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_4348753
_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         'C60 H92 Ge P2, C7 H14'
_chemical_formula_sum            'C67 H106 Ge P2'
_chemical_formula_weight         1046.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           30
_space_group_name_Hall           'P 2 -2bc'
_space_group_name_H-M_alt        'P n c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.3723(6)
_cell_length_b                   19.1347(3)
_cell_length_c                   12.3204(3)
_cell_measurement_reflns_used    12087
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      66.1390
_cell_measurement_theta_min      3.1750
_cell_volume                     6452.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0413483000
_diffrn_orient_matrix_UB_12      0.0154028000
_diffrn_orient_matrix_UB_13      -0.0812631000
_diffrn_orient_matrix_UB_21      0.0378525000
_diffrn_orient_matrix_UB_22      -0.0067483000
_diffrn_orient_matrix_UB_23      0.0920299000
_diffrn_orient_matrix_UB_31      0.0048871000
_diffrn_orient_matrix_UB_32      -0.0787278000
_diffrn_orient_matrix_UB_33      -0.0239052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30686
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.213
_diffrn_reflns_theta_min         1.614
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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            'blackish red'
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       plate
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.3866
_exptl_crystal_size_mid          0.3326
_exptl_crystal_size_min          0.0714
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 3286 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         10175
_refine_ls_number_restraints     548
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0770P)^2^+15.4294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.766
_reflns_Friedel_fraction_max     0.792
_reflns_number_gt                8834
_reflns_number_total             10175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01566_si_002.cif
_cod_data_source_block           7Ge.C7H14_kji140008_face_abs
_cod_original_cell_volume        6453.0(2)
_cod_database_code               4348753
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C60 H92 Ge1 P2'
_reflns_odcompleteness_completeness 95.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.052) H5(0.053) H7(0.059) H8A(0.096) H8B(0.096) H8C(0.096)
 H9A(0.086) H9B(0.086) H9C(0.086) H10(0.067) H11A(0.146) H11B(0.146)
 H11C(0.146) H12A(0.124) H12B(0.124) H12C(0.124) H13(0.05) H14A(0.087)
