Remote Substituent Effects on the Structures and Stabilities of P═E π-Stabilized Diphosphatetrylenes (R<sub>2</sub>P)<sub>2</sub>E (E = Ge, Sn).
Izod, Keith; Evans, Peter; Waddell, Paul G.; Probert, Michael R.; Inorganic chemistry 55 (2016) 10510–10522; doi:10.1021/acs.inorgchem.6b01566

data_4348756
_publ_section_title
;
 Remote Substituent Effects on the Structures and Stabilities of
 P&#x2550;E \p-Stabilized Diphosphatetrylenes
 (R<sub>2</sub>P)<sub>2</sub>E (E = Ge, Sn).
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10510
_journal_page_last               10522
_journal_paper_doi               10.1021/acs.inorgchem.6b01566
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C48 H68 P2'
_chemical_formula_sum            'C48 H68 P2'
_chemical_formula_weight         706.96
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.33377(10)
_cell_length_b                   18.41362(15)
_cell_length_c                   17.51452(14)
_cell_measurement_reflns_used    27240
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.8340
_cell_measurement_theta_min      3.3500
_cell_volume                     4243.74(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
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_diffrn_detector_area_resol_mean 10.3968
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_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   15.00  110.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   38.0000   60.0000 95

  2 omega  -30.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155  -38.0000 -120.0000 93

  3 omega  -21.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155  -99.0000  150.0000 101

  4 omega    9.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -120.4251 30

  5 omega   83.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -80.8612 26

  6 omega   66.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -171.1087 41

  7 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   42.3170 26

  8 omega   33.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   30.0000 87

  9 omega  143.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   30.0000 34

 10 omega   18.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   30.0000 43

 11 omega   41.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 76

 12 omega   80.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 43

 13 omega   41.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  120.0000 35

 14 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   30.0000 26

 15 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -150.0000 27

 16 omega   17.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  120.0000 34

 17 omega   21.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  150.0000 27

 18 omega    9.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  150.0000 74

 19 omega   65.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   60.0000 57

 20 omega  135.00  171.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   60.0000 36

 21 omega   19.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -120.0000 44

 22 omega   74.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -120.0000 35

 23 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 27

 24 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   90.0000 26

 25 omega   88.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -120.4251 25

 26 omega   73.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   90.0000 54

 27 omega   16.00  126.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000 -120.0000 110

 28 omega   39.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 32

 29 omega   94.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 26

 30 omega  124.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 28

 31 omega    9.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000    8.4925 106

 32 omega   66.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 31

 33 omega  108.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 26

 34 omega   20.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000 -150.0000 62

 35 omega   62.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000    0.0000 26

 36 omega   89.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000    0.0000 25

 37 omega   50.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 26

 38 omega   48.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  120.0000 26

 39 omega   84.00  132.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  115.5669 48

 40 omega -116.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7155  -57.0000 -120.0000 104

 41 omega -120.00   -8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7155  -77.0000    0.0000 112

 42 omega  -99.00  -18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7155  125.0000    0.0000 81

 43 omega    8.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   77.0000 -120.0000 91

 44 omega    8.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7155   77.0000  150.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0066376000
_diffrn_orient_matrix_UB_12      0.0799514000
_diffrn_orient_matrix_UB_13      -0.0246844000
_diffrn_orient_matrix_UB_21      -0.0476920000
_diffrn_orient_matrix_UB_22      0.0240763000
_diffrn_orient_matrix_UB_23      0.0703892000
_diffrn_orient_matrix_UB_31      0.1067026000
_diffrn_orient_matrix_UB_32      0.0057430000
_diffrn_orient_matrix_UB_33      0.0487262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57954
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.975
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7512
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0450P)^2^+1.4196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6334
_reflns_number_total             7512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01566_si_002.cif
_cod_data_source_block           10_kji150005_fa_2
_cod_original_cell_volume        4243.75(6)
_cod_database_code               4348756
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C48 H68 P2'
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C12B-C10 \\sim C12A-C10
 with sigma of 0.02
 C11B-C10 \\sim C11A-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12A) = Uanis(C12B)
Uanis(C11A) = Uanis(C11B)
4. Others
 Fixed Sof: H10(0.51277) H10A(0.48723) C11A(0.51277) H11A(0.51277)
 H11B(0.51277) H11C(0.51277) C12A(0.51277) H12A(0.51277) H12B(0.51277)
 H12C(0.51277) C11B(0.48723) H11D(0.48723) H11E(0.48723) H11F(0.48723)
 C12B(0.48723) H12D(0.48723) H12E(0.48723) H12F(0.48723)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C10(H10A), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43),
  C46(H46)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C39(H39), C40(H40), C41(H41)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C11A(H11A,H11B,H11C),
 C12A(H12A,H12B,H12C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F)
;
_shelx_res_checksum              14027
_shelx_hkl_checksum              50033
_olex2_submission_special_instructions 'No special instructions were received'