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_7123948
_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
'1(Cl4 Ga), C68 H86 N4 P2, C4 H8 O, 1[C6 H14]'
_chemical_formula_sum            'C78 H108 Cl4 Ga N4 O P2'
_chemical_formula_weight         1391.14
_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             2019-02-18
_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                78.6124(14)
_cell_angle_beta                 83.7585(15)
_cell_angle_gamma                76.4065(16)
_cell_formula_units_Z            2
_cell_length_a                   12.5647(3)
_cell_length_b                   15.8474(3)
_cell_length_c                   20.4584(3)
_cell_measurement_reflns_used    49006
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.7260
_cell_measurement_theta_min      3.0090
_cell_volume                     3873.26(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (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 0.999
_diffrn_measured_fraction_theta_max 0.945
_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    -76.00 -27.00   1.00   66.50    --  -17.14 132.00  30.98   49
  2  \w     -4.00  88.00   1.00   66.50    --   17.14  38.00 -90.00   92
  3  \w    -54.00  47.00   1.00   66.50    --   17.14 -77.00-180.00  101
  4  \w     -6.00  66.00   1.00   66.50    --   17.14-116.00 -70.29   72
  5  \w     -4.00  88.00   1.00   66.50    --   17.14  38.00  90.00   92
  6  \w    -54.00  38.00   1.00   66.50    --   17.14 -38.00  60.00   92
  7  \w    -13.00  88.00   1.00   66.50    --   17.14  77.00 120.00  101
  8  \w    -51.00  42.00   1.00   66.50    --   17.14 -57.00 -30.00   93
  9  \w    -13.00  88.00   1.00   66.50    --   17.14  77.00 -30.00  101
 10  \w    -75.00 -27.00   1.00   66.50    --  -17.14 131.00 120.57   48
 11  \w    -86.00   8.00   1.00   66.50    --  -17.14 -57.00  90.00   94
 12  \w    -69.00 -20.00   1.00   66.50    --  -17.14 121.00 -67.64   49
 13  \w     -1.00  69.00   1.00   66.50    --   17.14-121.00-168.04   70
 14  \w      6.00  76.00   1.00   66.50    --   17.14-132.00  76.39   70
 15  \w      6.00  76.00   1.00   66.50    --   17.14-132.00 -10.74   70
 16  \w     35.00 101.00   1.00   66.50    --   17.14 178.00  30.00   66
 17  \w   -102.00 -55.00   1.00   66.50    --  -17.14 178.00 -30.00   47
 18  \w     35.00 101.00   1.00   66.50    --   17.14 178.00-120.00   66
 19  \w    -20.00  56.00   1.00   66.50    --   17.14 -99.00  90.00   76
 20  \w      6.00  76.00   1.00   66.50    --   17.14-132.00-107.24   70
;
_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      0.0568502000
_diffrn_orient_matrix_UB_12      -0.0097325000
_diffrn_orient_matrix_UB_13      0.0051212000
_diffrn_orient_matrix_UB_21      -0.0016194000
_diffrn_orient_matrix_UB_22      -0.0447981000
_diffrn_orient_matrix_UB_23      0.0123522000
_diffrn_orient_matrix_UB_31      0.0123705000
_diffrn_orient_matrix_UB_32      -0.0093880000
_diffrn_orient_matrix_UB_33      -0.0328232000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            194103
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.886
_diffrn_reflns_theta_min         2.518
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (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    1.193
_exptl_crystal_description       plate
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         27354
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0626P)^2^+1.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20054
_reflns_number_total             27354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04701h2.cif
_cod_data_source_block           compound2b
_cod_original_cell_volume        3873.28(13)
_cod_database_code               7123948
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C74 H66 Cl4 Ga N4 P2'
_diffrn_oxdiff_digest_frames
;
011175ce5bfe7917d8c6900a525e318ef401583ffbe
;
_diffrn_oxdiff_digest_hkl
;
016c0f0d1fb2d427b4b7d83d3e77b94f49bbbd
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_shelx_res_checksum              97070
_shelx_fab_checksum              29928
_olex2_date_sample_data_collection 2019-02-15
_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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.893