Electrochemical collective synthesis of labeled pyrroloindoline alkaloids with Freon-type methanes as functional C1 synthons
Chen, Chao; Liu, Ru-Xin; Xiong, Feng; Li, Zi-Hao; Kang, Jun-Chen; Ding, Tong-Mei; Zhang, Shu-Yu; Chemical Communications  (2022) –; doi:10.1039/D2CC03301A

data_7130435
_publ_section_title
;
 Electrochemical collective synthesis of labeled pyrroloindoline alkaloids
 with Freon-type methanes as functional C1 synthons
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03301A
_journal_year                    2022
_chemical_formula_moiety         'C31 H36 N4 O2'
_chemical_formula_sum            'C31 H36 N4 O2'
_chemical_formula_weight         496.64
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.591(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.3413(16)
_cell_length_b                   5.7873(3)
_cell_length_c                   15.6520(8)
_cell_measurement_reflns_used    7165
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      63.57
_cell_measurement_theta_min      2.94
_cell_volume                     2724.3(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25412
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        63.773
_diffrn_reflns_theta_max         63.773
_diffrn_reflns_theta_min         2.938
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.7524
_exptl_transmission_factor_min   0.5144
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0829
_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^)+(0.1214P)^2^+3.8751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3137
_reflns_number_total             4464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03301a2.cif
_cod_data_source_block           t_a_CCDC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7130435
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.915
_shelx_res_checksum              43614
_shelx_hkl_checksum              20603