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_7712029
_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         '2(C0.5 F2 I), C12 H12 N2'
_chemical_formula_sum            'C13 H12 F4 I2 N2'
_chemical_formula_weight         526.05
_chemical_name_systematic
1,2-di(pyridine-4-yl)ethane.1,2-diiodotetrafluoroethane
_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_date             2022-12-13
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.12.07 svn.r85f57a8f for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                94.188(6)
_cell_angle_beta                 96.753(7)
_cell_angle_gamma                105.647(7)
_cell_formula_units_Z            1
_cell_length_a                   6.6506(7)
_cell_length_b                   7.5300(8)
_cell_length_c                   9.1546(10)
_cell_measurement_reflns_used    3640
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.83
_cell_volume                     435.76(8)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7820
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.555
_diffrn_reflns_theta_min         2.826
_exptl_absorpt_coefficient_mu    3.640
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       block
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2153
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1530
_reflns_number_total             2153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03819f2.cif
_cod_data_source_block           2a-diiodotetrafluoroethane
_cod_depositor_comments
'Adding full bibliography for 7712027--7712031.cif.'
_cod_database_code               7712029
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 I2-C7 \\sim I1-C7B
 with sigma of 0.02
 F2B-C7 \\sim C7-F1
 with sigma of 0.02
 F2-C7B \\sim C7B-F1A
 with sigma of 0.02
 F1A-C7 \\sim F2B-C7B \\sim F1-C7B \\sim F2-C7
 with sigma of 0.02
 F1A-F1 \\sim F2B-F2
 with sigma of 0.02
 I1-C7B \\sim I1A-C7C
 with sigma of 0.02
 F2B-C7B \\sim F2C-C7C
 with sigma of 0.02
 F1A-C7 \\sim F1B-C7A
 with sigma of 0.02
 C7B-C7 \\sim C7C-C7A
 with sigma of 0.02
 C7B-F1 \\sim C7C-F3
 with sigma of 0.02
 C7-I2 \\sim C7A-I2A
 with sigma of 0.02
 C7-F2 \\sim C7A-F2A
 with sigma of 0.02
 I1-F2B \\sim I1A-F2C
 with sigma of 0.04
 I1-C7 \\sim I1A-C7A
 with sigma of 0.04
 I1-F1 \\sim I1A-F3
 with sigma of 0.04
 F2B-C7 \\sim F2C-C7A
 with sigma of 0.04
 F2B-F1 \\sim F2C-F3
 with sigma of 0.04
 F1A-C7B \\sim F1B-C7C
 with sigma of 0.04
 F1A-I2 \\sim F1B-I2A
 with sigma of 0.04
 F1A-F2 \\sim F1B-F2A
 with sigma of 0.04
 C7B-I2 \\sim C7C-I2A
 with sigma of 0.04
 C7B-F2 \\sim C7C-F2A
 with sigma of 0.04
 C7-F1 \\sim C7A-F3
 with sigma of 0.04
 I2-F2 \\sim I2A-F2A
 with sigma of 0.04
 F1A-F2 \\sim F2B-F1
 with sigma of 0.02
 F1-C7B \\sim F2B-C7B \\sim F1A-C7 \\sim F2-C7
 with sigma of 0.02
 F2C-F3 \\sim F2A-F1B
 with sigma of 0.02
 F3-C7C \\sim F2C-C7C \\sim F1B-C7A \\sim F2A-C7A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7C \\sim C7 \\sim C7A \\sim C7B: within 2A with sigma of 2 and sigma for
terminal atoms of 4 within 2A
Uanis(C7) \\sim Ueq, Uanis(C7B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(F1)
\\sim Ueq, Uanis(F2B) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Rigid body (RIGU) restrains
 C5, N1, C1, C2, C4, C3, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I2, I1, C7B, F2B, C7, F1, F1A, F2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7C, C7A, F1B, I2A, F2A, I1A, F2C, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I2A, C7A, C7C, F1B, F2A, I1A, F2C, F3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: I1(0.25) F2B(0.25) F1A(0.25) C7B(0.125) C7(0.125) F1(0.25)
 I2(0.25) F2(0.25) C7A(0.125) I1A(0.25) C7C(0.125) F2C(0.25) F3(0.25) F1B(0.25)
 I2A(0.25) F2A(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C4(H4)
;
_shelx_res_checksum              46033
_olex2_submission_special_instructions 'No special instructions were received'