Rauhut-currier-type reaction with morita-baylis-hillman carbonates of 2-cyclohexenone and alkylidenemalononitriles to access chromene derivatives.
Peng, Jing; Huang, Xin; Zheng, Peng-Fei; Chen, Ying-Chun; Organic letters 15 (2013) 5534–5537; doi:10.1021/ol402694b

data_1512593
_publ_section_title
;
 Rauhut-currier-type reaction with morita-baylis-hillman carbonates of
 2-cyclohexenone and alkylidenemalononitriles to access chromene
 derivatives.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5534
_journal_page_last               5537
_journal_paper_doi               10.1021/ol402694b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C27 H22 N2 O2'
_chemical_formula_weight         406.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.025(4)
_cell_angle_beta                 98.840(3)
_cell_angle_gamma                102.091(4)
_cell_formula_units_Z            2
_cell_length_a                   8.156(3)
_cell_length_b                   11.100(4)
_cell_length_c                   13.054(4)
_cell_measurement_reflns_used    2574
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.118
_cell_measurement_theta_min      2.624
_cell_volume                     1075.3(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  AFC10/Saturn724+
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13193
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5661
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.6300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                4368
_reflns_number_total             5661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402694b_si_003.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1075.2(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512593