Synthesis and Characterization of Binucleating Bis(amidinate) Ligands and Their Dialuminum Complexes
Bronya Clare; Niladri Sarker; Richard Shoemaker; John R. Hagadorn; Inorganic Chemistry 43 (2004) 1159–1166; doi:10.1021/ic035035p

data_4310554
_publ_contact_author_address     '215 UCB, Boulder, CO, 80309-0215, USA'
_publ_contact_author_name        'John R. Hagadorn'
_publ_section_title
;
 Synthesis and Characterization of Binucleating Bis(amidinate) Ligands and
 Their Dialuminum Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1159
_journal_page_last               1166
_journal_paper_doi               10.1021/ic035035p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C47 H46 N4 O2'
_chemical_formula_weight         698.88
_chemical_name_common            Ph,Mes-L-DBF-H2acetone
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.247(2)
_cell_angle_beta                 92.611(3)
_cell_angle_gamma                111.536(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8708(10)
_cell_length_b                   14.0678(14)
_cell_length_c                   14.1881(13)
_cell_measurement_reflns_used    795
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      22.339
_cell_measurement_theta_min      2.739
_cell_volume                     1910.8(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\w 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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10965
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption correction applied using SADABS 
(Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1719
_reflns_number_gt                2998
_reflns_number_total             5478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035035psi20031120_045438_3.cif
_cod_data_source_block           jrh026
_cod_database_code               4310554