The first crystallographically characterised ruthenium(vi) alkylimido porphyrin competent for aerobic epoxidation and hydrogen atom abstraction.
Shing, Ka-Pan; Wan, Qingyun; Chang, Xiao-Yong; Che, Chi-Ming; Chemical communications (Cambridge, England) 56 (2020) 4428–4431; doi:10.1039/c9cc09972g

data_7126173
_publ_section_title
;
 The first crystallographically characterised ruthenium(vi) alkylimido
 porphyrin competent for aerobic epoxidation and hydrogen atom
 abstraction.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4428
_journal_page_last               4431
_journal_paper_doi               10.1039/c9cc09972g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C48 H26 F8 N6 Ru, 3(C6 H6)'
_chemical_formula_sum            'C66 H44 F8 N6 Ru'
_chemical_formula_weight         1174.14
_chemical_properties_physical    Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6211(4)
_cell_length_b                   12.9645(4)
_cell_length_c                   17.2046(5)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.31
_cell_measurement_theta_min      3.50
_cell_volume                     2815.12(15)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32379
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.300
_diffrn_reflns_theta_max         67.300
_diffrn_reflns_theta_min         4.270
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1011 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.7055. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0606
_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/[\s^2^(Fo^2^)+(0.1047P)^2^+5.5861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2282
_reflns_number_total             2609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09972g2.cif
_cod_data_source_block           cxy380_0m
_cod_depositor_comments
'Adding full bibliography for 7126171--7126173.cif.'
_cod_database_code               7126173
_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
 C18_$1-C17 = C18-C17 = C18_$2-C18 = C18_$2-C17_$2
 1.39 with sigma of 0.02
 C25-C24 = C24-C23 = C21-C20 = C23-C22 = C20-C19
 1.39 with sigma of 0.02
 C14-C14_$1 = C15_$1-C14_$1 = C16_$1-C15_$1 = C16-C16_$1
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F2) = Uanis(F2A)
Uanis(F1) = Uanis(F1A)
Uanis(C10A) = Uanis(C10)
Uanis(C9A) = Uanis(C9)
Uanis(C8A) = Uanis(C8)
Uanis(C6A) = Uanis(C6)
Uanis(C7A) = Uanis(C7)
Uanis(C11A) = Uanis(C11)
Uanis(C22) = Uanis(C21) = Uanis(C23) = Uanis(C20) = Uanis(C24) = Uanis(C19) =
Uanis(C25)
4. Others
 Sof(F1A)=Sof(F2A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=
 Sof(H10A)=Sof(C11A)=Sof(C6A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=FVAR(1)
 Sof(C18)=Sof(H18)=1-FVAR(2)
 Sof(C17)=Sof(H17)=0.5*(1-FVAR(3))
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=0.5*FVAR(3)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=1-FVAR(3)
 Sof(C22)=Sof(H22)=Sof(C25)=Sof(H25)=0.5*(1-FVAR(4))
 Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(3)
 Fixed Sof: H13A(0.5) H13B(0.5) H13C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C8(H8), C9(H9), C10(H10), C8A(H8A), C9A(H9A), C10A(H10A),
 C22(H22), C23(H23), C24(H24), C25(H25), C14(H14), C15(H15), C16(H16), C19(H19),
  C20(H20), C21(H21), C17(H17), C18(H18)
5.b Fitted hexagon refined as free rotating group:
 C7A(C8A,C9A,C10A,C11A,C6A)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'