Synthesis of digermylene-stabilized linear tetraboronate and boroxine.
Wu, Yile; Liu, Liu; Su, Jue; Yan, Kaili; Zhu, Jun; Zhao, Yufen; Chemical communications (Cambridge, England) 52 (2016) 1582–1585; doi:10.1039/c5cc09330a

data_7118520
_publ_section_title
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 Synthesis of digermylene-stabilized linear tetraboronate and boroxine.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1582
_journal_page_last               1585
_journal_paper_doi               10.1039/c5cc09330a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C82 H102 B4 Ge2 N4 O5, C6 H14, C7 H8'
_chemical_formula_sum            'C95 H124 B4 Ge2 N4 O5'
_chemical_formula_weight         1590.40
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-13 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                110.972(3)
_cell_angle_beta                 94.490(3)
_cell_angle_gamma                95.764(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1574(18)
_cell_length_b                   16.907(3)
_cell_length_c                   23.516(4)
_cell_measurement_reflns_used    5600
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.28
_cell_volume                     4456.5(13)
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.1456
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32847
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.93
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.901135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.1016 before and 0.0425 after correction.
The Ratio of minimum to maximum transmission is 0.9011.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene and hexane'
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         15618
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+6.0195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2314
_reflns_number_gt                11253
_reflns_number_total             15618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc09330a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4456.5(12)
_cod_database_code               7118520
_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
 C207-C206
 2.5 with sigma of 0.02
 C207-C202
 2.5 with sigma of 0.02
 C201-C207
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C77, C78, C79, C80, C81, C82
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C71, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C65, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C51, C50, C52, C50A, C52A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C36, C35, C37, C35A, C37A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C19, C21, C19A, C21A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C51 \\sim C50 \\sim C52 \\sim C50A \\sim C52A: within 1.7A with sigma of 0.005
and sigma for terminal atoms of 0.01
C36 \\sim C35 \\sim C37 \\sim C35A \\sim C37A: within 1.7A with sigma of 0.005
and sigma for terminal atoms of 0.01
C20 \\sim C19 \\sim C21 \\sim C19A \\sim C21A: within 1.7A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C205) \\sim Ueq, Uanis(C204) \\sim Ueq, Uanis(C203) \\sim Ueq,
Uanis(C207) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C206) \\sim Ueq,
Uanis(C202) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C202) = Uanis(C203) = Uanis(C204) = Uanis(C205) = Uanis(C207) =
Uanis(C201) = Uanis(C206)
5. Others
 Fixed Sof: H20(0.5) H20A(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5) C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5)
 C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5) H36(0.5) H36A(0.5) C35(0.5) H35A(0.5)
 H35B(0.5) H35C(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C35A(0.5) H35D(0.5)
 H35E(0.5) H35F(0.5) C37A(0.5) H37D(0.5) H37E(0.5) H37F(0.5) H51(0.5) H51A(0.5)
 C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
 C50A(0.5) H50D(0.5) H50E(0.5) H50F(0.5) C52A(0.5) H52D(0.5) H52E(0.5) H52F(0.5)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C20(H20A), C23(H23), C36(H36), C36(H36A),
 C39(H39), C48(H48), C51(H51), C51(H51A)
6.b Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C31(H31),
 C32(H32), C33(H33), C43(H43), C44(H44), C45(H45), C55(H55), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69),
 C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C79(H79),
  C80(H80), C81(H81), C82(H82), C202(H202), C203(H203), C204(H204), C205(H205),
 C206(H206)
6.d Fitted hexagon refined as free rotating group:
 C201(C202,C203,C204,C205,C206)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C19A(H19D,H19E,H19F), C21A(H21D,H21E,
 H21F), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,
 H28B,H28C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C35A(H35D,H35E,H35F),
 C37A(H37D,H37E,H37F), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C50A(H50D,H50E,H50F), C52A(H52D,H52E,H52F), C53(H53A,H53B,H53C), C57(H57A,H57B,
 H57C), C91(H91A,H91B,H91C), C96(H96A,H96B,H96C), C207(H20B,H20C,H20D)
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_olex2_submission_special_instructions 'No special instructions were received'