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_7001101
_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           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.068(3)
_cell_length_b                   13.970(3)
_cell_length_c                   13.023(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      15.1
_cell_volume                     3105.2(11)
_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    SIR92
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6016
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.50
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 560 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4281
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.3405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                3035
_reflns_number_total             4281
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b821179e.txt
_cod_data_source_block           '_IZI0211'
_cod_original_cell_volume        3105.1(10)
_cod_original_formula_sum        'C24 H43 Cl2 O5 P3 Ru '
_cod_database_code               7001101