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_7133528
_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         'C25 H21 F3 O2'
_chemical_formula_sum            'C25 H21 F3 O2'
_chemical_formula_weight         410.43
_chemical_melting_point          ?
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2023-06-12
_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                 92.8739(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0864(2)
_cell_length_b                   6.0321(1)
_cell_length_c                   13.7269(2)
_cell_measurement_reflns_used    7525
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.37
_cell_measurement_theta_min      4.72
_cell_volume                     999.52(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.017
_diffrn_reflns_av_unetI/netI     0.023
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8958
_diffrn_reflns_theta_full        74.680
_diffrn_reflns_theta_max         76.204
_diffrn_reflns_theta_min         3.662
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2021) 
;
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             427.998
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 777 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9745
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3178
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.0005290
_refine_ls_shift/su_mean         0.0000377
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.31P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0944
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              4
_reflns_limit_k_min              -7
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3116
_reflns_number_total             3178
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_scale          9.8(4)
_oxford_structure_analysis_title 027tjd23MJ04
_cod_data_source_file            d4cc02472a2.cif
_cod_data_source_block           2t
_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 '
_cod_database_code               7133528
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0361
_reflns_number_all               3178
_oxford_hooft_y                  0.04(5)
_oxford_bijvoet_difference       0.05(5)
_oxford_refined_flack_x          0.21(16)