#------------------------------------------------------------------------------
#$Date: 2023-09-21 10:58:45 +0300 (Thu, 21 Sep 2023) $
#$Revision: 286445 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/75/8107525.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_8107525
loop_
_publ_author_name
'Mkhatshwa, Marcus'
'Malan, Frederick P.'
'Makgopa, Katlego'
'Manicum, Amanda-Lee E.'
_publ_section_title
;
 The crystal structure of fac-tricarbonyl(6-bromo-2,2-bipyridine-κ2
 N,N)-(nitrato-\kO)rhenium(I), C13H7BrN3O6Re
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              667
_journal_page_last               669
_journal_paper_doi               10.1515/ncrs-2023-0141
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         C13H7BrN3O6Re
_chemical_formula_sum            'C13 H7 Br N3 O6 Re'
_chemical_formula_weight         567.33
_chemical_melting_point          150
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-20 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.26450(10)
_cell_length_b                   10.06070(10)
_cell_length_c                   20.7717(2)
_cell_measurement_reflns_used    32995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.998
_cell_measurement_theta_min      2.144
_cell_volume                     1506.22(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31772
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.999
_diffrn_reflns_theta_min         4.291
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_number         32995
_exptl_absorpt_coefficient_mu    19.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29763
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.163
_exptl_transmission_factor_max   0
_exptl_transmission_factor_min   0
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.770
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0165P)²+19.6465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3171
_reflns_number_total             3207
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0141_suppl_001.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1506.21(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8107525
_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.
;
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Br Br 0.43740(13) 0.42345(8) 0.23869(4) 0.0422(2) Uani 1 1 d . . . . .
C1 C 0.9142(9) 0.2668(6) 0.3426(3) 0.0250(13) Uani 1 1 d . . . . .
C2 C 0.5909(11) 0.1549(7) 0.2933(4) 0.0335(15) Uani 1 1 d . . . . .
C3 C 0.7723(9) 0.0558(6) 0.3957(3) 0.0281(14) Uani 1 1 d . . . . .
C4 C 0.5092(9) 0.5121(7) 0.3178(3) 0.0250(13) Uani 1 1 d . . . . .
C5 C 0.4639(9) 0.6462(7) 0.3174(3) 0.0278(14) Uani 1 1 d . . . . .
H5 H 0.397156 0.686662 0.280209 0.033 Uiso 1 1 calc R U . . .
C6 C 0.5191(10) 0.7184(7) 0.3726(4) 0.0302(15) Uani 1 1 d . . . . .
H6 H 0.494111 0.810959 0.373956 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6114(9) 0.6547(6) 0.4265(3) 0.0253(13) Uani 1 1 d . . . . .
H7 H 0.650459 0.703263 0.464980 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6464(8) 0.5190(6) 0.4235(3) 0.0201(12) Uani 1 1 d . . . . .
C9 C 0.7411(8) 0.4480(6) 0.4797(3) 0.0177(11) Uani 1 1 d . . . . .
C10 C 0.7921(8) 0.5097(6) 0.5399(3) 0.0224(12) Uani 1 1 d . . . . .
H10 H 0.766977 0.601191 0.545959 0.027 Uiso 1 1 calc R U . . .
C11 C 0.8796(8) 0.4341(6) 0.5901(3) 0.0228(12) Uani 1 1 d . . . . .
H11 H 0.915376 0.473716 0.631276 0.027 Uiso 1 1 calc R U . . .
C12 C 0.9153(9) 0.3022(7) 0.5809(3) 0.0253(13) Uani 1 1 d . . . . .
H12 H 0.975079 0.249559 0.615314 0.030 Uiso 1 1 calc R U . . .
C13 C 0.8622(8) 0.2471(6) 0.5200(3) 0.0220(12) Uani 1 1 d . . . . .
H13 H 0.887517 0.155860 0.513203 0.026 Uiso 1 1 calc R U . . .
N1 N 0.5976(7) 0.4461(5) 0.3681(2) 0.0201(10) Uani 1 1 d . . . . .
N2 N 0.7766(7) 0.3182(5) 0.4707(2) 0.0175(10) Uani 1 1 d . . . . .
N3 N 0.3340(8) 0.1199(6) 0.4218(3) 0.0287(12) Uani 1 1 d . . . . .
O1 O 1.0532(7) 0.2873(5) 0.3235(3) 0.0363(12) Uani 1 1 d . . . . .
O2 O 0.5439(9) 0.1010(6) 0.2457(3) 0.0506(16) Uani 1 1 d . . . . .
O3 O 0.8263(7) -0.0483(5) 0.4069(3) 0.0371(12) Uani 1 1 d . . . . .
O4 O 0.4323(6) 0.2199(4) 0.4206(2) 0.0253(9) Uani 1 1 d . . . . .
O5 O 0.3642(8) 0.0158(6) 0.3934(3) 0.0523(16) Uani 1 1 d . . . . .
O6 O 0.1981(8) 0.1273(6) 0.4536(3) 0.0511(15) Uani 1 1 d . . . . .
