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_4081347
_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            'C56 H82 Ba N4 O2'
_chemical_formula_weight         980.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.306(5)
_cell_length_b                   13.282(3)
_cell_length_c                   20.093(4)
_cell_measurement_reflns_used    95141
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      1.92
_cell_volume                     5476(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58318
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.530
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         13579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+4.3646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                11851
_reflns_number_total             13579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400622d_si_002.cif
_cod_data_source_block           ip128
_cod_original_cell_volume        5475.3(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4081347