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_7044608
_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         'C49 H41 P3, 2(C F3 O3 S), 2(C6 H4 F2)'
_chemical_formula_sum            'C63 H49 F10 O6 P3 S2'
_chemical_formula_weight         1249.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-03
_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                 102.8998(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9661(2)
_cell_length_b                   19.1154(2)
_cell_length_c                   19.1052(3)
_cell_measurement_reflns_used    16896
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      76.1960
_cell_measurement_theta_min      3.6590
_cell_volume                     5683.72(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      air
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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   -108.00 -12.00   0.50   12.00    --  -38.50 -57.00-150.00  192
  2  \w    -62.00  32.00   0.50   12.00    --  -38.50  57.00   0.00  188
  3  \w     43.00  98.00   0.50   12.00    --   42.75-125.00-180.00  110
  4  \w     84.00 109.00   0.50   48.00    --  111.00 -94.00 -90.00   50
  5  \w    114.00 141.00   0.50   48.00    --  111.00 -77.00-150.00   54
  6  \w     30.00 108.00   0.50   48.00    --  111.00 -94.00-180.00  156
  7  \w     37.00  72.00   0.50   48.00    --  111.00 -77.00-150.00   70
  8  \w     64.00 107.00   0.50   48.00    --  111.00 -94.00   0.00   86
  9  \w    139.00 177.00   0.50   48.00    --  111.00   0.00-120.00   76
 10  \w     41.00  70.00   0.50   48.00    --  111.00 -61.00 120.00   58
 11  \w     90.00 118.00   0.50   48.00    --  111.00 -61.00 120.00   56
 12  \w     36.00 133.00   0.50   48.00    --  111.00 -30.00-180.00  194
 13  \w     26.00  53.00   0.50   48.00    --  111.00   0.00-120.00   54
 14  \w     70.00 112.00   0.50   48.00    --  111.00   0.00-120.00   84
 15  \w     30.00  99.00   0.50   48.00    --  111.00 -94.00  60.00  138
 16  \w     40.00 129.00   0.50   48.00    --  111.00 -45.00 -60.00  178
 17  \w     50.00  98.00   0.50   48.00    --  111.00 -94.00-120.00   96
 18  \w     30.00  67.00   0.50   48.00    --  111.00 -94.00 -90.00   74
;
_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      -0.0705287000
_diffrn_orient_matrix_UB_12      -0.0372765000
_diffrn_orient_matrix_UB_13      -0.0557865000
_diffrn_orient_matrix_UB_21      -0.0671111000
_diffrn_orient_matrix_UB_22      0.0209388000
_diffrn_orient_matrix_UB_23      0.0427930000
_diffrn_orient_matrix_UB_31      -0.0178987000
_diffrn_orient_matrix_UB_32      0.0683772000
_diffrn_orient_matrix_UB_33      -0.0435526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34123
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.794
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         11801
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0592P)^2^+3.0565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10249
_reflns_number_total             11801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03271d2.cif
_cod_data_source_block           8
_cod_original_cell_volume        5683.74(14)
_cod_database_code               7044608
_chemical_oxdiff_formula         'C252 H196 F40 O24 P12 S8 '
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C53A \\sim C54A \\sim C52A \\sim F11A \\sim C55A \\sim C57A \\sim F10A \\sim
C56A \\sim C55B \\sim C52B \\sim C57B \\sim C53B \\sim F7B \\sim C56B \\sim
C54B \\sim F8B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
F12A \\sim C59A \\sim C60A \\sim C58A \\sim F13A \\sim C61A \\sim C63A \\sim
C62A \\sim C59B \\sim C60B \\sim C58B \\sim F10B \\sim C61B \\sim C63B \\sim
F9B \\sim C62B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F8A) = Uanis(F6B)
Uanis(O6A) = Uanis(O4B)
3. Others
 Sof(S2B)=Sof(F4B)=Sof(O6B)=Sof(F5B)=Sof(C51B)=Sof(F6B)=Sof(O5B)=Sof(O4B)=1-
 FVAR(1)
 Sof(S2A)=Sof(O5A)=Sof(O6A)=Sof(F8A)=Sof(F7A)=Sof(F9A)=Sof(O4A)=Sof(C51A)=
 FVAR(1)
 Sof(C59B)=Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=Sof(H62B)=
 Sof(C63B)=Sof(H63B)=Sof(C58B)=Sof(F9B)=Sof(F10B)=1-FVAR(2)
 Sof(C59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=
 Sof(C63A)=Sof(H63A)=Sof(C58A)=Sof(F12A)=Sof(F13A)=FVAR(2)
 Sof(C52B)=Sof(C57B)=Sof(H57B)=Sof(C56B)=Sof(H56B)=Sof(C55B)=Sof(H55B)=
 Sof(C54B)=Sof(H54B)=Sof(C53B)=Sof(F8B)=Sof(F7B)=1-FVAR(3)
 Sof(C53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=
 Sof(C57A)=Sof(H57A)=Sof(C52A)=Sof(F10A)=Sof(F11A)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C60B(H60B), C61B(H61B), C62B(H62B), C63B(H63B), C60A(H60A), C61A(H61A),
 C62A(H62A), C63A(H63A), C57B(H57B), C56B(H56B), C55B(H55B), C54B(H54B),
 C54A(H54A), C55A(H55A), C56A(H56A), C57A(H57A), C30(H30), C16(H16), C40(H40),
 C3(H3), C42(H42), C31(H31), C37(H37), C43(H43), C15(H15), C27(H27), C29(H29),
 C19(H19), C33(H33), C9(H9), C41(H41), C28(H28), C17(H17), C34(H34), C12(H12),
 C36(H36), C5(H5), C25(H25), C7(H7), C13(H13), C6(H6), C11(H11), C39(H39),
 C4(H4), C10(H10), C23(H23), C46(H46), C48(H48), C24(H24), C18(H18), C45(H45),
 C35(H35), C49(H49), C47(H47), C21(H21), C22(H22)
;
_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 2.488
_oxdiff_exptl_absorpt_empirical_full_min 0.525