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_7121139
_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         'C34 H46 N4 P2 S2 Se2'
_chemical_formula_sum            'C34 H46 N4 P2 S2 Se2'
_chemical_formula_weight         794.73
_chemical_name_systematic        ABK-466
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.2796(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5972(7)
_cell_length_b                   13.2665(5)
_cell_length_c                   15.6185(6)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.57
_cell_measurement_theta_min      2.66
_cell_volume                     3750.4(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0775
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -24
_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            61648
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.174
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.197
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5809
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0907 before and 0.0570 after correction. The Ratio of minimum to maximum transmission is 0.7788. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         9047
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+2.7453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6293
_reflns_number_total             9047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09349g2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7121136--7121139.cif.'
_cod_database_code               7121139
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.621
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C11 \\sim C10 \\sim C9 \\sim C8: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C4'(H4'A,H4'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B), C8'(H8'A,H8'B),
 C9'(H9'A,H9'B), C10'(H10C,H10D)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C13'(H13'), C14'(H14'),
 C15'(H15'), C16'(H16'), C17'(H17')
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C7'(H7'A,H7'B,H7'C), C11'(H11D,H11E,H11F)
;
_shelx_res_checksum              82464
_shelx_hkl_checksum              76640
_olex2_submission_special_instructions 'No special instructions were received'