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#$Date: 2023-05-05 04:53:07 +0300 (Fri, 05 May 2023) $
#$Revision: 283265 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/20/7712027.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_7712027
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         'C7 H9 N O3 Re'
_chemical_formula_sum            'C7 H9 N O3 Re'
_chemical_formula_weight         341.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                79.5150(10)
_cell_angle_beta                 76.4570(10)
_cell_angle_gamma                77.5250(10)
_cell_formula_units_Z            2
_cell_length_a                   6.02510(10)
_cell_length_b                   6.7106(2)
_cell_length_c                   11.4878(3)
_cell_measurement_reflns_used    6704
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      3.14
_cell_volume                     436.655(19)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9026
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         3.413
_exptl_absorpt_coefficient_mu    13.880
_exptl_absorpt_correction_T_max  0.0330
_exptl_absorpt_correction_T_min  0.0288
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.596
_exptl_crystal_description       block
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0186
_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)+(0.0180P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2524
_reflns_number_total             2684
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03819f2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7712027--7712031.cif.'
_cod_database_code               7712027
_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.
;
_exptl_absorpt_factor_mur        3.470
_exptl_absorpt_correction_t_ave  0.0307
_exptl_absorpt_rmerge_before     0.0196
_exptl_absorpt_rmerge_after      0.0218
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.26720(2) 0.79023(2) 0.67152(2) 0.03199(5) Uani 1 1 d . . . . .
N1 N 0.3880(5) 1.0219(4) 0.7768(2) 0.0354(5) Uani 1 1 d . . . . .
C3 C 0.5137(5) 1.3032(4) 0.8915(2) 0.0333(5) Uani 1 1 d . . . . .
C6 C 0.5895(5) 1.4542(5) 0.9491(3) 0.0399(6) Uani 1 1 d . . . . .
H6A H 0.632948 1.565813 0.887057 0.048 Uiso 1 1 calc R U . . .
H6B H 0.727087 1.385526 0.980189 0.048 Uiso 1 1 calc R U . . .
C2 C 0.6571(5) 1.2277(5) 0.7885(3) 0.0377(6) Uani 1 1 d . . . . .
H2 H 0.798214 1.271061 0.756152 0.045 Uiso 1 1 calc R U . . .
C1 C 0.5901(5) 1.0894(5) 0.7349(3) 0.0401(6) Uani 1 1 d . . . . .
H1 H 0.688788 1.040640 0.666714 0.048 Uiso 1 1 calc R U . . .
C5 C 0.2507(6) 1.0944(5) 0.8752(3) 0.0413(7) Uani 1 1 d . . . . .
H5 H 0.109890 1.049569 0.905401 0.050 Uiso 1 1 calc R U . . .
C4 C 0.3066(6) 1.2316(5) 0.9341(3) 0.0413(7) Uani 1 1 d . . . . .
H4 H 0.205294 1.276337 1.002651 0.050 Uiso 1 1 calc R U . . .
O1 O 0.5567(4) 0.6896(4) 0.6488(2) 0.0494(6) Uani 1 1 d . . . . .
O2 O 0.0980(4) 0.7357(4) 0.8104(2) 0.0508(6) Uani 1 1 d . . . . .
O3 O 0.1788(5) 1.0121(4) 0.5831(2) 0.0558(6) Uani 1 1 d . . . . .
C7 C 0.1675(7) 0.5858(6) 0.5854(4) 0.0538(9) Uani 1 1 d . . . . .
H7A H 0.005213 0.626541 0.583890 0.081 Uiso 1 1 calc R U . . .
H7B H 0.195556 0.449182 0.628471 0.081 Uiso 1 1 calc R U . . .
H7C H 0.255830 0.587661 0.504053 0.081 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 118.09(13) . . ?
O3 Re1 O1 117.92(14) . . ?
O2 Re1 O1 118.83(13) . . ?
O3 Re1 C7 98.12(15) . . ?
O2 Re1 C7 97.05(14) . . ?
O1 Re1 C7 97.65(14) . . ?
O3 Re1 N1 83.52(11) . . ?
O2 Re1 N1 82.09(10) . . ?
O1 Re1 N1 81.59(10) . . ?
C7 Re1 N1 178.36(12) . . ?
C5 N1 C1 117.1(3) . . ?
C5 N1 Re1 121.4(2) . . ?
C1 N1 Re1 121.40(18) . . ?
C4 C3 C2 116.5(3) . . ?
C4 C3 C6 124.0(3) . . ?
C2 C3 C6 119.5(3) . . ?
C3 C6 C6 115.4(3) . 2_687 ?
C3 C6 H6A 108.4 . . ?
C6 C6 H6A 108.4 2_687 . ?
C3 C6 H6B 108.4 . . ?
C6 C6 H6B 108.4 2_687 . ?
H6A C6 H6B 107.5 . . ?
C1 C2 C3 120.1(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
N1 C5 C4 123.4(3) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
Re1 C7 H7A 109.5 . . ?
Re1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Re1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
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 1.701(2) . ?
Re1 O2 1.704(2) . ?
Re1 O1 1.705(2) . ?
Re1 C7 2.086(3) . ?
Re1 N1 2.449(2) . ?
N1 C5 1.337(3) . ?
N1 C1 1.343(4) . ?
C3 C4 1.384(4) . ?
C3 C2 1.398(4) . ?
C3 C6 1.503(4) . ?
C6 C6 1.514(6) 2_687 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2 C1 1.374(4) . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C5 C4 1.373(4) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
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
C4 C3 C6 C6 -6.9(6) . . . 2_687 ?
C2 C3 C6 C6 173.1(3) . . . 2_687 ?
C4 C3 C2 C1 -0.1(5) . . . . ?
C6 C3 C2 C1 180.0(3) . . . . ?
C5 N1 C1 C2 -0.3(5) . . . . ?
Re1 N1 C1 C2 176.6(2) . . . . ?
C3 C2 C1 N1 0.4(5) . . . . ?
C1 N1 C5 C4 -0.2(5) . . . . ?
Re1 N1 C5 C4 -177.0(3) . . . . ?
N1 C5 C4 C3 0.5(5) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
C6 C3 C4 C5 179.6(3) . . . . ?
