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_4089012
_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         'C28 H45 B F2'
_chemical_formula_sum            'C28 H45 B F2'
_chemical_formula_weight         430.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 111.566(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   20.1669(6)
_cell_length_b                   8.6860(2)
_cell_length_c                   15.4565(5)
_cell_measurement_reflns_used    13177
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.80
_cell_measurement_theta_min      2.73
_cell_volume                     2517.97(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_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    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25806
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.584
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.3b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            nONE
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nONE
_exptl_crystal_F_000             944.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2892
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0823P)^2^+2.5359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2586
_reflns_number_total             2892
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00633_si_002.cif
_cod_data_source_block           1_EindBF2
_cod_database_code               4089012
_shelxl_version_number           2013-4
_shelx_res_checksum              27685
_shelx_hkl_checksum              32344