Diverse reactivity of a tricoordinate organoboron L2PhB: (L = oxazol-2-ylidene) towards alkali metal, group 9 metal, and coinage metal precursors
Kong, Lingbing; Ganguly, Rakesh; Li, Yongxin; Kinjo, Rei; Chem. Sci. 6 (2015) 2893–; doi:10.1039/C5SC00404G

data_1518758
_publ_section_title
;
 Diverse reactivity of a tricoordinate organoboron L2PhB: (L =
 oxazol-2-ylidene) towards alkali metal, group 9 metal, and coinage metal
 precursors
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              2893
_journal_paper_doi               10.1039/C5SC00404G
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C26 H38.73 B Cl N2 O2 Rh'
_chemical_formula_sum            'C26 H39 B Cl N2 O2 Rh'
_chemical_formula_weight         560.76
_chemical_name_systematic
;
 ?
;
_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             2014-12-10
_audit_creation_method           'APEX2 v2013.10-0'
_audit_update_record
;
2014-12-10 deposited with the CCDC.
2015-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.628(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.460(2)
_cell_length_b                   13.8072(16)
_cell_length_c                   11.9483(18)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      20.8707
_cell_measurement_theta_min      2.5577
_cell_volume                     2627.4(6)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      103.15
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1241
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5132
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.952
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.298
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+26.1341P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2950
_reflns_number_total             4810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00404g2.cif
_cod_data_source_block           rei184
_cod_depositor_comments
'Adding full bibliography for 1518755--1518759.cif.'
_cod_database_code               1518758
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-C15 \\sim B1-C15A
 with sigma of 0.02
 Rh1-C9 \\sim Rh1A-C9
 with sigma of 0.02
3. Rigid bond restraints
 Rh1, Cl1, C1, C2, C3, C4, C5, C6, C7, C8, Rh1A, Cl1A, C1A, C2A, C3A, C4A, C5A,
  C6A, C7A, C8A, N2, O2, C15, C16, C17, C18, C19, C20, N2A, O2A, C15A, C16A,
 C17A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Rh1 \\sim Cl1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim N2 \\sim O2 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N2A \\sim O2A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A
\\sim Rh1A \\sim Cl1A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim
C6A \\sim C7A \\sim C8A: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Rh1 \\sim Rh1A: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(Rh1) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(O2) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N2A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16A)
\\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C19A) \\sim Ueq,
Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C8) = Uanis(C8A)
5. Same fragment restrains
{Rh1, Cl1, C1, C2, C3, C4, C5, C6, C7, C8} sigma for 1-2: 0.02, 1-3: 0.04
as
{Rh1A, Cl1A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A}
{N2, O2, C15, C16, C17, C18, C19, C20} sigma for 1-2: 0.02, 1-3: 0.04
as
{N2A, O2A, C15A, C16A, C17A, C18A, C19A, C20A}
6. Others
 Sof(Rh1A)=Sof(Cl1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8A)=1-FVAR(1)
 Sof(Rh1)=Sof(Cl1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8)=Sof(H9A)=Sof(H9B)=FVAR(1)
 Sof(H1B)=Sof(N2A)=Sof(O2A)=Sof(C15A)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(H1AA)=Sof(N2)=Sof(O2)=Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C1A(H1A), C4A(H4A), C5A(H5A), C8A(H8A),
 B1(H1AA), B1(H1B)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C2A(H2AA,H2AB), C3A(H3AA,
 H3AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C9(H9A,H9B), C11(H11A,H11B), C16(H16A,
 H16B), C16A(H16C,H16D)
7.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
7.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F),
 C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              52066
_shelx_hkl_checksum              90039
_olex2_submission_special_instructions 'No special instructions were received'