Dearomatized BIAN Alkaline-Earth Alkyl Catalysts for the Intramolecular Hydroamination of Hindered Aminoalkenes
Arrowsmith, Merle; Hill, Michael S.; Kociok-Köhn, Gabriele; Organometallics 33 (2014) 206–; doi:10.1021/om400955v

data_4082615
_publ_section_title
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 Dearomatized BIAN Alkaline-Earth Alkyl Catalysts for the Intramolecular
 Hydroamination of Hindered Aminoalkenes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              206
_journal_paper_doi               10.1021/om400955v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C48 H60 N3 Si-, K+'
_chemical_formula_sum            'C48 H60 K N3 Si'
_chemical_formula_weight         746.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           206
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            48
_cell_length_a                   39.6750(7)
_cell_length_b                   39.6750(7)
_cell_length_c                   39.6750(7)
_cell_measurement_reflns_used    61220
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     62452.6(19)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). 
 Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, 
 Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '143 0.9 degree images with \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1026
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            55758
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'blue green'
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             19296
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.55
_platon_squeeze_details
;
the asymmetric unit contains one disordered toluene solvent molecule 
with 50% occupation factor which is disordered over a two fold axis.
Another toluene molecule is disordered about a three fold axis with 
occupation factor 33%. A trace of a further solvent molecule found 
to be located over a three fold axis but could not properly be solved.
;
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.1001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+65.3209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2848
_reflns_number_gt                4891
_reflns_number_total             9182
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C288 H360 K6 N18 Si6'
_cod_original_formula_weight         4477.08
_cod_original_formula_moiety         'C288 H360 K6 N18 Si6'
_cod_original_formula_units_Z            8
_cod_data_source_file            om400955v_si_002.cif
_cod_data_source_block           2
_cod_database_code               4082615