Structures, Electronics, and Reactivity of Strained Phosphazane Cages: A Combined Experimental and Computational Study.
Roth, Torsten; Vasilenko, Vladislav; Wadepohl, Hubert; Wright, Dominic S.; Gade, Lutz H.; Inorganic chemistry 54 (2015) 7636–7644; doi:10.1021/acs.inorgchem.5b01292

data_4343966
_publ_section_title
;
 Structures, Electronics, and Reactivity of Strained Phosphazane Cages: A
 Combined Experimental and Computational Study.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7636
_journal_page_last               7644
_journal_paper_doi               10.1021/acs.inorgchem.5b01292
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C51 H57 N4 P2, C F3 O3 S, 3(C H2 Cl2)'
_chemical_formula_sum            'C55 H63 Cl6 F3 N4 O3 P2 S'
_chemical_formula_weight         1191.79
_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_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tro115
_audit_creation_date
;
'Mon Nov 17 15:06:03 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'18.05.2015 16:14:11 CEST UTC+02:00  encif 1.32'
_cell_angle_alpha                90
_cell_angle_beta                 111.046(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1547(6)
_cell_length_b                   15.5003(4)
_cell_length_c                   20.9894(7)
_cell_measurement_reflns_used    21414
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.3320
_cell_measurement_theta_min      3.4610
_cell_volume                     5816.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega    1.00   84.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000  -30.0000 166

  2 omega   21.00   57.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000   30.0000 72

  3 omega   30.00   57.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000   60.0000 54

  4 omega  -37.00    2.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000   60.0000 78

  5 omega  -43.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000   -1.1995 204

  6 omega   -3.00   94.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000   90.0000 194

  7 omega    6.00   95.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   30.0000 178

  8 omega  -42.00   13.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -57.0000 -120.0000 110

  9 omega    1.00   44.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  -90.0000 86

 10 omega   -1.00   97.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -180.0000 196

 11 omega    1.00   31.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000    0.0000 60

 12 omega    1.00   40.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000 -150.0000 78

 13 omega  -26.00   58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -77.0000  -55.3728 168

 14 omega  -39.00   58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -77.0000  164.6144 194

 15 omega   18.00   60.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  109.1002 84

 16 omega  -35.00    6.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  109.1002 82

 17 omega   25.00   60.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -133.2945 70

 18 omega  -42.00  -16.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -133.2945 52

 19 omega  -46.00   52.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -38.0000  150.0000 196

 20 omega  -43.00   55.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000  -30.0000 196

 21 omega    6.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000 -150.0000 180

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0038895000
_diffrn_orient_matrix_UB_12      0.0384347000
_diffrn_orient_matrix_UB_13      -0.0193053000
_diffrn_orient_matrix_UB_21      0.0311738000
_diffrn_orient_matrix_UB_22      -0.0120640000
_diffrn_orient_matrix_UB_23      -0.0086996000
_diffrn_orient_matrix_UB_31      -0.0242463000
_diffrn_orient_matrix_UB_32      -0.0216871000
_diffrn_orient_matrix_UB_33      -0.0293739000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.161
_diffrn_reflns_av_unetI/netI     0.1358
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            164217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.218
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         19358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1936
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11013
_reflns_number_total             19358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01292_si_003.cif
_cod_data_source_block           ga_tro115_5
_cod_depositor_comments
'Adding full bibliography for 4343960--4343970.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4343966
_audit_block_refno               2260
_audit_block_usercomment         'trvv93 colourless needle'
_chemical_oxdiff_formula         'C55 H63 Cl6 F3 N4 O3 P2 S1'
_chemical_oxdiff_usercomment     'trvv93 colourless needle'
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.957
_diffrn_oxdiff_twin_integration_method simultaneous
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7932(10) 0.2068(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C23(H23), C26(H26), C39(H39)
3.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C81(H81A,H81B), C61(H61A,H61B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C)
;
_shelx_res_checksum              58211
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            19.1515(4)
_cell_oxdiff_length_b            15.5037(3)
_cell_oxdiff_length_c            20.9886(6)
_cell_oxdiff_angle_alpha         89.9967(18)
_cell_oxdiff_angle_beta          111.048(2)
_cell_oxdiff_angle_gamma         90.0088(16)
_cell_oxdiff_volume              5816.1(2)
_cell_oxdiff_measurement_reflns_used 21414
_cell_oxdiff_twin_number         2