One-pot construction of dispirocyclohexanes via K<sub>2</sub>CO<sub>3</sub>-mediated desulfonylative Michael-Michael-aldol (2 + 2 + 2) annulation of sulfonyl 2-pyridyl flavanones and methylketones.
Chang, Meng-Yang; Chen, Kuan-Ting; Chen, Han-Yu; Organic & biomolecular chemistry 18 (2020) 6297–6311; doi:10.1039/d0ob01404d

data_7157617
_publ_section_title
;
 One-pot construction of dispirocyclohexanes via
 K<sub>2</sub>CO<sub>3</sub>-mediated desulfonylative
 Michael-Michael-aldol (2 + 2 + 2) annulation of sulfonyl 2-pyridyl
 flavanones and methylketones.
;
_journal_issue                   32
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6297
_journal_page_last               6311
_journal_paper_doi               10.1039/d0ob01404d
_journal_volume                  18
_journal_year                    2020
_chemical_formula_sum            'C33 H24 Br2 Cl3 N2 O5'
_chemical_formula_weight         794.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-11-15 deposited with the CCDC.	2020-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.3340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5330(4)
_cell_length_b                   26.8610(11)
_cell_length_c                   12.2233(5)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.5051
_cell_measurement_theta_min      3.2906
_cell_volume                     3125.7(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
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_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
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_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.898
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13631
_diffrn_reflns_point_group_measured_fraction_full 0.898
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_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.562
_diffrn_reflns_theta_min         3.290
_exptl_absorpt_coefficient_mu    6.036
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lump
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+17.9656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5008
_reflns_number_total             5087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01404d2.cif
_cod_data_source_block           cu_190705LT_0m
_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 7157612--7157619.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7157617
_shelxl_version_number           2014/6
_shelx_res_checksum              49991
_shelx_hkl_checksum              21268