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#$Date: 2022-03-30 10:24:21 +0300 (Wed, 30 Mar 2022) $
#$Revision: 274100 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/49/8104937.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.
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data_8104937
loop_
_publ_author_name
'Jacobs, Francois J. F.'
'Brink, Alice'
_publ_section_title
;
 Crystal structure of fac-tricarbonyl-(nitrato-k1
 O)-bis(pyridine-\kN)-rhenium, C13H10O6N3Re
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              253
_journal_page_last               255
_journal_paper_doi               10.1515/ncrs-2020-0475
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C13 H10 N3 O6 Re'
_chemical_formula_sum            'C13 H10 N3 O6 Re'
_chemical_formula_weight         490.44
_chemical_name_systematic
fac-Tricarbonyl-(nitrato)-bis(pyridine-N)-rhenium
_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     'intrinsic phasing'
_cell_angle_alpha                90
_cell_angle_beta                 92.637(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9325(9)
_cell_length_b                   13.8112(16)
_cell_length_c                   13.4577(15)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    101.0
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.57
_cell_volume                     1472.8(3)
_computing_cell_refinement       'Apex3 (Bruker AXS Inc., 2016)'
_computing_data_collection       'Apex3 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'Apex3 (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Mercury 4.0 (MacRae et al., 2020)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 Quest Eco Chi Photon II CPAD diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.286
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int)
 was 0.1079 before and 0.0779 after correction. The Ratio of minimum to 
 maximum transmission is 0.8069. The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0249
_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)+3.2025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3221
_reflns_number_total             3551
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0475_suppl.cif
_cod_data_source_block           q1_20ffj4_0m
_cod_database_code               8104937
_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   0.529
_shelx_estimated_absorpt_t_min   0.436
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13)
;
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 0.82346(2) 0.60717(2) 0.23467(2) 0.01993(6) Uani 1 1 d . . . . .
O1 O 0.9999(4) 0.7809(2) 0.3355(3) 0.0446(8) Uani 1 1 d . . . . .
O2 O 0.8813(4) 0.7187(3) 0.0431(2) 0.0434(8) Uani 1 1 d . . . . .
O3 O 1.1633(4) 0.5106(2) 0.2097(3) 0.0400(8) Uani 1 1 d . . . . .
O4 O 0.5694(3) 0.65047(19) 0.2630(2) 0.0259(6) Uani 1 1 d . . . . .
O5 O 0.5590(4) 0.7776(2) 0.1658(2) 0.0408(8) Uani 1 1 d . . . . .
O6 O 0.3334(4) 0.7254(3) 0.2329(3) 0.0407(8) Uani 1 1 d . . . . .
N1 N 0.6918(4) 0.4887(2) 0.1523(2) 0.0203(6) Uani 1 1 d . . . . .
N2 N 0.7788(4) 0.5261(2) 0.3727(2) 0.0204(6) Uani 1 1 d . . . . .
N3 N 0.4848(4) 0.7193(2) 0.2186(3) 0.0266(7) Uani 1 1 d . . . . .
C1 C 0.9329(5) 0.7147(3) 0.3013(3) 0.0279(9) Uani 1 1 d . . . . .
C2 C 0.8561(5) 0.6769(3) 0.1148(3) 0.0297(9) Uani 1 1 d . . . . .
C3 C 1.0357(5) 0.5481(3) 0.2198(3) 0.0249(8) Uani 1 1 d . . . . .
C4 C 0.7270(6) 0.5722(3) 0.4530(3) 0.0285(9) Uani 1 1 d . . . . .
H4 H 0.703536 0.639508 0.448206 0.034 Uiso 1 1 calc R . . . .
C5 C 0.7061(6) 0.5265(3) 0.5426(3) 0.0349(10) Uani 1 1 d . . . . .
H5 H 0.669290 0.562043 0.598025 0.042 Uiso 1 1 calc R . . . .
C6 C 0.7389(6) 0.4287(3) 0.5512(3) 0.0315(9) Uani 1 1 d . . . . .
H6 H 0.725332 0.395332 0.612100 0.038 Uiso 1 1 calc R . . . .
C7 C 0.7924(6) 0.3809(3) 0.4680(4) 0.0353(10) Uani 1 1 d . . . . .
H7 H 0.816355 0.313577 0.471064 0.042 Uiso 1 1 calc R . . . .
C8 C 0.8107(5) 0.4309(3) 0.3811(3) 0.0285(9) Uani 1 1 d . . . . .
H8 H 0.847268 0.396869 0.324635 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5407(5) 0.4549(3) 0.1772(3) 0.0275(8) Uani 1 1 d . . . . .
H9 H 0.491407 0.480334 0.234745 0.033 Uiso 1 1 calc R . . . .
C10 C 0.4537(6) 0.3844(3) 0.1223(3) 0.0310(9) Uani 1 1 d . . . . .
H10 H 0.347529 0.361627 0.142356 0.037 Uiso 1 1 calc R . . . .
C11 C 0.5234(6) 0.3479(3) 0.0381(3) 0.0325(10) Uani 1 1 d . . . . .
H11 H 0.466412 0.299450 -0.000679 0.039 Uiso 1 1 calc R . . . .
C12 C 0.6782(6) 0.3833(3) 0.0111(3) 0.0330(10) Uani 1 1 d . . . . .
