Two isomers of a bis(diphenylphosphino)phosphinine, and the synthesis and reactivity of Ru arene/Cp* phosphinophosphinine complexes
Newland, Robert J.; Delve, Matthew P.; Wingad, Richard L.; Mansell, Stephen M.; New Journal of Chemistry 42 (2018) 19625–; doi:10.1039/C8NJ03632B

data_7057882
_publ_section_title
;
 Two isomers of a bis(diphenylphosphino)phosphinine, and the synthesis and
 reactivity of Ru arene/Cp* phosphinophosphinine complexes
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19625
_journal_paper_doi               10.1039/C8NJ03632B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C31 H41 Cl O P2 Ru Si'
_chemical_formula_sum            'C31 H41 Cl O P2 Ru Si'
_chemical_formula_weight         656.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                92.281(2)
_cell_angle_beta                 105.461(2)
_cell_angle_gamma                101.298(2)
_cell_formula_units_Z            4
_cell_length_a                   14.6758(5)
_cell_length_b                   14.7658(4)
_cell_length_c                   15.2176(3)
_cell_measurement_reflns_used    16772
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.6620
_cell_measurement_theta_min      3.8980
_cell_volume                     3101.92(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -68.00  28.00   1.00    3.00    --  -41.67  57.00  60.00   96
  2  \w    -64.00  31.00   1.00    3.00    --  -41.67  38.00-150.00   95
  3  \w   -116.00 -10.00   1.00    3.00    --  -41.67 -77.00  60.00  106
  4  \w   -112.00 -15.00   1.00    3.00    --  -41.67 -57.00 -90.00   97
  5  \w      1.00  82.00   1.00    3.00    --   41.67 -99.00-180.00   81
  6  \w     41.00 139.00   1.00   10.00    --  111.00 -61.00-120.00   98
  7  \w     32.00 111.00   1.00   10.00    --  111.00 -99.00-130.00   79
  8  \w     40.00 135.00   1.00   10.00    --  111.00 -45.00  60.00   95
  9  \w     36.00 135.00   1.00   10.00    --  111.00 -30.00   0.00   99
 10  \w     39.00 121.00   1.00   10.00    --  111.00-125.00 120.00   82
 11  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00 -30.00   79
 12  \w     39.00 121.00   1.00   10.00    --  111.00-125.00  60.00   82
 13  \w     36.00 135.00   1.00   10.00    --  111.00 -30.00 150.00   99
 14  \w     39.00 121.00   1.00   10.00    --  111.00-125.00 -30.00   82
 15  \w     87.00 178.00   1.00   10.00    --  111.00  45.00  30.00   91
 16  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00   0.00   79
 17  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00-180.00   79
 18  \w     88.00 155.00   1.00   10.00    --  111.00 -15.00 120.00   67
 19  \w     89.00 178.00   1.00   10.00    --  111.00  36.00   2.29   89
 20  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00-120.00   79
 21  \w     39.00 121.00   1.00   10.00    --  111.00-125.00-120.00   82
 22  \w     30.00 109.00   1.00   10.00    --  111.00 -94.00 150.00   79
 23  \w     39.00 121.00   1.00   10.00    --  111.00-125.00 150.00   82
 24  \w     37.00 142.00   1.00   10.00    --  111.00 -77.00  30.00  105
 25  \w     24.00 178.00   1.00   10.00    --  111.00   0.00-180.00  154
 26  \w     88.00 155.00   1.00   10.00    --  111.00 -15.00 120.00   67
 27  \w    140.00 165.00   1.00   10.00    --  111.00  56.00  80.61   25
 28  \w    124.00 160.00   1.00   10.00    --  111.00 125.00 -90.00   36
 29  \w     92.00 121.00   1.00   10.00    --  111.00-125.00-180.00   29
 30  \w     81.00 109.00   1.00   10.00    --  111.00 -94.00  30.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0783294000
_diffrn_orient_matrix_UB_12      -0.0453638000
_diffrn_orient_matrix_UB_13      -0.0221109000
_diffrn_orient_matrix_UB_21      0.0667883000
_diffrn_orient_matrix_UB_22      0.0330823000
_diffrn_orient_matrix_UB_23      0.0973144000
_diffrn_orient_matrix_UB_31      -0.0428707000
_diffrn_orient_matrix_UB_32      -0.0909716000
_diffrn_orient_matrix_UB_33      0.0343404000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.143
_diffrn_reflns_theta_min         3.739
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.394
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12852
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10562
_reflns_number_total             12852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03632b2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7057881--7057886.cif.'
_cod_original_cell_volume        3101.93(15)
_cod_database_code               7057882
_chemical_oxdiff_formula         'C31 H39 Cl P2 Ru Si'
_chemical_oxdiff_usercomment     '@ 120 K RJN331'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C34(H34), C35(H35), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              59396
_shelx_hkl_checksum              37466
_shelx_shelxl_version_number     2014/7
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.845