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_7717427
_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         'C32 H48 Al N O5, 0.5(O H2)'
_chemical_formula_sum            'C32 H49 Al N O5.5'
_chemical_formula_weight         562.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           32
_space_group_name_Hall           'P 2 -2ab'
_space_group_name_H-M_alt        'P b a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-24
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5149(4)
_cell_length_b                   34.1550(5)
_cell_length_c                   8.83250(10)
_cell_measurement_reflns_used    9258
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      3.93
_cell_volume                     6792.16(17)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            60639
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.187
_diffrn_reflns_theta_min         2.350
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1394 before and 0.0748 after correction.
The Ratio of minimum to maximum transmission is 0.6622.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 4020 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13113
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.1009
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2738
_refine_ls_wR_factor_ref         0.2961
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                10698
_reflns_number_total             13113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02831g2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7717427--7717429.cif.'
_cod_original_formula_sum        'C32 H49 Al N O5.50'
_cod_database_code               7717427
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.724
_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, All O(H,H) groups
2. Restrained distances
 C15-C16 \\sim C15-C17 \\sim C16-C17 \\sim C16A-C17A \\sim C16A-C15A \\sim
C17A-C15A
 with sigma of 0.04
 C14-C15 \\sim C14-C16 \\sim C14-C17 \\sim C14-C16A \\sim C14-C17A \\sim
C14-C15A \\sim C14-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C16)
Uanis(C15A) = Uanis(C17)
Uanis(C16A) = Uanis(C8)
4. Others
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Fixed Sof: O7(0.5) O6(0.5)
5.a Rotating group:
 O4(H4A,H4B), O4'(H4'A,H4'B)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C18(H18A,H18B), C2'(H2'A,H2'B), C3'(H3'A,H3'B),
 C18'(H18C,H18D)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C22(H22), C24(H24), C7'(H7'), C9'(H9'), C22'(H22'), C24'(H24')
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F), C17A(H17D,
 H17E,H17F), C11'(H11D,H11E,H11F), C12'(H12D,H12E,H12F), C13'(H13D,H13E,H13F),
 C15'(H15G,H15H,H15I), C16'(H16G,H16H,H16I), C17'(H17G,H17H,H17I), C26'(H26D,
 H26E,H26F), C27'(H27D,H27E,H27F), C28'(H28D,H28E,H28F), C30'(H30D,H30E,H30F),
 C31'(H31D,H31E,H31F), C32'(H32D,H32E,H32F)
;
_shelx_res_checksum              24371
_shelx_hkl_checksum              53300
_olex2_submission_special_instructions 'No special instructions were received'