<i>cis</i>-Oxoruthenium complexes supported by chiral tetradentate amine (N<sub>4</sub>) ligands for hydrocarbon oxidations.
Tse, Chun-Wai; Liu, Yungen; Wai-Shan Chow, Toby; Ma, Chaoqun; Yip, Wing-Ping; Chang, Xiao-Yong; Low, Kam-Hung; Huang, Jie-Sheng; Che, Chi-Ming; Chemical science 9 (2018) 2803–2816; doi:10.1039/c7sc05224c

data_1548914
_publ_section_title
;
 <i>cis</i>-Oxoruthenium complexes supported by chiral tetradentate amine
 (N<sub>4</sub>) ligands for hydrocarbon oxidations.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2803
_journal_page_last               2816
_journal_paper_doi               10.1039/c7sc05224c
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C30 H34 N6 Ru, 2(Cl O4), 0.83(C2 H3 N)'
_chemical_formula_sum            'C31.65 H36.48 Cl2 N6.83 O8 Ru'
_chemical_formula_weight         812.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                81.245(5)
_cell_angle_beta                 80.941(6)
_cell_angle_gamma                83.022(6)
_cell_formula_units_Z            4
_cell_length_a                   9.9120(7)
_cell_length_b                   17.5103(14)
_cell_length_c                   21.2883(17)
_cell_measurement_reflns_used    3452
_cell_measurement_temperature    100
_cell_measurement_theta_max      50.68
_cell_measurement_theta_min      3.10
_cell_volume                     3588.2(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15658
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        50.711
_diffrn_reflns_theta_max         50.711
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.402
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0908 before and 0.0650 after correction. The Ratio of minimum to maximum transmission is 0.7528. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             1665
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.640
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0682
_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^)+(0.1161P)^2^+9.6700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5361
_reflns_number_total             7360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05224c2.cif
_cod_data_source_block           cxy420_0m
_cod_depositor_comments
'Adding full bibliography for 1548910--1548914.cif.'
_cod_database_code               1548914
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45-C44
 1.53 with sigma of 0.02
 C44-C43
 1.53 with sigma of 0.02
 N10A-C56A = N10-C56
 1.34 with sigma of 0.02
 C50-C49 = C50A-C49A = C52A-C54A = C52-C54
 1.44 with sigma of 0.02
 C49-C48 = C49A-C48A = C51-C50 = C50A-C51A = C51-C52 = C52A-C51A = C55-C54 =
 C55A-C54A = C55-C56 = C55A-C56A = N10A-C53A = N10-C53
 1.39 with sigma of 0.02
 C44-C42
 2.52 with sigma of 0.04
 C43-C45
 2.52 with sigma of 0.04
 C53A-C49A = C53-C49 = C48-C50 = C48A-C50A
 2.42 with sigma of 0.04
 C54-C56 = C55-N10 = C54A-C56A = C55A-N10A
 2.42 with sigma of 0.04
 C56A-C53A = N10A-C48A = C56-C53 = N10-C48
 2.42 with sigma of 0.04
 C49-C51 = C49A-C51A = C50-C52 = C50A-C52A
 2.42 with sigma of 0.04
 C51-C54 = C51A-C54A = C52A-C55A = C52-C55
 2.42 with sigma of 0.04
 O6A-O7A \\sim O6-O7 \\sim O7A-O8A \\sim O7-O8 \\sim O8A-O6A \\sim O8-O6
 with sigma of 0.02
3. Restrained planarity
 N10, C48, C49, C50, C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 N10A, C48A, C49A, C50A, C51A, C52A, C53A, C54A, C55A, C56A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C1AA \\sim C2AA \\sim C3AA \\sim C42 \\sim C45: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
N7 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim
C38 \\sim C39: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N10A \\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim
C54A \\sim C55A \\sim C56A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7A) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C64) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C63) \\sim Ueq, : with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C44) = Uanis(C0AA)
Uanis(C43) = Uanis(C1AA)
Uanis(C46) = Uanis(C2AA)
Uanis(C41) = Uanis(C3AA)
Uanis(N10) = Uanis(N10A)
Uanis(C56) = Uanis(C56A)
Uanis(C55) = Uanis(C55A)
Uanis(C54) = Uanis(C54A)
Uanis(C52) = Uanis(C52A)
Uanis(C53) = Uanis(C53A)
Uanis(C50) = Uanis(C50A)
Uanis(C49) = Uanis(C49A)
Uanis(C48) = Uanis(C48A)
Uanis(O7) = Uanis(O7A)
Uanis(O6) = Uanis(O6A)
Uanis(O8) = Uanis(O8A)
Uanis(C51) = Uanis(C51A)
5. Others
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(C2AA)=
 Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=Sof(H42C)=Sof(H42D)=Sof(H45C)=Sof(H45D)=1-FVAR(1)
 Sof(C41)=Sof(H41)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=
 Sof(H44A)=Sof(H44B)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46)=FVAR(1)
 Sof(N10A)=Sof(C48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=
 Sof(H51A)=Sof(C52A)=Sof(C53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=
 Sof(C56A)=Sof(H56A)=Sof(N14)=Sof(C63)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=1-
 FVAR(2)
 Sof(N10)=Sof(C48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=
 Sof(C52)=Sof(C53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=FVAR(2)
 Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(3)
 Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C2AA(H2AA), C3AA(H3AA), C41(H41), C46(H46), C11(H11), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C42(H42A,H42B), C42(H42C,H42D), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C45(H45C,H45D), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C49(H49),
 C49A(H49A), C50(H50), C50A(H50A), C51(H51), C51A(H51A), C54(H54), C54A(H54A),
 C55(H55), C55A(H55A), C56(H56), C56A(H56A), C1(H1), C2(H2), C3(H3), C6(H6),
 C7(H7), C8(H8), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26)
6.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              57040
_olex2_submission_special_instructions 'No special instructions were received'