#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:52:20 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262597 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/64/7706401.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_7706401
loop_
_publ_author_name
'Henke, Wade C.'
'Kerr, Tyler A.'
'Sheridan, Thomas R.'
'Henling, Lawrence M.'
'Takase, Michael K.'
'Day, Victor W.'
'Gray, Harry B.'
'Blakemore, James D.'
_publ_section_title
;
 Synthesis, structural studies, and redox chemistry of bimetallic
 [Mn(CO)₃] and [Re(CO)₃] complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2746
_journal_page_last               2756
_journal_paper_doi               10.1039/d0dt03666h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C11 H6 Cl N4 O3 Re'
_chemical_formula_sum            'C11 H6 Cl N4 O3 Re'
_chemical_formula_weight         463.85
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2021-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.408(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2872(3)
_cell_length_b                   14.9679(7)
_cell_length_c                   13.4775(7)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100
_cell_measurement_theta_max      49.15
_cell_measurement_theta_min      2.72
_cell_volume                     1238.69(11)
_computing_cell_refinement       'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2014.11-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.992
_diffrn_reflns_theta_min         2.060
_exptl_absorpt_coefficient_mu    10.038
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1152 before and 0.0658 after correction. The Ratio of minimum to maximum transmission is 0.6301. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.487
_exptl_crystal_description       blade
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+3.5069P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3459
_reflns_number_total             3602
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03666h3.cif
_cod_data_source_block           cmpd1_a15100
_cod_depositor_comments
'Adding full bibliography for 7706395--7706401.cif.'
_cod_database_code               7706401
_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_max   0.824
_shelx_estimated_absorpt_t_min   0.108
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(Cl1)
3. Others
 Sof(Cl1A)=Sof(O3A)=Sof(C11A)=1-FVAR(1)
 Sof(Cl1)=Sof(O3)=Sof(C11)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.61838(2) 0.34643(2) 0.37847(2) 0.01147(4) Uani 1 1 d . . . . .
Cl1 Cl 0.73492(13) 0.29884(6) 0.22178(7) 0.0144(3) Uani 0.944(6) 1 d . . P A 1
Cl1A Cl 0.534(4) 0.3804(18) 0.5330(19) 0.019(6) Uiso 0.056(6) 1 d . . P A 2
O1 O 0.9161(4) 0.51031(16) 0.39549(18) 0.0194(5) Uani 1 1 d . . . . .
O2 O 0.2390(4) 0.46228(18) 0.26640(19) 0.0220(5) Uani 1 1 d . . . . .
O3 O 0.4983(5) 0.39777(19) 0.5797(3) 0.0221(6) Uani 0.944(6) 1 d . . P A 1
O3A O 0.763(9) 0.303(4) 0.174(5) 0.029(12) Uiso 0.056(6) 1 d . . P A 2
N1 N 0.8539(4) 0.25057(17) 0.45785(19) 0.0115(4) Uani 1 1 d . . . . .
N2 N 0.4501(4) 0.21884(17) 0.36027(19) 0.0116(4) Uani 1 1 d . . . . .
N3 N 0.9158(4) 0.09581(18) 0.4928(2) 0.0147(5) Uani 1 1 d . . . . .
N4 N 0.4970(4) 0.06218(18) 0.3881(2) 0.0156(5) Uani 1 1 d . . . . .
C1 C 1.0532(5) 0.2694(2) 0.5130(2) 0.0138(5) Uani 1 1 d . . . . .
H1 H 1.0997 0.3299 0.5208 0.017 Uiso 1 1 calc R U . . .
C2 C 1.1917(5) 0.2028(2) 0.5586(2) 0.0142(5) Uani 1 1 d . . . . .
H2 H 1.3324 0.2162 0.5980 0.017 Uiso 1 1 calc R U . . .
C3 C 1.1179(5) 0.1153(2) 0.5448(2) 0.0160(6) Uani 1 1 d . . . . .
H3 H 1.2126 0.0680 0.5728 0.019 Uiso 1 1 calc R U . . .
C4 C 0.7936(5) 0.1639(2) 0.4529(2) 0.0126(5) Uani 1 1 d . . . . .
C5 C 0.5674(5) 0.1459(2) 0.3969(2) 0.0125(5) Uani 1 1 d . . . . .
C6 C 0.2905(5) 0.0498(2) 0.3384(2) 0.0172(6) Uani 1 1 d . . . . .
H6 H 0.2335 -0.0092 0.3314 0.021 Uiso 1 1 calc R U . . .
C7 C 0.1578(5) 0.1198(2) 0.2968(2) 0.0163(6) Uani 1 1 d . . . . .
H7 H 0.0126 0.1097 0.2607 0.020 Uiso 1 1 calc R U . . .
C8 C 0.2436(5) 0.2050(2) 0.3098(2) 0.0139(5) Uani 1 1 d . . . . .
H8 H 0.1556 0.2545 0.2827 0.017 Uiso 1 1 calc R U . . .
C9 C 0.8034(5) 0.4497(2) 0.3905(2) 0.0154(6) Uani 1 1 d . . . . .
C10 C 0.3832(5) 0.4197(2) 0.3067(2) 0.0147(5) Uani 1 1 d . . . . .
C11 C 0.5416(7) 0.3777(3) 0.5024(5) 0.0160(9) Uani 0.944(6) 1 d . . P A 1
C11A C 0.713(10) 0.319(5) 0.256(6) 0.0144(3) Uani 0.056(6) 1 d . . P A 2
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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.1880
1.00 0.00 -1.00 0.1790
0.00 0.00 1.00 0.0160
0.00 0.00 -1.00 0.0270
0.00 -1.00 0.00 0.0070
0.00 1.00 0.00 0.0080
1.00 1.00 -5.00 0.0760
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
N1 Re1 Cl1 86.27(7) . . ?
