Crystal structure of 13-(4-fluorophenyl)-11,13-dihydro-1H-benzo[h]indazolo[6,7-b] [1, 6]naphthyridin-12(6H)-one — dimethylformamide — water (1/2/1), C29H31FN6O4
Xie, Heng-Shen; Wang, Jun-qiang; Su, Ling; Lu, Jing-yang; Zhao, Xiao-qian; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 541–543; doi:10.1515/ncrs-2015-0179

data_8106933
_publ_section_title
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 Crystal structure of
 13-(4-fluorophenyl)-11,13-dihydro-1H-benzo[h]indazolo[6,7-b] [1,
 6]naphthyridin-12(6H)-one --- dimethylformamide --- water (1/2/1),
 C29H31FN6O4
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              541
_journal_page_last               543
_journal_paper_doi               10.1515/ncrs-2015-0179
_journal_volume                  231
_journal_year                    2016
_chemical_formula_sum            'C29 H31 F N6 O4'
_chemical_formula_weight         546.60
_chemical_name_systematic
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3-(4-fluorophenyl)-11,13-dihydro-1H-benzo[h]indazolo[6,7-b] 
[1, 6]naphthyridin-12(6H)-one - dimethylformamide - water (1/2/1)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.358(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.405(2)
_cell_length_b                   11.5703(18)
_cell_length_c                   19.459(3)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.41
_cell_volume                     2775.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19427
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4962
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0577
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                3948
_reflns_number_total             4962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2015-0179_suppl.cif
_cod_data_source_block           Xie
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        2775.9(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               8106933