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#$Date: 2019-11-23 12:13:16 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233240 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/86/4348664.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_4348664
loop_
_publ_author_name
'Frei, Angelo'
'Sidler, David'
'Mokolokolo, Pennie'
'Braband, Henrik'
'Fox, Thomas'
'Spingler, Bernhard'
'Roodt, Andreas'
'Alberto, Roger'
_publ_section_title
;
 Kinetics and Mechanism of CO Exchange in fac-[MBr2(solvent)(CO)3](-) (M =
 Re, (99)Tc).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9352
_journal_page_last               9360
_journal_paper_doi               10.1021/acs.inorgchem.6b01503
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C12 H20 Br2 N O4 Re'
_chemical_formula_weight         588.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.754(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3143(3)
_cell_length_b                   20.0387(6)
_cell_length_c                   12.5146(4)
_cell_measurement_reflns_used    7202
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.3870
_cell_measurement_theta_min      2.9380
_cell_volume                     1781.66(11)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2014)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2014)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2014)'
_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    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.810
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    11.315
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.049
_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            colourless
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.244
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         6074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0261P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5270
_reflns_number_total             6074
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01503_si_003.cif
_cod_data_source_block           afx141215
_cod_original_cell_volume        1781.65(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348664
_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   0.078
_shelx_estimated_absorpt_t_max   0.429
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Re1 Re -0.24156(2) 0.45091(2) 0.17351(2) 0.02200(4) Uani 1 1 d . .
C1 C 0.0293(5) 0.47351(16) 0.2406(3) 0.0304(7) Uani 1 1 d . .
C2 C -0.5105(4) 0.42462(14) 0.1309(3) 0.0268(6) Uani 1 1 d . .
C3 C -0.2058(5) 0.44515(14) 0.0272(3) 0.0300(7) Uani 1 1 d . .
C4 C -0.3103(5) 0.54223(14) 0.1522(3) 0.0271(6) Uani 1 1 d . .
C5 C -0.1474(4) 0.64140(14) 0.4842(3) 0.0272(6) Uani 1 1 d . .
H5A H -0.0538 0.6474 0.5550 0.033 Uiso 1 1 calc R U
H5B H -0.2026 0.5963 0.4848 0.033 Uiso 1 1 calc R U
C6 C -0.0462(5) 0.64429(18) 0.3924(3) 0.0381(8) Uani 1 1 d . .
H6C H 0.0189 0.6872 0.3948 0.057 Uiso 1 1 calc R U
H6B H -0.1376 0.6396 0.3215 0.057 Uiso 1 1 calc R U
H6A H 0.0458 0.6079 0.4013 0.057 Uiso 1 1 calc R U
C7 C -0.4545(4) 0.68372(15) 0.3732(3) 0.0305(7) Uani 1 1 d . .
H7B H -0.5498 0.7192 0.3704 0.037 Uiso 1 1 calc R U
H7A H -0.3977 0.6905 0.3096 0.037 Uiso 1 1 calc R U
C8 C -0.5538(5) 0.61710(17) 0.3597(3) 0.0394(8) Uani 1 1 d . .
H8C H -0.6159 0.6104 0.4202 0.059 Uiso 1 1 calc R U
H8B H -0.4618 0.5814 0.3607 0.059 Uiso 1 1 calc R U
H8A H -0.6482 0.6162 0.2895 0.059 Uiso 1 1 calc R U
C9 C -0.2282(4) 0.76292(14) 0.4734(3) 0.0311(7) Uani 1 1 d . .
H9A H -0.1834 0.7677 0.4051 0.037 Uiso 1 1 calc R U
H9B H -0.3341 0.7944 0.4685 0.037 Uiso 1 1 calc R U
C10 C -0.0720(5) 0.78327(16) 0.5686(3) 0.0395(8) Uani 1 1 d . .
H10A H -0.0345 0.8293 0.5580 0.059 Uiso 1 1 calc R U
H10B H 0.0360 0.7535 0.5733 0.059 Uiso 1 1 calc R U
H10C H -0.1152 0.7803 0.6368 0.059 Uiso 1 1 calc R U
C11 C -0.3783(4) 0.68213(15) 0.5788(3) 0.0279(6) Uani 1 1 d . .
H11A H -0.2737 0.6879 0.6448 0.033 Uiso 1 1 calc R U
H11B H -0.4234 0.6356 0.5787 0.033 Uiso 1 1 calc R U
C12 C -0.5371(5) 0.72859(18) 0.5882(3) 0.0400(8) Uani 1 1 d . .
H12A H -0.4886 0.7742 0.6015 0.060 Uiso 1 1 calc R U
H12B H -0.5897 0.7143 0.6496 0.060 Uiso 1 1 calc R U
H12C H -0.6356 0.7273 0.5198 0.060 Uiso 1 1 calc R U
N1 N -0.3023(3) 0.69250(11) 0.4775(2) 0.0230(5) Uani 1 1 d . .
