<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_1548913
_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_absolute_configuration ad
_chemical_formula_moiety         'C32 H38 N6 Ru, 2(Cl O4)'
_chemical_formula_sum            'C32 H38 Cl2 N6 O8 Ru'
_chemical_formula_weight         806.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-03
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.016(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1503(6)
_cell_length_b                   16.4241(13)
_cell_length_c                   12.8050(11)
_cell_measurement_reflns_used    1296
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.27
_cell_measurement_theta_min      27.43
_cell_volume                     1692.9(2)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0382
_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       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27030
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.685
_diffrn_reflns_theta_min         3.495
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.712
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1100 before and 0.0775 after correction.
The Ratio of minimum to maximum transmission is 0.6845.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         5959
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0311P)^2^+1.5540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                5934
_reflns_number_total             5959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05224c2.cif
_cod_data_source_block           cxy433
_cod_depositor_comments
'Adding full bibliography for 1548910--1548914.cif.'
_cod_database_code               1548913
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Cl2 \\sim O5 \\sim O6 \\sim O7 \\sim O8: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Cl2) = Uanis(Cl2A)
Uanis(O8) = Uanis(O8A)
Uanis(O7) = Uanis(O7A)
3. Others
 Sof(Cl2A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(Cl2)=Sof(O7)=Sof(O8)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C20(H20), C21(H21), C22(H22),
 C24(H24), C25(H25)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'