Carbodicarbenes: Unexpected π-Accepting Ability during Re-activity with Small Molecules.
Chen, Wen-Ching; Shih, Wei-Chih; Jurca, Titel; Zhao, Lili; Andrada, Diego M.; Peng, Chun-Jung; Chang, Chun-Chi; Liu, Shu-Kai; Wang, Yi-Ping; Wen, Yuh-Sheng; Yap, Glenn P. A.; Hsu, Chao-Ping; Frenking, Gernot; Ong, Tiow-Gan; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08031

data_4126338
_publ_section_title
;
 Carbodicarbenes: Unexpected \p-Accepting Ability during Re-activity with
 Small Molecules.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08031
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C31 H43 B N4'
_chemical_formula_sum            'C31 H43 B N4'
_chemical_formula_weight         482.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_Int_Tables_number      76
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_audit_creation_date             2015-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8086(4)
_cell_length_b                   15.8086(4)
_cell_length_c                   11.7043(3)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      23.68
_cell_measurement_theta_min      2.52
_cell_volume                     2925.04(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            70404
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.9107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0730 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.9384.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.0956
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048.3408
_exptl_crystal_recrystallization_method
'Dissolved in diethyl ether and recrystallized at -15 oC.'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.1817
_refine_diff_density_min         -0.1323
_refine_diff_density_rms         0.0298
_refine_ls_d_res_high            0.7801
_refine_ls_d_res_low             15.8086
_refine_ls_goodness_of_fit_ref   1.0468
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0468
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.3960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         1.000
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                5985
_reflns_number_total             6457
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja7b08031_si_003.cif
_cod_data_source_block           i15863
_cod_original_sg_symbol_Hall     ' P 4w'
_cod_database_code               4126338
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C21(H21), C24(H24), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b), C29(H29a,H29b), C30(H30a,
 H30b), C31(H31a,H31b)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C16(H16), C17(H17), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C10(H10a,H10b,H10c), C13(H13a,H13b,H13c), C14(H14a,H14b,
 H14c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c)
;
_olex2_submission_special_instructions 'No special instructions were received'