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_4084273
_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         'C33 H33 Al N2'
_chemical_formula_sum            'C33 H33 Al N2'
_chemical_formula_weight         484.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.05560(10)
_cell_length_b                   17.8662(4)
_cell_length_c                   14.0256(2)
_cell_measurement_reflns_used    6307
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      54.5
_cell_measurement_theta_min      4
_cell_volume                     2770.36(8)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.628
_diffrn_measured_fraction_theta_max 0.702
_diffrn_measurement_device_type  'Duo with Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.628
_diffrn_reflns_Laue_measured_fraction_max 0.702
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15130
_diffrn_reflns_point_group_measured_fraction_full 0.624
_diffrn_reflns_point_group_measured_fraction_max 0.699
_diffrn_reflns_theta_full        58.000
_diffrn_reflns_theta_max         54.781
_diffrn_reflns_theta_min         4.007
_diffrn_source                   'ImuS microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       'cut piece of larger parallelepiped'
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.133
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 1106 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.7237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.620
_reflns_Friedel_fraction_max     0.695
_reflns_number_gt                2371
_reflns_number_total             2409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500730g_si_002.cif
_cod_data_source_block           6
_cod_database_code               4084273
_shelxl_version_number           2014-3
_shelx_res_checksum              89307
_shelx_hkl_checksum              48407