Syntheses and Thermolysis of Arylpalladium Hydroxide Complexes: Implications for C(sp2)–OH Bond-Forming Reductive Elimination To Generate Phenol Derivatives
Hayashi, Yumi; Wada, Shinji; Yamashita, Makoto; Nozaki, Kyoko; Organometallics 31 (2012) 1073–; doi:10.1021/om201142s

data_4068141
_publ_section_title
;
 Syntheses and Thermolysis of Arylpalladium Hydroxide Complexes:
 Implications for C(sp2)--OH Bond-Forming Reductive Elimination To
 Generate Phenol Derivatives
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              1073
_journal_paper_doi               10.1021/om201142s
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C58 H110 O7 P4 Pd2'
_chemical_formula_weight         1256.14
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.83(2)
_cell_angle_beta                 84.948(20)
_cell_angle_gamma                82.368(19)
_cell_formula_units_Z            1
_cell_length_a                   8.958(5)
_cell_length_b                   10.801(6)
_cell_length_c                   16.399(10)
_cell_measurement_reflns_used    5070
_cell_measurement_temperature    103.1500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0724
_cell_volume                     1565.0(16)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0370
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_diffrn_reflns_limit_l_max       19
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_diffrn_reflns_number            10321
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_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.9312
_exptl_absorpt_correction_T_min  0.7366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.45
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_refine_diff_density_max         0.770
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_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     362
_refine_ls_number_reflns         5383
_refine_ls_number_restraints     61
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_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0407
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+1.6779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                4606
_reflns_number_total             5383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201142s_si_002.cif
_cod_data_source_block           5-CO2Me
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1565.1(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068141