HFIP promoted carbo-lactonisation as a new route to functionalised lactones.
Aynetdinova, Daniya; Jaschinski, Megan; Jenkins, Timothy C.; Donohoe, Timothy J.; Chemical communications (Cambridge, England) 60 (2024) 9997–10000; doi:10.1039/d4cc02472a

data_7133525
_publ_section_title
;
 HFIP promoted carbo-lactonisation as a new route to functionalised
 lactones.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9997
_journal_page_last               10000
_journal_paper_doi               10.1039/d4cc02472a
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H20 O3'
_chemical_formula_sum            'C19 H20 O3'
_chemical_formula_weight         296.37
_chemical_melting_point          ?
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2024-04-11
_audit_creation_method           'CRYSTALS_ver_14_build_c42b451 '
_audit_update_record
;
2024-04-17 deposited with the CCDC.	2024-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6987(2)
_cell_length_b                   7.5431(3)
_cell_length_c                   35.7122(11)
_cell_measurement_reflns_used    4183
_cell_measurement_temperature    150
_cell_measurement_theta_max      75.94
_cell_measurement_theta_min      4.93
_cell_volume                     1535.12(9)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2021) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2021) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.049
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            7339
_diffrn_reflns_theta_full        74.555
_diffrn_reflns_theta_max         76.077
_diffrn_reflns_theta_min         4.954
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2021) 
;
_exptl_crystal_colour            'translucent pale yellow'
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.21
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 866 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.07(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0244
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.0004723
_refine_ls_shift/su_mean         0.0000299
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 1.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1151
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1151
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                2739
_reflns_number_total             2946
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.31
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_scale          8.9(3)
_oxford_structure_analysis_title 001tjd23MJ01
_cod_data_source_file            d4cc02472a2.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133525--7133530.cif.
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               7133525
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0473
_reflns_number_all               2946
_oxford_hooft_y                  0.10(17)
_oxford_bijvoet_difference       0.07(14)
_oxford_refined_flack_x          -0.0(3)