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_7053455
_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         'C43 H76 Al2 Ca N2'
_chemical_formula_sum            'C43 H76 Al2 Ca N2'
_chemical_formula_weight         715.1
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_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             2007-04-18T15:29:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.304(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1238(2)
_cell_length_b                   20.7676(4)
_cell_length_c                   19.6414(3)
_cell_measurement_reflns_used    30011
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     4489.88(14)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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      -0.66057E-2
_diffrn_orient_matrix_UB_12      -0.334156E-1
_diffrn_orient_matrix_UB_13      0.359302E-1
_diffrn_orient_matrix_UB_21      -0.35229E-1
_diffrn_orient_matrix_UB_22      0.328104E-1
_diffrn_orient_matrix_UB_23      0.287228E-1
_diffrn_orient_matrix_UB_31      -0.834804E-1
_diffrn_orient_matrix_UB_32      -0.11202E-1
_diffrn_orient_matrix_UB_33      -0.230513E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40326
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_correction_T_min  0.892
_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    1.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8781
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.1004
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+9.8219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2539
_refine_ls_wR_factor_ref         0.2742
_reflns_number_gt                6713
_reflns_number_total             8781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00042f.txt
_cod_data_source_block           apr507
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7053455