Bis[1-(2-hydroxyethyl)-4,10-diazapyrazolo[4,3-<i>b</i>]fluoren-5(1<i>H</i>)-one thiosemicarbazonato]zinc(II) dimethylformamide trisolvate monohydrate
Xi-Quan Che; Acta Crystallographica Section C 64 (2008) m5–m7; doi:10.1107/S0108270107052602

data_2016412
_publ_section_title
;Bis[1-(2-hydroxyethyl)-4,10-diazapyrazolo[4,3-<i>b</i>]fluoren-5(1<i>H</i>)-one
 thiosemicarbazonato]zinc(II) dimethylformamide trisolvate monohydrate
;
_journal_coeditor_code           SQ3102
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m5
_journal_page_last               m7
_journal_paper_doi               10.1107/S0108270107052602
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zn (C15 H12 N7 O S)2], 3C3 H7 N O, H2 O'
_chemical_formula_moiety         'C30 H24 N14 O2 S2 Zn, 3(C3 H7 N O), H2 O '
_chemical_formula_sum            'C39 H47 N17 O6 S2 Zn'
_chemical_formula_weight         979.43
_chemical_name_systematic
;
Bis[3-(2-hydroxyethyl)-4,10-diazapyrazolo[3,4-<i>b</i>]fluoren-9(3H)-one
thiosemicarbazonato]zinc(II) dimethylformamide trisolvate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 95.191(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.530(5)
_cell_length_b                   12.104(5)
_cell_length_c                   23.601(5)
_cell_measurement_reflns_used    1864
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.84
_cell_measurement_theta_min      3.68
_cell_volume                     4703(3)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28631
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.8770
_exptl_absorpt_correction_T_min  0.8340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11219
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.5414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                5488
_reflns_number_total             11219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sq3102.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-11-30
;
_cod_original_sg_symbol_H-M      'P 21/ c'
_cod_database_code               2016412
_cod_database_fobs_code          2016412