Re Re 0.68498(4) 0.23286(2) 0.37591(2) 0.01883(9) 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 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
C1 Re C3 87.9(3) . .
C1 Re C2 88.8(3) . .
C3 Re C2 83.4(3) . .
C1 Re O4 172.2(2) . .
C3 Re O4 97.3(2) . .
C2 Re O4 97.6(3) . .
C1 Re N2 94.3(2) . .
C3 Re N2 96.7(2) . .
C2 Re N2 176.9(3) . .
O4 Re N2 79.33(18) . .
C1 Re N1 93.1(2) . .
C3 Re N1 171.6(2) . .
C2 Re N1 105.0(2) . .
O4 Re N1 80.84(18) . .
N2 Re N1 74.88(18) . .
N3 O4 Re 125.5(4) . .
C4 N1 C8 116.0(5) . .
C4 N1 Re 129.7(4) . .
C8 N1 Re 114.2(4) . .
C13 N2 C9 119.4(5) . .
C13 N2 Re 122.9(4) . .
C9 N2 Re 117.8(4) . .
O4 N3 O5 122.9(6) . .
O4 N3 O6 117.1(6) . .
O5 N3 O6 120.0(6) . .
N2 C9 C10 121.2(5) . .
N2 C9 C8 116.2(5) . .
C10 C9 C8 122.6(5) . .
C6 C7 C8 119.4(6) . .
O1 C1 Re 179.0(6) . .
N1 C8 C7 122.1(6) . .
N1 C8 C9 117.0(5) . .
C7 C8 C9 120.9(6) . .
C11 C10 C9 118.3(6) . .
N2 C13 C12 122.2(6) . .
C11 C12 C13 118.5(6) . .
O3 C3 Re 178.8(7) . .
C12 C11 C10 120.4(6) . .
N1 C4 C5 125.4(6) . .
N1 C4 Br 120.1(5) . .
C5 C4 Br 114.5(5) . .
C5 C6 C7 119.4(6) . .
C6 C5 C4 117.6(6) . .
O2 C2 Re 174.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re C1 1.912(7) .
Re C3 1.918(7) .
Re C2 1.931(7) .
Re O4 2.163(4) .
Re N2 2.174(4) .
Re N1 2.237(5) .
Br C4 1.885(6) .
O4 N3 1.236(7) .
N1 C4 1.333(8) .
N1 C8 1.374(8) .
N2 C13 1.338(8) .
N2 C9 1.348(7) .
O1 C1 1.149(8) .
O3 C3 1.132(8) .
N3 O5 1.236(8) .
N3 O6 1.256(8) .
O2 C2 1.143(9) .
C9 C10 1.404(8) .
C9 C8 1.465(8) .
C7 C6 1.387(9) .
C7 C8 1.391(9) .
C10 C11 1.380(9) .
C13 C12 1.391(9) .
C12 C11 1.370(9) .
C4 C5 1.389(9) .
C6 C5 1.375(10) .
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
Re O4 N3 O5 -4.7(9) . . . .
Re O4 N3 O6 175.5(5) . . . .
C13 N2 C9 C10 -0.1(8) . . . .
Re N2 C9 C10 178.6(4) . . . .
C13 N2 C9 C8 -179.8(5) . . . .
Re N2 C9 C8 -1.1(7) . . . .
C4 N1 C8 C7 -2.1(9) . . . .
Re N1 C8 C7 176.8(5) . . . .
C4 N1 C8 C9 179.0(5) . . . .
Re N1 C8 C9 -2.1(6) . . . .
C6 C7 C8 N1 2.1(10) . . . .
C6 C7 C8 C9 -179.0(6) . . . .
N2 C9 C8 N1 2.2(8) . . . .
C10 C9 C8 N1 -177.6(5) . . . .
N2 C9 C8 C7 -176.7(6) . . . .
C10 C9 C8 C7 3.5(9) . . . .
N2 C9 C10 C11 -0.1(9) . . . .
C8 C9 C10 C11 179.6(5) . . . .
C9 N2 C13 C12 0.4(9) . . . .
Re N2 C13 C12 -178.2(5) . . . .
N2 C13 C12 C11 -0.5(10) . . . .
C13 C12 C11 C10 0.3(10) . . . .
C9 C10 C11 C12 0.0(9) . . . .
C8 N1 C4 C5 0.0(9) . . . .
Re N1 C4 C5 -178.7(5) . . . .
C8 N1 C4 Br 179.3(4) . . . .
Re N1 C4 Br 0.6(8) . . . .
C8 C7 C6 C5 0.0(10) . . . .
C7 C6 C5 C4 -1.9(10) . . . .
N1 C4 C5 C6 2.0(10) . . . .
Br C4 C5 C6 -177.3(5) . . . .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{b478de1f-2a1d-4d3e-a869-ffdb2b71e7d6} ? ? ?
{df3d5821-5cb4-48dd-aa57-0dd78efcf533} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{b478de1f-2a1d-4d3e-a869-ffdb2b71e7d6} '_publcif_info_datablock.publ_exptl'
loop_
_publcif_info_cif.paper_type
CE
;
;
