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_7044609
_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 H40 F2 P3, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C52 H43 F5 N O3 P3 S'
_chemical_formula_weight         949.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-24
_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                 101.354(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9625(4)
_cell_length_b                   18.9800(10)
_cell_length_c                   24.0879(11)
_cell_measurement_reflns_used    17903
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.4740
_cell_measurement_theta_min      2.0220
_cell_volume                     4465.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 phi   -344.66   15.04   0.3000   19.9960
omega____ theta____ kappa____ phi______ frames
 -29.6591  -19.0000  -46.2250     -     1199

  2 phi     34.16  344.36   0.3000   19.9990
omega____ theta____ kappa____ phi______ frames
  29.6584  -19.0000   46.2250     -     1034
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\p scans'
_diffrn_orient_matrix_UB_11      0.0681477000
_diffrn_orient_matrix_UB_12      0.0046219000
_diffrn_orient_matrix_UB_13      -0.0039849000
_diffrn_orient_matrix_UB_21      -0.0248026000
_diffrn_orient_matrix_UB_22      0.0191548000
_diffrn_orient_matrix_UB_23      -0.0252463000
_diffrn_orient_matrix_UB_31      0.0048457000
_diffrn_orient_matrix_UB_32      0.0317163000
_diffrn_orient_matrix_UB_33      0.0157786000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48030
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.730
_diffrn_reflns_theta_min         2.031
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
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    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0829P)^2^+8.2711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7458
_reflns_number_total             9473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03271d2.cif
_cod_data_source_block           18
_cod_database_code               7044609
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C52H43F3N1O3P3S
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H30(0.037) H10(0.035) H11(0.036) H37(0.029) H46(0.04) H45(0.033)
 H12(0.034) H5(0.051) H31(0.03) H9(0.031) H13(0.031) H27(0.03) H48(0.036)
 H29(0.045) H28(0.041) H36(0.034) H47(0.039) H19(0.031) H21(0.028) H16(0.039)
 H34(0.037) H24(0.035) H22(0.033) H49(0.033) H18(0.038) H35(0.036) H25(0.029)
 H52A(0.133) H52B(0.133) H52C(0.133) H41(0.055) H7(0.037) H15(0.034) H17(0.041)
 H23(0.037) H33(0.032) H6(0.047) H42(0.048) H40(0.049) H43(0.039) H3(0.037)
 H4(0.046) H39(0.04)
 Fixed X: H30(0.669) H10(0.5788) H11(0.4939) H37(0.3854) H46(0.9169)
 H45(0.784) H12(0.3345) H5(0.0596) H31(0.5397) H9(0.4987) H13(0.2568)
 H27(0.6187) H48(0.7487) H29(0.7699) H28(0.7483) H36(0.4665) H47(0.9025)
 H19(0.2494) H21(0.3308) H16(-0.1104) H34(0.7649) H24(-0.002) H22(0.1187)
 H49(0.6069) H18(0.0806) H35(0.6568) H25(0.2107) H52A(0.677) H52B(0.6605)
 H52C(0.808) H41(0.6972) H7(0.03) H15(0.0551) H17(-0.0942) H23(-0.0467)
 H33(0.6875) H6(-0.0711) H42(0.488) H40(0.8546) H43(0.4415) H3(0.3932)
 H4(0.2926) H39(0.8056)
 Fixed Y: H30(0.4926) H10(0.0308) H11(-0.0737) H37(0.3308) H46(0.0882)
 H45(0.1801) H12(-0.0698) H5(0.3147) H31(0.4588) H9(0.1387) H13(0.0377)
 H27(0.2533) H48(-0.0464) H29(0.4073) H28(0.288) H36(0.3878) H47(-0.0239)
 H19(0.2219) H21(0.398) H16(0.0735) H34(0.4786) H24(0.3967) H22(0.452)
 H49(0.0429) H18(0.1917) H35(0.4618) H25(0.3437) H52A(0.3852) H52B(0.407)
 H52C(0.4095) H41(0.2735) H7(0.235) H15(0.1048) H17(0.1136) H23(0.4525)
 H33(0.4211) H6(0.2879) H42(0.2188) H40(0.2921) H43(0.1792) H3(0.229)
 H4(0.2853) H39(0.2587)
 Fixed Z: H30(0.7205) H10(0.7151) H11(0.6707) H37(0.4571) H46(0.6878)
 H45(0.6417) H12(0.5855) H5(0.74) H31(0.633) H9(0.6767) H13(0.5459) H27(0.674)
 H48(0.5647) H29(0.7848) H28(0.7617) H36(0.3847) H47(0.6496) H19(0.4602)
 H21(0.6596) H16(0.4821) H34(0.4997) H24(0.4931) H22(0.6574) H49(0.5198)
 H18(0.3818) H35(0.4065) H25(0.4943) H52A(0.2263) H52B(0.2888) H52C(0.272)
 H41(0.3317) H7(0.5823) H15(0.5614) H17(0.3924) H23(0.5738) H33(0.573)
 H6(0.6516) H42(0.3345) H40(0.4151) H43(0.4206) H3(0.6939) H4(0.7617)
 H39(0.5017)
;
_olex2_submission_special_instructions 'No special instructions were received'