The crystal structure of the Matrine derivative: 12-(1H-indol-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one hydrate, C23H29N3O
Xing-An, Cheng; Zhan-Mei, Liu; Wei-Xin, Liang; Bo, Wu; Xu-Hong, Jiang; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 1017–1019; doi:10.1515/ncrs-2017-0144

data_8106754
_publ_section_title
;
 The crystal structure of the Matrine derivative:
 12-(1H-indol-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3&#x2032;,2&#x2032;,1&#x2032;-ij][1,6]naphthyridin-10-one
 hydrate, C23H29N3O
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1017
_journal_page_last               1019
_journal_paper_doi               10.1515/ncrs-2017-0144
_journal_volume                  232
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H29 N3 O, H2 O'
_chemical_formula_sum            'C23 H31 N3 O2'
_chemical_formula_weight         381.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.62130(10)
_cell_length_b                   18.25770(10)
_cell_length_c                   25.6873(2)
_cell_measurement_reflns_used    23900
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8850
_cell_measurement_theta_min      4.8120
_cell_volume                     4043.31(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38567
_diffrn_reflns_theta_full        74.06
_diffrn_reflns_theta_max         74.06
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03068
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                7843
_reflns_number_total             8120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0144_suppl.cif
_cod_data_source_block           p212121
_cod_database_code               8106754
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11'(H11'), C13'(H13'), C6'(H6'), C5'(H5'), C7'(H7'), C11(H11), C6(H6),
 C7(H7), C13(H13), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C14'(H14A,H14B), C2'(H2'A,H2'B), C17'(H17A,H17B), C8'(H8'A,H8'B), C10'(H10A,
 H10B), C9'(H9'A,H9'B), C4'(H4'A,H4'B), C12'(H12A,H12B), C3'(H3'A,H3'B),
 C17(H17C,H17D), C9(H9A,H9B), C8(H8A,H8B), C3(H3A,H3B), C2(H2A,H2B), C12(H12C,
 H12D), C10(H10C,H10D), C14(H14C,H14D), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C25'(H25'), C23'(H23'), C22'(H22'), C20'(H20'), C21'(H21'), C24'(H24'),
 C25(H25), C23(H23), C24(H24), C21(H21), C20(H20), C22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'