Efficient strategy for construction of 6-carbamoylfulvene-6-carboxylate skeletons via [3 + 2] cycloaddition of 1-cyanocyclopropane 1-ester with β-nitrostyrenes
Tan, Chen; Ye, Weijian; Yao, Juan; Liu, Juanjuan; Xue, Shuwen; Li, Yang; Wang, Cunde; RSC Advances 5 (2015) 26491–; doi:10.1039/C5RA02918J

data_7235892
_publ_section_title
;
 Efficient strategy for construction of 6-carbamoylfulvene-6-carboxylate
 skeletons via [3&#x00A0;+ 2] cycloaddition of 1-cyanocyclopropane 1-ester
 with \b-nitrostyrenes
;
_journal_issue                   34
_journal_name_full               'RSC Advances'
_journal_page_first              26491
_journal_paper_doi               10.1039/C5RA02918J
_journal_volume                  5
_journal_year                    2015
_chemical_formula_sum            'C30 H26 Cl N O5'
_chemical_formula_weight         515.97
_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   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2014-12-21 deposited with the CCDC.
2015-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.596(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.841(5)
_cell_length_b                   14.847(4)
_cell_length_c                   8.918(2)
_cell_measurement_reflns_used    2919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.51
_cell_measurement_theta_min      2.47
_cell_volume                     2626.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1707
_diffrn_reflns_av_unetI/netI     0.1929
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24139
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.053
_exptl_absorpt_coefficient_mu    0.186
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.2109
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1924
_reflns_number_total             4612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra02918j2.cif
_cod_data_source_block           001
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7235892
_shelxl_version_number           2014/6
_shelx_res_checksum              56057
_shelx_hkl_checksum              29099