The crystal structure of 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino [3,2-a]isoquinolin-7-ium (E)-3-(4-nitrophenyl)acrylate pentahydrate, C29H34N2O13
Chen, Shi-Yun; Wang, Wei; He, Yong; Yin, Deng-ke; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1089–1091; doi:10.1515/ncrs-2023-0331

data_8107668
_publ_section_title
;
 The crystal structure of
 9,10-dimethoxy-5,6-dihydro-[1,3]dioxolo[4,5-g]isoquinolino
 [3,2-a]isoquinolin-7-ium (E)-3-(4-nitrophenyl)acrylate pentahydrate,
 C29H34N2O13
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1089
_journal_page_last               1091
_journal_paper_doi               10.1515/ncrs-2023-0331
_journal_volume                  238
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C20 H18 N O4, C9 H6 N O4, 5(H2 O)'
_chemical_formula_sum            'C29 H34 N2 O13'
_chemical_formula_weight         618.58
_chemical_name_systematic
;
3-((1<i>R</i>,2<i>S</i>)-1-methylpyrrolidin-1-ium-2-yl)pyridin-1-ium
tetrachloridocobaltate(II) monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                94.2080(10)
_cell_angle_beta                 99.7870(10)
_cell_angle_gamma                90.2470(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1996(2)
_cell_length_b                   13.1993(3)
_cell_length_c                   13.5119(3)
_cell_measurement_reflns_used    7535
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      59.23
_cell_measurement_theta_min      2.90
_cell_volume                     1437.00(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      193
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2711
_diffrn_detector_type            EOS
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       'w and \f shutterless scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13791
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.305
_diffrn_reflns_theta_min         2.895
_diffrn_source                   MetalJet
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.35.
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Crystallogr. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0457
_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^)+(0.015P)^2^+3.2P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4466
_reflns_number_total             6231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0331_suppl_001.cif
_cod_data_source_block           exp_1115
_cod_database_code               8107668
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.924
_shelx_res_checksum              76867