Phosphine-catalyzed divergent domino processes between γ-substituted allenoates and carbonyl-activated alkenes
Wu, Mingyue; Han, Zhaobin; Ni, Huanzhen; Wang, Nengzhong; Ding, Kuiling; Lu, Yixin; Chemical Science  (2022) –; doi:10.1039/D1SC06364B

data_1566404
_publ_section_title
;
 Phosphine-catalyzed divergent domino processes between \g-substituted
 allenoates and carbonyl-activated alkenes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06364B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_sum            'C37 H31 F O5'
_chemical_formula_weight         574.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2022-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.804(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9625(16)
_cell_length_b                   9.5991(14)
_cell_length_c                   14.075(2)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.72
_cell_measurement_theta_min      3.17
_cell_volume                     1467.4(4)
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.715
_diffrn_reflns_theta_max         66.715
_diffrn_reflns_theta_min         3.169
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
; 
 Flack x determined using 2402 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.056(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0345P)^2^+0.3143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5166
_reflns_number_total             5171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06364b2.cif
_cod_data_source_block           J014
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1566404
_shelx_shelxl_version_number     2017/1
_computing_bruker_data_scaling   'SADABS V2018/1 (Bruker AXS Inc.)'
_shelx_res_checksum              9819