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

data_7714365
_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         'C32 H40 B2 N2 O2'
_chemical_formula_sum            'C32 H40 B2 N2 O2'
_chemical_formula_weight         506.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-04
_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                 105.5900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5820(2)
_cell_length_b                   11.08990(10)
_cell_length_c                   16.7948(2)
_cell_measurement_reflns_used    14895
_cell_measurement_temperature    150.01(16)
_cell_measurement_theta_max      76.1620
_cell_measurement_theta_min      4.3570
_cell_volume                     2974.82(6)
_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      150.01(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -22.00  28.00   1.00    2.00    --  -42.66  38.00-180.00   50
  2  \w      2.00  36.00   1.00    2.00    --  -42.66  19.00 120.00   34
  3  \w     -1.00  29.00   1.00    2.00    --  -42.66  19.00-150.00   30
  4  \w     -1.00  31.00   1.00    2.00    --  -42.66  19.00 -30.00   32
  5  \w    -22.00  10.00   1.00    2.00    --  -42.66  38.00-120.00   32
  6  \w     79.00 125.00   1.00    2.00    --   42.66 178.00 -90.00   46
  7  \w     70.00 103.00   1.00    2.00    --   42.66 169.00  10.00   33
  8  \w    105.00 168.00   1.00    5.00    --  111.00  77.00-120.00   63
  9  \w     40.00  66.00   1.00    5.00    --  111.00 -45.00-180.00   26
 10  \w     43.00  71.00   1.00    5.00    --  111.00 -45.00 120.00   28
 11  \w     70.00 112.00   1.00    5.00    --  111.00-125.00-150.00   42
 12  \w     55.00  81.00   1.00    5.00    --  111.00 -77.00-180.00   26
 13  \w    102.00 127.00   1.00    5.00    --  111.00 -77.00-180.00   25
 14  \w     41.00  89.00   1.00    5.00    --  111.00 -61.00  90.00   48
 15  \w     87.00 168.00   1.00    5.00    --  111.00  45.00 -60.00   81
 16  \w     46.00  71.00   1.00    5.00    --  111.00 -45.00 -90.00   25
 17  \w     40.00  68.00   1.00    5.00    --  111.00 -45.00-150.00   28
 18  \w     83.00 112.00   1.00    5.00    --  111.00-125.00-180.00   29
 19  \w     46.00  72.00   1.00    5.00    --  111.00 -45.00 150.00   26
 20  \w     42.00  68.00   1.00    5.00    --  111.00 -45.00   0.00   26
 21  \w     71.00 112.00   1.00    5.00    --  111.00-125.00 -90.00   41
 22  \w     39.00  65.00   1.00    5.00    --  111.00-125.00 120.00   26
 23  \w     41.00  67.00   1.00    5.00    --  111.00-125.00-180.00   26
 24  \w    105.00 133.00   1.00    5.00    --  111.00  77.00   0.00   28
 25  \w     86.00 111.00   1.00    5.00    --  111.00-125.00-120.00   25
 26  \w     88.00 165.00   1.00    5.00    --  111.00  30.00-150.00   77
 27  \w      9.00  36.00   1.00    2.00    --  -42.66  19.00-180.00   27
 28  \w      4.00  36.00   1.00    2.00    --  -42.66  19.00  60.00   32
 29  \w      4.00  36.00   1.00    2.00    --  -42.66  19.00  90.00   32
 30  \w      1.00  27.00   1.00    2.00    --  -42.66  19.00 -90.00   26
 31  \w     70.00  98.00   1.00    2.00    --   42.66 178.00 150.00   28
 32  \w     62.00 127.00   1.00    2.00    --   42.66 178.00  90.00   65
 33  \w     62.00  88.00   1.00    5.00    --  111.00 -95.00 -30.00   26
 34  \w     82.00 108.00   1.00    5.00    --  111.00-108.00-138.28   26
 35  \w     77.00 107.00   1.00    5.00    --  111.00-103.00  90.85   30
 36  \w     40.00  72.00   1.00    5.00    --  111.00 -45.00 -60.00   32
 37  \w     66.00 109.00   1.00    5.00    --  111.00-125.00 -60.00   43
 38  \w    111.00 150.00   1.00    5.00    --  111.00  77.00  30.00   39
 39  \w    119.00 146.00   1.00    5.00    --  111.00  30.00 -30.00   27
 40  \w     40.00  72.00   1.00    5.00    --  111.00 -45.00 -30.00   32
 41  \w     76.00 117.00   1.00    5.00    --  111.00-132.00  39.75   41
 42  \w     64.00  92.00   1.00    5.00    --  111.00 -61.00   0.00   28
 43  \w    149.00 175.00   1.00    5.00    --  111.00  30.00 -90.00   26
 44  \w     90.00 105.00   1.00    5.00    --  111.00  30.00 -90.00   15
;
_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      -0.0044172000
_diffrn_orient_matrix_UB_12      -0.1367910000
_diffrn_orient_matrix_UB_13      0.0139494000
_diffrn_orient_matrix_UB_21      -0.0829067000
_diffrn_orient_matrix_UB_22      -0.0062968000
_diffrn_orient_matrix_UB_23      -0.0687689000
_diffrn_orient_matrix_UB_31      0.0491453000
_diffrn_orient_matrix_UB_32      -0.0228610000
_diffrn_orient_matrix_UB_33      -0.0644439000
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25640
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.134
_diffrn_reflns_theta_min         4.835
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.413
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0551P)^2^+0.8624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5495
_reflns_number_total             6152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03416j1.cif
_cod_data_source_block           212xzme22_mp_num
_cod_database_code               7714365
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H40 B2 O2 N2'
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.785
_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:
 C9(H9), C12(H12), C21(H21), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19),
 C31(H31), C32(H32), C33(H33), C34(H34)
2.c 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)
;
_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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.798