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_7121306
_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         'C48 H68 As2 Ge, C7 H8'
_chemical_formula_sum            'C55 H76 As2 Ge'
_chemical_formula_weight         959.58
_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     dual
_audit_creation_date             2017-02-28
_audit_creation_method
;
Olex2 1.2
(compiled Feb 23 2017 12:29:26 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                77.0882(17)
_cell_angle_beta                 78.4162(17)
_cell_angle_gamma                71.263(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6717(3)
_cell_length_b                   12.8423(3)
_cell_length_c                   16.8971(3)
_cell_measurement_reflns_used    24399
_cell_measurement_temperature    190.0(2)
_cell_measurement_theta_max      66.7530
_cell_measurement_theta_min      3.6550
_cell_volume                     2513.24(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      190.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     12.00 116.00   1.00    2.00    --   41.59  57.00-180.00  104
  2  \w    -32.00  71.00   1.00    2.00    --   41.59 -57.00  30.00  103
  3  \w     -3.00  96.00   1.00    2.00    --   41.59-125.00 -30.00   99
  4  \w      8.00 132.00   1.00    8.00    --   93.50 -90.00 162.18  124
  5  \w      9.00 133.00   1.00    8.00    --   93.50 -93.00  17.32  124
  6  \w      9.00 133.00   1.00    8.00    --   93.50 -93.00-102.15  124
  7  \w      9.00 133.00   1.00    8.00    --   93.50 -92.00  47.49  124
  8  \w      8.00 132.00   1.00    8.00    --   93.50 -91.00-117.69  124
  9  \w     15.00 127.00   1.00    8.00    --   93.50 -77.00-150.00  112
 10  \w     63.00 171.00   1.00    8.00    --   93.50  30.00  90.00  108
 11  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00 -60.00   74
 12  \w     19.00 121.00   1.00    8.00    --   93.50 -45.00  60.00  102
 13  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00  60.00   74
 14  \w     66.00 168.00   1.00    8.00    --   93.50  45.00 120.00  102
 15  \w     19.00  96.00   1.00    8.00    --   93.50-125.00-120.00   77
 16  \w     19.00  96.00   1.00    8.00    --   93.50-125.00 -60.00   77
 17  \w     63.00 171.00   1.00    8.00    --   93.50  30.00   0.00  108
 18  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00  90.00   74
 19  \w     73.00 168.00   1.00    8.00    --   93.50 125.00 -60.00   95
 20  \w     66.00 168.00   1.00    8.00    --   93.50  45.00 -60.00  102
 21  \w     32.00 177.00   1.00    8.00    --   93.50  15.00 -30.00  145
 22  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00   0.00   74
 23  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00 150.00   74
 24  \w     19.00 121.00   1.00    8.00    --   93.50 -45.00 -60.00  102
 25  \w      9.00 133.00   1.00    8.00    --   93.50 -93.00 119.25  124
 26  \w      8.00 132.00   1.00    8.00    --   93.50 -91.00 -22.21  124
 27  \w   -120.00  -8.00   1.00    2.00    --  -41.59 -77.00  30.00  112
 28  \w   -116.00 -12.00   1.00    2.00    --  -41.59 -57.00 120.00  104
 29  \w      8.00 120.00   1.00    2.00    --   41.59  77.00 -30.00  112
 30  \w      8.00 120.00   1.00    2.00    --   41.59  77.00 -90.00  112
 31  \w     63.00 168.00   1.00    8.00    --   93.50  61.00-180.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1013369000
_diffrn_orient_matrix_UB_12      -0.0937649000
_diffrn_orient_matrix_UB_13      0.0312976000
_diffrn_orient_matrix_UB_21      -0.0719531000
_diffrn_orient_matrix_UB_22      -0.0817206000
_diffrn_orient_matrix_UB_23      0.0237955000
_diffrn_orient_matrix_UB_31      0.0369217000
_diffrn_orient_matrix_UB_32      -0.0325770000
_diffrn_orient_matrix_UB_33      -0.0858953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53120
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.820
_diffrn_reflns_theta_max         66.820
_diffrn_reflns_theta_min         3.689
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.870
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         8893
_refine_ls_number_restraints     762
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+2.4680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7861
_reflns_number_total             8893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09564c2.cif
_cod_data_source_block           8Ge
_cod_depositor_comments
'Adding full bibliography for 7121305--7121307.cif.'
_cod_database_code               7121306
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C55 H76 As2 Ge1'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
 C47B-C46 \\sim C47A-C46
 with sigma of 0.02
 C48A-C46 \\sim C48B-C46
 with sigma of 0.02
 C48B-C47B \\sim C47A-C48A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49A \\sim C49A \\sim C49A \\sim C49A \\sim C50A \\sim C50A \\sim C50A \\sim
C51A \\sim C51A \\sim C51A \\sim C52A \\sim C52A \\sim C52A \\sim C53A \\sim
C53A \\sim C53A \\sim C54A \\sim C54A \\sim C54A \\sim C55A \\sim C55A \\sim
C49B \\sim C49B \\sim C49B \\sim C49B \\sim C50B \\sim C50B \\sim C50B \\sim
C51B \\sim C51B \\sim C51B \\sim C52B \\sim C52B \\sim C52B \\sim C53B \\sim
C53B \\sim C53B \\sim C54B \\sim C54B \\sim C54B \\sim C55B \\sim C55B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C47A \\sim C47B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C48A \\sim C48B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C49A, C50A, C51A, C52A, C53A, C54A, C55A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C49B, C50B, C51B, C52B, C53B, C54B, C55B}
6. Others
 Fixed Sof: H46A(0.32213) H46(0.67787) C47A(0.67787) H47A(0.67787)
 H47B(0.67787) H47C(0.67787) C48A(0.67787) H48A(0.67787) H48B(0.67787)
 H48C(0.67787) C49A(0.58352) C50A(0.58352) H50A(0.58352) C51A(0.58352)
 H51A(0.58352) C52A(0.58352) H52A(0.58352) C53A(0.58352) H53A(0.58352)
 C54A(0.58352) H54A(0.58352) C55A(0.58352) H55A(0.58352) H55B(0.58352)
 H55C(0.58352) C47B(0.32213) H47D(0.32213) H47E(0.32213) H47F(0.32213)
 C48B(0.32213) H48D(0.32213) H48E(0.32213) H48F(0.32213) C49B(0.41648)
 C50B(0.41648) H50B(0.41648) C51B(0.41648) H51B(0.41648) C52B(0.41648)
 H52B(0.41648) C53B(0.41648) H53B(0.41648) C54B(0.41648) H54B(0.41648)
 C55B(0.41648) H55D(0.41648) H55E(0.41648) H55F(0.41648)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43), C46(H46A),
  C46(H46)
7.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), C50A(H50A), C51A(H51A), C52A(H52A),
 C53A(H53A), C54A(H54A), C50B(H50B), C51B(H51B), C52B(H52B), C53B(H53B),
 C54B(H54B)
7.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), C47A(H47A,H47B,H47C),
 C48A(H48A,H48B,H48C), C55A(H55A,H55B,H55C), C47B(H47D,H47E,H47F), C48B(H48D,
 H48E,H48F), C55B(H55D,H55E,H55F)
;
_shelx_res_checksum              97343
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.908