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_4519105
_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            'C11 H30 Ca Cl2 N2 O8'
_chemical_formula_weight         429.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.779(2)
_cell_length_b                   8.8435(10)
_cell_length_c                   13.4059(17)
_cell_measurement_reflns_used    2722
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5420
_cell_measurement_theta_min      3.8110
_cell_volume                     1870.7(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.965
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6684
_diffrn_reflns_point_group_measured_fraction_full 0.812
_diffrn_reflns_point_group_measured_fraction_max 0.765
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95277
_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    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
; 
 Flack x determined using 605 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_coef       0.022(4)
_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   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3288
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+1.4194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.518
_reflns_Friedel_fraction_full    0.608
_reflns_Friedel_fraction_max     0.546
_reflns_number_gt                2299
_reflns_number_total             3288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c04086_si_002.cif
_cod_data_source_block           ic20143
_cod_database_code               4519105
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              16611
_shelx_hkl_checksum              31890