N1 Re1 Cl1A 88.0(6) . . ?
N1 Re1 N2 74.85(9) . . ?
N2 Re1 Cl1 82.96(7) . . ?
N2 Re1 Cl1A 95.4(6) . . ?
C9 Re1 Cl1 91.06(10) . . ?
C9 Re1 Cl1A 90.0(6) . . ?
C9 Re1 N1 98.84(11) . . ?
C9 Re1 N2 171.52(11) . . ?
C9 Re1 C10 88.28(13) . . ?
C9 Re1 C11A 87(2) . . ?
C10 Re1 Cl1 94.09(10) . . ?
C10 Re1 Cl1A 91.6(6) . . ?
C10 Re1 N1 172.86(11) . . ?
C10 Re1 N2 98.10(11) . . ?
C11 Re1 Cl1 176.54(13) . . ?
C11 Re1 N1 90.27(15) . . ?
C11 Re1 N2 96.12(14) . . ?
C11 Re1 C9 89.50(16) . . ?
C11 Re1 C10 89.34(16) . . ?
C11A Re1 Cl1A 175.3(19) . . ?
C11A Re1 N1 88.8(19) . . ?
C11A Re1 N2 87(2) . . ?
C11A Re1 C10 92.1(18) . . ?
C1 N1 Re1 126.2(2) . . ?
C1 N1 C4 116.7(3) . . ?
C4 N1 Re1 117.14(19) . . ?
C5 N2 Re1 117.06(19) . . ?
C8 N2 Re1 125.9(2) . . ?
C8 N2 C5 116.9(3) . . ?
C4 N3 C3 116.6(3) . . ?
C5 N4 C6 116.4(3) . . ?
N1 C1 H1 119.3 . . ?
N1 C1 C2 121.3(3) . . ?
C2 C1 H1 119.3 . . ?
C1 C2 H2 121.3 . . ?
C1 C2 C3 117.5(3) . . ?
C3 C2 H2 121.3 . . ?
N3 C3 C2 121.7(3) . . ?
N3 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
N1 C4 C5 115.4(3) . . ?
N3 C4 N1 126.1(3) . . ?
N3 C4 C5 118.5(3) . . ?
N2 C5 C4 115.3(3) . . ?
N4 C5 N2 125.8(3) . . ?
N4 C5 C4 118.8(3) . . ?
N4 C6 H6 118.9 . . ?
N4 C6 C7 122.2(3) . . ?
C7 C6 H6 118.9 . . ?
C6 C7 H7 121.2 . . ?
C8 C7 C6 117.7(3) . . ?
C8 C7 H7 121.2 . . ?
N2 C8 C7 120.9(3) . . ?
N2 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
O1 C9 Re1 178.1(3) . . ?
O2 C10 Re1 177.6(3) . . ?
O3 C11 Re1 178.6(4) . . ?
O3A C11A Re1 177(5) . . ?
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 Cl1 2.4837(10) . ?
Re1 Cl1A 2.31(3) . ?
Re1 N1 2.171(2) . ?
Re1 N2 2.172(3) . ?
Re1 C9 1.920(3) . ?
Re1 C10 1.926(3) . ?
Re1 C11 1.894(6) . ?
Re1 C11A 1.92(8) . ?
O1 C9 1.145(4) . ?
O2 C10 1.146(4) . ?
O3 C11 1.171(7) . ?
O3A C11A 1.23(11) . ?
N1 C1 1.342(4) . ?
N1 C4 1.349(4) . ?
N2 C5 1.351(4) . ?
N2 C8 1.346(4) . ?
N3 C3 1.345(4) . ?
N3 C4 1.320(4) . ?
N4 C5 1.326(4) . ?
N4 C6 1.340(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.379(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.484(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(4) . ?
C8 H8 0.9500 . ?
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
Re1 N1 C1 C2 -178.6(2) . . . . ?
Re1 N1 C4 N3 177.5(2) . . . . ?
Re1 N1 C4 C5 -2.7(3) . . . . ?
Re1 N2 C5 N4 -176.1(2) . . . . ?
Re1 N2 C5 C4 4.9(3) . . . . ?
Re1 N2 C8 C7 175.3(2) . . . . ?
N1 C1 C2 C3 0.4(5) . . . . ?
N1 C4 C5 N2 -1.4(4) . . . . ?
N1 C4 C5 N4 179.5(3) . . . . ?
N3 C4 C5 N2 178.4(3) . . . . ?
N3 C4 C5 N4 -0.7(4) . . . . ?
N4 C6 C7 C8 -1.2(5) . . . . ?
C1 N1 C4 N3 -3.6(5) . . . . ?
C1 N1 C4 C5 176.2(3) . . . . ?
C1 C2 C3 N3 -2.8(5) . . . . ?
C3 N3 C4 N1 1.2(5) . . . . ?
C3 N3 C4 C5 -178.6(3) . . . . ?
C4 N1 C1 C2 2.6(4) . . . . ?
C4 N3 C3 C2 2.1(5) . . . . ?
C5 N2 C8 C7 0.2(4) . . . . ?
C5 N4 C6 C7 0.9(5) . . . . ?
C6 N4 C5 N2 0.0(5) . . . . ?
C6 N4 C5 C4 178.9(3) . . . . ?
C6 C7 C8 N2 0.7(5) . . . . ?
C8 N2 C5 N4 -0.5(5) . . . . ?
C8 N2 C5 C4 -179.5(3) . . . . ?
