Hydrochlorination of Ruthenaphosphaalkenyls: Unexpectedly Facile Access to Alkylchlorohydrophosphane Complexes
Greenacre, Victoria K.; Day, Iain J.; Crossley, Ian R.; Organometallics 36 (2017) 435–; doi:10.1021/acs.organomet.6b00829

data_4089175
_publ_section_title
;
 Hydrochlorination of Ruthenaphosphaalkenyls: Unexpectedly Facile Access
 to Alkylchlorohydrophosphane Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              435
_journal_paper_doi               10.1021/acs.organomet.6b00829
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C41 H42 Cl3 O P3 Ru Si, C H2 Cl2'
_chemical_formula_sum            'C42 H44 Cl5 O P3 Ru Si'
_chemical_formula_weight         964.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                99.390(6)
_cell_angle_beta                 101.138(5)
_cell_angle_gamma                116.048(7)
_cell_formula_units_Z            2
_cell_length_a                   12.5318(8)
_cell_length_b                   13.0932(11)
_cell_length_c                   15.9653(10)
_cell_measurement_reflns_used    3372
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.5730
_cell_measurement_theta_min      3.9120
_cell_volume                     2215.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     10.00 104.00   1.00    1.87    --   36.63  77.00  90.00   94
  2  \w     41.00 176.00   1.00    7.49    --  107.00   0.00  60.00  135
  3  \w    110.00 167.00   1.00    7.49    --  107.00  45.00 -90.00   57
  4  \w     87.00 124.00   1.00    7.49    --  107.00 -45.00  30.00   37
  5  \w     45.00 143.00   1.00    7.49    --  107.00 -93.00 116.62   98
  6  \w     41.00 124.00   1.00    7.49    --  107.00 -45.00 -60.00   83
  7  \w     45.00 122.00   1.00    7.49    --  107.00 -45.00-150.00   77
  8  \w     43.00 142.00   1.00    7.49    --  107.00 -92.00 -61.25   99
  9  \w     39.00  76.00   1.00    1.87    --   36.63 -99.00-150.00   37
 10  \w     42.00  84.00   1.00    7.49    --  107.00 -45.00  30.00   42
 11  \w     41.00 124.00   1.00    7.49    --  107.00 -45.00 120.00   83
 12  \w    -24.00   6.00   1.00    1.87    --   36.63 -99.00-150.00   30
 13  \w    -31.00  63.00   1.00    1.87    --   36.63 -77.00 -30.00   94
 14  \w   -106.00 -22.00   1.00    1.87    --  -36.63 -38.00-150.00   84
 15  \w   -104.00 -53.00   1.00    1.87    --  -36.63 178.00  60.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.1070
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11632
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.129
_diffrn_reflns_theta_min         3.916
_exptl_absorpt_coefficient_mu    7.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8091
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1214P)^2^+5.5894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6059
_reflns_number_total             8091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00829_si_003.cif
_cod_data_source_block           vg-15-067_2
_cod_database_code               4089175
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-H1
 1.2 with sigma of 0.02
3. Others
 Fixed Sof: Cl5(0.5) Cl6(0.5) H42A(0.5) H42B(0.5) H42C(0.5) H42D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C42(H42A,H42B), C42(H42C,H42D)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;