Reaction of an oxaruthenacycle with DMAD. Stoichiometric transformations of 2,6-xylenol to allylic phenols and benzopyrans via sp3 C‒H bond cleavage reaction
Hirano, Masafumi; Izhab, Izirwan Bin; Kurata, Naoki; Koizumi, Kaori; Komine, Nobuyuki; Komiya, Sanshiro; Dalton Transactions  (2009) 3270–3279; doi:10.1039/b821179e

data_7001100
_publ_section_title
;
 Reaction of an oxaruthenacycle with DMAD. Stoichiometric
 transformations of 2,6-xylenol to allylic phenols and benzopyrans via
 sp3 C--H bond cleavage reaction
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3270
_journal_page_last               3279
_journal_paper_doi               10.1039/b821179e
_journal_year                    2009
_chemical_formula_moiety         'C24 H43 Cl2 O5 P3 Ru '
_chemical_formula_sum            'C24 H43 Cl2 O5 P3 Ru'
_chemical_formula_weight         676.50
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.11(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   22.265(8)
_cell_length_b                   15.629(14)
_cell_length_c                   9.049(3)
_cell_measurement_reflns_used    4
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      15.3
_cell_volume                     3148(3)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8584
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1400.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     315
_refine_ls_number_reflns         7233
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                2968
_reflns_number_total             7233
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b821179e.txt
_cod_data_source_block           '_complex3'
_cod_original_formula_sum        'C24 H43 Cl2 O5 P3 Ru '
_cod_database_code               7001100