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#$Date: 2020-04-05 13:47:37 +0300 (Sun, 05 Apr 2020) $
#$Revision: 250285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/35/7703524.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_7703524
loop_
_publ_author_name
'Bonfiglio, Anna'
'Magra, Kévin'
'Cebrián, Cristina'
'Polo, Federico'
'Gros, Philippe C.'
'Mercandelli, Pierluigi'
'Mauro, Matteo'
_publ_section_title
;
 Red-emitting neutral rhenium(i) complexes bearing a pyridyl
 pyridoannelated N-heterocyclic carbene.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3102
_journal_page_last               3111
_journal_paper_doi               10.1039/c9dt04890a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C15 H9 Br N3 O3 Re'
_chemical_formula_sum            'C15 H9 Br N3 O3 Re'
_chemical_formula_weight         545.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-01-30 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                88.7910(10)
_cell_angle_beta                 76.4800(10)
_cell_angle_gamma                72.1440(10)
_cell_formula_units_Z            2
_cell_length_a                   6.7338(3)
_cell_length_b                   10.8986(4)
_cell_length_c                   11.3120(5)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.63
_cell_volume                     767.14(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            54752
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.168
_diffrn_reflns_theta_min         1.966
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_exptl_absorpt_coefficient_mu    10.542
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.361
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.362
_refine_diff_density_min         -1.941
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0295
_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)+(0.0144P)²+5.6487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3829
_reflns_number_total             4137
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04890a2.cif
_cod_data_source_block           mmab191219
_cod_depositor_comments
'Adding full bibliography for 7703523--7703524.cif.'
_cod_database_code               7703524
_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   0.253
_shelx_estimated_absorpt_t_max   0.364
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2704(8) 0.9477(5) 0.5186(5) 0.0209(9) Uani 1 1 d . . . . .
H1 H 0.1578 0.9908 0.5859 0.025 Uiso 1 1 calc R U . . .
C2 C 0.3014(9) 1.0042(5) 0.4117(5) 0.0261(10) Uani 1 1 d . . . . .
H2 H 0.2080 1.0876 0.4035 0.031 Uiso 1 1 calc R U . . .
C3 C 0.4734(9) 0.9406(6) 0.3096(5) 0.0287(11) Uani 1 1 d . . . . .
H3 H 0.4923 0.9828 0.2353 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6071(8) 0.8227(5) 0.3176(4) 0.0251(10) Uani 1 1 d . . . . .
H4 H 0.7215 0.7820 0.2501 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5758(7) 0.7588(5) 0.4287(4) 0.0206(9) Uani 1 1 d . . . . .
C6 C 0.6683(8) 0.6403(5) 0.4665(4) 0.0210(9) Uani 1 1 d . . . . .
H6 H 0.7862 0.5730 0.4207 0.025 Uiso 1 1 calc R U . . .
C7 C 0.3955(7) 0.7514(4) 0.6259(4) 0.0178(8) Uani 1 1 d . . . . .
C8 C 0.5851(7) 0.5339(4) 0.6632(4) 0.0180(9) Uani 1 1 d . . . . .
C9 C 0.7475(8) 0.4185(5) 0.6292(5) 0.0231(10) Uani 1 1 d . . . . .
H9 H 0.8456 0.4050 0.5517 0.028 Uiso 1 1 calc R U . . .
C10 C 0.7619(9) 0.3229(5) 0.7124(5) 0.0272(11) Uani 1 1 d . . . . .
H10 H 0.8726 0.2425 0.6934 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6137(9) 0.3456(5) 0.8234(5) 0.0283(11) Uani 1 1 d . . . . .
H11 H 0.6204 0.2808 0.8811 0.034 Uiso 1 1 calc R U . . .
C12 C 0.4558(9) 0.4638(5) 0.8494(5) 0.0254(10) Uani 1 1 d . . . . .
H12 H 0.3541 0.4784 0.9257 0.030 Uiso 1 1 calc R U . . .
C13 C 0.0220(8) 0.9307(5) 0.8223(4) 0.0238(10) Uani 1 1 d . . . . .
C14 C 0.0388(8) 0.7220(5) 0.9618(5) 0.0263(10) Uani 1 1 d . . . . .
C15 C 0.3869(8) 0.8136(5) 0.8835(4) 0.0233(10) Uani 1 1 d . . . . .
N1 N 0.4072(6) 0.8243(4) 0.5283(3) 0.0181(7) Uani 1 1 d . . . . .
N2 N 0.5557(6) 0.6375(4) 0.5852(3) 0.0174(7) Uani 1 1 d . . . . .
N3 N 0.4397(6) 0.5598(4) 0.7707(4) 0.0195(8) Uani 1 1 d . . . . .
O1 O -0.0825(7) 1.0377(4) 0.8318(4) 0.0369(9) Uani 1 1 d . . . . .
O2 O -0.0609(7) 0.6990(5) 1.0517(4) 0.0427(11) Uani 1 1 d . . . . .
O3 O 0.4901(6) 0.8507(4) 0.9323(3) 0.0297(8) Uani 1 1 d . . . . .
Br1 Br -0.03486(8) 0.66548(5) 0.70294(5) 0.02731(11) Uani 1 1 d . . . . .
Re1 Re 0.20602(3) 0.75565(2) 0.80595(2) 0.01832(6) 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 C1 N1 118.6(5) . . ?
C2 C1 H1 120.7 . . ?
N1 C1 H1 120.7 . . ?
C1 C2 C3 121.2(5) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C4 C3 C2 121.0(5) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 119.3(5) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 N1 106.2(4) . . ?
C6 C5 C4 135.2(5) . . ?
