σ-Hole interactions in organometallic catalysts: the case of methyltrioxorhenium(VII).
Calabrese, Miriam; Pizzi, Andrea; Daolio, Andrea; Frontera, Antonio; Resnati, Giuseppe; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1030–1035; doi:10.1039/d2dt03819f

data_7712031
_publ_section_title
;
 &#x3c3;-Hole interactions in organometallic catalysts: the case of
 methyltrioxorhenium(VII).
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1030
_journal_page_last               1035
_journal_paper_doi               10.1039/d2dt03819f
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C5 H7 N2 O4 Re'
_chemical_formula_sum            'C5 H7 N2 O4 Re'
_chemical_formula_weight         345.33
_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   geom
_audit_creation_date             2022-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.156(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0455(5)
_cell_length_b                   10.9263(6)
_cell_length_c                   8.6505(5)
_cell_measurement_reflns_used    6704
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      3.14
_cell_volume                     802.60(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16559
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.640
_diffrn_reflns_theta_min         3.038
_exptl_absorpt_coefficient_mu    15.116
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1267 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.4324.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.858
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.140
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0443P)^2^+1.1524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2347
_reflns_number_total             2464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03819f2.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 7712027--7712031.cif.'
_cod_database_code               7712031
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C2(H2), C3(H3)
1.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              74174
_olex2_submission_special_instructions 'No special instructions were received'