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_7700852
_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         'C49 H39 N2 O3 P2 Ru, Cl, 3(C H2 Cl2)'
_chemical_formula_sum            'C52 H45 Cl7 N2 O3 P2 Ru'
_chemical_formula_weight         1157.06
_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
_audit_creation_date             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.    2019-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                83.417(3)
_cell_angle_beta                 87.037(3)
_cell_angle_gamma                74.939(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8566(5)
_cell_length_b                   14.8810(5)
_cell_length_c                   15.3961(5)
_cell_measurement_reflns_used    7673
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.2360
_cell_measurement_theta_min      3.4640
_cell_volume                     2605.17(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9737
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  40.00   1.00   15.00    --   18.81 -57.00   0.00   90
  2  \w     -2.00  69.00   1.00   15.00    --   18.81-113.00-140.00   71
  3  \w     41.00  88.00   1.00   15.00    --   18.81  57.00 150.00   47
  4  \w     -4.00  76.00   1.00   15.00    --   18.81  77.00  90.00   80
  5  \w    -92.00 -66.00   1.00   15.00    --  -19.74 -37.00  90.00   26
  6  \w    -57.00 -30.00   1.00   15.00    --  -19.74 -57.00 -30.00   27
  7  \w    -84.00  10.00   1.00   15.00    --  -19.74 -77.00 -90.00   94
  8  \w    -15.00  32.00   1.00   15.00    --  -19.74  19.00  90.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388915000
_diffrn_orient_matrix_UB_12      -0.0293769000
_diffrn_orient_matrix_UB_13      0.0042437000
_diffrn_orient_matrix_UB_21      0.0109952000
_diffrn_orient_matrix_UB_22      -0.0098452000
_diffrn_orient_matrix_UB_23      0.0454029000
_diffrn_orient_matrix_UB_31      -0.0469733000
_diffrn_orient_matrix_UB_32      0.0387770000
_diffrn_orient_matrix_UB_33      0.0085105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24051
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.154
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         11974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1149P)^2^+7.3346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9201
_reflns_number_total             11974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03020d2.cif
_cod_data_source_block           20170619c-ddf2022
_cod_depositor_comments
'Adding full bibliography for 7700852--7700855.cif.'
_cod_original_cell_volume        2605.17(16)
_cod_database_code               7700852
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B)
2.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C13(H13), C32(H32), C38(H38), C9(H9), C36(H36), C29(H29), C35(H35),
 C7(H7), C19(H19), C45(H45), C40(H40), C47(H47), C8(H8), C42(H42), C3(H3),
 C39(H39), C48(H48), C41(H41), C4(H4), C46(H46), C25(H25), C2(H2), C23(H23),
 C16(H16), C26(H26), C33(H33), C34(H34), C28(H28), C14(H14), C20(H20), C15(H15),
  C27(H27), C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              30587
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.798