N1 C5 C4 118.6(5) . . ?
C5 C6 N2 106.0(4) . . ?
C5 C6 H6 127.0 . . ?
N2 C6 H6 127.0 . . ?
N1 C7 N2 103.3(4) . . ?
N1 C7 Re1 140.7(3) . . ?
N2 C7 Re1 115.8(3) . . ?
N3 C8 C9 124.7(4) . . ?
N3 C8 N2 113.2(4) . . ?
C9 C8 N2 122.1(4) . . ?
C8 C9 C10 117.5(5) . . ?
C8 C9 H9 121.2 . . ?
C10 C9 H9 121.2 . . ?
C11 C10 C9 119.4(5) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C12 C11 C10 119.1(5) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N3 C12 C11 122.8(5) . . ?
N3 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
O1 C13 Re1 177.5(5) . . ?
O2 C14 Re1 177.8(5) . . ?
O3 C15 Re1 177.9(5) . . ?
C7 N1 C1 126.8(4) . . ?
C7 N1 C5 111.8(4) . . ?
C1 N1 C5 121.4(4) . . ?
C7 N2 C6 112.7(4) . . ?
C7 N2 C8 119.3(4) . . ?
C6 N2 C8 128.0(4) . . ?
C8 N3 C12 116.4(4) . . ?
C8 N3 Re1 117.5(3) . . ?
C12 N3 Re1 126.0(3) . . ?
C15 Re1 C13 87.4(2) . . ?
C15 Re1 C14 91.9(2) . . ?
C13 Re1 C14 89.8(2) . . ?
C15 Re1 C7 95.33(19) . . ?
C13 Re1 C7 100.16(19) . . ?
C14 Re1 C7 167.9(2) . . ?
C15 Re1 N3 91.48(18) . . ?
C13 Re1 N3 174.05(18) . . ?
C14 Re1 N3 96.07(19) . . ?
C7 Re1 N3 74.11(16) . . ?
C15 Re1 Br1 177.35(16) . . ?
C13 Re1 Br1 95.01(15) . . ?
C14 Re1 Br1 87.03(15) . . ?
C7 Re1 Br1 85.31(12) . . ?
N3 Re1 Br1 86.22(10) . . ?
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
C1 C2 1.347(7) . ?
C1 N1 1.396(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.440(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.339(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.428(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.359(7) . ?
C5 N1 1.416(6) . ?
C6 N2 1.384(6) . ?
C6 H6 0.9500 . ?
C7 N1 1.349(6) . ?
C7 N2 1.374(6) . ?
C7 Re1 2.129(4) . ?
C8 N3 1.344(6) . ?
C8 C9 1.381(7) . ?
C8 N2 1.411(6) . ?
C9 C10 1.385(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(8) . ?
C11 H11 0.9500 . ?
C12 N3 1.355(6) . ?
C12 H12 0.9500 . ?
C13 O1 1.154(6) . ?
C13 Re1 1.915(5) . ?
C14 O2 1.150(6) . ?
C14 Re1 1.951(5) . ?
C15 O3 1.146(6) . ?
C15 Re1 1.910(5) . ?
N3 Re1 2.208(4) . ?
Br1 Re1 2.6199(5) . ?
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
N1 C1 C2 C3 -0.9(7) . . . . ?
C1 C2 C3 C4 0.4(8) . . . . ?
C2 C3 C4 C5 1.0(7) . . . . ?
C3 C4 C5 C6 175.4(5) . . . . ?
C3 C4 C5 N1 -1.8(7) . . . . ?
N1 C5 C6 N2 0.0(5) . . . . ?
C4 C5 C6 N2 -177.5(5) . . . . ?
N3 C8 C9 C10 -0.4(7) . . . . ?
N2 C8 C9 C10 -179.8(4) . . . . ?
C8 C9 C10 C11 1.1(7) . . . . ?
C9 C10 C11 C12 -0.7(8) . . . . ?
C10 C11 C12 N3 -0.4(8) . . . . ?
N2 C7 N1 C1 175.9(4) . . . . ?
Re1 C7 N1 C1 0.7(8) . . . . ?
N2 C7 N1 C5 -1.6(5) . . . . ?
Re1 C7 N1 C5 -176.9(4) . . . . ?
C2 C1 N1 C7 -177.3(4) . . . . ?
C2 C1 N1 C5 0.0(7) . . . . ?
C6 C5 N1 C7 1.1(5) . . . . ?
C4 C5 N1 C7 179.0(4) . . . . ?
C6 C5 N1 C1 -176.6(4) . . . . ?
C4 C5 N1 C1 1.3(6) . . . . ?
N1 C7 N2 C6 1.6(5) . . . . ?
Re1 C7 N2 C6 178.3(3) . . . . ?
N1 C7 N2 C8 -177.2(4) . . . . ?
Re1 C7 N2 C8 -0.6(5) . . . . ?
C5 C6 N2 C7 -1.0(5) . . . . ?
C5 C6 N2 C8 177.7(4) . . . . ?
N3 C8 N2 C7 2.7(6) . . . . ?
C9 C8 N2 C7 -177.8(4) . . . . ?
N3 C8 N2 C6 -175.9(4) . . . . ?
C9 C8 N2 C6 3.5(7) . . . . ?
C9 C8 N3 C12 -0.6(7) . . . . ?
N2 C8 N3 C12 178.9(4) . . . . ?
C9 C8 N3 Re1 177.0(4) . . . . ?
N2 C8 N3 Re1 -3.5(5) . . . . ?
C11 C12 N3 C8 1.0(7) . . . . ?
C11 C12 N3 Re1 -176.4(4) . . . . ?
