[RuCl2(η(6)-p-cymene)] complexes bearing phosphinous acid ligands: preparation, application in C-H bond functionalization and mechanistic investigations.
Graux, Lionel V.; Giorgi, Michel; Buono, Gérard; Clavier, Hervé; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6491–6502; doi:10.1039/c5dt04683a

data_7038585
_publ_section_title
;
 [RuCl2(\h(6)-p-cymene)] complexes bearing phosphinous acid ligands:
 preparation, application in C-H bond functionalization and mechanistic
 investigations.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6491
_journal_page_last               6502
_journal_paper_doi               10.1039/c5dt04683a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C22 H23 Cl2 F2 O P Ru'
_chemical_formula_sum            'C22 H23 Cl2 F2 O P Ru'
_chemical_formula_weight         544.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date
;
'Tue Mar 04 19:35:45 2014'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_audit_update_record
;
2015-10-29 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 95.422(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.0912(3)
_cell_length_b                   11.0395(2)
_cell_length_c                   16.0317(4)
_cell_measurement_reflns_used    8038
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0090
_cell_measurement_theta_min      3.6950
_cell_volume                     2306.54(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
  1 omega  -78.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        9.6643    0.0000  150.0000 176

  2 omega  -84.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987  -38.0000  -90.0000 99

  3 omega  -65.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        9.6643  -38.0000    0.0000 56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0054027000
_diffrn_orient_matrix_UB_12      0.0490990000
_diffrn_orient_matrix_UB_13      -0.0286159000
_diffrn_orient_matrix_UB_21      0.0344707000
_diffrn_orient_matrix_UB_22      -0.0286283000
_diffrn_orient_matrix_UB_23      -0.0253208000
_diffrn_orient_matrix_UB_31      -0.0417713000
_diffrn_orient_matrix_UB_32      -0.0299814000
_diffrn_orient_matrix_UB_33      -0.0226863000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19215
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.796
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0359P)^2^+1.7663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4096
_reflns_number_total             5279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04683a2.cif
_cod_data_source_block           lgr2044b
_cod_depositor_comments
'Adding full bibliography for 7038583--7038589.cif.'
_cod_database_code               7038585
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.839
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C18(H18), C19(H19), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'