#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:29:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179751 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/47/7004756.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_7004756
loop_
_publ_author_name
'Zobi, Fabio'
'Spingler, Bernhard'
'Alberto, Roger'
_publ_section_title
;
 Ligand-mediated decarbonylation as an efficient synthetic method to
 Re(i) and Re(ii) dicarbonyl complexes
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              5287
_journal_page_last               5289
_journal_paper_doi               10.1039/b811766g
_journal_year                    2008
_chemical_formula_sum            'C6 H13 Br N3 O2 Re'
_chemical_formula_weight         425.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.295(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1668(1)
_cell_length_b                   12.1894(3)
_cell_length_c                   11.8617(2)
_cell_measurement_reflns_used    5057
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      34.6759
_cell_measurement_theta_min      2.4292
_cell_volume                     1004.14(3)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '/o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9092
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    16.054
_exptl_absorpt_correction_T_max  0.38000
_exptl_absorpt_correction_T_min  0.06421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.883
_refine_diff_density_min         -2.761
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0329
_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)+(0.0431P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                3024
_reflns_number_total             3808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811766g.txt
_cod_data_source_block           fz250308
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7004756
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.76405(2) 0.152177(14) 0.366181(14) 0.01484(6) Uani 1 1 d . . .
Br1 Br 0.71987(7) 0.11156(4) 0.57284(4) 0.02262(11) Uani 1 1 d . . .
C1 C 1.0278(7) 0.1854(4) 0.4108(4) 0.0205(9) Uani 1 1 d . . .
C2 C 0.7292(6) 0.3034(5) 0.3657(4) 0.0208(10) Uani 1 1 d . . .
C3 C 0.3965(7) 0.1661(4) 0.1802(4) 0.0222(10) Uani 1 1 d . . .
H3A H 0.4046 0.2470 0.1865 0.027 Uiso 1 1 calc R . .
H3B H 0.2626 0.1458 0.1405 0.027 Uiso 1 1 calc R . .
C4 C 0.5342(7) 0.1240(4) 0.1118(4) 0.0200(9) Uani 1 1 d . . .
H4A H 0.5033 0.0466 0.0895 0.024 Uiso 1 1 calc R . .
H4B H 0.5187 0.1675 0.0395 0.024 Uiso 1 1 calc R . .
C5 C 0.8522(7) 0.0336(4) 0.1651(4) 0.0232(10) Uani 1 1 d . . .
H5A H 0.9914 0.0490 0.1948 0.028 Uiso 1 1 calc R . .
H5B H 0.8274 0.0161 0.0812 0.028 Uiso 1 1 calc R . .
C6 C 0.7962(8) -0.0622(4) 0.2295(4) 0.0255(10) Uani 1 1 d . . .
H6A H 0.6636 -0.0860 0.1912 0.031 Uiso 1 1 calc R . .
H6B H 0.8844 -0.1246 0.2288 0.031 Uiso 1 1 calc R . .
N1 N 0.4510(6) 0.1160(4) 0.2972(3) 0.0207(8) Uani 1 1 d . . .
H1C H 0.4299 0.0415 0.2927 0.025 Uiso 1 1 calc R . .
H1D H 0.3804 0.1461 0.3446 0.025 Uiso 1 1 calc R . .
N2 N 0.7381(6) 0.1318(3) 0.1819(3) 0.0191(8) Uani 1 1 d . . .
H2C H 0.7935 0.1928 0.1560 0.023 Uiso 1 1 calc R . .
N3 N 0.8070(6) -0.0285(4) 0.3510(3) 0.0218(8) Uani 1 1 d . . .
H3C H 0.9253 -0.0478 0.3973 0.026 Uiso 1 1 calc R . .
H3D H 0.7143 -0.0654 0.3776 0.026 Uiso 1 1 calc R . .
O1 O 1.1896(5) 0.2103(3) 0.4388(3) 0.0275(8) Uani 1 1 d . . .
O2 O 0.7153(6) 0.4000(3) 0.3647(3) 0.0293(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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Re1 C1 85.0(2) . . ?
C2 Re1 N2 97.62(17) . . ?
C1 Re1 N2 97.99(17) . . ?
C2 Re1 N1 94.15(18) . . ?
C1 Re1 N1 175.02(17) . . ?
N2 Re1 N1 77.25(15) . . ?
C2 Re1 N3 175.14(17) . . ?
C1 Re1 N3 94.93(19) . . ?
N2 Re1 N3 77.57(15) . . ?
N1 Re1 N3 85.53(16) . . ?
C2 Re1 Br1 98.30(14) . . ?
C1 Re1 Br1 97.13(14) . . ?
