C‒H versus O‒H Bond Activation in Phosphino-alcohol Ligands: Synthesis of the α-Hydroxy-alkyl Ruthenium(II) Derivatives [RuCl{κ2(P,C)-Ph2PC6H4C(R)OH}(η6-arene)]
Díaz-Álvarez, Alba E.; Vidal, Cristian; Suárez, Francisco J.; Díez, Josefina; Cadierno, Victorio; Crochet, Pascale; Organometallics 34 (2015) 3670–; doi:10.1021/acs.organomet.5b00074

data_4086105
_publ_section_title
;
 C--H versus O--H Bond Activation in Phosphino-alcohol Ligands: Synthesis
 of the \a-Hydroxy-alkyl Ruthenium(II) Derivatives
 [RuCl{\k2(P,C)-Ph2PC6H4C(R)OH}(\h6-arene)]
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3670
_journal_paper_doi               10.1021/acs.organomet.5b00074
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C29 H31 Cl O P Ru, F6 P'
_chemical_formula_sum            'C29 H31 Cl F6 O P2 Ru'
_chemical_formula_weight         708.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5393(4)
_cell_length_b                   14.8640(5)
_cell_length_c                   15.3966(5)
_cell_measurement_reflns_used    2995
_cell_measurement_temperature    150(2)
_cell_volume                     2869.68(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    DIRDIF-2008
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_laue_measured_fraction_full 1.000
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32806
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.902
_diffrn_reflns_theta_min         4.134
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.888
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  0.3066
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       Prisme
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 1976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5357
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+10.1645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.758
_reflns_friedel_fraction_full    0.993
_reflns_friedel_fraction_max     0.973
_reflns_number_gt                4882
_reflns_number_total             5357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00074_si_001.cif
_cod_data_source_block           6b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4086105.cif.
;
_cod_database_code               4086105
_shelxl_version_number           2014-3
_shelx_res_checksum              32011
_shelx_hkl_checksum              37285