Zirconium-Catalyzed Amine Borane Dehydrocoupling and Transfer Hydrogenation
Erickson, Karla A.; Stelmach, John P. W.; Mucha, Neil T.; Waterman, Rory; Organometallics 34 (2015) 4693–; doi:10.1021/acs.organomet.5b00415

data_4086182
_publ_section_title
;
 Zirconium-Catalyzed Amine Borane Dehydrocoupling and Transfer
 Hydrogenation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4693
_journal_paper_doi               10.1021/acs.organomet.5b00415
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C17 H48 B N5 Si3 Zr'
_chemical_formula_sum            'C17 H48 B N5 Si3 Zr'
_chemical_formula_weight         508.90
_chemical_name_common            '[Zr]NMe2BH3'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 132.7510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.936(3)
_cell_length_b                   17.7815(18)
_cell_length_c                   17.424(3)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    125.(2)
_cell_measurement_theta_max      29.0466
_cell_measurement_theta_min      2.7364
_cell_volume                     5673.1(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2012.6.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0138
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29842
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light colourless-yellow'
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+6.5407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                5215
_reflns_number_total             5600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00415_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 4086182.cif.'
_cod_database_code               4086182
_shelx_res_checksum              36648
_shelx_hkl_checksum              1237