Donor–acceptor interactions in tri(phosphonio)methanide dications [(Ph3P)2CP(X)Ph2]2+ (X = H, Me, CN, NCS, OH, Cl, OTf, F)
Yogendra, S.; Hennersdorf, F.; Bauzá, A.; Frontera, A.; Fischer, R.; Weigand, J. J.; Dalton Transactions  (2017) –; doi:10.1039/C7DT03271D

data_7044607
_publ_section_title
;
 Donor--acceptor interactions in tri(phosphonio)methanide dications
 [(Ph3P)2CP(X)Ph2]2+ (X = H, Me, CN, NCS, OH, Cl, OTf, F)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03271D
_journal_year                    2017
_chemical_formula_moiety         'C50 H43 P3, 2(C F3 O3 S), 0.5(C6 H4 F2)'
_chemical_formula_sum            'C55 H45 F7 O6 P3 S2'
_chemical_formula_weight         1091.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-10-04 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.84904(19)
_cell_length_b                   30.9248(3)
_cell_length_c                   18.15886(14)
_cell_measurement_reflns_used    32822
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.5290
_cell_measurement_theta_min      2.4490
_cell_volume                     10023.29(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -94.00  -2.00   0.50    1.00    --  -38.50 125.00 -30.00  184
  2  \w    -94.00  -2.00   0.50    1.00    --  -38.50 125.00-180.00  184
  3  \w     23.00  98.00   0.50    1.00    --   42.75-125.00  90.00  150
  4  \w     94.00 178.00   0.50    4.00    --  111.00 125.00 -60.00  168
  5  \w     39.00 121.00   0.50    4.00    --  111.00-125.00-180.00  164
  6  \w     30.00 109.00   0.50    4.00    --  111.00 -94.00 -30.00  158
  7  \w     83.00 178.00   0.50    4.00    --  111.00  61.00   0.00  190
  8  \w     80.00 178.00   0.50    4.00    --  111.00  77.00-150.00  196
  9  \w     30.00 109.00   0.50    4.00    --  111.00 -94.00-150.00  158
 10  \w     31.00 156.00   0.50    4.00    --  111.00 -15.00 -30.00  250
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0670121000
_diffrn_orient_matrix_UB_12      -0.0066583000
_diffrn_orient_matrix_UB_13      0.0522110000
_diffrn_orient_matrix_UB_21      -0.0328591000
_diffrn_orient_matrix_UB_22      -0.0437721000
_diffrn_orient_matrix_UB_23      0.0245610000
_diffrn_orient_matrix_UB_31      0.0433583000
_diffrn_orient_matrix_UB_32      -0.0228150000
_diffrn_orient_matrix_UB_33      -0.0622090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55427
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.888
_diffrn_reflns_theta_min         2.858
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_T_max  0.510
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.568
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.377
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         10480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0464P)^2^+9.3373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10404
_reflns_number_total             10480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03271d2.cif
_cod_data_source_block           9
_cod_database_code               7044607
_chemical_oxdiff_formula         C55H47F7O6P3S2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F7(0.5) F8(0.5) C53(0.5) C58(0.5) H58(0.5) C57(0.5) H57(0.5)
 C56(0.5) H56(0.5) C55(0.5) H55(0.5) C54(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C58(H58), C57(H57), C56(H56), C55(H55)
3.b Fitted hexagon refined as free rotating group:
 C53(C58,C57,C56,C55,C54)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_checksum              17117
_shelx_shelxl_version_number     2014/7
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.771