Aluminum complexes with Schiff base bridged bis(indolyl) ligands: synthesis, structure, and catalytic activity for polymerization of rac-lactide.
Wei, Yun; Song, Lulu; Jiang, Ling; Huang, Zeming; Wang, Shaowu; Yuan, Qingbing; Mu, Xiaolong; Zhu, Xiancui; Zhou, Shuangliu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15290–15299; doi:10.1039/c9dt02724f

data_7701244
_publ_section_title
;
 Aluminum complexes with Schiff base bridged bis(indolyl) ligands:
 synthesis, structure, and catalytic activity for polymerization of
 rac-lactide.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15290
_journal_page_last               15299
_journal_paper_doi               10.1039/c9dt02724f
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ramd
_chemical_formula_moiety         'C32 H37 Al N4 O5'
_chemical_formula_sum            'C32 H37 Al N4 O5'
_chemical_formula_weight         584.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-18 deposited with the CCDC.    2019-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.716(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8797(12)
_cell_length_b                   17.8443(17)
_cell_length_c                   15.4734(15)
_cell_measurement_reflns_used    6827
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      2.93
_cell_volume                     3439.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1400
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49516
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.934
_exptl_absorpt_coefficient_mu    0.100
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1908 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         11718
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1159P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.2255
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                5574
_reflns_number_total             11718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02724f2.cif
_cod_data_source_block           20190814b_sq
_cod_depositor_comments
'Adding full bibliography for 7701238--7701244.cif.'
_cod_database_code               7701244
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O10-C70 = O10A-C70A
 1.46 with sigma of 0.01
 C70-C69 = C70A-C69A = C71A-C70A = C71-C70
 1.54 with sigma of 0.01
 O10A-C70A \\sim O10-C70
 with sigma of 0.02
 C68-O10 \\sim C68-O10A
 with sigma of 0.02
 O9A-O10A \\sim O9-O10
 with sigma of 0.02
 O10-C69 \\sim O10-C71
 with sigma of 0.02
 O10A-C69A \\sim O10A-C71A
 with sigma of 0.02
 C69A-C71A \\sim C71-C69
 with sigma of 0.02
 C68-C69 \\sim C68-C71
 with sigma of 0.02
 C68-C69A \\sim C68-C71A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4A \\sim O5A \\sim C73A \\sim C72A \\sim C74A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O4 \\sim O5 \\sim C73 \\sim C72 \\sim C74: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O9A \\sim O10A \\sim C70A \\sim C71A \\sim C69A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C69A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) = Uanis(O4A)
Uanis(O9) = Uanis(O9A)
Uanis(O10A) = Uanis(O10)
4. Rigid body (RIGU) restrains
 O4, C62, O5, C73, C72, C74
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O4A, C62, O5A, C73A, C74A, C72A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O9, C68, O10, C70, C71, C69
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C68, O9A, O10A, C70A, C71A, C69A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O4A)=Sof(O5A)=Sof(C73A)=Sof(H73A)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=
 Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(1)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74A)=
 Sof(H74B)=Sof(H74C)=Sof(O4)=Sof(O5)=FVAR(1)
 Sof(O9A)=Sof(O10A)=Sof(C70A)=Sof(H70A)=Sof(C71A)=Sof(H71D)=Sof(H71E)=
 Sof(H71F)=Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=1-FVAR(2)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(H71C)=Sof(O9)=Sof(O10)=FVAR(2)
6.a Riding coordinates:
 C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C71A(H71D,H71E,H71F), C69A(H69D,
 H69E,H69F)
6.b Ternary CH refined with riding coordinates:
 C58(H58), C61(H61), C64(H64), C67(H67), C70(H70), C73(H73), C73A(H73A),
 C70A(H70A)
6.c Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C52(H52A,H52B), C54(H54A,H54B)
6.d Aromatic/amide H refined with riding coordinates:
 C47(H47), C48(H48), C49(H49), C50(H50), C35(H35), C36(H36), C37(H37),
 C38(H38), C24(H24), C25(H25), C26(H26), C27(H27), C12(H12), C13(H13), C14(H14),
  C15(H15), C17(H17), C19(H19), C20(H20), C22(H22), C40(H40), C42(H42),
 C43(H43), C45(H45)
6.e Fitted hexagon refined as free rotating group:
 C46(C47,C48,C49,C50,C51)
6.f Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C66(H66A,
 H66B,H66C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C72A(H72D,H72E,H72F),
 C74A(H74D,H74E,H74F)
;
_shelx_res_checksum              71845
_shelx_fab_checksum              41323
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'