Catalytic Nitrile Hydration with [Ru(η6-p-cymene)Cl2(PR2R′)] Complexes: Secondary Coordination Sphere Effects with Phosphine Oxide and Phosphinite Ligands
Knapp, Spring Melody M.; Sherbow, Tobias J.; Yelle, Robert B.; Juliette, J. Jerrick; Tyler, David R.; Organometallics 32 (2013) 3744–; doi:10.1021/om400380j

data_4081041
_publ_section_title
;
 Catalytic Nitrile Hydration with [Ru(\h6-p-cymene)Cl2(PR2R&#x2032;)]
 Complexes: Secondary Coordination Sphere Effects with Phosphine Oxide and
 Phosphinite Ligands
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3744
_journal_paper_doi               10.1021/om400380j
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H28 Cl2 O1 P2 Ru1'
_chemical_formula_sum            'C15 H28 Cl2 O P2 Ru'
_chemical_formula_weight         458.31
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-01-18
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90.0
_cell_angle_beta                 107.006(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.00000
_cell_length_a                   6.47519(14)
_cell_length_b                   32.4129(6)
_cell_length_c                   9.8840(3)
_cell_measurement_reflns_used    15621
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.4233
_cell_measurement_theta_min      3.7642
_cell_volume                     1983.74(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.3533
_diffrn_detector_type            'Oxford Diffraction Ruby CCD'
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.9662
_diffrn_measurement_details
;
  1 omega  -63.00   32.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -57.0000   30.0000 95

  2 omega   -5.00   22.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000  -90.0000 27

  3 omega  -10.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000 -150.0000 63

  4 omega   -4.00   38.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   37.0000 -180.0000 42

  5 omega  -82.00  -23.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208  -57.0000 -120.0000 59

  6 omega  -66.00    6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208  -57.0000  -90.0000 72

  7 omega  -63.00   39.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -46.0000   94.0000 102

  8 omega  -65.00   37.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -37.0000 -180.0000 102

  9 omega  -18.00   85.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000   60.0000 103

 10 omega  -18.00   66.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000 -120.0000 84

 11 omega  -42.00   62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   57.0000  -60.0000 104

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0340665000
_diffrn_orient_matrix_UB_12      -0.0109095000
_diffrn_orient_matrix_UB_13      0.0649769000
_diffrn_orient_matrix_UB_21      0.0604551000
_diffrn_orient_matrix_UB_22      -0.0136701000
_diffrn_orient_matrix_UB_23      -0.0297076000
_diffrn_orient_matrix_UB_31      0.0911475000
_diffrn_orient_matrix_UB_32      0.0131441000
_diffrn_orient_matrix_UB_33      0.0229769000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22395
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         29.4233
_diffrn_reflns_theta_min         3.7642
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.3975
_exptl_crystal_size_mid          0.1377
_exptl_crystal_size_min          0.0751
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.50
_refine_ls_abs_structure_details 'Flack (1983), 2348 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0103
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4966
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.0063355
_refine_ls_shift/su_mean         0.0003062
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 4.88P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0678
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0678
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              43
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                4845
_reflns_number_total             4966
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.25
_oxford_diffrn_Wilson_scale      0.39
_oxford_refine_ls_r_factor_ref   0.0295
_oxford_refine_ls_scale          1.701(6)
_oxford_reflns_number_all        4966
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om400380j_si_002.cif
_cod_data_source_block           RuDMPMO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1983.74(8)
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_sum        'C15 H28 Cl2 O1 P2 Ru1'
_cod_database_code               4081041
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;