Ruthenium(v) terminal arylimido corroles: isolation, spectroscopic characterization and reactivity.
Shing, Ka-Pan; Qin, Lin; Wu, Liang-Liang; Huang, Jie-Sheng; Che, Chi-Ming; Chemical science 14 (2023) 10602–10609; doi:10.1039/d3sc02266h

data_1569764
_publ_section_title
;
 Ruthenium(v) terminal arylimido corroles: isolation, spectroscopic
 characterization and reactivity.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              10602
_journal_page_last               10609
_journal_paper_doi               10.1039/d3sc02266h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C82 H54 N8 Ru2, 2(C0.667 H1.333 Cl), 0.667(C H2 Cl2), 0.667(Cl)'
_chemical_formula_sum            'C84 H58 Cl4 N8 Ru2'
_chemical_formula_weight         1523.32
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2022-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-21 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.427(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4207(6)
_cell_length_b                   12.7439(7)
_cell_length_c                   26.3116(13)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.30
_cell_measurement_theta_min      3.37
_cell_volume                     3487.9(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5039
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.365
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.329
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1223 before and 0.0809 after correction.
 
For component 2:
 wR2(int) was 0.1208 before and 0.0812 after correction.
 The Ratio of minimum to maximum transmission is 0.57.

Final HKLF 4 output contains 27448 reflections, Rint = 0.0722
 (19417 with I > 3sig(I), Rint = 0.0668)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       plate
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.711
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0473P)^2^+33.1510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4534
_reflns_number_total             5039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02266h2.cif
_cod_data_source_block           twin4
_cod_depositor_comments          'Adding full bibliography for 1569764.cif.'
_cod_database_code               1569764
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.547(2)
 0.453(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C23A-C21A = C23-C21 = C22A-C21A = C22-C21 = C24A-C21A = C24-C21
 1.53 with sigma of 0.02
 C23-C24
 2.52 with sigma of 0.04
 C23-C22
 2.52 with sigma of 0.04
 C24-C22
 2.52 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl4 \\sim C42 \\sim Cl1 \\sim Cl2 \\sim C42A \\sim Cl5: within 2.1A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.1A
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) = Uanis(C23A)
Uanis(C22) = Uanis(C22A)
Uanis(C24) = Uanis(C24A)
Uanis(C21) = Uanis(C21A)
Uanis(C42) = Uanis(C42A)
Uanis(Cl3) = Uanis(Cl5)
5. Others
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(C21A)=1-FVAR(2)
 Sof(C21)=FVAR(2)
 Fixed Sof: Cl3(0.33333) Cl4(0.66667) C42(0.66667) H42A(0.66667) H42B(0.66667)
 Cl1(0.33333) Cl2(0.33333) C42A(0.33333) H42C(0.33333) H42D(0.33333)
 Cl5(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C42A(H42C,H42D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14),
 C18(H18), C19(H19), C25(H25), C26(H26), C28(H28), C29(H29), C34(H34), C36(H36),
  C39(H39), C40(H40)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C22A(H22D,H22E,
 H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              64525
_olex2_submission_special_instructions 'No special instructions were received'