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_7700853
_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
'C48 H36 N2 O3 P2 Ru, 0.5(C H2 Cl2), 2.5(C H4 O)'
_chemical_formula_sum            'C51 H47 Cl N2 O5.5 P2 Ru'
_chemical_formula_weight         974.36
_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
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-22 deposited with the CCDC.    2019-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                72.075(2)
_cell_angle_beta                 79.871(2)
_cell_angle_gamma                89.554(2)
_cell_formula_units_Z            4
_cell_length_a                   11.7433(6)
_cell_length_b                   19.4520(9)
_cell_length_c                   21.6447(11)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.225
_cell_measurement_theta_min      2.277
_cell_volume                     4625.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       '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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON \/c\`o detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            75693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_min         2.033
_diffrn_source                   'ImuS 3.0'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1430 before and 0.0859 after correction.
The Ratio of minimum to maximum transmission is 0.6765.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.108
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         22855
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0803P)^2^+12.1996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16005
_reflns_number_total             22855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03020d2.cif
_cod_data_source_block           20181018f_0m
_cod_depositor_comments
'Adding full bibliography for 7700852--7700855.cif.'
_cod_original_formula_sum        'C51 H47 Cl N2 O5.50 P2 Ru'
_cod_database_code               7700853
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H11A of O11, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H12 of O12, H10 of O10, H9A of O9, H8A of O8, H7A of O7
2. Restrained distances
 H11A-O3
 2.4 with sigma of 0.01
 H11A-O11
 0.84 with sigma of 0.001
3. Rigid bond restraints
 O11, C102, O12, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O11 \\sim C102 \\sim O12 \\sim C103: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(O12)=Sof(H12)=Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(H10L)=1-FVAR(1)
 Sof(O11)=Sof(H11A)=Sof(C102)=Sof(H10G)=Sof(H10H)=Sof(H10I)=FVAR(1)
 Fixed Y: O12(0.0849) C103(0.02208)
6.a Riding coordinates:
 O7(H7A), O8(H8A), O9(H9A), O10(H10)
6.b Rotating group:
 O11(H11A)
6.c Ternary CH refined with riding coordinates:
 C11(H11), C58(H58)
6.d Secondary CH2 refined with riding coordinates:
 C97(H97A,H97B)
6.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C54(H54),
 C55(H55), C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67),
  C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94)
6.f Idealised Me refined as rotating group:
 C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C101(H10D,
 H10E,H10F), C102(H10G,H10H,H10I), C103(H10J,H10K,H10L)
6.g Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_shelx_res_checksum              71483
_olex2_submission_special_instructions 'No special instructions were received'