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_4343967
_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_absolute_configuration ad
_chemical_formula_moiety         'C39 H37 N4 P2, C F3 O3 S'
_chemical_formula_sum            'C40 H37 F3 N4 O3 P2 S'
_chemical_formula_weight         772.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tro128
_audit_creation_date             2015-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'18.05.2015 16:25:42 CEST UTC+02:00  encif 1.32'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.467(6)
_cell_length_b                   17.866(10)
_cell_length_c                   19.990(12)
_cell_measurement_reflns_used    8005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.37
_cell_measurement_theta_min      2.26
_cell_volume                     3738(4)
_computing_cell_refinement
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_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      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            93087
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.998
_diffrn_reflns_theta_min         1.529
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 4235 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         11888
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0533P)^2^+1.0417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10363
_reflns_number_total             11888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01292_si_003.cif
_cod_data_source_block           ga_tro128
_cod_depositor_comments
'Adding full bibliography for 4343960--4343970.cif.'
_cod_database_code               4343967
_audit_block_refno               2394
_audit_block_usercomment         trvvsi
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.907
_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
 C50-F1 \\sim C50-F2 \\sim C50-F3
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3
 with sigma of 0.02
 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
 C28-C29A \\sim C28-C29B
 with sigma of 0.005
3. Rigid body (RIGU) restrains
 S, O1, O2, O3, C50, F1, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39, C29B,
 C30B, C31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H28A)=Sof(C29B)=Sof(C30B)=Sof(H30B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=
 Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=
 Sof(H36B)=Sof(C37B)=Sof(C38B)=Sof(H38B)=1-FVAR(1)
 Sof(H28)=Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(C32A)=Sof(H32A)=
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C28(H28), C28(H28A)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
 C30A(H30A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C37A(H37A),
 C38A(H38A), C30B(H30B), C31B(H31B), C33B(H33B), C34B(H34B), C35B(H35B),
 C36B(H36B), C38B(H38B)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              6541
_olex2_submission_special_instructions 'No special instructions were received'