Diastereoselective synthesis of spiro[carbazole-3,5'-pyrimidines] and spiro[carbazole-3,1'-cyclohexanes] <i>via</i> four-component reaction.
Zhan, Shao-Cong; Fang, Ren-Jie; Sun, Jing; Yan, Chao-Guo; Organic & biomolecular chemistry 19 (2021) 6322–6327; doi:10.1039/d1ob01113h

data_7158144
_publ_section_title
;
 Diastereoselective synthesis of spiro[carbazole-3,5'-pyrimidines] and
 spiro[carbazole-3,1'-cyclohexanes] <i>via</i> four-component reaction.
;
_journal_issue                   28
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6322
_journal_page_last               6327
_journal_paper_doi               10.1039/d1ob01113h
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C34 H31 N3 O8'
_chemical_formula_sum            'C34 H31 N3 O8'
_chemical_formula_weight         609.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-04-20 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(4)
_cell_angle_beta                 96.176(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3152(19)
_cell_length_b                   11.0682(15)
_cell_length_c                   20.681
_cell_measurement_reflns_used    7763
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.02
_cell_measurement_theta_min      2.38
_cell_volume                     3030.2(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2259
_diffrn_reflns_av_unetI/netI     0.1334
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23239
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.090
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0141(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5934
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1741
_refine_ls_R_factor_gt           0.1208
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+7.6362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3480
_reflns_number_total             5934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob01113h2.cif
_cod_data_source_block           3o
_cod_depositor_comments
'Adding full bibliography for 7158139--7158148.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7158144
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              50431