Construction of dispirocyclohexanes via amine-catalyzed [2 + 2 + 2] annulations of Morita-Baylis-Hillman acetates with exocyclic alkenes.
Chen, Rongshun; Xu, Silong; Fan, Xia; Li, Hanyuan; Tang, Yuhai; He, Zhengjie; Organic & biomolecular chemistry 13 (2015) 398–408; doi:10.1039/c4ob01927j

data_7154142
_publ_section_title
;
 Construction of dispirocyclohexanes via amine-catalyzed [2 + 2 + 2]
 annulations of Morita-Baylis-Hillman acetates with exocyclic alkenes.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              398
_journal_page_last               408
_journal_paper_doi               10.1039/c4ob01927j
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C43.25 H32.5 Cl0.5 F6 O6'
_chemical_formula_weight         779.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 92.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_b                   21.206(4)
_cell_length_c                   14.570(3)
_cell_measurement_reflns_used    7748
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9344
_cell_measurement_theta_min      1.6971
_cell_volume                     3757.4(12)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0778
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_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37451
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.9716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0106(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1590
_reflns_number_gt                5215
_reflns_number_total             8963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob01927j2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7154142--7154143.cif.
;
_cod_original_cell_volume        3757.4(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C43.25 H32.50 Cl0.50 F6 O6'
_cod_database_code               7154142