Synthesis and Structural Characteristics of Discrete Organoboron and Organoaluminum Hydrides Incorporating Bulky Eind Groups
Murosaki, Takahiro; Kaneda, Shohei; Maruhashi, Ryota; Sadamori, Kazuya; Shoji, Yoshiaki; Tamao, Kohei; Hashizume, Daisuke; Hayakawa, Naoki; Matsuo, Tsukasa; Organometallics 35 (2016) 3397–; doi:10.1021/acs.organomet.6b00633

data_4089017
_publ_section_title
;
 Synthesis and Structural Characteristics of Discrete Organoboron and
 Organoaluminum Hydrides Incorporating Bulky Eind Groups
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3397
_journal_paper_doi               10.1021/acs.organomet.6b00633
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C64 H116 Al2 Li2 O2'
_chemical_formula_sum            'C64 H116 Al2 Li2 O2'
_chemical_formula_weight         985.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.0125(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   20.016(2)
_cell_length_b                   16.3120(17)
_cell_length_c                   20.747(2)
_cell_measurement_reflns_used    17202
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.01
_cell_measurement_theta_min      2.50
_cell_volume                     6542.7(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            105209
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.161
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192.00
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     675
_refine_ls_number_reflns         14873
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0534P)^2^+3.1080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13637
_reflns_number_total             14873
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00633_si_002.cif
_cod_data_source_block           5_LiEindAlH3
_cod_original_cell_volume        6542.9(12)
_cod_database_code               4089017
_shelxl_version_number           2013-4
_shelx_res_checksum              22162
_shelx_hkl_checksum              23320