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_7122593
_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         'C12 H14 N2 P2 S4'
_chemical_formula_sum            'C12 H14 N2 P2 S4'
_chemical_formula_weight         376.43
_chemical_name_systematic        IB-266
_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     dual
_audit_creation_date             2017-05-17
_audit_creation_method
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Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-09-07 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                91.108(3)
_cell_angle_beta                 99.021(3)
_cell_angle_gamma                104.050(3)
_cell_formula_units_Z            1
_cell_length_a                   4.6979(3)
_cell_length_b                   7.2032(4)
_cell_length_c                   12.1580(7)
_cell_measurement_reflns_used    6150
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.92
_cell_volume                     393.47(4)
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_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    'XT (Sheldrick, 2015)'
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
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_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9986
_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         27.994
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'sealed tube'
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_exptl_absorpt_coefficient_mu    0.796
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_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1055 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.8272. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
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_exptl_crystal_description       plate
_exptl_crystal_F_000             194
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0196P)^2^+0.2844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1815
_reflns_number_total             1893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08158a2.cif
_cod_data_source_block           5184f
_cod_depositor_comments
'Adding full bibliography for 7122593--7122597.cif.'
_cod_database_code               7122593
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.762
_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.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              11335
_shelx_hkl_checksum              8391
_olex2_submission_special_instructions 'No special instructions were received'