 H14B(0.087) H14C(0.087) H15A(0.087) H15B(0.087) H15C(0.087) H18(0.048)
 H20(0.047) H22(0.045) H23A(0.075) H23B(0.075) H23C(0.075) H24A(0.072)
 H24B(0.072) H24C(0.072) H25(0.064) H26A(0.084) H26B(0.084) H26C(0.084)
 H27A(0.132) H27B(0.132) H27C(0.132) H28(0.062) H29A(0.102) H29B(0.102)
 H29C(0.102) H30A(0.108) H30B(0.108) H30C(0.108) H33(0.048) H35(0.048)
 H37(0.06) H38A(0.092) H38B(0.092) H38C(0.092) H39A(0.092) H39B(0.092)
 H39C(0.092) H40(0.063) H41A(0.129) H41B(0.129) H41C(0.129) H42A(0.118)
 H42B(0.118) H42C(0.118) H43(0.049) H44A(0.075) H44B(0.075) H44C(0.075)
 H45A(0.075) H45B(0.075) H45C(0.075) H48(0.05) H50(0.053) H52(0.048)
 H53A(0.076) H53B(0.076) H53C(0.076) H54A(0.08) H54B(0.08) H54C(0.08)
 H55(0.064) H56A(0.095) H56B(0.095) H56C(0.095) H57A(0.124) H57B(0.124)
 H57C(0.124) H58(0.05) H59A(0.096) H59B(0.096) H59C(0.096) H60A(0.087)
 H60B(0.087) H60C(0.087) H1SA(0.284) H1SB(0.284) H1SC(0.284) H2S(0.214)
 H3SA(0.254) H3SB(0.254) H4SA(0.277) H4SB(0.277) H5SA(0.279) H5SB(0.279)
 H6SA(0.255) H6SB(0.255) H7SA(0.179) H7SB(0.179)
 Fixed X: H3(0.6108) H5(0.5585) H7(0.6935) H8A(0.6971) H8B(0.7356) H8C(0.7312)
 H9A(0.633) H9B(0.6666) H9C(0.6196) H10(0.5139) H11A(0.5952) H11B(0.5419)
 H11C(0.5684) H12A(0.5167) H12B(0.5055) H12C(0.558) H13(0.6377) H14A(0.5946)
 H14B(0.6244) H14C(0.6509) H15A(0.5613) H15B(0.5623) H15C(0.5365) H18(0.5611)
 H20(0.6372) H22(0.6296) H23A(0.5546) H23B(0.5493) H23C(0.5294) H24A(0.5792)
 H24B(0.6047) H24C(0.6363) H25(0.5364) H26A(0.514) H26B(0.513) H26C(0.5568)
 H27A(0.6117) H27B(0.5677) H27C(0.608) H28(0.7207) H29A(0.6642) H29B(0.7089)
 H29C(0.6611) H30A(0.7504) H30B(0.7638) H30C(0.7205) H33(0.8999) H35(0.9409)
 H37(0.8138) H38A(0.78) H38B(0.7803) H38C(0.8193) H39A(0.8866) H39B(0.8463)
 H39C(0.8869) H40(0.992) H41A(0.9129) H41B(0.9655) H41C(0.9337) H42A(0.9922)
 H42B(1.0045) H42C(0.9523) H43(0.8573) H44A(0.9351) H44B(0.9265) H44C(0.9581)
 H45A(0.8994) H45B(0.871) H45C(0.8432) H48(0.9359) H50(0.8508) H52(0.879)
 H53A(0.9536) H53B(0.9603) H53C(0.9761) H54A(0.9221) H54B(0.9055) H54C(0.8664)
 H55(0.9496) H56A(0.9793) H56B(0.9748) H56C(0.9356) H57A(0.8715) H57B(0.9133)
 H57C(0.876) H58(0.7843) H59A(0.8041) H59B(0.7772) H59C(0.8332) H60A(0.7347)
 H60B(0.7188) H60C(0.7507) H1SA(0.6838) H1SB(0.7287) H1SC(0.7028) H2S(0.7684)
 H3SA(0.6841) H3SB(0.7002) H4SA(0.7625) H4SB(0.7187) H5SA(0.7534) H5SB(0.7944)
 H6SA(0.8262) H6SB(0.8186) H7SA(0.7498) H7SB(0.7943)
 Fixed Y: H3(0.1746) H5(-0.0169) H7(0.1456) H8A(0.2065) H8B(0.1545)
 H8C(0.2304) H9A(0.2538) H9B(0.2564) H9C(0.2096) H10(0.0788) H11A(0.1088)
 H11B(0.101) H11C(0.0365) H12A(0.1905) H12B(0.19) H12C(0.2091) H13(-0.0957)
