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_7121305
_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 Sn, C7 H8'
_chemical_formula_sum            'C55 H76 As2 Sn'
_chemical_formula_weight         1005.68
_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             2017-02-13
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:58:59 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                75.874(3)
_cell_angle_beta                 77.693(3)
_cell_angle_gamma                69.763(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7953(4)
_cell_length_b                   12.9297(3)
_cell_length_c                   16.8382(6)
_cell_measurement_reflns_used    13247
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.3890
_cell_measurement_theta_min      3.6290
_cell_volume                     2509.21(14)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.859
_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    -23.00  89.00   1.00    4.50    --   10.16  77.00  30.00  112
  2  \w    -55.00  -6.00   1.00    4.50    --   10.16 139.00 133.00   49
  3  \w    -19.00  84.00   1.00    4.50    --   10.16  57.00   0.00  103
  4  \w    -69.00  44.00   1.00    4.50    --   10.16 -77.00-120.00  113
  5  \w    -64.00  40.00   1.00    4.50    --   10.16 -57.00 120.00  104
  6  \w    -70.00  -1.00   1.00    4.50    --   -9.14 131.00 -41.00   69
  7  \w    -19.00  53.00   1.00    4.50    --   10.16  57.00-120.00   72
;
_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      0.0439584000
_diffrn_orient_matrix_UB_12      0.0245773000
_diffrn_orient_matrix_UB_13      -0.0097613000
_diffrn_orient_matrix_UB_21      0.0000595000
_diffrn_orient_matrix_UB_22      -0.0039802000
_diffrn_orient_matrix_UB_23      0.0427573000
_diffrn_orient_matrix_UB_31      0.0403678000
_diffrn_orient_matrix_UB_32      -0.0540443000
_diffrn_orient_matrix_UB_33      0.0013887000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40464
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.812
_diffrn_reflns_theta_min         3.242
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.852
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.630
_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    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         11268
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0261P)^2^+2.4748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8671
_reflns_number_total             11268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09564c2.cif
_cod_data_source_block           8Sn
_cod_depositor_comments
'Adding full bibliography for 7121305--7121307.cif.'
_cod_original_cell_volume        2509.21(15)
_cod_database_code               7121305
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C55 H76 As2 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. Uiso/Uaniso restraints and constraints
C49A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim C54A \\sim C55A \\sim
C49B \\sim C50B \\sim C51B \\sim C52B \\sim C53B \\sim C54B \\sim C55B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C49A, C50A, C51A, C52A, C53A, C54A, C55A, C49B, C50B, C51B, C52B, C53B, C54B,
 C55B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. 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}
5. Others
 Fixed Sof: C49A(0.8516) C50A(0.8516) H50A(0.8516) C51A(0.8516) H51A(0.8516)
 C52A(0.8516) H52A(0.8516) C53A(0.8516) H53A(0.8516) C54A(0.8516) H54A(0.8516)
 C55A(0.8516) H55A(0.8516) H55B(0.8516) H55C(0.8516) C49B(0.1484) C50B(0.1484)
 H50B(0.1484) C51B(0.1484) H51B(0.1484) C52B(0.1484) H52B(0.1484) C53B(0.1484)
 H53B(0.1484) C54B(0.1484) H54B(0.1484) C55B(0.1484) H55D(0.1484) H55E(0.1484)
 H55F(0.1484)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43), C46(H46)
6.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)
6.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), C55A(H55A,H55B,H55C), C55B(H55D,H55E,H55F)
;
_shelx_res_checksum              4601
_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 1.042
_oxdiff_exptl_absorpt_empirical_full_min 0.975