Triazenide Complexes of the Heavier Alkaline Earths: Synthesis, Characterization, And Suitability for Hydroamination Catalysis
Anthony G. M. Barrett; Mark R. Crimmin; Michael S. Hill; Peter B. Hitchcock; Gabriele Kociok-Köhn; Panayiotis A. Procopiou; Inorganic Chemistry 47 (2008) 7366–7376; doi:10.1021/ic800789x

data_4305863
_publ_contact_author_address
;
Department of Chemistry
University of Bath
Bath, BA2 7AY
United Kingdom
;
_publ_contact_author_email       m.s.hill@bath.ac.uk
_publ_contact_author_fax         '44 1225 82 6231'
_publ_contact_author_name        'Michael S. Hill'
_publ_contact_author_phone       '44 1225 38 3394'
_publ_section_title
;
Triazenide Complexes of the Heavier Alkaline Earths: Synthesis,
Characterization, And Suitability for Hydroamination Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7366
_journal_page_last               7376
_journal_paper_doi               10.1021/ic800789x
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C52 H99 Ba K N5 O4 Si4'
_chemical_formula_sum            'C52 H99 Ba K N5 O4 Si4'
_chemical_formula_weight         1147.16
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.9340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7430(5)
_cell_length_b                   16.5050(5)
_cell_length_c                   21.2450(8)
_cell_measurement_reflns_used    48107
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     6586.5(4)
_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., Instit\"ut 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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '202 1.3 degree images with \f and\w 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  0.1594
_diffrn_reflns_av_sigmaI/netI    0.1754
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46651
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements 

 Sortav (Blessing 1995)

;
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11625
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.2108
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.2364
_reflns_number_gt                4935
_reflns_number_total             11625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800789x-file001_1.cif
_cod_data_source_block           k08msh18
_cod_database_code               4305863