Sustainable Synthesis of Cyclic Carbonates from Terminal Epoxides by a Highly Efficient CaI<sub>2</sub>/1,3-Bis[tris(hydroxymethyl)-methylamino]-propane Catalyst.
Liu, Kuan-Ting; Chuang, Jia-Yu; Jeng, Ru-Jong; Leung, Man-Kit; ACS omega 6 (2021) 27279–27287; doi:10.1021/acsomega.1c04086

data_4519106
_publ_section_title
;
 Sustainable Synthesis of Cyclic Carbonates from Terminal Epoxides by a
 Highly Efficient
 CaI<sub>2</sub>/1,3-Bis[tris(hydroxymethyl)-methylamino]-propane
 Catalyst.
;
_journal_issue                   41
_journal_name_full               'ACS omega'
_journal_page_first              27279
_journal_page_last               27287
_journal_paper_doi               10.1021/acsomega.1c04086
_journal_volume                  6
_journal_year                    2021
_chemical_formula_sum            'C23 H24 O8'
_chemical_formula_weight         428.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
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_cell_angle_beta                 108.828(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.327(6)
_cell_length_b                   5.8690(9)
_cell_length_c                   12.6542(17)
_cell_measurement_reflns_used    2048
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      4.4530
_cell_volume                     2061.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.2496
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.879
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1061P)^2^+2.1205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1809
_reflns_number_total             2300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c04086_si_004.cif
_cod_data_source_block           ic20187
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4519106
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              96629
_shelx_hkl_checksum              92233