Macrocyclic Binucleating β-Diketiminate Ligands and their Lithium, Aluminum, and Zinc Complexes.
Vela, Javier; Zhu, Liwei; Flaschenriem, Christine J.; Brennessel, William W.; Lachicotte, Rene J.; Holland, Patrick L.; Organometallics 26 (2007) 3416–3423; doi:10.1021/om0700258

data_4089350
_publ_section_title
;
 Macrocyclic Binucleating \b-Diketiminate Ligands and their Lithium,
 Aluminum, and Zinc Complexes.
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3416
_journal_page_last               3423
_journal_paper_doi               10.1021/om0700258
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C42 H62 Li2 N4 O4'
_chemical_formula_sum            'C42 H62 Li2 N4 O4'
_chemical_formula_weight         700.84
_chemical_name_common            holjv64
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.9985(16)
_cell_length_b                   20.5761(18)
_cell_length_c                   22.744(2)
_cell_measurement_reflns_used    3985
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.34
_cell_volume                     8423.0(13)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            112657
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_correction_T_min  0.9760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10442
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.810
_refine_ls_R_factor_all          0.1971
_refine_ls_R_factor_gt           0.1459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4443
_refine_ls_wR_factor_ref         0.4922
_reflns_number_gt                5822
_reflns_number_total             10442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0700258-file003.cif
_cod_data_source_block           mBinLi2THF4
_cod_original_cell_volume        8422.8(13)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4089350