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_4343970
_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         'C47 H69 Cl2 N4 P2 Rh2, C F3 O3 S'
_chemical_formula_sum            'C55 H77 Cl2 F3 N4 O3 P2 Rh2 S'
_chemical_formula_weight         1269.92
_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_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tro123
_audit_creation_date
;
'Tue Mar 17 11:47:54 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'18.05.2015 17:13:27 CEST UTC+02:00  encif 1.32'
_cell_angle_alpha                90
_cell_angle_beta                 99.0958(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.08913(10)
_cell_length_b                   20.49420(14)
_cell_length_c                   20.83769(15)
_cell_measurement_reflns_used    60825
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.0640
_cell_measurement_theta_min      3.5850
_cell_volume                     5519.45(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_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 0.943
_diffrn_measurement_details
;
  1 omega  -42.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -80.0000  -11.2539 202

  2 omega    2.00   54.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   38.0000 -180.0000 104

  3 omega   -5.00   22.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   80.0000  168.0814 54

  4 omega  -43.00   57.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -77.0000  137.6130 200

  5 omega   13.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000 -150.0000 128

  6 omega    6.00   36.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000   60.0000 60

  7 omega   60.00   86.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000   60.0000 52

  8 omega   -3.00   73.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000    0.0000 152

  9 omega    4.00   96.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000 -120.0000 184

 10 omega    8.00   74.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000   60.0000 132

 11 omega  -31.00   -5.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -77.0000   90.0000 52

 12 omega   29.00   57.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -77.0000   90.0000 56

 13 omega    2.00   41.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   38.0000    0.0000 78

 14 omega   49.00   85.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   38.0000    0.0000 72

 15 omega  -43.00   12.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -77.0000 -150.0000 110

 16 omega   29.00   55.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -77.0000 -150.0000 52

 17 omega   19.00   45.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000  -30.0000 52

 18 omega   31.00   60.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  175.3761 58

 19 omega  -43.00   60.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  -83.3821 206

 20 omega  -40.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000   46.9628 198

 21 omega   -3.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000 -150.0000 200

 22 omega   -3.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000    0.0000 200

 23 omega  -42.00   48.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -57.0000   60.0000 180

 24 omega    6.00   96.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000  120.0000 180

 25 omega    6.00   63.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000  -30.0000 114

 26 omega  -46.00    5.50   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -38.0000 -150.0000 103

;
_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      0.0362295000
_diffrn_orient_matrix_UB_12      -0.0019790000
_diffrn_orient_matrix_UB_13      0.0290963000
_diffrn_orient_matrix_UB_21      0.0314705000
_diffrn_orient_matrix_UB_22      0.0236029000
_diffrn_orient_matrix_UB_23      -0.0123037000
_diffrn_orient_matrix_UB_31      -0.0266071000
_diffrn_orient_matrix_UB_32      0.0252332000
_diffrn_orient_matrix_UB_33      0.0138172000
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            220308
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.861
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         19392
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+2.2307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16072
_reflns_number_total             19392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01292_si_003.cif
_cod_data_source_block           ga_tro123_sq
_cod_depositor_comments
'Adding full bibliography for 4343960--4343970.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4343970
_audit_block_refno               2380
_audit_block_usercomment         'tr1550 orange irregular'
_chemical_oxdiff_formula         'C55 H77 Cl2 F3 N4 O3 P2 Rh2 S1'
_chemical_oxdiff_usercomment     'tr1550 orange irregular'
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.920
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. 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
2. Restrained distances
 S-O1 \\sim S-O2 \\sim S-O3
 with sigma of 0.02
 O1-O2 \\sim O1-O3 \\sim O2-O3
 with sigma of 0.02
 C51-F1 \\sim C51-F2 \\sim C51-F3
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C23(H23), C28(H28), C31(H31), C43(H43), C46(H46)
3.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18)
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), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              53121
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            13.09137(13)
_cell_oxdiff_length_b            20.49516(15)
_cell_oxdiff_length_c            20.83352(13)
_cell_oxdiff_angle_alpha         90.0337(5)
_cell_oxdiff_angle_beta          99.1021(7)
_cell_oxdiff_angle_gamma         89.9861(7)
_cell_oxdiff_volume              5519.45(8)
_cell_oxdiff_measurement_reflns_used 60825
_platon_squeeze_void_probe_radius 1.20