H12 H 0.728798 0.359978 -0.046907 0.040 Uiso 1 1 calc R . . . .
C13 C 0.7571(5) 0.4526(3) 0.0697(3) 0.0280(9) Uani 1 1 d . . . . .
H13 H 0.863475 0.476323 0.050879 0.034 Uiso 1 1 calc R . . . .
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'
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
O4 Re1 N1 82.53(11) . .
O4 Re1 N2 78.72(11) . .
N1 Re1 N2 87.51(11) . .
C1 Re1 O4 96.26(15) . .
C1 Re1 N1 177.05(15) . .
C1 Re1 N2 94.91(15) . .
C2 Re1 O4 100.05(15) . .
C2 Re1 N1 91.65(15) . .
C2 Re1 N2 178.59(14) . .
C2 Re1 C1 85.90(18) . .
C3 Re1 O4 169.88(14) . .
C3 Re1 N1 91.71(14) . .
C3 Re1 N2 92.77(14) . .
C3 Re1 C1 89.87(17) . .
C3 Re1 C2 88.39(18) . .
N3 O4 Re1 126.3(2) . .
C9 N1 Re1 122.6(3) . .
C9 N1 C13 117.4(3) . .
C13 N1 Re1 119.9(3) . .
C4 N2 Re1 120.4(3) . .
C4 N2 C8 117.5(3) . .
C8 N2 Re1 121.9(3) . .
O5 N3 O4 119.5(3) . .
O6 N3 O4 117.9(3) . .
O6 N3 O5 122.6(4) . .
O1 C1 Re1 175.9(4) . .
O2 C2 Re1 177.8(4) . .
O3 C3 Re1 178.6(4) . .
N2 C4 H4 118.5 . .
N2 C4 C5 123.0(4) . .
C5 C4 H4 118.5 . .
C4 C5 H5 120.3 . .
C4 C5 C6 119.5(4) . .
C6 C5 H5 120.3 . .
C5 C6 H6 121.2 . .
C5 C6 C7 117.5(4) . .
C7 C6 H6 121.2 . .
C6 C7 H7 120.0 . .
C8 C7 C6 120.0(4) . .
C8 C7 H7 120.0 . .
N2 C8 C7 122.5(4) . .
N2 C8 H8 118.8 . .
C7 C8 H8 118.8 . .
N1 C9 H9 118.7 . .
N1 C9 C10 122.6(4) . .
C10 C9 H9 118.7 . .
C9 C10 H10 120.4 . .
C11 C10 C9 119.1(4) . .
C11 C10 H10 120.4 . .
C10 C11 H11 120.7 . .
C10 C11 C12 118.7(4) . .
C12 C11 H11 120.7 . .
C11 C12 H12 120.6 . .
C13 C12 C11 118.8(4) . .
C13 C12 H12 120.6 . .
N1 C13 C12 123.4(4) . .
N1 C13 H13 118.3 . .
C12 C13 H13 118.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O4 2.153(3) .
Re1 N1 2.211(3) .
Re1 N2 2.211(3) .
Re1 C1 1.921(4) .
Re1 C2 1.907(4) .
Re1 C3 1.890(4) .
O1 C1 1.144(5) .
O2 C2 1.149(5) .
O3 C3 1.151(5) .
O4 N3 1.294(4) .
O5 N3 1.241(4) .
O6 N3 1.228(4) .
N1 C9 1.344(5) .
N1 C13 1.344(5) .
N2 C4 1.335(5) .
N2 C8 1.343(5) .
C4 H4 0.9500 .
C4 C5 1.377(6) .
C5 H5 0.9500 .
C5 C6 1.380(6) .
C6 H6 0.9500 .
C6 C7 1.383(7) .
C7 H7 0.9500 .
C7 C8 1.372(6) .
C8 H8 0.9500 .
C9 H9 0.9500 .
C9 C10 1.387(6) .
C10 H10 0.9500 .
C10 C11 1.379(6) .
C11 H11 0.9500 .
C11 C12 1.385(6) .
C12 H12 0.9500 .
C12 C13 1.374(6) .
C13 H13 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C9 H9 O4 0.95 2.46 2.941(5) 111.7 . yes
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
Re1 O4 N3 O5 -12.3(5) . . . .
Re1 O4 N3 O6 169.3(3) . . . .
Re1 N1 C9 C10 176.3(3) . . . .
Re1 N1 C13 C12 -175.9(3) . . . .
Re1 N2 C4 C5 -176.3(3) . . . .
Re1 N2 C8 C7 176.3(3) . . . .
N1 C9 C10 C11 -0.7(6) . . . .
N2 C4 C5 C6 -0.2(7) . . . .
C4 N2 C8 C7 -0.2(6) . . . .
C4 C5 C6 C7 0.1(7) . . . .
C5 C6 C7 C8 -0.1(7) . . . .
C6 C7 C8 N2 0.1(7) . . . .
C8 N2 C4 C5 0.3(6) . . . .
C9 N1 C13 C12 -0.6(6) . . . .
C9 C10 C11 C12 -0.2(6) . . . .
C10 C11 C12 C13 0.6(6) . . . .
C11 C12 C13 N1 -0.3(7) . . . .
C13 N1 C9 C10 1.1(6) . . . .
