Cycloaddition of carbon dioxide to epoxides by highly active constrained aluminum chloride complexes.
Laiwattanapaisarn, Nattiya; Virachotikul, Arnut; Phomphrai, Khamphee; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11039–11048; doi:10.1039/d1dt01903a

data_7707698
_publ_section_title
;
 Cycloaddition of carbon dioxide to epoxides by highly active constrained
 aluminum chloride complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11039
_journal_page_last               11048
_journal_paper_doi               10.1039/d1dt01903a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '4(C24 H26 Al Cl N2 O2), 2(C H2 Cl2)'
_chemical_formula_sum            'C98 H108 Al4 Cl8 N8 O8'
_chemical_formula_weight         1917.44
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-24 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.279(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7139(13)
_cell_length_b                   10.2393(8)
_cell_length_c                   25.3441(19)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.39
_cell_volume                     4559.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      120
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            134693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.030
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1062 before and 0.0550 after correction. The Ratio of minimum to maximum transmission is 0.9349. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_recrystallization_method
'Vapor diffusion crystallization using DCM as solvent and hexane as anti-solvent'
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0414P)^2^+2.2882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8011
_reflns_number_total             8984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01903a2.cif
_cod_data_source_block           p2n_a
_cod_depositor_comments
'Adding full bibliography for 7707698--7707700.cif.'
_cod_database_code               7707698
_shelx_shelxl_version_number     2018/3
_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. Others
 Fixed Sof: Cl05(0.5) Cl06(0.5) Cl1A(0.5) Cl0A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C12(H12A,H12B), C45(H45A,H45B), C13(H13A,H13B), C30(H30A,
 H30B), C4(H4A,H4B), C33(H33A,H33B), C32(H32A,H32B), C21(H21A,H21B), C22(H22A,
 H22B), C5(H5A,H5B), C44(H44A,H44B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C18(H18), C37(H37), C27(H27)
3.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C48(H48A,H48B,
 H48C), C11(H11A,H11B,H11C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
_shelx_res_checksum              42038
_shelx_hkl_checksum              84824
_olex2_submission_special_instructions 'No special instructions were received'