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_7057884
_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         'C49 H52 Cl3 Fe N2 O P3, 4(C H2 Cl2)'
_chemical_formula_sum            'C53 H60 Cl11 Fe N2 O P3'
_chemical_formula_weight         1279.74
_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
_audit_creation_date             2016-01-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                104.833(2)
_cell_angle_beta                 93.541(2)
_cell_angle_gamma                114.316(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3741(5)
_cell_length_b                   14.0430(5)
_cell_length_c                   19.6151(7)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.31
_cell_volume                     2948.1(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51076
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.810
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0571 before and 0.0463 after correction.
The Ratio of minimum to maximum transmission is 0.9217.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       Block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         13575
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0299P)^2^+4.5836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12190
_reflns_number_total             13575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03632b2.cif
_cod_data_source_block           7_HCl_H2O_FeCl2
_cod_depositor_comments
'Adding full bibliography for 7057881--7057886.cif.'
_cod_database_code               7057884
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.02
 N2-H2
 0.9 with sigma of 0.02
3. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C50(H50A,H50B), C53(H53A,H53B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C24(H24), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C43(H43), C45(H45)
4.c Disordered Me refined with riding coordinates:
 C26(H26A,H26B,H26C,H26D,H26E,H26F)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              23104
_shelx_hkl_checksum              49514
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'