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_4305865
_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_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H68 Ca N4 O2 Si2, C7 H8'
_chemical_formula_sum            'C45 H76 Ca N4 O2 Si2'
_chemical_formula_weight         801.36
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2007-06-27T09:41:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.391(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8380(3)
_cell_length_b                   24.3827(7)
_cell_length_c                   18.8459(5)
_cell_measurement_reflns_used    15106
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     4913.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.43911E-1
_diffrn_orient_matrix_UB_12      0.5913E-3
_diffrn_orient_matrix_UB_13      0.427224E-1
_diffrn_orient_matrix_UB_21      -0.825648E-1
_diffrn_orient_matrix_UB_22      0.213E-3
_diffrn_orient_matrix_UB_23      -0.326678E-1
_diffrn_orient_matrix_UB_31      -0.10621E-2
_diffrn_orient_matrix_UB_32      -0.410079E-1
_diffrn_orient_matrix_UB_33      0.4464E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19331
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.8319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.25(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7833
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+4.2762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                6737
_reflns_number_total             7833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800789x-file001_3.cif
_cod_data_source_block           jun2307
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4305865