Iron-catalyzed domino Knoevenagel-hetero-Diels-Alder reaction: facile access to oxabicyclo[3.3.1]nonene derivatives.
Wu, Mingchang; Yang, Junhang; Luo, Fang; Cheng, Cungui; Zhu, Gangguo; Organic & biomolecular chemistry 17 (2019) 5684–5687; doi:10.1039/c9ob00836e

data_7156871
_publ_section_title
;
 Iron-catalyzed domino Knoevenagel-hetero-Diels-Alder reaction: facile
 access to oxabicyclo[3.3.1]nonene derivatives.
;
_journal_issue                   23
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5684
_journal_page_last               5687
_journal_paper_doi               10.1039/c9ob00836e
_journal_volume                  17
_journal_year                    2019
_chemical_formula_sum            'C17 H18 O2'
_chemical_formula_weight         254.31
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_space_group_name_Hall           '-C 2yc'
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_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-04-10 deposited with the CCDC.    2019-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
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_cell_angle_gamma                90.00
_cell_formula_units_Z            8
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_cell_length_c                   16.4364(5)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      49.5
_cell_measurement_theta_min      2.23
_cell_volume                     2732.90(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.997
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_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_av_sigmaI/netI    0.0277
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_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48432
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.3
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_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0743
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_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2455
_refine_ls_wR_factor_ref         0.2738
_reflns_number_gt                2184
_reflns_number_total             3140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ob00836e2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

 Adding full bibliography for 7156871.cif.
;
_cod_original_cell_volume        2732.90(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7156871