Mono- and Bimetallic Aluminum Alkyl, Aryl, and Hydride Complexes of a Bulky Dipyrromethene Ligand
Gianopoulos, Christopher G.; Kirschbaum, Kristin; Mason, Mark R.; Organometallics 33 (2014) 4503–; doi:10.1021/om500730g

data_4084274
_publ_section_title
;
 Mono- and Bimetallic Aluminum Alkyl, Aryl, and Hydride Complexes of a
 Bulky Dipyrromethene Ligand
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4503
_journal_paper_doi               10.1021/om500730g
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C66 H64 Al2 N4 O , C7 H8 , 0.5 C7 H8'
_chemical_formula_sum            'C76.5 H76 Al2 N4 O'
_chemical_formula_weight         1121.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                95.103(1)
_cell_angle_beta                 96.525(1)
_cell_angle_gamma                96.276(1)
_cell_formula_units_Z            2
_cell_length_a                   11.4137(2)
_cell_length_b                   13.7788(2)
_cell_length_c                   20.9666(3)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      69.314
_cell_measurement_theta_min      3.244
_cell_volume                     3239.16(9)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker Duo with Apex II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50495
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         69.597
_diffrn_reflns_theta_min         2.132
_diffrn_source                   'ImuS microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.7017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         11559
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+1.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9482
_reflns_number_total             11559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500730g_si_002.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C76.50 H76 Al2 N4 O'
_cod_database_code               4084274
_shelxl_version_number           2014-3
_shelx_res_checksum              72732
_shelx_hkl_checksum              60414