Aluminum methyl, alkoxide and α-alkoxy ester complexes supported by 6,6'-dimethylbiphenyl-bridged salen ligands: synthesis, characterization and catalysis for rac-lactide polymerization.
Kan, Chao; Ge, Jilei; Ma, Haiyan; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6682–6695; doi:10.1039/c5dt04633e

data_7702049
_publ_section_title
;
 Aluminum methyl, alkoxide and \a-alkoxy ester complexes supported by
 6,6'-dimethylbiphenyl-bridged salen ligands: synthesis, characterization
 and catalysis for rac-lactide polymerization.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6682
_journal_page_last               6695
_journal_paper_doi               10.1039/c5dt04633e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C42 H48 Al N2 O5'
_chemical_formula_sum            'C42 H48 Al N2 O5'
_chemical_formula_weight         687.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-05-05 deposited with the CCDC.
2016-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                91.070(3)
_cell_angle_beta                 95.849(3)
_cell_angle_gamma                114.041(3)
_cell_formula_units_Z            4
_cell_length_a                   13.950(3)
_cell_length_b                   16.296(3)
_cell_length_c                   21.630(4)
_cell_measurement_reflns_used    6368
_cell_measurement_temperature    130
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.34
_cell_volume                     4457.4(15)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.1319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         0.948
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.7709.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         17512
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+2.0144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11125
_reflns_number_total             17512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04633e2.cif
_cod_data_source_block           mo_dm14606_0m
_cod_original_cell_volume        4457.2(14)
_cod_database_code               7702049
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C40 = C39'-C40 = C81-C82 = C81'-C82
 1.5 with sigma of 0.01
 H39C-H49C
 2.05 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C39 \\sim C39' \\sim C40 \\sim C41: within 1.7A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C81 \\sim C81' \\sim C82 \\sim C83: within 1.7A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Fixed Sof: C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C81'(0.5) H81D(0.5)
 H81E(0.5) H81F(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C39'(0.5) H39D(0.5)
 H39E(0.5) H39F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C57(H57),
 C59(H59), C61(H61), C69(H69), C71(H71), C73(H73), C2(H2), C3(H3), C4(H4),
 C10(H10), C11(H11), C12(H12), C15(H15), C17(H17), C19(H19), C27(H27), C29(H29),
  C31(H31)
5.b Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C81'(H81D,H81E,H81F), C84(H84A,H84B,H84C), C7(H7A,H7B,H7C), C14(H14A,H14B,
 H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C39'(H39D,H39E,H39F), C42(H42A,H42B,
 H42C)
;
_shelx_res_checksum              65411
_olex2_submission_special_instructions 'No special instructions were received'