Synthesis of β-diketiminato calcium silylamides and their reactions with triethylaluminium
Crimmin, Mark R.; Hill, Michael S.; Hitchcock, Peter B.; Mahon, Mary F.; New Journal of Chemistry 34 (2010) 1572–; doi:10.1039/c0nj00042f

data_7053454
_publ_section_title
;
 Synthesis of \b-diketiminato calcium silylamides and their reactions with
 triethylaluminium
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1572
_journal_paper_doi               10.1039/c0nj00042f
_journal_volume                  34
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H59 Ca N3 Si2, 0.5(C5 H12)'
_chemical_formula_sum            'C37.5 H65 Ca N3 Si2'
_chemical_formula_weight         654.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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      2.3
_audit_creation_date             2006-08-24T11:21:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.9889(11)
_cell_length_b                   26.9889(11)
_cell_length_c                   11.5798(3)
_cell_measurement_reflns_used    19623
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     8434.7(5)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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      0.315383E-1
_diffrn_orient_matrix_UB_12      0.58376E-2
_diffrn_orient_matrix_UB_13      0.43236E-1
_diffrn_orient_matrix_UB_21      0.181677E-1
_diffrn_orient_matrix_UB_22      0.37659E-2
_diffrn_orient_matrix_UB_23      -0.747502E-1
_diffrn_orient_matrix_UB_31      -0.69385E-2
_diffrn_orient_matrix_UB_32      0.363952E-1
_diffrn_orient_matrix_UB_33      0.7997E-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  0.0931
_diffrn_reflns_av_unetI/netI     0.1244
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26227
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.8862
_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    1.03
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8203
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1658
_refine_ls_R_factor_gt           0.0807
_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^)+(0.0806P)^2^+10.1501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                4367
_reflns_number_total             8203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00042f.txt
_cod_data_source_block           aug1906
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7053454