Switchable, chiral aluminium catalysts for ring opening polymerisations.
Jenkins, David T.; Trodden, Elizabeth C.; Andresen, John M.; Mansell, Stephen M.; McIntosh, Ruaraidh D.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18089–18093; doi:10.1039/d4dt02831g

data_7717428
_publ_section_title
;
 Switchable, chiral aluminium catalysts for ring opening polymerisations.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18089
_journal_page_last               18093
_journal_paper_doi               10.1039/d4dt02831g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C68 H104 Al2 N2 O10, 2(C7 H8), 2(C2 H3 N)'
_chemical_formula_sum            'C86 H126 Al2 N4 O10'
_chemical_formula_weight         1429.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-24 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.155(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.866(5)
_cell_length_b                   31.717(15)
_cell_length_c                   13.243(6)
_cell_measurement_reflns_used    9255
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.11
_cell_measurement_theta_min      4.52
_cell_volume                     4285(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65171
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.587
_diffrn_reflns_theta_min         4.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1382 before and 0.0923 after correction. The Ratio of minimum to maximum transmission is 0.7120. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0055(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         8384
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1264P)^2^+3.6384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7292
_reflns_number_total             8384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02831g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7717427--7717429.cif.'
_cod_original_cell_volume        4284(3)
_cod_database_code               7717428
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.755
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 C33A-C34A
 1.5 with sigma of 0.01
 Al1-H5
 2.241886 with sigma of 0.02
 C31-C32A \\sim C31-C32B
 with sigma of 0.02
 C32A-O3A \\sim C32B-O3B
 with sigma of 0.02
 C32A-O4A \\sim C32B-O4B
 with sigma of 0.02
 C33A-C34A \\sim C33B-C34B
 with sigma of 0.02
3. Rigid bond restraints
 O3A, O4A, C31, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3B, O4B, C31, C32B, C33B, C34B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3A \\sim O4A \\sim C31 \\sim C32A \\sim C33A \\sim C34A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
O3B \\sim O4B \\sim C31 \\sim C32B \\sim C33B \\sim C34B: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(O3B)=Sof(O4B)=Sof(H31A)=Sof(H31B)=Sof(C32B)=Sof(C33B)=Sof(H33C)=Sof(H33D)=
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(O3A)=Sof(O4A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=
 Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B), C31(H31C,H31D), C31(H31A,H31B), C33A(H33A,H33B),
 C33B(H33C,H33D)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C7(H7), C20(H20), C22(H22), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C34A(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C43(H43A,H43B,
 H43C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              81481
_shelx_hkl_checksum              71190
_olex2_submission_special_instructions 'No special instructions were received'