik'
'Jordi, Sara'
'Fox, Thomas'
'Blacque, Oliver'
'Spingler, Bernhard'
_publ_section_title
;
 Structure and Reactivities of Rhenium and Technetium bis-Arene Sandwich
 Complexes [M(η6-arene)2]+
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02072D
_journal_year                    2017
_chemical_formula_sum            'C15 H16 B N6 Re'
_chemical_formula_weight         477.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.507(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2517(4)
_cell_length_b                   10.2422(6)
_cell_length_c                   8.9263(5)
_cell_measurement_reflns_used    4135
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.2970
_cell_measurement_theta_min      2.9820
_cell_volume                     753.69(7)
_computing_cell_refinement       'CrysAlisPro (Oxford, 2007)'
_computing_data_collection       'CrysAlisPro (Oxford, 2007)'
_computing_data_reduction        'CrysAlisPro (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby CCD'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9097
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         32.874
_diffrn_reflns_theta_min         2.284
_exptl_absorpt_coefficient_mu    8.069
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.324
_refine_diff_density_min         -2.491
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0237P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2473
_reflns_number_total             2736
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02072d2.cif
_cod_data_source_block           GIM210616
_cod_database_code               7043692
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.444
_shelx_estimated_absorpt_t_max   0.738
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Re1 Re 0.15231(2) 0.2500 0.51808(2) 0.01627(7) Uani 1 2 d S T P
C1 C 0.0053(7) 0.2500 0.3086(6) 0.0320(15) Uani 1 2 d S T P
H1A H -0.1095 0.2500 0.2947 0.038 Uiso 1 2 calc R U P
C2 C 0.0887(6) 0.1287(5) 0.3186(4) 0.0322(10) Uani 1 1 d . . .
H2A H 0.0320 0.0484 0.3067 0.039 Uiso 1 1 calc R U .
C3 C 0.2596(5) 0.1311(4) 0.3472(4) 0.0269(9) Uani 1 1 d . . .
H3A H 0.3166 0.0509 0.3596 0.032 Uiso 1 1 calc R U .
C4 C 0.3470(7) 0.2500 0.3576(7) 0.0295(14) Uani 1 2 d S T P
H4A H 0.4618 0.2500 0.3714 0.035 Uiso 1 2 calc R U P
C5 C -0.2249(7) 0.2500 0.5964(8) 0.0317(14) Uani 1 2 d S T P
H5A H -0.2650 0.2500 0.4950 0.038 Uiso 1 2 calc R U P
C6 C -0.3210(8) 0.2500 0.7208(8) 0.0362(17) Uani 1 2 d S T P
H6A H -0.4361 0.2500 0.7206 0.043 Uiso 1 2 calc R U P
C7 C -0.2149(8) 0.2500 0.8440(8) 0.0334(15) Uani 1 2 d S T P
H7A H -0.2438 0.2500 0.9459 0.040 Uiso 1 2 calc R U P
C8 C 0.3294(4) 0.0077(4) 0.6884(5) 0.0233(8) Uani 1 1 d . . .
H8 H 0.3724 -0.0280 0.6003 0.028 Uiso 1 1 calc R U .
C9 C 0.3563(5) -0.0429(4) 0.8314(5) 0.0286(9) Uani 1 1 d . . .
H9 H 0.4206 -0.1164 0.8603 0.034 Uiso 1 1 calc R U .
C10 C 0.2694(5) 0.0368(4) 0.9217(5) 0.0292(9) Uani 1 1 d . . .
H10 H 0.2619 0.0278 1.0271 0.035 Uiso 1 1 calc R U .
B1 B 0.1004(9) 0.2500 0.8824(7) 0.0259(14) Uani 1 2 d S T P
H11 H 0.079(8) 0.2500 0.999(7) 0.039 Uiso 1 2 d S U P
N1 N -0.0673(5) 0.2500 0.6410(5) 0.0217(10) Uani 1 2 d S T P
N2 N -0.0625(6) 0.2500 0.7947(5) 0.0241(10) Uani 1 2 d S T P
N3 N 0.2353(4) 0.1126(3) 0.6912(4) 0.0201(6) Uani 1 1 d . . .
