Heavier Alkaline Earth Metal Borohydride Complexes Stabilized by β-Diketiminate Ligand
Sankaranarayana Pillai Sarish; Anukul Jana; Herbert W. Roesky; Thomas Schulz; Michael John; Dietmar Stalke; Inorganic Chemistry 49 (2010) 3816–3820; doi:10.1021/ic902338r

data_4315373
_publ_contact_author             'Prof. Dr. Dietmar Stalke'
_publ_contact_author_email       dstalke@chemie.uni-goettingen.de
_publ_section_title
;
 Heavier Alkaline Earth Metal Borohydride Complexes Stabilized by
 \b-Diketiminate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3816
_journal_page_last               3820
_journal_paper_doi               10.1021/ic902338r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C45 H77 B Ca N2 O'
_chemical_formula_weight         712.98
_chemical_name_systematic
; 
 ? 
;
_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                 99.155(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.749(5)
_cell_length_b                   13.176(3)
_cell_length_c                   16.106(4)
_cell_measurement_reflns_used    8233
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.33
_cell_volume                     4347.1(18)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.10'
_computing_publication_material  'XP in SHELXTL ver. 6.10'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.10'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.10'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'INCOATEC Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31406
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4503
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.8065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                4447
_reflns_number_total             7992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902338r_si_002.cif
_cod_data_source_block           CaH
_cod_database_code               4315373