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_7707700
_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_absolute_configuration syn
_chemical_formula_moiety         'C36 H50 Al Cl N2 O2, C6 H6'
_chemical_formula_sum            'C42 H56 Al Cl N2 O2'
_chemical_formula_weight         683.31
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-13
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9908(6)
_cell_length_b                   12.7225(7)
_cell_length_c                   29.7257(18)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.59
_cell_volume                     3778.4(4)
_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    'XT (Sheldrick, 2015)'
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            133165
_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         30.564
_diffrn_reflns_theta_min         2.456
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.9405. 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    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method
'slow evaporation using benzene as solvent'
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 4716 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         11587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.7180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10998
_reflns_number_total             11587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01903a2.cif
_cod_data_source_block           p212121
_cod_depositor_comments
'Adding full bibliography for 7707698--7707700.cif.'
_cod_database_code               7707700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.962
_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.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C23(H23A,H23B), C22(H22A,H22B), C21(H21A,H21B),
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C27(H27), C39(H39), C40(H40), C41(H41), C42(H42), C37(H37), C38(H38)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C18(H18A,H18B,
 H18C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C35(H35A,
 H35B,H35C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C12(H12A,H12B,H12C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              29310
_shelx_hkl_checksum              70603
_olex2_submission_special_instructions 'No special instructions were received'