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_7126171
_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_absolute_configuration ad
_chemical_formula_moiety         'C54 H35 F8 N5 O Ru, C6 H6'
_chemical_formula_sum            'C60 H41 F8 N5 O Ru'
_chemical_formula_weight         1101.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            4
_cell_length_a                   10.8463(2)
_cell_length_b                   20.3999(4)
_cell_length_c                   21.4989(4)
_cell_measurement_reflns_used    9620
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.58
_cell_measurement_theta_min      2.99
_cell_volume                     4756.92(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0465
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62228
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.598
_diffrn_reflns_theta_max         67.598
_diffrn_reflns_theta_min         2.986
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.370
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0861 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.7486. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 3636 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         8519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0598P)^2^+7.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                8375
_reflns_number_total             8519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09972g2.cif
_cod_data_source_block           cxy369_0m
_cod_depositor_comments
'Adding full bibliography for 7126171--7126173.cif.'
_cod_database_code               7126171
_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.a Ternary CH refined with riding coordinates:
 C47(H47), C49(H49), C51(H51)
2.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C48(H48A,H48B), C50(H50A,H50B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C19(H19),
 C20(H20), C21(H21), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C35(H35),
  C36(H36), C41(H41), C42(H42), C43(H43), C60(H60), C55(H55), C56(H56),
 C57(H57), C58(H58), C59(H59)
2.d Fitted hexagon refined as free rotating group:
 C60(C55,C56,C57,C58,C59)
;
_olex2_submission_special_instructions 'No special instructions were received'