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_7115278
_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         'C38 H64 B F3 N3 O3 S, C24 H20 B'
_chemical_formula_sum            'C62 H84 B2 F3 N3 O3 S'
_chemical_formula_weight         1030.00
_chemical_name_systematic
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 ?
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_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.570(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.260(12)
_cell_length_b                   13.788(7)
_cell_length_c                   19.769(10)
_cell_measurement_temperature    100(2)
_cell_volume                     5816(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1417
_diffrn_reflns_av_unetI/netI     0.2426
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24181
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00202(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         8342
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.1833
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                3230
_reflns_number_total             8342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc03497j2.cif
_cod_data_source_block           shelxl_a
_cod_database_code               7115278
_olex2_refinement_description
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1. Shared sites
{O2A, O2B}
2. Others
 Fixed Sof: S1A(0.6) O1A(0.6) O2A(0.6) O3A(0.6) C3A(0.6) F1A(0.6) F2A(0.6)
 F3A(0.6) H1A(0.6) S1B(0.4) O1B(0.4) O2B(0.4) O3B(0.4) C3B(0.4) F1B(0.4)
 F2B(0.4) F3B(0.4) H1B(0.4)
 Fixed Uiso: H3A(0.032) H3B(0.032) H10(0.033) H11(0.035) H12(0.035)
 H14A(0.029) H14B(0.029) H15A(0.07) H15B(0.07) H15C(0.07) H16A(0.033)
 H16B(0.033) H17A(0.071) H17B(0.071) H17C(0.071) H18A(0.061) H18B(0.061)
 H18C(0.061) H19A(0.06) H19B(0.06) H19C(0.06) H20A(0.053) H20B(0.053)
 H20C(0.053) H21(0.071) H22A(0.256) H22B(0.256) H22C(0.256) H23(0.034)
 H24A(0.067) H24B(0.067) H24C(0.067) H25A(0.073) H25B(0.073) H25C(0.073)
 H26(0.035) H27A(0.069) H27B(0.069) H27C(0.069) H28A(0.062) H28B(0.062)
 H28C(0.062) H29(0.037) H30A(0.052) H30B(0.052) H30C(0.052) H31A(0.067)
 H31B(0.067) H31C(0.067) H32(0.027) H33A(0.05) H33B(0.05) H33C(0.05)
 H34A(0.053) H34B(0.053) H34C(0.053) H35(0.033) H36A(0.058) H36B(0.058)
 H36C(0.058) H37A(0.054) H37B(0.054) H37C(0.054) H112(0.036) H113(0.043)
 H114(0.045) H115(0.041) H116(0.036) H118(0.03) H119(0.036) H120(0.037)
 H121(0.034) H122(0.033) H124(0.032) H125(0.029) H126(0.032) H127(0.029)
 H128(0.028) H130(0.034) H131(0.044) H132(0.044) H133(0.042) H134(0.038)
 Fixed X: H3A(0.8333) H3B(0.769) H10(0.9368) H11(1.0384) H12(1.0574)
 H14A(0.7093) H14B(0.6961) H15A(0.6625) H15B(0.6205) H15C(0.6737) H16A(0.7558)
 H16B(0.7641) H17A(0.8758) H17B(0.8456) H17C(0.8638) H18A(0.7792) H18B(0.7593)
 H18C(0.8182) H19A(0.9208) H19B(0.8809) H19C(0.9187) H20A(0.7094) H20B(0.6798)
 H20C(0.7438) H21(0.6256) H22A(0.6872) H22B(0.6142) H22C(0.6477) H23(0.6016)
