Mechanistic insights into dehydrocoupling of amine boranes using dinuclear zirconocene complexes
Lindenau, Kevin; Jannsen, Nora; Rippke, Mirko; Al Hamwi, Hanan; Selle, Carmen; Drexler, Hans-Joachim; Spannenberg, Anke; Sawall, Mathias; Neymeyr, Klaus; Heller, Detlef; Reiß, Fabian; Beweries, Torsten; Catalysis Science & Technology 11 (2021) 4034–4050; doi:10.1039/D1CY00531F

data_1562551
_publ_section_title
;
 Mechanistic insights into dehydrocoupling of amine boranes using
 dinuclear zirconocene complexes
;
_journal_issue                   12
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4034
_journal_page_last               4050
_journal_paper_doi               10.1039/D1CY00531F
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety
'0.89 (C30 H41 Cl1 Si2 Zr2), 0.11 (C31 H44 Si2 Zr2)'
_chemical_formula_sum            'C30.11 H41.33 Cl0.89 Si2 Zr2'
_chemical_formula_weight         673.45
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-11-24 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                73.455(3)
_cell_angle_beta                 74.142(3)
_cell_angle_gamma                82.668(3)
_cell_formula_units_Z            4
_cell_length_a                   12.9147(8)
_cell_length_b                   16.0454(11)
_cell_length_c                   16.0971(10)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.59
_cell_volume                     3071.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            159799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.363
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       'Part of plate'
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.218
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         14071
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+4.0696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12879
_reflns_number_total             14071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00531f3.cif
_cod_data_source_block           AX1945abs
_cod_depositor_comments
'Adding full bibliography for 1562548--1562551.cif.'
_cod_database_code               1562551
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.698
_shelx_estimated_absorpt_t_max   0.836
_shelx_res_checksum              93172