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

data_7714364
_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         'C74 H112 B2 Ge2 Li2 N8, C5 H12'
_chemical_formula_sum            'C79 H124 B2 Ge2 Li2 N8'
_chemical_formula_weight         1366.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.994(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8726(8)
_cell_length_b                   16.5014(3)
_cell_length_c                   25.3097(7)
_cell_measurement_reflns_used    7695
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      74.2710
_cell_measurement_theta_min      3.2400
_cell_volume                     8279.5(5)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_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    -44.00  19.00   1.00    5.50    --  -42.16  57.00   0.00   63
  2  \w   -103.00 -16.00   1.00    5.50    --  -42.16 -57.00 -90.00   87
  3  \w   -103.00 -27.00   1.00    5.50    --  -42.16 -38.00-180.00   76
  4  \w    -27.00   0.00   1.00    5.50    --  -42.16 118.00  89.00   27
  5  \w     -5.00  20.00   1.00    5.50    --  -42.16  19.00   0.00   25
  6  \w     88.00 174.00   1.00   18.00    --  111.00  30.00 -90.00   86
  7  \w     50.00 111.00   1.00   18.00    --  111.00 -77.00 -30.00   61
  8  \w     62.00  89.00   1.00   18.00    --  111.00 -61.00 -30.00   27
  9  \w     56.00  90.00   1.00   18.00    --  111.00 -61.00-180.00   34
 10  \w     44.00  72.00   1.00   18.00    --  111.00 -45.00  60.00   28
 11  \w     41.00  70.00   1.00   18.00    --  111.00 -45.00  30.00   29
 12  \w     57.00  93.00   1.00   18.00    --  111.00 -61.00 120.00   36
 13  \w     66.00 136.00   1.00   18.00    --  111.00  15.00-150.00   70
 14  \w     40.00  67.00   1.00   18.00    --  111.00 -45.00 -30.00   27
 15  \w     63.00  89.00   1.00   18.00    --  111.00 -61.00  90.00   26
 16  \w     48.00  87.00   1.00   18.00    --  111.00 -95.00 -60.00   39
 17  \w     48.00  88.00   1.00   18.00    --  111.00 -61.00-150.00   40
 18  \w     55.00 108.00   1.00   18.00    --  111.00-118.00   3.00   53
 19  \w     40.00  70.00   1.00   18.00    --  111.00 -45.00  90.00   30
 20  \w     95.00 122.00   1.00   18.00    --  111.00  45.00   0.00   27
 21  \w    127.00 170.00   1.00   18.00    --  111.00  45.00   0.00   43
 22  \w     68.00  98.00   1.00   18.00    --  111.00-125.00 150.00   30
 23  \w    100.00 125.00   1.00   18.00    --  111.00  61.00-180.00   25
 24  \w    -12.00  -9.00   1.00    5.50    --  -42.16  38.00  30.00    3
;
_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      0.0249827000
_diffrn_orient_matrix_UB_12      0.0259472000
_diffrn_orient_matrix_UB_13      -0.0459740000
_diffrn_orient_matrix_UB_21      -0.0723333000
_diffrn_orient_matrix_UB_22      -0.0076200000
_diffrn_orient_matrix_UB_23      -0.0480841000
_diffrn_orient_matrix_UB_31      -0.0134010000
_diffrn_orient_matrix_UB_32      0.0893629000
_diffrn_orient_matrix_UB_33      0.0092928000
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.145
_diffrn_reflns_theta_min         3.299
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.718
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       plate
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8516
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0491P)^2^+6.2267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6363
_reflns_number_total             8516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03416j1.cif
_cod_data_source_block           215xzme22_mi_single_num
_cod_database_code               7714364
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H56 Ge1 Li1 B1 N4'
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.801
_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
 C54S-C53S = C53S-C52S = C52S-C51S = C51S-C50S
 1.52 with sigma of 0.02
 C54S-C52S = C53S-C51S = C52S-C50S
 2.54 with sigma of 0.04
 C54S-C53S \\sim C53S-C52S \\sim C52S-C51S \\sim C51S-C50S
 with sigma of 0.02
 C54S-C52S \\sim C52S-C50S \\sim C53S-C51S
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C50S \\sim C51S \\sim C52S \\sim C53S \\sim C54S: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C50S) \\sim Ueq, Uanis(C51S) \\sim Ueq, Uanis(C52S) \\sim Ueq,
Uanis(C53S) \\sim Ueq, Uanis(C54S) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.03
4. Rigid body (RIGU) restrains
 C50S, C51S, C52S, C53S, C54S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C50S(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C51S(0.5) H51A(0.5)
 H51B(0.5) C52S(0.5) H52A(0.5) H52B(0.5) C53S(0.5) H53B(0.5) H53A(0.5)
 C54S(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24), C33(H33), C38(H38)
6.b Secondary CH2 refined with riding coordinates:
 C51S(H51A,H51B), C52S(H52A,H52B), C53S(H53B,H53A)
6.c Me refined with riding coordinates:
 C50S(H50A,H50B,H50C), C54S(H54A,H54B,H54C)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19)
6.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_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 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.755