A planar per-borylated digermene
Zheng, Xiongfei; Crumpton, Agamemnon; Ellwanger, Mathias; Aldridge, Simon; Dalton Transactions  (2023) –; doi:10.1039/D3DT03416J

data_7714366
_publ_section_title
;
 A planar per-borylated digermene
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03416J
_journal_year                    2023
_chemical_formula_moiety         'C64 H80 B4 Ge2 N4 O4'
_chemical_formula_sum            'C64 H80 B4 Ge2 N4 O4'
_chemical_formula_weight         1157.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.1440(10)
_cell_angle_beta                 94.3580(10)
_cell_angle_gamma                92.4280(10)
_cell_formula_units_Z            6
_cell_length_a                   11.9393(2)
_cell_length_b                   22.4852(2)
_cell_length_c                   36.1463(5)
_cell_measurement_reflns_used    51597
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.3190
_cell_measurement_theta_min      3.6480
_cell_volume                     9538.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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      7.00  35.00   1.00    3.00    --  -41.40  19.00 -30.00   28
  2  \w     -2.00  37.00   1.00    3.00    --  -41.40  19.00 120.00   39
  3  \w     -5.00  31.00   1.00    3.00    --  -41.40  19.00  30.00   36
  4  \w     -2.00  35.00   1.00    3.00    --  -41.40  19.00  90.00   37
  5  \w      0.00  36.00   1.00    3.00    --  -41.40  19.00-180.00   36
  6  \w     -5.00  37.00   1.00    3.00    --  -41.40  19.00  60.00   42
  7  \w    -85.00 -18.00   1.00    3.00    --  -41.40 125.00 150.00   67
  8  \w     30.00  90.00   1.00    3.00    --   41.40-125.00  60.00   60
  9  \w     16.00  45.00   1.00    3.00    --   41.40 -99.00 150.00   29
 10  \w     26.00  82.00   1.00    3.00    --   41.40  57.00 -60.00   56
 11  \w     44.00  72.00   1.00   12.00    --  111.00 -45.00 120.00   28
 12  \w    113.00 174.00   1.00   12.00    --  111.00  45.00 150.00   61
 13  \w     41.00  71.00   1.00   12.00    --  111.00 -45.00-150.00   30
 14  \w     74.00 109.00   1.00   12.00    --  111.00-111.00-150.00   35
 15  \w     71.00  96.00   1.00   12.00    --  111.00-111.00-120.00   25
 16  \w    105.00 174.00   1.00   12.00    --  111.00  45.00 120.00   69
 17  \w     88.00 177.00   1.00   12.00    --  111.00  45.00-150.00   89
 18  \w     40.00  65.00   1.00   12.00    --  111.00 -45.00-120.00   25
 19  \w     51.00  77.00   1.00   12.00    --  111.00 -61.00 -60.00   26
 20  \w     83.00 109.00   1.00   12.00    --  111.00-111.00 120.00   26
 21  \w     97.00 177.00   1.00   12.00    --  111.00  30.00 -90.00   80
 22  \w     40.00  72.00   1.00   12.00    --  111.00 -45.00   0.00   32
 23  \w     40.00  65.00   1.00   12.00    --  111.00 -45.00 -60.00   25
 24  \w     61.00 109.00   1.00   12.00    --  111.00-111.00  90.00   48
 25  \w     59.00 109.00   1.00   12.00    --  111.00-111.00 150.00   50
 26  \w     41.00 109.00   1.00   12.00    --  111.00-111.00   0.00   68
 27  \w     44.00  71.00   1.00   12.00    --  111.00 -45.00-180.00   27
 28  \w     49.00  74.00   1.00   12.00    --  111.00 -61.00-150.00   25
 29  \w     36.00 108.00   1.00   12.00    --  111.00-111.00 -30.00   72
 30  \w     70.00 109.00   1.00   12.00    --  111.00-111.00 -90.00   39
 31  \w     74.00 101.00   1.00   12.00    --  111.00 178.00 -90.00   27
 32  \w     34.00  61.00   1.00   12.00    --  111.00 -94.00  90.00   27
 33  \w     61.00 109.00   1.00   12.00    --  111.00-111.00-180.00   48
 34  \w    138.00 173.00   1.00   12.00    --  111.00  77.00  90.00   35
 35  \w     61.00  89.00   1.00   12.00    --  111.00 -61.00  60.00   28
 36  \w     56.00  88.00   1.00   12.00    --  111.00 -61.00 150.00   32
 37  \w     87.00 121.00   1.00   12.00    --  111.00  30.00  60.00   34
 38  \w    125.00 151.00   1.00   12.00    --  111.00  30.00  60.00   26
 39  \w     62.00 109.00   1.00   12.00    --  111.00-111.00  60.00   47
 40  \w    116.00 144.00   1.00   12.00    --  111.00 111.00 150.00   28
 41  \w     42.00  72.00   1.00   12.00    --  111.00 -45.00  90.00   30
 42  \w     48.00  92.00   1.00   12.00    --  111.00-111.00 -60.00   44
 43  \w     46.00  85.00   1.00   12.00    --  111.00-137.00 146.00   39
 44  \w     97.00 122.00   1.00   12.00    --  111.00-137.00 146.00   25
 45  \w     40.00  94.00   1.00   12.00    --  111.00-111.00  30.00   54
 46  \w      3.00  28.00   1.00    3.00    --   38.00  88.00 -66.91   25
