[4+1] cyclization of α-diazo esters and mesoionic N-heterocyclic olefins.
Liang, Qiuming; Zeng, Yimin; Mendez Ocampo, Pedro A.; Zhu, Hui; Qu, Zheng-Wang; Grimme, Stefan; Song, Datong; Chemical communications (Cambridge, England) 59 (2023) 4770–4773; doi:10.1039/d3cc01139a

data_7131484
_publ_section_title
;
 [4+1] cyclization of &#x3b1;-diazo esters and mesoionic N-heterocyclic
 olefins.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4770
_journal_page_last               4773
_journal_paper_doi               10.1039/d3cc01139a
_journal_volume                  59
_journal_year                    2023
_chemical_formula_sum            'C27 H25 N5 O'
_chemical_formula_weight         435.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.084(7)
_cell_length_b                   17.067(5)
_cell_length_c                   11.802(3)
_cell_measurement_reflns_used    58567
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.444
_cell_measurement_theta_min      3.145
_cell_volume                     5254(2)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa Photon II'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            58567
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         3.145
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0105(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0903P)^2^+1.9069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3854
_reflns_number_total             5976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01139a2.cif
_cod_data_source_block           wl499_sq
_cod_depositor_comments
'Adding full bibliography for 7131480--7131487.cif.'
_cod_original_cell_volume        5254(3)
_cod_database_code               7131484
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              64963
_shelx_hkl_checksum              67547
_shelx_fab_checksum              72290