N4 N 0.1968(4) 0.1296(4) 0.8368(3) 0.0232(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'
N N 0.0061 0.0033 '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
N1 Re1 C3 137.24(14) . .
N1 Re1 C3 137.24(14) . 4_565
C3 Re1 C3 68.3(2) . 4_565
N1 Re1 N3 83.34(13) . 4_565
C3 Re1 N3 137.38(14) . 4_565
C3 Re1 N3 90.64(14) 4_565 4_565
N1 Re1 N3 83.34(13) . .
C3 Re1 N3 90.64(14) . .
C3 Re1 N3 137.38(14) 4_565 .
N3 Re1 N3 80.46(18) 4_565 .
N1 Re1 C1 89.3(2) . .
C3 Re1 C1 68.07(16) . .
C3 Re1 C1 68.07(16) 4_565 .
N3 Re1 C1 138.86(9) 4_565 .
N3 Re1 C1 138.86(9) . .
N1 Re1 C4 169.9(2) . .
C3 Re1 C4 37.82(13) . .
C3 Re1 C4 37.82(13) 4_565 .
N3 Re1 C4 104.27(15) 4_565 .
N3 Re1 C4 104.27(15) . .
C1 Re1 C4 80.6(2) . .
N1 Re1 C2 103.51(16) . 4_565
C3 Re1 C2 80.77(16) . 4_565
C3 Re1 C2 37.83(17) 4_565 4_565
N3 Re1 C2 105.31(17) 4_565 4_565
N3 Re1 C2 171.37(13) . 4_565
C1 Re1 C2 37.69(15) . 4_565
C4 Re1 C2 68.32(18) . 4_565
N1 Re1 C2 103.51(16) . .
C3 Re1 C2 37.83(17) . .
C3 Re1 C2 80.77(16) 4_565 .
N3 Re1 C2 171.37(13) 4_565 .
N3 Re1 C2 105.31(17) . .
C1 Re1 C2 37.69(15) . .
C4 Re1 C2 68.32(18) . .
C2 Re1 C2 68.2(3) 4_565 .
C2 C1 C2 121.9(5) . 4_565
C2 C1 Re1 72.3(3) . .
C2 C1 Re1 72.3(3) 4_565 .
C2 C1 H1A 119.0 . .
C2 C1 H1A 119.0 4_565 .
Re1 C1 H1A 128.7 . .
C1 C2 C3 118.0(4) . .
C1 C2 Re1 70.0(3) . .
C3 C2 Re1 69.4(2) . .
C1 C2 H2A 121.0 . .
C3 C2 H2A 121.0 . .
Re1 C2 H2A 132.4 . .
C4 C3 C2 121.6(4) . .
C4 C3 Re1 72.1(3) . .
C2 C3 Re1 72.8(2) . .
C4 C3 H3A 119.2 . .
C2 C3 H3A 119.2 . .
Re1 C3 H3A 128.2 . .
C3 C4 C3 118.6(5) . 4_565
C3 C4 Re1 70.0(3) . .
C3 C4 Re1 70.0(3) 4_565 .
C3 C4 H4A 120.7 . .
C3 C4 H4A 120.7 4_565 .
Re1 C4 H4A 132.0 . .
N1 C5 C6 110.0(6) . .
N1 C5 H5A 125.0 . .
C6 C5 H5A 125.0 . .
C7 C6 C5 105.9(5) . .
C7 C6 H6A 127.1 . .
C5 C6 H6A 127.1 . .
N2 C7 C6 107.9(5) . .
N2 C7 H7A 126.0 . .
C6 C7 H7A 126.0 . .
N3 C8 C9 110.8(4) . .
N3 C8 H8 124.6 . .
C9 C8 H8 124.6 . .
C10 C9 C8 104.6(4) . .
C10 C9 H9 127.7 . .
C8 C9 H9 127.7 . .
N4 C10 C9 108.8(4) . .
N4 C10 H10 125.6 . .
C9 C10 H10 125.6 . .
N2 B1 N4 108.6(3) . .
N2 B1 N4 108.6(3) . 4_565
N4 B1 N4 107.2(5) . 4_565
N2 B1 H11 109(4) . .
