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_7115279
_publ_section_title
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 An efficient synthetic route to stable bis(carbene)borylenes [(L1)(L2)BH]
;
_journal_name_full               Chem.Commun.
_journal_page_first              7837
_journal_paper_doi               10.1039/C4CC03497J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C36 H54 B F3 N3 O3 S, C24 H20 B'
_chemical_formula_sum            'C60 H74 B2 F3 N3 O3 S'
_chemical_formula_weight         995.90
_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
_audit_creation_date             2014-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2853 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2524(5)
_cell_length_b                   13.4771(5)
_cell_length_c                   28.1965(9)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.56
_cell_volume                     5413.6(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      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34655
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         2.509
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.118
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+2.1800P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8741
_reflns_number_total             10835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03497j2.cif
_cod_data_source_block           gb_mm1
_cod_database_code               7115279
_shelxl_version_number           2013-2
_olex2_refinement_description
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1. Others
 Fixed Uiso: H12(0.018) H13(0.019) H15(0.016) H17(0.02) H21(0.019) H22(0.02)
 H24A(0.027) H24B(0.027) H24C(0.027) H25(0.02) H26A(0.027) H26B(0.027)
 H26C(0.027) H28A(0.022) H28B(0.022) H28C(0.022) H29(0.02) H30(0.026)
 H31(0.016) H32A(0.019) H32B(0.019) H33(0.018) H36(0.022) H37(0.022) H38(0.02)
 H39(0.025) H40(0.02) H42A(0.026) H42B(0.026) H42C(0.026) H43A(0.038)
 H43B(0.038) H43C(0.038) H44A(0.029) H44B(0.029) H44C(0.029) H45(0.019)
 H47A(0.026) H47B(0.026) H47C(0.026) H48(0.023) H49(0.022) H51A(0.022)
 H51B(0.022) H52(0.021) H53A(0.021) H53B(0.021) H54(0.023) H55(0.025) H56(0.03)
 H58(0.019) H59A(0.028) H59B(0.028) H59C(0.028) H60(0.017) H61(0.036)
 H62(0.032) H63(0.041) H64(0.025) H65A(0.031) H65B(0.031) H65C(0.031)
 H66(0.039) H67A(0.035) H67B(0.035) H67C(0.035) H68(0.036) H69A(0.044)
 H69B(0.044) H69C(0.044) H70A(0.037) H70B(0.037) H70C(0.037) H71(0.037)
 Fixed X: H12(-0.3248) H13(0.2593) H15(0.4983) H17(-0.4037) H21(0.4954) H22(-
 0.5316) H24A(0.1411) H24B(0.2165) H24C(0.1282) H25(0.388) H26A(0.2293)
 H26B(0.3225) H26C(0.3028) H28A(0.5014) H28B(0.5342) H28C(0.5449) H29(-0.392)
 H30(-0.21) H31(0.2757) H32A(0.4727) H32B(0.4081) H33(0.2006) H36(-0.2523) H37(-
 0.5437) H38(0.1054) H39(-0.2615) H40(-0.61) H42A(0.4922) H42B(0.5314)
 H42C(0.4242) H43A(0.0535) H43B(0.0253) H43C(-0.0476) H44A(0.1132) H44B(0.0577)
 H44C(0.1102) H45(0.0753) H47A(0.6149) H47B(0.6487) H47C(0.6153) H48(-0.2138)
 H49(-0.1588) H51A(0.3048) H51B(0.3672) H52(-0.0731) H53A(0.1965) H53B(0.2134)
 H54(-0.3194) H55(-0.4194) H56(-0.0896) H58(-0.098) H59A(0.2907) H59B(0.3833)
 H59C(0.3503) H60(0.2992) H61(0.0255) H62(-0.1225) H63(-0.2952) H64(-0.15)
 H65A(0.2028) H65B(0.1413) H65C(0.2511) H66(0.0406) H67A(-0.0769) H67B(-0.0445)
 H67C(0.0002) H68(-0.1571) H69A(0.2864) H69B(0.1943) H69C(0.2911) H70A(0.4373)
 H70B(0.4991) H70C(0.452) H71(-0.4267)
 Fixed Y: H12(0.829) H13(0.4335) H15(0.6792) H17(0.6112) H21(0.5914)
 H22(0.7945) H24A(1.0223) H24B(1.1043) H24C(1.0944) H25(0.4859) H26A(1.0731)
 H26B(1.0802) H26C(0.9866) H28A(0.4701) H28B(0.4517) H28C(0.5572) H29(0.8428)
 H30(0.5091) H31(0.9552) H32A(0.6312) H32B(0.5578) H33(0.4848) H36(0.7199)
 H37(0.5634) H38(0.6287) H39(0.5886) H40(0.6545) H42A(0.7804) H42B(0.8268)
 H42C(0.8023) H43A(0.6233) H43B(0.5351) H43C(0.6188) H44A(0.5716) H44B(0.4783)
 H44C(0.4751) H45(1.0704) H47A(0.578) H47B(0.6875) H47C(0.6528) H48(0.59)
 H49(0.9155) H51A(0.8164) H51B(0.7671) H52(1.061) H53A(0.6875) H53B(0.5799)
 H54(0.7497) H55(0.905) H56(0.7529) H58(0.7719) H59A(0.4492) H59B(0.3943)
 H59C(0.3934) H60(0.8103) H61(0.674) H62(0.6777) H63(1.172) H64(0.9282)
 H65A(0.3248) H65B(0.3252) H65C(0.3226) H66(0.7134) H67A(0.7073) H67B(0.6049)
 H67C(0.7036) H68(1.0977) H69A(0.5339) H69B(0.5889) H69C(0.644) H70A(0.8287)
 H70B(0.7832) H70C(0.8873) H71(1.0744)
 Fixed Z: H12(0.4089) H13(0.1777) H15(0.2914) H17(0.4855) H21(0.1734)
 H22(0.606) H24A(0.2724) H24B(0.2838) H24C(0.3153) H25(0.1371) H26A(0.3896)
 H26B(0.3616) H26C(0.3927) H28A(0.3004) H28B(0.3533) H28C(0.3306) H29(0.5739)
 H30(0.4011) H31(0.3113) H32A(0.392) H32B(0.4197) H33(0.2958) H36(0.5986)
 H37(0.5166) H38(0.3189) H39(0.3317) H40(0.5769) H42A(0.2031) H42B(0.2507)
 H42C(0.2445) H43A(0.4024) H43B(0.3687) H43C(0.3791) H44A(0.2356) H44B(0.2525)
 H44C(0.2045) H45(0.388) H47A(0.2554) H47B(0.2637) H47C(0.2129) H48(0.4728)
 H49(0.4162) H51A(0.3986) H51B(0.4385) H52(0.4194) H53A(0.4094) H53B(0.3908)
 H54(0.3367) H55(0.4764) H56(0.4868) H58(0.384) H59A(0.3651) H59B(0.3812)
 H59C(0.3276) H60(0.3016) H61(0.6126) H62(0.6447) H63(0.4802) H64(0.5183)
 H65A(0.2301) H65B(0.2753) H65C(0.2808) H66(0.5329) H67A(0.304) H67B(0.2838)
 H67C(0.2655) H68(0.5073) H69A(0.4608) H69B(0.4746) H69C(0.4786) H70A(0.3509)
 H70B(0.3924) H70C(0.3986) H71(0.4654)
;
_shelx_res_checksum              57184