B(C6F5)3-catalysed cyclic carbonate editing
He, Yicheng; Unnikrishnan, Krishnapriya Anattil; Yin, Wenhao; Kuniyil, Rositha; Du, Haifeng; Guo, Wusheng; Green Chemistry 27 (2025) 6741–6746; doi:10.1039/D5GC01888A

data_7250441
_publ_section_title
;
 B(C6F5)3-catalysed cyclic carbonate editing
;
_journal_issue                   23
_journal_name_full               'Green Chemistry'
_journal_page_first              6741
_journal_page_last               6746
_journal_paper_doi               10.1039/D5GC01888A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C18 H16 O3'
_chemical_formula_sum            'C18 H16 O3'
_chemical_formula_weight         280.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-08
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2025-01-25 deposited with the CCDC.	2025-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                70.545(2)
_cell_angle_beta                 74.245(2)
_cell_angle_gamma                74.481(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9241(2)
_cell_length_b                   9.1060(2)
_cell_length_c                   10.2978(2)
_cell_measurement_reflns_used    5875
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.3170
_cell_measurement_theta_min      4.6430
_cell_volume                     744.80(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     51.00  86.00   0.50    0.50    --   42.10 -82.00 120.00   70
  2  \w    103.00 130.00   0.50    0.50    --   42.10  77.00-180.00   54
  3  \w     89.00 132.00   0.50    0.50    --   42.10  77.00-150.00   86
  4  \w     86.00 128.00   0.50    0.50    --   42.10  77.00 150.00   84
  5  \w    -29.00  35.00   0.50    0.50    --   42.10 -82.00 120.00  128
  6  \w    -22.00  39.00   0.50    0.50    --   42.10 -82.00 150.00  122
  7  \w    -36.00  72.00   0.50    0.50    --   42.10 -57.00 -60.00  216
  8  \w     -2.00  59.00   0.50    0.50    --   42.10 -82.00-150.00  122
  9  \w     18.00  87.00   0.50    0.50    --  101.60 -82.00 -90.00  138
 10  \w    148.00 180.00   0.50    0.50    --  101.60 -25.00  30.00   64
 11  \w     71.00  97.00   0.50    0.50    --  101.60  25.00-180.00   52
 12  \w    147.00 191.00   0.50    0.50    --  101.60  25.00-180.00   88
 13  \w     65.00 117.00   0.50    0.50    --  101.60 -82.00 150.00  104
 14  \w     90.00 143.00   0.50    0.50    --  101.60 -82.00 -90.00  106
 15  \w     90.00 115.00   0.50    0.50    --  101.60 -77.00-180.00   50
 16  \w     12.00 139.00   0.50    0.50    --  101.60 -82.00 120.00  254
 17  \w     33.00 144.00   0.50    0.50    --  101.60 -82.00 -60.00  222
 18  \w     32.00 109.00   0.50    0.50    --  101.60 -82.00  60.00  154
 19  \w    131.00 172.00   0.50    0.50    --  101.60  77.00 -30.00   82
 20  \w     79.00 126.00   0.50    0.50    --  101.60  77.00 -30.00   94
 21  \w     19.00 159.00   0.50    0.50    --  101.60 -25.00-180.00  280
 22  \w     26.00 111.00   0.50    0.50    --  101.60 -25.00  30.00  170
 23  \w     25.00  51.00   0.50    0.50    --  101.60 -77.00   0.00   52
 24  \w     79.00 105.00   0.50    0.50    --  101.60 -82.00-150.00   52
 25  \w     81.00 106.00   0.50    0.50    --  101.60 -82.00   0.00   50
 26  \w     62.00  87.00   0.50    0.50    --  101.60 -82.00  30.00   50
 27  \w     15.00  67.00   0.50    0.50    --  101.60 -77.00-180.00  104
 28  \w     14.00 163.00   0.50    0.50    --  101.60   0.00   0.00  298
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0406885000
_diffrn_orient_matrix_UB_12      0.0935703000
_diffrn_orient_matrix_UB_13      0.1091998000
_diffrn_orient_matrix_UB_21      -0.1781893000
_diffrn_orient_matrix_UB_22      0.0097217000
_diffrn_orient_matrix_UB_23      0.0126538000
_diffrn_orient_matrix_UB_31      0.0063134000
_diffrn_orient_matrix_UB_32      -0.1569035000
_diffrn_orient_matrix_UB_33      0.1189374000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6720
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.417
_diffrn_reflns_theta_min         4.649
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.084(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0587P)^2^+0.2472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2698
_reflns_number_total             2797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc01888a2.cif
_cod_data_source_block           606-4
_cod_depositor_comments          'Adding full bibliography for 7250441.cif.'
_cod_database_code               7250441
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.899
_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 Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84493
_shelx_hkl_checksum              33186
_shelx_fab_checksum              28443
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.468
_oxdiff_exptl_absorpt_empirical_full_min 0.525