O1 O 0.1786(3) 0.48600(14) 0.2838(2) 0.0468(7) Uani 1 1 d . .
O2 O -0.6646(3) 0.41040(12) 0.1102(2) 0.0406(6) Uani 1 1 d . .
O3 O -0.1830(4) 0.44083(12) -0.0603(2) 0.0457(7) Uani 1 1 d . .
O4 O -0.3536(4) 0.59728(11) 0.1375(2) 0.0400(6) Uani 1 1 d . .
Br1 Br -0.27535(5) 0.45133(2) 0.37729(3) 0.02940(7) Uani 1 1 d . .
Br2 Br -0.14851(4) 0.32352(2) 0.19602(3) 0.03065(8) 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'
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'
Br Br -0.2901 2.4595 '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
C4 Re1 C3 90.89(13)
C4 Re1 C2 90.33(13)
C3 Re1 C2 94.53(14)
C4 Re1 C1 92.47(13)
C3 Re1 C1 93.90(14)
C2 Re1 C1 171.08(13)
C4 Re1 Br1 92.89(10)
C3 Re1 Br1 175.96(9)
C2 Re1 Br1 86.89(9)
C1 Re1 Br1 84.52(9)
C4 Re1 Br2 178.12(10)
C3 Re1 Br2 87.33(9)
C2 Re1 Br2 89.20(8)
C1 Re1 Br2 88.27(9)
Br1 Re1 Br2 88.906(10)
O1 C1 Re1 176.1(3)
O2 C2 Re1 177.5(3)
O3 C3 Re1 179.0(3)
O4 C4 Re1 178.8(3)
C6 C5 N1 115.4(3)
C6 C5 H5A 108.4
N1 C5 H5A 108.4
C6 C5 H5B 108.4
N1 C5 H5B 108.4
H5A C5 H5B 107.5
C5 C6 H6C 109.5
C5 C6 H6B 109.5
H6C C6 H6B 109.5
C5 C6 H6A 109.5
H6C C6 H6A 109.5
H6B C6 H6A 109.5
C8 C7 N1 115.8(3)
C8 C7 H7B 108.3
N1 C7 H7B 108.3
C8 C7 H7A 108.3
N1 C7 H7A 108.3
H7B C7 H7A 107.4
C7 C8 H8C 109.5
C7 C8 H8B 109.5
H8C C8 H8B 109.5
C7 C8 H8A 109.5
H8C C8 H8A 109.5
H8B C8 H8A 109.5
C10 C9 N1 116.0(3)
C10 C9 H9A 108.3
N1 C9 H9A 108.3
C10 C9 H9B 108.3
N1 C9 H9B 108.3
H9A C9 H9B 107.4
C9 C10 H10A 109.5
C9 C10 H10B 109.5
H10A C10 H10B 109.5
C9 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
N1 C11 C12 115.0(3)
N1 C11 H11A 108.5
C12 C11 H11A 108.5
N1 C11 H11B 108.5
C12 C11 H11B 108.5
H11A C11 H11B 107.5
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
C7 N1 C11 111.4(2)
C7 N1 C5 110.9(2)
C11 N1 C5 106.2(2)
C7 N1 C9 106.0(2)
C11 N1 C9 111.2(2)
C5 N1 C9 111.2(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C4 1.900(3)
Re1 C3 1.914(4)
Re1 C2 1.983(3)
Re1 C1 2.011(3)
Re1 Br1 2.6200(4)
Re1 Br2 2.6395(3)
C1 O1 1.125(4)
C2 O2 1.131(4)
C3 O3 1.148(4)
C4 O4 1.150(3)
C5 C6 1.508(5)
C5 N1 1.515(3)
C5 H5A 0.9900
C5 H5B 0.9900
C6 H6C 0.9800
C6 H6B 0.9800
C6 H6A 0.9800
C7 C8 1.510(4)
C7 N1 1.511(4)
C7 H7B 0.9900
C7 H7A 0.9900
C8 H8C 0.9800
C8 H8B 0.9800
C8 H8A 0.9800
C9 C10 1.498(5)
C9 N1 1.517(4)
C9 H9A 0.9900
C9 H9B 0.9900
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 N1 1.514(4)
C11 C12 1.515(4)
C11 H11A 0.9900
C11 H11B 0.9900
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
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
C8 C7 N1 C11 -57.5(3)
C8 C7 N1 C5 60.6(3)
C8 C7 N1 C9 -178.6(3)
C12 C11 N1 C7 -58.9(3)
C12 C11 N1 C5 -179.8(3)
C12 C11 N1 C9 59.1(3)
C6 C5 N1 C7 60.8(3)
C6 C5 N1 C11 -178.0(3)
C6 C5 N1 C9 -56.8(4)
C10 C9 N1 C7 -179.1(3)
C10 C9 N1 C11 59.6(3)
C10 C9 N1 C5 -58.6(4)
