Unusual C-O bond cleavage of aromatic ethers in ruthenium complexes bearing a 2-alkoxypyridyl fragment.
Deng, Danfeng; Hu, Bowen; Yang, Min; Chen, Dafa; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13614–13621; doi:10.1039/c9dt03020d

data_7700854
_publ_section_title
;
 Unusual C-O bond cleavage of aromatic ethers in ruthenium complexes
 bearing a 2-alkoxypyridyl fragment.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13614
_journal_page_last               13621
_journal_paper_doi               10.1039/c9dt03020d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C47 H39 N2 O2 P2 Ru, Cl, C H2 Cl2'
_chemical_formula_sum            'C48 H41 Cl3 N2 O2 P2 Ru'
_chemical_formula_weight         947.19
_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   mixed
_audit_creation_date             2019-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-22 deposited with the CCDC.    2019-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                101.8130(10)
_cell_angle_beta                 106.7340(10)
_cell_angle_gamma                94.5840(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2506(4)
_cell_length_b                   13.7227(5)
_cell_length_c                   17.3369(6)
_cell_measurement_reflns_used    6421
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      26.897
_cell_measurement_theta_min      2.408
_cell_volume                     2260.75(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      303.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.1238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.532
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1297 before and 0.0749 after correction. The Ratio of minimum to maximum transmission is 0.7121. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         13837
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0681P)^2^+2.0601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7861
_reflns_number_total             13837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03020d2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 7700852--7700855.cif.'
_cod_database_code               7700854
_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
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 Cl2-Cl3 = Cl2A-Cl3A
 2.903 with sigma of 0.02
 C48-Cl2 = C48-Cl3 = C48A-Cl2A = C48A-Cl3A
 1.78 with sigma of 0.02
3. Rigid bond restraints
 Cl2A, Cl3A, Cl3, C48, Cl2, C48A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23, C28, C27, C26, C25, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim C48 \\sim Cl3 \\sim Cl3A \\sim C48A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C23 \\sim C28 \\sim C27 \\sim C26 \\sim C25 \\sim C24: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Cl3A)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl3)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(1)
6.a Riding coordinates:
 Ru1(H)
6.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C48A(H48C,H48D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C22(H22), C21(H21), C20(H20), C19(H19), C18(H18),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
6.d Fitted hexagon refined as free rotating group:
 C17(C22,C21,C20,C19,C18), C23(C24,C25,C26,C27,C28), C41(C42,C43,C44,C45,C46)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              11153
_olex2_submission_special_instructions 'No special instructions were received'