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_7118521
_publ_section_title
;
 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_absolute_configuration ad
_chemical_formula_moiety         'C67 H95 B3 Ge2 N4 O5'
_chemical_formula_sum            'C67 H95 B3 Ge2 N4 O5'
_chemical_formula_weight         1214.07
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2015-08-31 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.46(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.192(8)
_cell_length_b                   24.045
_cell_length_c                   13.298
_cell_measurement_temperature    293(2)
_cell_volume                     4210(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.929
_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  0.0754
_diffrn_reflns_av_unetI/netI     0.1984
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37308
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.586
_diffrn_reflns_theta_min         1.534
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 3663 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.073(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         19197
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2176
_reflns_Friedel_coverage         0.878
_reflns_friedel_fraction_full    0.985
_reflns_friedel_fraction_max     0.854
_reflns_number_gt                11553
_reflns_number_total             19197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc09330a2.cif
_cod_data_source_block           1_sq
_cod_database_code               7118521
_shelxl_version_number           2013-2
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C39(H39), C42(H42), C51(H51), C54(H54), C66(H66)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C29(H29A,H29B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C34(H34), C35(H35),
 C36(H36), C46(H46), C47(H47), C48(H48), C58(H58), C60(H60)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C)
;
_shelx_fab_checksum              49624
_olex2_submission_special_instructions 'No special instructions were received'