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_7122595
_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 Cl2 N2 P2 S4'
_chemical_formula_sum            'C12 H14 Cl2 N2 P2 S4'
_chemical_formula_weight         447.33
_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             2018-09-07
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2018-09-07 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                84.231(6)
_cell_angle_beta                 88.651(6)
_cell_angle_gamma                88.674(6)
_cell_formula_units_Z            1
_cell_length_a                   6.5353(5)
_cell_length_b                   6.6119(4)
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_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.5750
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35t (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,17:45:29)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35t (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,17:45:29)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35t (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,17:45:29)
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_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
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  1 omega   21.00  177.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  102.0000 156
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_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
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_diffrn_orient_matrix_UB_32      0.0360427000
_diffrn_orient_matrix_UB_33      -0.0448036000
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
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_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3033
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
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_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
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_exptl_absorpt_coefficient_mu    0.968
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35t (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,17:45:29)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
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_exptl_crystal_description       plank
_exptl_crystal_F_000             228
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_exptl_crystal_size_min          0.15
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_refine_ls_number_reflns         3033
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2210
_reflns_number_total             3033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08158a2.cif
_cod_data_source_block           5379
_cod_depositor_comments
'Adding full bibliography for 7122593--7122597.cif.'
_cod_database_code               7122595
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C12 H13 Cl2 N2 P2 S4'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.760
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9038(7)
 0.0962(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              86991
_shelx_hkl_checksum              28473
_olex2_submission_special_instructions 'No special instructions were received'