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_4348752
_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 Sn'
_chemical_formula_sum            'C48 H68 P2 Sn'
_chemical_formula_weight         825.65
_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             2015-04-17
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
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_cell_angle_alpha                90
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_cell_formula_units_Z            4
_cell_length_a                   13.9682(3)
_cell_length_b                   17.3921(3)
_cell_length_c                   18.5886(4)
_cell_measurement_reflns_used    8010
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0150
_cell_measurement_theta_min      3.3110
_cell_volume                     4515.66(16)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -23.00   69.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.0633   19.0000  150.0000 92

  2 omega  -90.00    0.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.0633  -19.0000  -30.0000 90

  3 omega   -4.00   21.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008  -99.0000  -60.0000 25

  4 omega  -24.00   34.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008   77.0000 -180.0000 58

  5 omega   -4.00   52.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008  -99.0000   30.0000 56
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0331647000
_diffrn_orient_matrix_UB_12      0.0291369000
_diffrn_orient_matrix_UB_13      0.0098009000
_diffrn_orient_matrix_UB_21      -0.0360039000
_diffrn_orient_matrix_UB_22      0.0188050000
_diffrn_orient_matrix_UB_23      0.0201222000
_diffrn_orient_matrix_UB_31      0.0135063000
_diffrn_orient_matrix_UB_32      -0.0214657000
_diffrn_orient_matrix_UB_33      0.0309059000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33747
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0226P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5966
_reflns_number_total             8259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01566_si_002.cif
_cod_data_source_block           6Sn_kji150010_fa
_cod_original_cell_volume        4515.67(15)
_cod_database_code               4348752
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C48 H34 P2 Sn1'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43), C46(H46)
2.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)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 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)
;
_shelx_res_checksum              94482
_shelx_hkl_checksum              37678
_olex2_submission_special_instructions 'No special instructions were received'