N2 Re1 Br1 158.89(11) . . ?
N1 Re1 Br1 87.85(10) . . ?
N3 Re1 Br1 86.54(10) . . ?
O1 C1 Re1 177.3(5) . . ?
O2 C2 Re1 177.0(4) . . ?
N1 C3 C4 107.9(4) . . ?
N1 C3 H3A 110.1 . . ?
C4 C3 H3A 110.1 . . ?
N1 C3 H3B 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
N2 C4 C3 110.9(4) . . ?
N2 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 109.4(4) . . ?
N2 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N2 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N3 C6 C5 108.8(4) . . ?
N3 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N3 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C3 N1 Re1 105.7(3) . . ?
C3 N1 H1C 110.6 . . ?
Re1 N1 H1C 110.6 . . ?
C3 N1 H1D 110.6 . . ?
Re1 N1 H1D 110.6 . . ?
H1C N1 H1D 108.7 . . ?
C5 N2 C4 111.6(4) . . ?
C5 N2 Re1 108.3(3) . . ?
C4 N2 Re1 113.5(3) . . ?
C5 N2 H2C 107.8 . . ?
C4 N2 H2C 107.8 . . ?
Re1 N2 H2C 107.8 . . ?
C6 N3 Re1 112.1(3) . . ?
C6 N3 H3C 109.2 . . ?
Re1 N3 H3C 109.2 . . ?
C6 N3 H3D 109.2 . . ?
Re1 N3 H3D 109.2 . . ?
H3C N3 H3D 107.9 . . ?
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 1.859(6) . ?
Re1 C1 1.877(5) . ?
Re1 N2 2.162(4) . ?
Re1 N1 2.234(4) . ?
Re1 N3 2.237(4) . ?
Re1 Br1 2.5958(5) . ?
C1 O1 1.165(6) . ?
C2 O2 1.182(7) . ?
C3 N1 1.478(6) . ?
C3 C4 1.515(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N2 1.495(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.490(6) . ?
C5 C6 1.504(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N3 1.482(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N1 H1C 0.9200 . ?
N1 H1D 0.9200 . ?
N2 H2C 0.9300 . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Re1 C1 O1 5(9) . . . . ?
N2 Re1 C1 O1 102(9) . . . . ?
N1 Re1 C1 O1 85(9) . . . . ?
N3 Re1 C1 O1 -180(100) . . . . ?
Br1 Re1 C1 O1 -92(9) . . . . ?
C1 Re1 C2 O2 23(7) . . . . ?
N2 Re1 C2 O2 -74(7) . . . . ?
N1 Re1 C2 O2 -152(7) . . . . ?
N3 Re1 C2 O2 -66(8) . . . . ?
Br1 Re1 C2 O2 120(7) . . . . ?
N1 C3 C4 N2 -47.4(5) . . . . ?
N2 C5 C6 N3 -51.1(5) . . . . ?
C4 C3 N1 Re1 53.2(4) . . . . ?
C2 Re1 N1 C3 63.0(3) . . . . ?
C1 Re1 N1 C3 -17(2) . . . . ?
N2 Re1 N1 C3 -33.9(3) . . . . ?
N3 Re1 N1 C3 -112.2(3) . . . . ?
Br1 Re1 N1 C3 161.2(3) . . . . ?
C6 C5 N2 C4 -74.4(5) . . . . ?
C6 C5 N2 Re1 51.2(4) . . . . ?
C3 C4 N2 C5 139.9(4) . . . . ?
C3 C4 N2 Re1 17.2(5) . . . . ?
C2 Re1 N2 C5 152.1(3) . . . . ?
C1 Re1 N2 C5 66.1(3) . . . . ?
N1 Re1 N2 C5 -115.4(3) . . . . ?
N3 Re1 N2 C5 -27.2(3) . . . . ?
Br1 Re1 N2 C5 -69.2(4) . . . . ?
C2 Re1 N2 C4 -83.5(3) . . . . ?
C1 Re1 N2 C4 -169.4(3) . . . . ?
N1 Re1 N2 C4 9.1(3) . . . . ?
N3 Re1 N2 C4 97.2(3) . . . . ?
Br1 Re1 N2 C4 55.2(5) . . . . ?
C5 C6 N3 Re1 26.4(5) . . . . ?
C2 Re1 N3 C6 -8(2) . . . . ?
C1 Re1 N3 C6 -96.8(3) . . . . ?
N2 Re1 N3 C6 0.3(3) . . . . ?
N1 Re1 N3 C6 78.2(3) . . . . ?
Br1 Re1 N3 C6 166.4(3) . . . . ?