 H14A(-0.1288) H14B(-0.181) H14C(-0.1181) H15A(-0.0849) H15B(-0.1573) H15C(-
 0.0931) H18(0.0046) H20(-0.1725) H22(0.1008) H23A(0.0652) H23B(0.1408)
 H23C(0.0764) H24A(0.1214) H24B(0.18) H24C(0.1238) H25(-0.0869) H26A(-0.1714)
 H26B(-0.2044) H26C(-0.22) H27A(-0.1777) H27B(-0.1541) H27C(-0.1) H28(-0.12)
 H29A(-0.2391) H29B(-0.2406) H29C(-0.2004) H30A(-0.1242) H30B(-0.193) H30C(-
 0.1928) H33(-0.1795) H35(0.0183) H37(-0.1611) H38A(-0.172) H38B(-0.2445) H38C(-
 0.2281) H39A(-0.2565) H39B(-0.2724) H39C(-0.2169) H40(-0.071) H41A(-0.1046)
 H41B(-0.0859) H41C(-0.029) H42A(-0.1873) H42B(-0.1808) H42C(-0.2046)
 H43(0.0867) H44A(0.0803) H44B(0.1554) H44C(0.1014) H45A(0.121) H45B(0.1743)
 H45C(0.1113) H48(0.0036) H50(0.1698) H52(-0.1038) H53A(-0.0562) H53B(-0.1332)
 H53C(-0.0707) H54A(-0.1161) H54B(-0.1789) H54C(-0.1286) H55(0.0966)
 H56A(0.1719) H56B(0.2122) H56C(0.2235) H57A(0.1889) H57B(0.1747) H57C(0.1154)
 H58(0.1099) H59A(0.2329) H59B(0.2276) H59C(0.2113) H60A(0.0759) H60B(0.1517)
 H60C(0.1398) H1SA(0.0872) H1SB(0.1372) H1SC(0.1068) H2S(0.0431) H3SA(-0.0236)
 H3SB(-0.0192) H4SA(-0.089) H4SB(-0.1254) H5SA(-0.1128) H5SB(-0.142) H6SA(-
 0.036) H6SB(-0.0424) H7SA(0.0294) H7SB(0.0686)
 Fixed Z: H3(-0.1776) H5(-0.2016) H7(0.037) H8A(-0.1714) H8B(-0.1232) H8C(-
 0.0762) H9A(-0.0395) H9B(0.0635) H9C(0.0634) H10(-0.284) H11A(-0.4144) H11B(-
 0.4594) H11C(-0.4075) H12A(-0.2175) H12B(-0.3423) H12C(-0.3007) H13(-0.0109)
 H14A(-0.213) H14B(-0.1408) H14C(-0.1972) H15A(0.0613) H15B(0.0018) H15C(-
 0.0527) H18(0.3375) H20(0.3179) H22(0.146) H23A(0.0752) H23B(0.1229)
 H23C(0.1882) H24A(0.3434) H24B(0.2747) H24C(0.335) H25(0.4477) H26A(0.3217)
 H26B(0.4381) H26C(0.3598) H27A(0.5112) H27B(0.5841) H27C(0.5504) H28(0.1167)
 H29A(0.1719) H29B(0.0923) H29C(0.06) H30A(0.2947) H30B(0.2324) H30C(0.3157)
 H33(-0.1255) H35(-0.1436) H37(0.0844) H38A(-0.0878) H38B(-0.0287) H38C(-
 0.1183) H39A(0.0186) H39B(0.1054) H39C(0.1299) H40(-0.2265) H41A(-0.3626)
 H41B(-0.4039) H41C(-0.3457) H42A(-0.1704) H42B(-0.2943) H42C(-0.2575)
 H43(0.0466) H44A(0.1193) H44B(0.0723) H44C(0.0075) H45A(-0.1559) H45B(-0.0824)
 H45C(-0.1355) H48(0.3996) H50(0.361) H52(0.2043) H53A(0.1462) H53B(0.1867)
 H53C(0.261) H54A(0.4117) H54B(0.3388) H54C(0.3895) H55(0.5137) H56A(0.3833)
 H56B(0.4937) H56C(0.4025) H57A(0.5455) H57B(0.6296) H57C(0.6008) H58(0.1363)
 H59A(0.2517) H59B(0.1397) H59C(0.1474) H60A(0.2764) H60B(0.2437) H60C(0.3477)
 H1SA(0.537) H1SB(0.5501) H1SC(0.6531) H2S(0.5178) H3SA(0.5995) H3SB(0.4769)
 H4SA(0.5015) H4SB(0.558) H5SA(0.7248) H5SB(0.6468) H6SA(0.6213) H6SB(0.7467)
 H7SA(0.7381) H7SB(0.6857)
;
_shelx_res_checksum              64277
_shelx_hkl_checksum              60270