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_4343968
_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
'C43 H65 Cl2 Ir2 N4 P2, C F3 O3 S, C H2 Cl2, C7 H8'
_chemical_formula_sum            'C52 H75 Cl4 F3 Ir2 N4 O3 P2 S'
_chemical_formula_weight         1481.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_vv3
_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 16:35:57 CEST UTC+02:00  encif 1.32'
_cell_angle_alpha                98.124(12)
_cell_angle_beta                 92.831(13)
_cell_angle_gamma                91.799(13)
_cell_formula_units_Z            2
_cell_length_a                   10.610(5)
_cell_length_b                   15.089(7)
_cell_length_c                   17.314(8)
_cell_measurement_reflns_used    8020
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.21
_cell_volume                     2739(2)
_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    'DIRDIF (Beurskens et al., 1999-2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         1.934
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.203
_exptl_absorpt_correction_T_max  0.6478
_exptl_absorpt_correction_T_min  0.5296
_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            red
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         7.592
_refine_diff_density_min         -2.870
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         15330
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0546P)^2^+31.3211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12357
_reflns_number_total             15330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01292_si_003.cif
_cod_data_source_block           ga_vv3
_cod_depositor_comments
'Adding full bibliography for 4343960--4343970.cif.'
_cod_database_code               4343968
_audit_block_refno               2299
_audit_block_usercomment         VV58
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.551
_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. Uiso/Uaniso restraints and constraints
C67 \\sim S2: within 1A with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 C61, C62, C63, C64, C65, C66, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C81, C82, C83, C84, C85, C86, C87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, O11, O12, O13, C51, F11, F12, F13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, O21, O22, O23, C52, F21, F22, F23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: S1(0.5) F11(0.5) F12(0.5) F13(0.5) O11(0.5) O12(0.5) O13(0.5)
 C51(0.5) S2(0.5) F21(0.5) F22(0.5) F23(0.5) O21(0.5) O22(0.5) O23(0.5)
 C52(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C87(0.5) H87A(0.5) H87B(0.5)
 H87C(0.5) C61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5) C64(0.5) H64(0.5)
 C65(0.5) H65(0.5) C66(0.5) H66(0.5) C81(0.5) C82(0.5) H82(0.5) C83(0.5)
 H83(0.5) C84(0.5) H84(0.5) C85(0.5) H85(0.5) C86(0.5) H86(0.5)
5.a Free rotating group:
 S1(F11,F12,F13,O11,O12,O13,C51), S2(F21,F22,F23,O21,O22,O23,C52,Cl71,Cl72,C71,
 C67,H67A,H67B,H67C,C87,H87A,H87B,H87C)
5.b Ternary CH refined with riding coordinates:
 C28(H28), C29(H29), C32(H32), C33(H33), C36(H36), C37(H37), C40(H40), C41(H41)
5.c Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C34(H34A,H34B), C35(H35A,H35B), C38(H38A,
 H38B), C39(H39A,H39B), C42(H42A,H42B), C43(H43A,H43B), C71(H71A,H71B)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C13(H13), C15(H15), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
5.e Fitted hexagon refined as free rotating group:
 C61(C62,C63,C64,C65,C66), C81(C82,C83,C84,C85,C86)
5.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              48807
_olex2_submission_special_instructions 'No special instructions were received'