N4 B1 H11 112(2) . .
N4 B1 H11 112(2) 4_565 .
C5 N1 N2 106.3(5) . .
C5 N1 Re1 132.3(4) . .
N2 N1 Re1 121.4(3) . .
C7 N2 N1 109.9(5) . .
C7 N2 B1 130.1(5) . .
N1 N2 B1 120.0(4) . .
C8 N3 N4 106.4(3) . .
C8 N3 Re1 132.5(3) . .
N4 N3 Re1 121.0(3) . .
C10 N4 N3 109.4(3) . .
C10 N4 B1 130.1(4) . .
N3 N4 B1 120.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 N1 2.159(4) .
Re1 C3 2.171(4) .
Re1 C3 2.171(4) 4_565
Re1 N3 2.178(3) 4_565
Re1 N3 2.178(3) .
Re1 C1 2.184(6) .
Re1 C4 2.198(5) .
Re1 C2 2.215(4) 4_565
Re1 C2 2.215(4) .
C1 C2 1.421(6) .
C1 C2 1.421(6) 4_565
C1 H1A 0.9500 .
C2 C3 1.422(6) .
C2 H2A 0.9500 .
C3 C4 1.416(5) .
C3 H3A 0.9500 .
C4 C3 1.416(5) 4_565
C4 H4A 0.9500 .
C5 N1 1.344(8) .
C5 C6 1.391(8) .
C5 H5A 0.9500 .
C6 C7 1.376(10) .
C6 H6A 0.9500 .
C7 N2 1.351(7) .
C7 H7A 0.9500 .
C8 N3 1.327(5) .
C8 C9 1.386(5) .
C8 H8 0.9500 .
C9 C10 1.372(6) .
C9 H9 0.9500 .
C10 N4 1.340(5) .
C10 H10 0.9500 .
B1 N2 1.526(9) .
B1 N4 1.532(5) .
B1 N4 1.532(5) 4_565
B1 H11 1.06(6) .
N1 N2 1.371(6) .
N3 N4 1.362(4) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 C1 C2 C3 3.2(8) 4_565 .
Re1 C1 C2 C3 -51.8(4) . .
C2 C1 C2 Re1 55.0(5) 4_565 .
C1 C2 C3 C4 -3.3(6) . .
Re1 C2 C3 C4 -55.4(4) . .
C1 C2 C3 Re1 52.1(4) . .
C2 C3 C4 C3 3.4(8) . 4_565
Re1 C3 C4 C3 -52.3(5) . 4_565
C2 C3 C4 Re1 55.7(4) . .
N1 C5 C6 C7 0.000(2) . .
C5 C6 C7 N2 0.000(2) . .
N3 C8 C9 C10 1.2(5) . .
C8 C9 C10 N4 -0.5(5) . .
C6 C5 N1 N2 0.000(1) . .
C6 C5 N1 Re1 180.000(1) . .
C6 C7 N2 N1 0.000(2) . .
C6 C7 N2 B1 180.000(2) . .
C5 N1 N2 C7 0.000(2) . .
Re1 N1 N2 C7 180.000(2) . .
C5 N1 N2 B1 180.000(2) . .
Re1 N1 N2 B1 0.000(2) . .
N4 B1 N2 C7 121.9(3) . .
N4 B1 N2 C7 -121.9(3) 4_565 .
N4 B1 N2 N1 -58.1(3) . .
N4 B1 N2 N1 58.1(3) 4_565 .
C9 C8 N3 N4 -1.4(5) . .
C9 C8 N3 Re1 175.8(3) . .
C9 C10 N4 N3 -0.3(5) . .
C9 C10 N4 B1 -173.2(4) . .
C8 N3 N4 C10 1.0(4) . .
Re1 N3 N4 C10 -176.6(3) . .
C8 N3 N4 B1 174.7(4) . .
Re1 N3 N4 B1 -2.8(5) . .
N2 B1 N4 C10 -128.0(5) . .
N4 B1 N4 C10 114.8(5) 4_565 .
N2 B1 N4 N3 59.7(5) . .
N4 B1 N4 N3 -57.5(6) 4_565 .
