Intermolecular non-covalent interactions in the organic perrhenates crystal structures: from theory to practice
Novikov, Anton P.; Sitanskaia, Anastasiia V.; Volkov, Mikhail A.; Nevolin, Iurii M.; Grigoriev, Mikhail S.; CrystEngComm 26 (2024) 6640–6649; doi:10.1039/D4CE00951G

data_7249581
_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, C5 H12 N'
_chemical_formula_sum            'C5 H12 N O4 Re'
_chemical_formula_weight         336.36
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-01 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                95.814(11)
_cell_angle_beta                 94.570(11)
_cell_angle_gamma                100.825(11)
_cell_formula_units_Z            1
_cell_length_a                   5.807(2)
_cell_length_b                   6.087(2)
_cell_length_c                   6.157(2)
_cell_measurement_reflns_used    3433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      3.343
_cell_volume                     211.57(12)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4129
_diffrn_reflns_point_group_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.452
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    14.328
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0794 before and 0.0390 after correction.
The Ratio of minimum to maximum transmission is 0.8181.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.640
_exptl_crystal_description       block
_exptl_crystal_F_000             156
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_coef       0.0190(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2042
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0187
_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/[\s^2^(Fo^2^)+(0.0037P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0333
_refine_ls_wR_factor_ref         0.0333
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    0.705
_reflns_Friedel_fraction_max     0.654
_reflns_number_gt                2042
_reflns_number_total             2042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00951g2.cif
_cod_data_source_block           mv137
_cod_depositor_comments
'Adding full bibliography for 7249580--7249590.cif.'
_cod_database_code               7249581
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.926
 0.074
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C3) = Uanis(C4)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              28969
_shelx_hkl_checksum              10467
_olex2_submission_special_instructions 'No special instructions were received'