Diverse saturated heterocycles from a hydroacylation/conjugate addition cascade
Iwumene, Ndidi U. N.; Moseley, Daniel. F.; Pullin, Robert D. C.; Willis, Michael C.; Chemical Science 13 (2022) 1504–1511; doi:10.1039/D1SC06900D

data_1566049
_publ_section_title
;
 Diverse saturated heterocycles from a hydroacylation/conjugate addition
 cascade
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1504
_journal_page_last               1511
_journal_paper_doi               10.1039/D1SC06900D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C20 H27 N1 O5'
_chemical_formula_sum            'C20 H27 N O5'
_chemical_formula_weight         361.44
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2021-06-24 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.936(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6377(4)
_cell_length_b                   19.0350(7)
_cell_length_c                   18.0198(7)
_cell_measurement_reflns_used    8500
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      1.84
_cell_volume                     3797.8(3)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_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      170
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50277
_diffrn_reflns_theta_full        27.196
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         1.839
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9801
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         11262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.0006463
_refine_ls_shift/su_mean         0.0000632
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 1.14P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1517
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1517
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7542
_reflns_number_total             11263
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.00
_oxford_diffrn_Wilson_scale      0.43
_oxford_refine_ls_r_factor_ref   0.0819
_oxford_refine_ls_scale          1.613(8)
_oxford_reflns_number_all        11263
_cod_data_source_file            d1sc06900d2.cif
_cod_data_source_block           DM3_067_v2
_cod_depositor_comments
;
The following automatic conversions were performed:

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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1566046--1566049.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C20 H27 N1 O5'
_cod_database_code               1566049
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0819
_oxford_refine_ls_wr_factor_all  0.1518