Diphosphene radical cations and dications with a π-conjugated C2P2C2-framework
Ghadwal, Rajendra S.; Sharma, Mahendra Kumar; Rottschäfer, Dennis; Blomeyer, Sebastian; Neumann, Beate; Stammler, Georg; Hinz, Alexander; van Gastel, Maurice; Chemical Communications  (2019) –; doi:10.1039/C9CC04701H

data_7123946
_publ_section_title
;
 Diphosphene radical cations and dications with a \p-conjugated
 C2P2C2-framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04701H
_journal_year                    2019
_chemical_formula_moiety         'C68 H82 N4 P2, Cl4 Ga, 2(C H2 Cl2)'
_chemical_formula_sum            'C70 H86 Cl8 Ga N4 P2'
_chemical_formula_weight         1398.68
_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             2019-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-09 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                100.208(3)
_cell_angle_beta                 91.640(3)
_cell_angle_gamma                96.981(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9028(4)
_cell_length_b                   15.6844(6)
_cell_length_c                   21.5392(8)
_cell_measurement_reflns_used    19354
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.9240
_cell_measurement_theta_min      2.6450
_cell_volume                     3593.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00   8.00   1.00   50.00    --  -17.08 -57.00-180.00   73
  2  \w    -83.00 -10.00   1.00   50.00    --  -17.08 -57.00  90.00   73
  3  \w    -53.00  81.00   1.00   50.00    --   17.08   0.00 -60.00  134
  4  \w     14.00  88.00   1.00   50.00    --   17.08  38.00 -30.00   74
  5  \w    -54.00  35.00   1.00   50.00    --   17.08 -38.00 150.00   89
  6  \w     10.00  75.00   1.00   50.00    --   17.08-131.00 174.42   65
  7  \w    -13.00  83.00   1.00   50.00    --   17.08  77.00  60.00   96
  8  \w    -31.00  53.00   1.00   50.00    --   17.08 -90.00 -84.69   84
  9  \w     30.00  71.00   1.00   50.00    --   17.08-125.00  44.96   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0644114000
_diffrn_orient_matrix_UB_12      -0.0136320000
_diffrn_orient_matrix_UB_13      0.0002717000
_diffrn_orient_matrix_UB_21      0.0022233000
_diffrn_orient_matrix_UB_22      -0.0280653000
_diffrn_orient_matrix_UB_23      -0.0295282000
_diffrn_orient_matrix_UB_31      0.0123853000
_diffrn_orient_matrix_UB_32      -0.0342570000
_diffrn_orient_matrix_UB_33      0.0158292000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.623
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         21022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+2.5495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14482
_reflns_number_total             21022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04701h2.cif
_cod_data_source_block           compound2a
_cod_database_code               7123946
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H44 Cl2 Ga P2 N2'
_diffrn_oxdiff_digest_frames
;
0128a3d6a6e882091b5f4e5f2f92d458db00027fbc3
;
_diffrn_oxdiff_digest_hkl
;
01c19c2f57c697361e830ed5fa12440ea226b3
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl2B)=Sof(Cl3B)=Sof(Cl4B)=Sof(Cl7B)=Sof(Cl8B)=Sof(C70A)=Sof(H70C)=
 Sof(H70D)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl3)=Sof(Cl4)=Sof(Cl7)=Sof(Cl8)=Sof(C70B)=Sof(H70A)=Sof(H70B)=
 FVAR(1)
 Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C44(H44), C47(H47), C56(H56), C59(H59)
3.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70A(H70C,H70D), C70B(H70A,H70B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C40(H40),
  C41(H41), C42(H42), C52(H52), C53(H53), C54(H54), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68)
3.d Disordered Me refined with riding coordinates:
 C11(H11A,H11B,H11C,H11D,H11E,H11F)
3.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C)
;
_shelx_res_checksum              79474
_olex2_date_sample_data_collection 2019-01-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.108
_oxdiff_exptl_absorpt_empirical_full_min 0.894