Ring Expansion Reactions of Electron-Rich Boron-Containing Heterocycles
Araneda, Juan F.; Piers, Warren E.; Sgro, Michael J.; Parvez, Masood; Organometallics 34 (2015) 3408–; doi:10.1021/acs.organomet.5b00390

data_4085951
_publ_section_title
;
 Ring Expansion Reactions of Electron-Rich Boron-Containing Heterocycles
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3408
_journal_paper_doi               10.1021/acs.organomet.5b00390
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C114 H156 B4 K4 O8, 2(C4 H8 O)'
_chemical_formula_sum            'C122 H172 B4 K4 O10'
_chemical_formula_weight         1998.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.390(3)
_cell_angle_beta                 78.224(3)
_cell_angle_gamma                64.155(3)
_cell_formula_units_Z            1
_cell_length_a                   14.3390(7)
_cell_length_b                   15.3414(7)
_cell_length_c                   16.5198(9)
_cell_measurement_reflns_used    6490
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      2.74
_cell_volume                     3194.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37367
_diffrn_reflns_theta_full        68.50
_diffrn_reflns_theta_max         68.50
_diffrn_reflns_theta_min         2.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  0.8544
_exptl_absorpt_correction_T_min  0.5699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure   ! 
RESPONSE: During the 
refinement of the structure, electron density peaks were located 
that were believed to be highly disordered 
solvent molecules (possibly tetrahydrofuran). Attempts 
made to model the solvent molecule were not successful. 
The SQUEEZE option in PLATON (Spek, 2009) indicated there was a 
large solvent cavity 363.7 Ang^3. In the final cycles of refinement, 
this contribution (82) to the 
electron density was removed from the observed data. The 
density, the F(000) value, the molecular weight and the formula are 
given without taking into account the results obtained with the 
SQUEEZE option PLATON (Spek, 2009). Similar treatments of disordered 
solvent molecules were carried out by St\"ahler et al. (2001), 
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). 
References: 
  
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
  
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). 
Acta Cryst. E61, m2014-m2017. 
  
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. 
(2003). Acta Cryst. E59, o975-o977. 
  
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. 
(2003). Acta Cryst. C59, m84-m86. 
  
Stahler, R., Nather, C. & Bensch, W. (2001). Acta Cryst. 
C57, 26-27.
;
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0612
_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^)+(0.1299P)^2^+0.4795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.1962
_reflns_number_gt                9609
_reflns_number_total             11410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00390_si_002.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085950--4085951.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085951