Syntheses and Structures of Bis-Amidinate‒Alane Complexes
Bayram, Melike; Bläser, Dieter; Wölper, Christoph; Schulz, Stephan; Organometallics 33 (2014) 2080–; doi:10.1021/om5002217

data_4083021
_publ_contact_author
;
          Prof. Dr. Schulz, Stephan
          Fachbereich Chemie der
          Universit\"at Duisburg-Essen
          Campus Essen, Universit\"atsstr. 7
          D-45141 Essen, Germany
;
_publ_section_title
;
 Syntheses and Structures of Bis-Amidinate--Alane Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2080
_journal_paper_doi               10.1021/om5002217
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H42 Al2 N4'
_chemical_formula_sum            'C19 H42 Al2 N4'
_chemical_formula_weight         380.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.4840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5270(2)
_cell_length_b                   11.6905(3)
_cell_length_c                   12.2380(3)
_cell_measurement_reflns_used    20550
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.41
_cell_volume                     1206.59(5)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37756
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'sealed X-RAY tube'
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 3087 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         7325
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0504P)^2^+0.0874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                6815
_reflns_number_total             7325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5002217_si_001.cif
_cod_data_source_block           mb_062m
_cod_depositor_comments
'Adding full bibliography for 4083015--4083021.cif.'
_cod_database_code               4083021
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2013-4
_shelx_res_checksum              58374
_shelx_hkl_checksum              65510