Brønsted Base-Catalyzed Annulation of Allyl Ketones and Alkynyl 1,2-Diketones
Fang, Xinqiang; Kong, Xiangwen; Liu, Jian; Yang, Shuang; Zeng, Min; Zhan, Xinyue; Li, Chunsen; Song, Jinshuai; Meng, Miao; Chemical Communications  (2018) –; doi:10.1039/C8CC01020J

data_7121463
_publ_section_title
;
 Br\/onsted Base-Catalyzed Annulation of Allyl Ketones and Alkynyl
 1,2-Diketones
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC01020J
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C32 H22 Cl2 O3'
_chemical_formula_sum            'C32 H22 Cl2 O3'
_chemical_formula_weight         525.4
_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'
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2017-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-01-20 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.290(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.200(4)
_cell_length_b                   21.427(7)
_cell_length_c                   12.408(5)
_cell_measurement_reflns_used    5752
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      27.4739
_cell_measurement_theta_min      2.7856
_cell_volume                     2659.4(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      293.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.8460
_diffrn_measured_fraction_theta_max 99.5000
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 28.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.2765
              2theta: -24.8484
scan:
    Number of images: 280
               Slice: -115.0000 - 25.0000
         Image width: 0.5000
            Exp time: 28.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.2765
              2theta: -24.8484
scan:
    Number of images: 160
               Slice: -115.0000 - -35.0000
         Image width: 0.5000
            Exp time: 28.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.2765
              2theta: -24.8484
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0365
_diffrn_orient_matrix_UB_12      0.0925
_diffrn_orient_matrix_UB_13      -0.0108
_diffrn_orient_matrix_UB_21      0.0356
_diffrn_orient_matrix_UB_22      0.0108
_diffrn_orient_matrix_UB_23      -0.0282
_diffrn_orient_matrix_UB_31      -0.0487
_diffrn_orient_matrix_UB_32      -0.0095
_diffrn_orient_matrix_UB_33      -0.0655
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22777
_diffrn_reflns_theta_full        27.4663
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           80.0000
_diffrn_source_power             4.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7051
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.3123
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1089.6639
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.4562
_refine_diff_density_min         -0.4315
_refine_diff_density_rms         0.0923
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.52(18)
_refine_ls_d_res_high            0.7705
_refine_ls_d_res_low             8.0408
_refine_ls_goodness_of_fit_ref   0.9930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    86
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9930
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.0089
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.692
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              -27
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                4648
_reflns_number_total             10319
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc01020j2.cif
_cod_data_source_block           data
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2659.2(17)
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7121463
_diffrn_number_total             6226
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(18) 0.52(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C41(H41a,H41b)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36),
 C37(H37), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C53(H53), C54(H54), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62),
 C63(H63), C64(H64)
;
_olex2_submission_special_instructions 'No special instructions were received'