An efficient synthetic route to stable bis(carbene)borylenes [(L1)(L2)BH]
David A. Ruiz; Mohand Melaimi; Guy Bertrand; Chem.Commun. 50 (2014) 7837–; doi:10.1039/C4CC03497J

data_7115276
_publ_section_title
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 An efficient synthetic route to stable bis(carbene)borylenes [(L1)(L2)BH]
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_journal_name_full               Chem.Commun.
_journal_page_first              7837
_journal_paper_doi               10.1039/C4CC03497J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C37 H64 B N3, C2.5 H5.5'
_chemical_formula_sum            'C39.5 H70 B N3'
_chemical_formula_weight         597.80
_chemical_name_systematic
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 ?
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_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-06
_audit_creation_method
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Olex2 1.2
(compiled 2013.12.10 svn.r2853 for OlexSys, GUI svn.r4736)
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_cell_angle_alpha                90.00
_cell_angle_beta                 114.471(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.415(5)
_cell_length_b                   18.243(4)
_cell_length_c                   17.305(3)
_cell_measurement_temperature    100(2)
_cell_volume                     7877(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32951
_diffrn_reflns_theta_full        34.36
_diffrn_reflns_theta_max         34.36
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         15374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                9443
_reflns_number_total             15374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc03497j2.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C39.50 H70 B N3'
_cod_database_code               7115276
_olex2_refinement_description
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1. Others
 Fixed Sof: H3S1(0.5) H3S2(0.5)
 Fixed U12: C3S(0)
 Fixed U23: C3S(0)
 Fixed Uiso: H1S1(0.207) H1S2(0.207) H1S3(0.207) H2S1(0.105) H2S2(0.105)
 H3S1(0.087) H3S2(0.087)
 Fixed X: H1S1(0.5033) H1S2(0.5605) H1S3(0.5562) H2S1(0.5609) H2S2(0.5778)
 C3S(0.5) H3S1(0.5104) H3S2(0.4896)
 Fixed Y: H1S1(0.0349) H1S2(-0.0012) H1S3(0.0683) H2S1(0.0682) H2S2(0.133)
 H3S1(0.1728) H3S2(0.1728)
 Fixed Z: H1S1(0.1487) H1S2(0.2037) H1S3(0.1447) H2S1(0.3103) H2S2(0.2645)
 C3S(0.25) H3S1(0.3004) H3S2(0.1996)
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