Structural studies of Schiff-base [2 + 2] macrocycles derived from 2,2'-oxydianiline and the ROP capability of their organoaluminium complexes.
Yang, Wenxue; Zhao, Ke-Qing; Prior, Timothy J.; Hughes, David L.; Arbaoui, Abdessamad; Elsegood, Mark R. J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11990–12005; doi:10.1039/c6dt01997h

data_7039841
_publ_section_title
;
 Structural studies of Schiff-base [2 + 2] macrocycles derived from
 2,2'-oxydianiline and the ROP capability of their organoaluminium
 complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11990
_journal_page_last               12005
_journal_paper_doi               10.1039/c6dt01997h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C55 H60 Al2 N4 O2, 2.25(C2 H3 N)'
_chemical_formula_sum            'C59.5 H66.75 Al2 N6.25 O2'
_chemical_formula_weight         955.40
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.9493(17)
_cell_angle_beta                 97.1008(16)
_cell_angle_gamma                112.5747(16)
_cell_formula_units_Z            4
_cell_length_a                   15.2938(19)
_cell_length_b                   15.671(2)
_cell_length_c                   25.086(3)
_cell_measurement_reflns_used    6207
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.56
_cell_measurement_theta_min      2.18
_cell_volume                     5464.5(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6884
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36298
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        22.554
_diffrn_reflns_theta_max         22.554
_diffrn_reflns_theta_min         1.374
_diffrn_source                   'Daresbury SRS station 9.8'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2038
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0088(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1319
_refine_ls_number_reflns         15657
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1524P)^2^+1.3373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9183
_reflns_number_total             15657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01997h2.cif
_cod_data_source_block           cr301
_cod_depositor_comments
'Adding full bibliography for 7039831--7039842.cif.'
_cod_original_formula_sum        'C59.50 H66.75 Al2 N6.25 O2'
_cod_database_code               7039841
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              55816