A diarsagermylene and a diarsastannylene stabilised by areneGe/Sn interactions.
Izod, Keith; Evans, Peter; Waddell, Paul G.; Chemical communications (Cambridge, England) 54 (2018) 2526–2529; doi:10.1039/c7cc09564c

data_7121307
_publ_section_title
;
 A diarsagermylene and a diarsastannylene stabilised by areneGe/Sn
 interactions.
;
_journal_issue                   20
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2526
_journal_page_last               2529
_journal_paper_doi               10.1039/c7cc09564c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C36 H58 As Li O3, C36.01 H58.97 As Li O3'
_chemical_formula_sum            'C72.01 H116.97 As2 Li2 O6'
_chemical_formula_weight         1242.46
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                68.376(2)
_cell_angle_beta                 80.7734(18)
_cell_angle_gamma                89.4407(16)
_cell_formula_units_Z            2
_cell_length_a                   11.4059(2)
_cell_length_b                   17.5174(3)
_cell_length_c                   19.3810(5)
_cell_measurement_reflns_used    23118
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.1210
_cell_measurement_theta_min      3.1970
_cell_volume                     3548.12(14)
_computing_cell_refinement
;
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
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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_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      150.0(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
  1 omega  -52.00  -10.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008  137.0000   13.0000 42

  2 omega   42.00   68.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008 -137.0000  -49.0000 26

  3 omega    4.00   35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008  -99.0000  150.0000 31

  4 omega   14.00   52.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008  -99.0000   60.0000 38

  5 omega  -36.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008   19.0000    0.0000 127

  6 omega  -79.00   -9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008    0.0000 -180.0000 70

  7 omega  -39.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.0633   57.0000  -60.0000 104

  8 omega  -85.00   17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.0633  -38.0000  150.0000 102

  9 omega  -39.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.0633   57.0000  150.0000 104

 10 omega  -16.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008   38.0000  120.0000 102

 11 omega   22.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0008 -132.0000  127.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0047463000
_diffrn_orient_matrix_UB_12      -0.0231063000
_diffrn_orient_matrix_UB_13      0.0380558000
_diffrn_orient_matrix_UB_21      0.0514525000
_diffrn_orient_matrix_UB_22      -0.0178115000
_diffrn_orient_matrix_UB_23      -0.0121133000
_diffrn_orient_matrix_UB_31      0.0362059000
_diffrn_orient_matrix_UB_32      0.0324271000
_diffrn_orient_matrix_UB_33      0.0004897000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71162
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.757
_diffrn_reflns_theta_min         2.920
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         16256
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0411P)^2^+1.2822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12267
_reflns_number_total             16256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09564c2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7121305--7121307.cif.'
_cod_original_cell_volume        3548.14(14)
_cod_database_code               7121307
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C36 H58 O3 As1 Li1'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6C-Li2 \\sim O6A-Li2 \\sim O6B-Li2
 with sigma of 0.02
 C36-C35B \\sim C35A-C36
 with sigma of 0.02
 C35A-C34 \\sim C34-C35B
 with sigma of 0.02
 O4A-Li2 \\sim O4B-Li2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O6A) = Uanis(O6B) = Uanis(O6C)
Uanis(C71C) = Uanis(C72A) = Uanis(C72B)
Uanis(C72C) = Uanis(C71A) = Uanis(C71B)
Uanis(C70A) = Uanis(C70C) = Uanis(C70B)
Uanis(C69C) = Uanis(C69A) = Uanis(C69B)
Uanis(C35B) = Uanis(C35A)
Uanis(O4A) = Uanis(O4B)
Uanis(C61A) = Uanis(C61B)
Uanis(C62A) = Uanis(C62B)
Uanis(C63A) = Uanis(C63B)
Uanis(C64A) = Uanis(C64B)
4. Rigid body (RIGU) restrains
 O6A, C69A, C70A, C71A, C72A, O6B, C69B, C70B, C71B, C72B, O6C, C69C, C70C,
 C71C, C72C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, C61A, C62A, C63A, C64A, O4B, C61B, C62B, C63B, C64B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O6B, C69B, C70B, C71B, C72B} sigma for 1-2: 0.02, 1-3: 0.02
as
{O6A, C69A, C70A, C71A, C72A}
{O4A, C61A, C62A, C63A, C64A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O4B, C61B, C62B, C63B, C64B}
6. Others
 Fixed Sof: H34A(0.72735) H34B(0.72735) H34C(0.27265) H34D(0.27265)
 H36A(0.72735) H36B(0.72735) H36C(0.27265) H36D(0.27265) O4A(0.42724)
 C61A(0.42724) H61A(0.42724) H61B(0.42724) C62A(0.42724) H62A(0.42724)
 H62B(0.42724) C63A(0.42724) H63A(0.42724) H63B(0.42724) C64A(0.42724)
 H64A(0.42724) H64B(0.42724) O6A(0.33598) C69A(0.33598) H69A(0.33598)
 H69B(0.33598) C70A(0.33598) H70A(0.33598) H70B(0.33598) C71A(0.33598)
 H71A(0.33598) H71B(0.33598) C72A(0.33598) H72A(0.33598) H72B(0.33598)
 C35A(0.65728) H35A(0.65728) H35B(0.65728) O4B(0.57276) C61B(0.57276)
 H61C(0.57276) H61D(0.57276) C62B(0.57276) H62C(0.57276) H62D(0.57276)
 C63B(0.57276) H63C(0.57276) H63D(0.57276) C64B(0.57276) H64C(0.57276)
 H64D(0.57276) O6B(0.18998) C69B(0.18998) H69C(0.18998) H69D(0.18998)
 C70B(0.18998) H70C(0.18998) H70D(0.18998) C71B(0.18998) H71C(0.18998)
 H71D(0.18998) C72B(0.18998) H72C(0.18998) H72D(0.18998) C35B(0.34272)
 H35C(0.34272) H35D(0.34272) O6C(0.47645) C69C(0.47645) H69E(0.47645)
 H69F(0.47645) C70C(0.47645) H70E(0.47645) H70F(0.47645) H70G(0.47645)
 C71C(0.47645) H71E(0.47645) H71F(0.47645) C72C(0.47645) H72E(0.47645)
 H72F(0.47645) H72G(0.47645)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C43(H43), C46(H46), C55(H55), C58(H58)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C34(H34C,H34D), C36(H36A,H36B), C36(H36C,H36D), C65(H65A,H65B),
  C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C61A(H61A,H61B), C62A(H62A,
 H62B), C63A(H63A,H63B), C64A(H64A,H64B), C69A(H69A,H69B), C70A(H70A,H70B),
 C71A(H71A,H71B), C72A(H72A,H72B), C35A(H35A,H35B), C61B(H61C,H61D), C62B(H62C,
 H62D), C63B(H63C,H63D), C64B(H64C,H64D), C69B(H69C,H69D), C70B(H70C,H70D),
 C71B(H71C,H71D), C72B(H72C,H72D), C35B(H35C,H35D), C69C(H69E,H69F), C71C(H71E,
 H71F)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C39(H39), C40(H40),
 C41(H41), C51(H51), C52(H52), C53(H53)
7.d 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), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C70C(H70E,H70F,H70G), C72C(H72E,H72F,H72G)
;
_shelx_res_checksum              50581
_olex2_submission_special_instructions 'No special instructions were received'