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_7115277
_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         'C35 H54 B N3'
_chemical_formula_sum            'C35 H54 B N3'
_chemical_formula_weight         527.62
_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 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.492(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2182(7)
_cell_length_b                   9.3515(4)
_cell_length_c                   21.6436(10)
_cell_measurement_reflns_used    6717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.54
_cell_volume                     3178.1(2)
_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      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22614
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         1.413
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0495 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.9686.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+0.5412P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4873
_reflns_number_total             6500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03497j2.cif
_cod_data_source_block           gb_mm3_0m
_cod_database_code               7115277
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.7454
_shelx_estimated_absorpt_t_min   0.7220
_olex2_refinement_description
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1. Others
 Fixed Uiso: H1A(0.035) H1B(0.035) H1C(0.035) H2(0.022) H9(0.03) H10(0.034)
 H11(0.031) H12(0.025) H14(0.023) H15A(0.041) H15B(0.041) H15C(0.041)
 H16A(0.04) H16B(0.04) H16C(0.04) H17(0.022) H18A(0.036) H18B(0.036)
 H18C(0.036) H19A(0.042) H19B(0.042) H19C(0.042) H20A(0.043) H20B(0.043)
 H22A(0.031) H22B(0.031) H23A(0.062) H23B(0.062) H23C(0.062) H24A(0.026)
 H24B(0.026) H25A(0.047) H25B(0.047) H25C(0.047) H26A(0.045) H26B(0.045)
 H26C(0.045) H27A(0.064) H27B(0.064) H27C(0.064) H28A(0.038) H28B(0.038)
 H28C(0.038) H29(0.024) H30(0.025) H31(0.023) H33(0.023) H34A(0.038)
 H34B(0.038) H34C(0.038) H35A(0.041) H35B(0.041) H35C(0.041) H1(0.017)
 Fixed X: H1A(0.2812) H1B(0.2418) H1C(0.2253) H2(0.1049) H9(-0.0032)
 H10(0.0704) H11(0.167) H12(0.1951) H14(0.1551) H15A(0.1727) H15B(0.1808)
 H15C(0.092) H16A(0.2712) H16B(0.2973) H16C(0.2795) H17(-0.0397) H18A(0.0471)
 H18B(0.0056) H18C(0.0852) H19A(-0.1356) H19B(-0.1443) H19C(-0.0956) H20A(-
 0.1442) H20B(-0.1905) H22A(-0.2) H22B(-0.1215) H23A(-0.1388) H23B(-0.2165)
 H23C(-0.2228) H24A(-0.0255) H24B(-0.0385) H25A(-0.178) H25B(-0.1167) H25C(-
 0.1694) H26A(-0.1522) H26B(-0.1717) H26C(-0.0888) H27A(-0.0083) H27B(-0.0955)
 H27C(-0.0202) H28A(0.1181) H28B(0.1753) H28C(0.2165) H29(0.2392) H30(0.2187)
 H31(0.1043) H33(-0.0645) H34A(0.0394) H34B(-0.0361) H34C(0.0496) H35A(-0.0331)
 H35B(-0.1188) H35C(-0.0903) H1(0.1038)
 Fixed Y: H1A(0.561) H1B(0.6774) H1C(0.5148) H2(0.6234) H9(0.1817) H10(0.2627)
 H11(0.447) H12(0.5563) H14(0.5883) H15A(0.7281) H15B(0.8) H15C(0.7454)
 H16A(0.4484) H16B(0.6102) H16C(0.5324) H17(0.1822) H18A(0.0196) H18B(-0.0425)
 H18C(0.0581) H19A(0.2364) H19B(0.0834) H19C(0.1042) H20A(0.6616) H20B(0.5126)
 H22A(0.4964) H22B(0.4153) H23A(0.2388) H23B(0.2458) H23C(0.3163) H24A(0.7114)
 H24B(0.6363) H25A(0.7206) H25B(0.8506) H25C(0.7885) H26A(0.3345) H26B(0.4659)
 H26C(0.3754) H27A(0.6022) H27B(0.6803) H27C(0.7039) H28A(0.7043) H28B(0.7945)
 H28C(0.6761) H29(0.4255) H30(0.1949) H31(0.0639) H33(0.1911) H34A(0.0743)
 H34B(-0.03) H34C(-0.0425) H35A(-0.0211) H35B(-0.0023) H35C(0.1135) H1(0.3462)
 Fixed Z: H1A(0.4019) H1B(0.3508) H1C(0.3348) H2(0.3591) H9(-0.0005) H10(-
 0.0726) H11(-0.047) H12(0.0525) H14(0.2269) H15A(0.1156) H15B(0.1823)
 H15C(0.1425) H16A(0.2204) H16B(0.2257) H16C(0.1595) H17(0.1759) H18A(0.1024)
 H18B(0.1548) H18C(0.1744) H19A(0.0732) H19B(0.1005) H19C(0.047) H20A(0.2934)
 H20B(0.2848) H22A(0.1649) H22B(0.1522) H23A(0.2273) H23B(0.1674) H23C(0.2317)
 H24A(0.2428) H24B(0.1765) H25A(0.1452) H25B(0.1673) H25C(0.2127) H26A(0.3641)
 H26B(0.4032) H26C(0.4291) H27A(0.4386) H27B(0.4118) H27C(0.3794) H28A(0.4651)
 H28B(0.4311) H28C(0.4805) H29(0.4857) H30(0.5158) H31(0.4587) H33(0.3321)
 H34A(0.2917) H34B(0.2922) H34C(0.345) H35A(0.4285) H35B(0.3762) H35C(0.4297)
 H1(0.2728)
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_shelx_res_checksum              85174