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#$Date: 2024-12-06 19:37:58 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296470 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/95/7249590.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_7249590
loop_
_publ_author_name
'Novikov, Anton P.'
'Sitanskaia, Anastasiia V.'
'Volkov, Mikhail A.'
'Nevolin, Iurii M.'
'Grigoriev, Mikhail S.'
_publ_section_title
;
 Intermolecular non-covalent interactions in the organic perrhenates
 crystal structures: from theory to practice
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              6640
_journal_page_last               6649
_journal_paper_doi               10.1039/D4CE00951G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'O4 Re, C4 H10 N'
_chemical_formula_sum            'C4 H10 N O4 Re'
_chemical_formula_weight         322.33
_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   mixed
_audit_creation_date             2024-10-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-01 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.576(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4974(3)
_cell_length_b                   8.7838(6)
_cell_length_c                   15.4679(10)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.108
_cell_measurement_theta_min      3.523
_cell_volume                     742.00(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'APEX3 v2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39441
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.498
_diffrn_reflns_theta_min         4.324
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.335
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1430 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.4952.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.885
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.739
_refine_diff_density_min         -2.360
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00132(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0197
_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)+3.1184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2551
_reflns_number_total             2684
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00951g2.cif
_cod_data_source_block           pirrolidreo4
_cod_depositor_comments
'Adding full bibliography for 7249580--7249590.cif.'
_cod_database_code               7249590
_shelx_shelxl_version_number     2018/3
_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   0.292
_shelx_estimated_absorpt_t_min   0.180
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B), C1(H1C,H1D)
;
_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 0.04617(2) 0.83835(2) 0.10753(2) 0.00716(4) Uani 1 1 d . . . . .
O1 O 0.3467(4) 0.8603(3) 0.08684(17) 0.0163(5) Uani 1 1 d . . . . .
O4 O 0.0433(5) 0.7539(3) 0.20765(16) 0.0162(5) Uani 1 1 d . . . . .
O5 O -0.1107(4) 0.7232(3) 0.02879(15) 0.0130(4) Uani 1 1 d . . . . .
O8 O -0.0931(5) 1.0152(3) 0.10824(18) 0.0186(5) Uani 1 1 d . . . . .
C2 C 0.5999(6) 0.4818(3) 0.1513(2) 0.0109(5) Uani 1 1 d . . . . .
H2A H 0.576395 0.583968 0.124587 0.013 Uiso 1 1 calc R U . . .
H2B H 0.724299 0.488878 0.202720 0.013 Uiso 1 1 calc R U . . .
N1 N 0.5213(5) 0.2277(3) 0.09407(18) 0.0111(5) Uani 1 1 d . . . . .
H1A H 0.418(8) 0.227(5) 0.051(3) 0.013 Uiso 1 1 d . U . . .
H1B H 0.612(8) 0.151(5) 0.098(3) 0.013 Uiso 1 1 d . U . . .
C4 C 0.3945(6) 0.2483(4) 0.1738(2) 0.0129(6) Uani 1 1 d . . . . .
H4A H 0.497391 0.211633 0.226360 0.015 Uiso 1 1 calc R U . . .
H4B H 0.235696 0.194029 0.168366 0.015 Uiso 1 1 calc R U . . .
C3 C 0.3581(6) 0.4197(4) 0.1768(2) 0.0155(6) Uani 1 1 d . . . . .
H3A H 0.330447 0.453553 0.235944 0.019 Uiso 1 1 calc R U . . .
H3B H 0.218095 0.452235 0.134930 0.019 Uiso 1 1 calc R U . . .
C1 C 0.6778(6) 0.3668(4) 0.0856(2) 0.0162(6) Uani 1 1 d . . . . .
H1C H 0.650028 0.408382 0.025804 0.019 Uiso 1 1 calc R U . . .
H1D H 0.853530 0.341274 0.098964 0.019 Uiso 1 1 calc R U . . .
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
_geom_angle_publ_flag
O1 Re1 O5 110.10(11) . . ?
O1 Re1 O8 109.49(12) . . ?
O4 Re1 O1 108.80(12) . . ?
O4 Re1 O5 109.03(12) . . ?
O4 Re1 O8 109.36(13) . . ?
O8 Re1 O5 110.03(12) . . ?
H2A C2 H2B 108.9 . . ?
C3 C2 H2A 110.8 . . ?
C3 C2 H2B 110.8 . . ?
C1 C2 H2A 110.8 . . ?
C1 C2 H2B 110.8 . . ?
C1 C2 C3 104.7(2) . . ?
H1A N1 H1B 114(4) . . ?
C4 N1 H1A 109(3) . . ?
C4 N1 H1B 111(3) . . ?
C4 N1 C1 107.3(2) . . ?
C1 N1 H1A 107(3) . . ?
C1 N1 H1B 109(3) . . ?
N1 C4 H4A 111.2 . . ?
N1 C4 H4B 111.2 . . ?
N1 C4 C3 102.8(3) . . ?
H4A C4 H4B 109.1 . . ?
C3 C4 H4A 111.2 . . ?
C3 C4 H4B 111.2 . . ?
C2 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
C4 C3 C2 102.9(3) . . ?
C4 C3 H3A 111.2 . . ?
C4 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C2 C1 H1C 110.6 . . ?
C2 C1 H1D 110.6 . . ?
N1 C1 C2 105.7(2) . . ?
N1 C1 H1C 110.6 . . ?
N1 C1 H1D 110.6 . . ?
H1C C1 H1D 108.7 . . ?
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 O1 1.729(2) . ?
Re1 O4 1.719(2) . ?
Re1 O5 1.735(2) . ?
Re1 O8 1.732(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.530(4) . ?
C2 C1 1.529(4) . ?
N1 H1A 0.83(5) . ?
N1 H1B 0.83(5) . ?
N1 C4 1.495(4) . ?
N1 C1 1.508(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.520(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
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
N1 H1A O5 0.83(5) 2.02(5) 2.812(4) 160(4) 3_565 yes
N1 H1B O8 0.83(5) 2.01(5) 2.815(4) 163(4) 1_645 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
_geom_torsion_publ_flag
N1 C4 C3 C2 -40.8(3) . . . . ?
C4 N1 C1 C2 -11.1(3) . . . . ?
C3 C2 C1 N1 -14.5(3) . . . . ?
C1 C2 C3 C4 34.2(3) . . . . ?
C1 N1 C4 C3 32.3(3) . . . . ?
