Expanding the chemistry of ring-fused 1,4-diphosphinines by stable mono anion formation.
Begum, Imtiaz; Schnakenburg, Gregor; Kelemen, Zsolt; Nyulászi, László; Boeré, René T; Streubel, Rainer; Chemical communications (Cambridge, England) 54 (2018) 13555–13558; doi:10.1039/c8cc08158a

data_7122594
_publ_section_title
;
 Expanding the chemistry of ring-fused 1,4-diphosphinines by stable mono
 anion formation.
;
_journal_issue                   96
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13555
_journal_page_last               13558
_journal_paper_doi               10.1039/c8cc08158a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C30 H62 K N3 O3 P2 S4 Si2'
_chemical_formula_sum            'C30 H62 K N3 O3 P2 S4 Si2'
_chemical_formula_weight         798.28
_chemical_name_systematic        IB-365
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-09-07 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                77.937(5)
_cell_angle_beta                 83.960(5)
_cell_angle_gamma                88.797(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9737(6)
_cell_length_b                   14.8907(9)
_cell_length_c                   16.9261(11)
_cell_measurement_reflns_used    6512
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.68
_cell_volume                     2199.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.1279
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14534
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.676
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.7658
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0785P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4338
_reflns_number_total             7756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08158a2.cif
_cod_data_source_block           5545
_cod_depositor_comments
'Adding full bibliography for 7122593--7122597.cif.'
_cod_database_code               7122594
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C29
 1.38 with sigma of 0.01
 O3S-C29S
 1.38 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(C27S) \\sim Ueq, Uanis(C28S) \\sim Ueq, Uanis(C29S) \\sim Ueq,
Uanis(C30S) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Sof(C28S)=Sof(H28C)=Sof(H28D)=Sof(C30S)=Sof(H30D)=Sof(H30E)=Sof(H30F)=
 Sof(C29S)=Sof(H29C)=Sof(H29D)=Sof(O3S)=Sof(C27S)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 1-FVAR(1)
 Sof(O3)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C10(H10A,H10B), C11(H11A,H11B), C20(H20A,H20B),
 C21(H21A,H21B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B), C29(H29A,H29B),
  C28S(H28C,H28D), C29S(H29C,H29D)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C30S(H30D,H30E,
 H30F), C27S(H27D,H27E,H27F)
;
_shelx_res_checksum              48263
_shelx_hkl_checksum              1267
_olex2_submission_special_instructions 'No special instructions were received'