 H24A(0.5713) H24B(0.5121) H24C(0.5407) H25A(0.5521) H25B(0.5263) H25C(0.5934)
 H26(0.8153) H27A(0.7389) H27B(0.8031) H27C(0.7448) H28A(0.8123) H28B(0.872)
 H28C(0.8445) H29(0.713) H30A(0.6669) H30B(0.6651) H30C(0.7308) H31A(0.6362)
 H31B(0.603) H31C(0.6095) H32(0.7965) H33A(0.848) H33B(0.8387) H33C(0.7791)
 H34A(0.8395) H34B(0.768) H34C(0.8166) H35(0.9455) H36A(1.0753) H36B(1.0406)
 H36C(1.0239) H37A(0.9733) H37B(1.014) H37C(1.0445) H112(0.7274) H113(0.8345)
 H114(0.8954) H115(0.848) H116(0.7413) H118(0.6863) H119(0.6571) H120(0.5765)
 H121(0.5266) H122(0.5567) H124(0.5279) H125(0.4939) H126(0.5668) H127(0.6738)
 H128(0.7067) H130(0.6064) H131(0.5601) H132(0.5295) H133(0.5509) H134(0.6008)
 Fixed Y: H3A(0.2729) H3B(0.3327) H10(0.6035) H11(0.5483) H12(0.4162)
 H14A(0.3651) H14B(0.2594) H15A(0.2076) H15B(0.2956) H15C(0.315) H16A(0.1336)
 H16B(0.1254) H17A(0.1362) H17B(0.0408) H17C(0.1308) H18A(0.5108) H18B(0.4824)
 H18C(0.5521) H19A(0.3759) H19B(0.4571) H19C(0.4845) H20A(0.4506) H20B(0.3535)
 H20C(0.3488) H21(0.3743) H22A(0.4321) H22B(0.4101) H22C(0.4932) H23(0.1412)
 H24A(0.2346) H24B(0.2063) H24C(0.3135) H25A(0.2941) H25B(0.1852) H25C(0.2071)
 H26(0.0271) H27A(-0.0632) H27B(-0.1225) H27C(-0.1493) H28A(-0.1268) H28B(-
 0.0937) H28C(-0.024) H29(-0.0987) H30A(0.0729) H30B(-0.0335) H30C(0.02) H31A(-
 0.0865) H31B(-0.0899) H31C(0.011) H32(0.5066) H33A(0.6958) H33B(0.6559)
 H33C(0.6737) H34A(0.5924) H34B(0.5687) H34C(0.4822) H35(0.2816) H36A(0.3382)
 H36B(0.274) H36C(0.3866) H37A(0.1984) H37B(0.1596) H37C(0.2329) H112(0.9485)
 H113(0.9639) H114(0.8266) H115(0.6739) H116(0.66) H118(0.7011) H119(0.5641)
 H120(0.464) H121(0.5028) H122(0.6406) H124(0.8004) H125(0.8078) H126(0.8067)
 H127(0.7977) H128(0.7863) H130(0.9749) H131(1.1069) H132(1.098) H133(0.9573)
 H134(0.8275)
 Fixed Z: H3A(0.3025) H3B(0.2883) H10(0.0758) H11(0.1243) H12(0.2001)
 H14A(0.1475) H14B(0.1134) H15A(0.2114) H15B(0.1706) H15C(0.2432) H16A(0.2344)
 H16B(0.1571) H17A(0.2091) H17B(0.2321) H17C(0.2851) H18A(0.2799) H18B(0.198)
 H18C(0.2296) H19A(0.3307) H19B(0.3566) H19C(0.3015) H20A(-0.1188) H20B(-
 0.1591) H20C(-0.0965) H21(-0.0982) H22A(0.0244) H22B(-0.0096) H22C(-0.0423)
 H23(-0.0711) H24A(0.0137) H24B(-0.0509) H24C(-0.0455) H25A(-0.1679) H25B(-
 0.1731) H25C(-0.1844) H26(0.0886) H27A(0.1247) H27B(0.1389) H27C(0.0727) H28A(-
 0.0089) H28B(0.0535) H28C(-0.0129) H29(-0.0494) H30A(-0.1263) H30B(-0.1591)
 H30C(-0.1266) H31A(0.0081) H31B(-0.0752) H31C(-0.0336) H32(0.1037)
 H33A(0.0934) H33B(0.1658) H33C(0.0992) H34A(-0.0065) H34B(-0.0114) H34C(-
 0.0083) H35(0.2599) H36A(0.3037) H36B(0.3487) H36C(0.3356) H37A(0.1675)
 H37B(0.2429) H37C(0.1992) H112(0.2828) H113(0.3389) H114(0.3814) H115(0.3647)
 H116(0.3135) H118(0.1687) H119(0.1001) H120(0.1127) H121(0.1991) H122(0.2688)
 H124(0.2968) H125(0.3974) H126(0.5094) H127(0.5186) H128(0.4165) H130(0.301)
 H131(0.2337) H132(0.1103) H133(0.0564) H134(0.1236)
;