Diazadiene Complexes of the Heavy Alkaline-Earth Metals Strontium and Barium: Structures and Reactivity
Lorenz, Volker; Hrib, Cristian G.; Grote, Dirk; Hilfert, Liane; Krasnopolski, Michael; Edelmann, Frank T.; Organometallics 32 (2013) 4636–; doi:10.1021/om400622d

data_4081345
_publ_section_title
;
 Diazadiene Complexes of the Heavy Alkaline-Earth Metals Strontium and
 Barium: Structures and Reactivity
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4636
_journal_paper_doi               10.1021/om400622d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C34 H56 N2 O4 Sr'
_chemical_formula_weight         644.43
_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                 91.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.860(2)
_cell_length_b                   17.602(4)
_cell_length_c                   20.310(4)
_cell_measurement_reflns_used    28416
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.07
_cell_volume                     3523.3(13)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22456
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  0.2956
_exptl_absorpt_correction_T_min  0.2774
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         9455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+3.1038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                7750
_reflns_number_total             9455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400622d_si_002.cif
_cod_data_source_block           ip121
_cod_original_cell_volume        3523.4(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081345