2,5-Bis{N-(2,6-diisopropylphenyl)iminomethyl}pyrrolyl Complexes of the Heavy Alkaline Earth Metals: Synthesis, Structures, and Hydroamination Catalysis
Jenter, Jelena; Köppe, Ralf; Roesky, Peter W.; Organometallics 30 (2011) 1404–; doi:10.1021/om100937c

data_4063779
_publ_section_title
;
 2,5-Bis{N-(2,6-diisopropylphenyl)iminomethyl}pyrrolyl Complexes of the
 Heavy Alkaline Earth Metals: Synthesis, Structures, and Hydroamination
 Catalysis
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1404
_journal_paper_doi               10.1021/om100937c
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C44 H72 Ca N4 O2 Si2, C4 H8 O'
_chemical_formula_sum            'C48 H80 Ca N4 O3 Si2'
_chemical_formula_weight         857.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             09-06-30
_audit_creation_method           'STOE X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.426(3)
_cell_length_b                   10.568(2)
_cell_length_c                   29.727(6)
_cell_measurement_reflns_used    23022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      1.38
_cell_volume                     5114.1(17)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e/3'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0919
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            22279
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.9452
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         10661
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                6139
_reflns_number_total             10661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100937c_si_001.cif
_cod_data_source_block           5
_cod_original_cell_volume        5114.2(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4063779