 47  \w      4.00  31.00   1.00    3.00    --   38.00  86.00 110.66   27
 48  \w      3.00  29.00   1.00    3.00    --   38.00  88.00  20.29   26
 49  \w    -51.00  32.00   1.00    3.00    --  -41.40  77.00-120.00   83
 50  \w   -109.00 -71.00   1.00    3.00    --  -41.40 -37.00  90.00   38
 51  \w    -76.00 -20.00   1.00    3.00    --  -41.40 -37.00-120.00   56
 52  \w    -66.00 -19.00   1.00    3.00    --  -41.40 -37.00  90.00   47
 53  \w      8.00  33.00   1.00    3.00    --   41.40  83.00-131.05   25
 54  \w     15.00  40.00   1.00    3.00    --   46.00  76.00-110.38   25
 55  \w     14.00  39.00   1.00    3.00    --   46.00  80.00   1.74   25
 56  \w     14.00  42.00   1.00    3.00    --   46.00  82.00  91.21   28
 57  \w     32.00  59.00   1.00    3.00    --   62.00  71.00 -89.47   27
 58  \w     33.00  60.00   1.00    3.00    --   62.00  70.00  81.40   27
 59  \w     32.00  40.00   1.00    3.00    --   62.00  71.00  24.50    8
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0047531000
_diffrn_orient_matrix_UB_12      0.0096580000
_diffrn_orient_matrix_UB_13      0.0432627000
_diffrn_orient_matrix_UB_21      -0.1292120000
_diffrn_orient_matrix_UB_22      0.0012438000
_diffrn_orient_matrix_UB_23      -0.0019780000
_diffrn_orient_matrix_UB_31      -0.0089072000
_diffrn_orient_matrix_UB_32      -0.0688174000
_diffrn_orient_matrix_UB_33      -0.0010852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            130031
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.350
_diffrn_reflns_theta_min         3.719
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2155
_refine_ls_number_reflns         39407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0537P)^2^+6.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31177
_reflns_number_total             39407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03416j1.cif
_cod_data_source_block           132xzme21_ap_1comp_num
_cod_database_code               7714366
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C210 H252 Ge6 B6 N12'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.610
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C9A(H9A), C12A(H12A), C21A(H21A), C24A(H24A), C47A(H47A), C50A(H50A),
 C59A(H59A), C62A(H62A), C9B(H9B), C12B(H12B), C21B(H21B), C24B(H24B),
 C47B(H47B), C50B(H50B), C59B(H59B), C62B(H62B), C9C(H9C), C12C(H12C),
 C21C(H21C), C24C(H24C), C9D(H9D), C12D(H12D), C21D(H21D), C24D(H24D)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C5A(H5A), C6A(H6A), C7A(H7A), C17A(H17A), C18A(H18A),
 C19A(H19A), C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A), C35A(H35A),
 C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A), C43A(H43A),
 C44A(H44A), C45A(H45A), C55A(H55A), C56A(H56A), C57A(H57A), C1B(H1B), C2B(H2B),
  C5B(H5B), C6B(H6B), C7B(H7B), C17B(H17B), C18B(H18B), C19B(H19B), C28B(H28B),
 C29B(H29B), C30B(H30B), C31B(H31B), C35B(H35B), C36B(H36B), C37B(H37B),
 C38B(H38B), C39B(H39B), C40B(H40B), C43B(H43B), C44B(H44B), C45B(H45B),
 C55B(H55B), C56B(H56B), C57B(H57B), C1C(H1C), C2C(H2C), C5C(H5C), C6C(H6C),
 C7C(H7C), C17C(H17C), C18C(H18C), C19C(H19C), C28C(H28C), C29C(H29C),
 C30C(H30C), C31C(H31C), C1D(H1D), C2D(H2D), C5D(H5D), C6D(H6D), C7D(H7D),
 C17D(H17D), C18D(H18D), C19D(H19D), C28D(H28D), C29D(H29D), C30D(H30D),
 C31D(H31D)
2.c Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C25A(H25A,H25B,H25C),
 C26A(H26A,H26B,H26C), C48A(H48A,H48B,H48C), C49A(H49A,H49B,H49C), C51A(H51A,
 H51B,H51C), C52A(H52A,H52B,H52C), C60A(H60A,H60B,H60C), C61A(H61A,H61B,H61C),
 C63A(H63A,H63B,H63C), C64A(H64A,H64B,H64C), C10B(H10D,H10E,H10F), C11B(H11D,
 H11E,H11F), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C22B(H22D,H22E,H22F),
 C23B(H23D,H23E,H23F), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F), C48B(H48D,
 H48E,H48F), C49B(H49D,H49E,H49F), C51B(H51D,H51E,H51F), C52B(H52D,H52E,H52F),
 C60B(H60D,H60E,H60F), C61B(H61D,H61E,H61F), C63B(H63D,H63E,H63F), C64B(H64D,
 H64E,H64F), C10C(H10G,H10H,H10I), C11C(H11G,H11H,H11I), C13C(H13G,H13H,H13I),
 C14C(H14G,H14H,H14I), C22C(H22G,H22H,H22I), C23C(H23G,H23H,H23I), C25C(H25G,
 H25H,H25I), C26C(H26G,H26H,H26I), C10D(H10J,H10K,H10L), C11D(H11J,H11K,H11L),
 C13D(H13J,H13K,H13L), C14D(H14J,H14K,H14L), C22D(H22J,H22K,H22L), C23D(H23J,
 H23K,H23L), C25D(H25J,H25K,H25L), C26D(H26J,H26K,H26L)
;
_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 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.783