Redox induced oxidative C-C coupling of non-innocent bis(heterocyclo)methanides
Lahiri, Goutam Kumar; Panda, Sanjib; Baliyan, Rupal; Dhara, Suman; Huang, Kuo-Wei; Dalton Transactions  (2021) –; doi:10.1039/D1DT03310G

data_7708776
_publ_section_title
;
 Redox induced oxidative C-C coupling of non-innocent
 bis(heterocyclo)methanides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03310G
_journal_year                    2021
_chemical_formula_moiety         'C26 H28 N4 O4 Ru, F6 P1'
_chemical_formula_sum            'C26 H28 F6 N4 O4 P Ru'
_chemical_formula_weight         706.56
_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             2021-10-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-10-14 deposited with the CCDC.	2021-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                72.540(4)
_cell_angle_beta                 85.511(3)
_cell_angle_gamma                86.024(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8784(3)
_cell_length_b                   12.9044(5)
_cell_length_c                   14.3059(6)
_cell_measurement_reflns_used    5454
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0950
_cell_measurement_theta_min      2.5340
_cell_volume                     1381.55(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  70.00   0.50    8.00    --  -20.00   0.00 -36.00  266
  2  \w    -60.00  19.00   0.50    8.00    --  -20.00 -72.00 108.00  158
  3  \w    -59.00   4.50   0.50    8.00    --  -20.00  72.00  36.00  127
  4  \w    -69.00  19.00   0.50    8.00    --  -20.00 -72.00-108.00  176
  5  \w   -101.00 -42.50   0.50    8.00    --  -20.00 -72.00-180.00  117
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11178
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.539
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       plate
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0540
_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/[\s^2^(Fo^2^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3704
_reflns_number_total             4827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03310g2.cif
_cod_data_source_block           3-h
_cod_database_code               7708776
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-F1 \\sim P1A-F1A
 with sigma of 0.02
 F12-F2 \\sim F12A-F2A
 with sigma of 0.04
 F3-F5 \\sim F3A-F5A
 with sigma of 0.04
 P1-F3 \\sim P1A-F3A
 with sigma of 0.02
 F2-F4 \\sim F2A-F4A
 with sigma of 0.04
 P1-F12 \\sim P1A-F12A
 with sigma of 0.02
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 P1-F5 \\sim P1A-F5A
 with sigma of 0.02
 F5-F2 \\sim F5A-F2A
 with sigma of 0.04
 P1-F2 \\sim P1A-F2A
 with sigma of 0.02
 F3-F12 \\sim F3A-F12A
 with sigma of 0.04
 P1-F4 \\sim P1A-F4A
 with sigma of 0.02
 F3-F2 \\sim F3A-F2A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F12-F5 \\sim F12A-F5A
 with sigma of 0.04
 F1-F12 \\sim F1A-F12A
 with sigma of 0.04
 F12-F4 \\sim F12A-F4A
 with sigma of 0.04
 F1-F5 \\sim F1A-F5A
 with sigma of 0.04
 F5-F4 \\sim F5A-F4A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F1-F4 \\sim F1A-F4A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P1 \\sim P1A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 F5, P1, F1, F3, F12, F2, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4A, P1A, F1A, F3A, F12A, F5A, F2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(P1A)=Sof(F1A)=Sof(F3A)=Sof(F12A)=Sof(F5A)=Sof(F2A)=Sof(F4A)=1-FVAR(1)
 Sof(P1)=Sof(F1)=Sof(F3)=Sof(F12)=Sof(F5)=Sof(F2)=Sof(F4)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C4(H4), C10(H10), C15(H15), C24(H24), C6(H6), C7(H7),
 C12(H12), C14(H14), C13(H13), C19(H19)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              86451
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;