1,4-Additions of tricyclic 1,4-diphosphinines - a novel system to study σ-bond activation and π-π dispersion interactions.
Koner, Abhishek; Kelemen, Zsolt; Schnakenburg, Gregor; Nyulászi, László; Streubel, Rainer; Chemical communications (Cambridge, England) 54 (2018) 1182–1184; doi:10.1039/c7cc09349g

data_7121138
_publ_section_title
;
 1,4-Additions of tricyclic 1,4-diphosphinines - a novel system to study
 \s-bond activation and \p-\p dispersion interactions.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1182
_journal_page_last               1184
_journal_paper_doi               10.1039/c7cc09349g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '4(C32 H43 N5 O2 P2 S2), C H2 Cl2'
_chemical_formula_sum            'C129 H174 Cl2 N20 O8 P8 S8'
_chemical_formula_weight         2708.01
_chemical_name_systematic        ABK-445
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.3663(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.7111(12)
_cell_length_b                   14.5378(7)
_cell_length_c                   21.9682(16)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.30
_cell_volume                     7126.5(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48634
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0850 before and 0.0586 after correction. The Ratio of minimum to maximum transmission is 0.9243. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8586
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1137P)^2^+17.3882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6399
_reflns_number_total             8586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09349g2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7121136--7121139.cif.'
_cod_database_code               7121138
_shelx_shelxl_version_number     2014/7
_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
 C33-Cl1 = C33-Cl2
 1.74 with sigma of 0.01
 C17S-C18S
 1.49 with sigma of 0.01
 C18-C17 = C18S-C17S = C17-C16 = C17S-C16
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C18S \\sim C18 \\sim C17 \\sim C17S \\sim C16 \\sim C15: within 2A with sigma
of 0.003 and sigma for terminal atoms of 0.006
4. Rigid body (RIGU) restrains
 C18S, C18, C33, Cl1, Cl2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H16C)=Sof(H16D)=Sof(C18S)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C17S)=
 Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(1)
 Fixed Sof: Cl1(0.25) C33(0.25) H33A(0.25) H33B(0.25) Cl2(0.25)
6.a Ternary CH refined with riding coordinates:
 C23(H23), C26(H26)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C15(H15A,H15B), C16(H16A,H16B), C16(H16C,H16D), C17(H17A,H17B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C33(H33A,H33B), C17S(H17C,H17D)
6.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C), C18S(H18D,H18E,H18F)
;
_shelx_res_checksum              87747
_shelx_hkl_checksum              96241
_olex2_submission_special_instructions 'No special instructions were received'