Isolation of the key intermediates of base-promoted borylene‒carbonyl coupling reactions
Braunschweig, Holger; Kramer, Thomas; Radacki, Krzysztof; Shang, Rong; Siedler, Eva; Werner, Christine; Chemical Science 5 (2014) 2271–; doi:10.1039/c4sc00183d

data_1516559
_publ_section_title
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 Isolation of the key intermediates of base-promoted borylene--carbonyl
 coupling reactions
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_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2271
_journal_paper_doi               10.1039/c4sc00183d
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C16 H22 B Mn N2 O2'
_chemical_formula_sum            'C16 H22 B Mn N2 O2'
_chemical_formula_weight         340.11
_chemical_name_common
;

?

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_chemical_name_systematic
; 

?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.815(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.4606(11)
_cell_length_b                   12.5027(9)
_cell_length_c                   18.2085(13)
_cell_measurement_reflns_used    5943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.39
_cell_volume                     3284.7(4)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6489
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.745686
_exptl_absorpt_correction_T_min  0.636132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TwinAbs 2008/3 (Bruker 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.362
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6489
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0218P)^2^+18.3314P] where
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1857
_reflns_number_gt                5244
_reflns_number_total             6489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00183d1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1516559