#------------------------------------------------------------------------------
#$Date: 2023-05-05 04:53:07 +0300 (Fri, 05 May 2023) $
#$Revision: 283265 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/20/7712031.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_7712031
loop_
_publ_author_name
'Calabrese, Miriam'
'Pizzi, Andrea'
'Daolio, Andrea'
'Frontera, Antonio'
'Resnati, Giuseppe'
_publ_section_title
;
 σ-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       'φ and ω 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 λ/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/[σ²(Fo²)+(0.0443P)²+1.1524P] where P=(Fo²+2Fc²)/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 > 2σ(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
_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.
;
_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)
;
_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 0.17440(2) 0.60288(2) 0.18656(2) 0.01095(6) Uani 1 1 d . . . . .
O3 O 0.3021(3) 0.7129(2) 0.2968(3) 0.0158(4) Uani 1 1 d . . . . .
O2 O 0.0668(3) 0.6716(2) 0.0041(3) 0.0205(5) Uani 1 1 d . . . . .
O1 O 0.2533(3) 0.4735(2) 0.1333(3) 0.0155(4) Uani 1 1 d . . . . .
C4 C 0.2791(4) 0.3844(3) 0.4620(4) 0.0125(6) Uani 1 1 d . . . . .
H4 H 0.237848 0.337240 0.367296 0.015 Uiso 1 1 calc R U . . .
C1 C 0.3339(4) 0.5713(3) 0.5871(4) 0.0128(5) Uani 1 1 d . . . . .
H1 H 0.333804 0.656224 0.580542 0.015 Uiso 1 1 calc R U . . .
C2 C 0.3927(4) 0.5178(3) 0.7391(4) 0.0129(5) Uani 1 1 d . . . . .
H2 H 0.429669 0.565738 0.833475 0.016 Uiso 1 1 calc R U . . .
C3 C 0.3400(4) 0.3260(3) 0.6104(4) 0.0131(5) Uani 1 1 d . . . . .
H3 H 0.342643 0.240967 0.615326 0.016 Uiso 1 1 calc R U . . .
N2 N 0.3966(4) 0.3933(2) 0.7506(4) 0.0114(5) Uani 1 1 d . . . . .
N1 N 0.2762(3) 0.5069(2) 0.4471(3) 0.0121(5) Uani 1 1 d . . . . .
O5 O 0.4553(3) 0.3404(2) 0.8911(3) 0.0173(4) Uani 1 1 d . . . . .
C5 C -0.0263(4) 0.5741(3) 0.2542(4) 0.0178(6) Uani 1 1 d . . . . .
H5A H -0.017687 0.622376 0.349614 0.027 Uiso 1 1 calc R U . . .
H5B H -0.033133 0.489030 0.278899 0.027 Uiso 1 1 calc R U . . .
H5C H -0.119083 0.597664 0.164888 0.027 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
O3 Re1 O2 105.39(12) . . ?
O3 Re1 O1 117.72(12) . . ?
O3 Re1 N1 79.29(10) . . ?
O3 Re1 C5 115.42(12) . . ?
O2 Re1 O1 105.65(12) . . ?
O2 Re1 N1 169.00(11) . . ?
O2 Re1 C5 92.91(13) . . ?
O1 Re1 N1 80.17(10) . . ?
O1 Re1 C5 115.32(13) . . ?
C5 Re1 N1 76.10(12) . . ?
N1 C4 C3 122.9(3) . . ?
N1 C1 C2 123.1(3) . . ?
N2 C2 C1 119.2(3) . . ?
N2 C3 C4 119.5(3) . . ?
C3 N2 C2 118.8(3) . . ?
O5 N2 C2 120.7(3) . . ?
O5 N2 C3 120.5(2) . . ?
C4 N1 Re1 121.4(2) . . ?
C1 N1 Re1 122.06(19) . . ?
C1 N1 C4 116.5(3) . . ?
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 O3 1.712(2) . ?
Re1 O2 1.716(2) . ?
Re1 O1 1.717(2) . ?
Re1 N1 2.365(2) . ?
Re1 C5 2.114(3) . ?
C4 C3 1.368(4) . ?
C4 N1 1.345(4) . ?
C1 C2 1.368(4) . ?
C1 N1 1.341(4) . ?
C2 N2 1.363(4) . ?
C3 N2 1.358(4) . ?
N2 O5 1.284(3) . ?
