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_7057886
_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         'C30 H36 Cl O P2 Ru, 0.5(C H2 Cl2), F6 P'
_chemical_formula_sum            'C30.5 H37 Cl2 F6 O P3 Ru'
_chemical_formula_weight         798.48
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-25
_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                90
_cell_angle_beta                 90.340(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.8172(4)
_cell_length_b                   37.4359(16)
_cell_length_c                   19.6657(9)
_cell_measurement_reflns_used    9157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.37
_cell_volume                     6491.1(5)
_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      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            222582
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.392
_diffrn_reflns_theta_min         2.340
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       orange
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.188
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         16043
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+16.2441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14225
_reflns_number_total             16043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03632b2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7057881--7057886.cif.'
_cod_original_formula_sum        'C30.50 H37 Cl2 F6 O P3 Ru'
_cod_database_code               7057886
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H61A,H61B,H1} of C61, All O(H) groups
 At 1.5 times of:
  {H25A,H25B,H25C} of C25, {H6A,H6B,H6C} of C6, {H36A,H36B,H36C} of C36,
  {H29A,H29B,H29C} of C29, {H27A,H27B,H27C} of C27, {H26A,H26B,H26C} of C26,
  {H28A,H28B,H28C} of C28, {H30A,H30B,H30C} of C30, {H57A,H57B,H57C} of C57,
  {H56A,H56B,H56C} of C56, {H60A,H60B,H60C} of C60, {H55A,H55B,H55C} of C55,
  {H58A,H58B,H58C} of C58, {H59A,H59B,H59C} of C59
2. Restrained distances
 O1-H1
 0.96 with sigma of 0.02
 O2-H2
 0.96 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C33(H33), C34(H34), C35(H35),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              57092
_shelx_hkl_checksum              37219
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'