Poly[[tetramethanolbis[4-oxo-3-(pyridin-4-yl)-1-(2,4,6-trichlorophenyl)-4,5-dihydro-1<i>H</i>-pyrazolo[3,4-<i>d</i>]pyrimidin-6-olato]disodium]–diethyl ether–methanol (1/1/2)]
Abu Thaher, Bassam; Schollmeyer, Dieter; Laufer, Stefan; IUCrData 1 (2016) x161081–; doi:10.1107/S2414314616010816

data_1543663
_publ_section_title
;
 Poly[[tetramethanolbis[4-oxo-3-(pyridin-4-yl)-1-(2,4,6-trichlorophenyl)-4,5-dihydro-1<i>H</i>-pyrazolo[3,4-<i>d</i>]pyrimidin-6-olato]disodium]--diethyl
 ether--methanol (1/1/2)]
;
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x161081
_journal_paper_doi               10.1107/S2414314616010816
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac
'[Na (C16 H7 Cl3 N5 O2) (C H4 O)2], 0.5(C4 H10 O), C H4 O'
_chemical_formula_moiety         'C16 H7 Cl3 N5 Na O2, 0.5(C4 H10 O), 3(C H4 O)'
_chemical_formula_sum            'C21 H24 Cl3 N5 Na O5.5'
_chemical_formula_weight         563.79
_chemical_name_systematic
'Poly[[tetramethanolbis[4-oxo-3-(pyridin-4-yl)-1-(2,4,6-trichlorophenyl)-4,5-dihydro-1<i>H</i>-pyrazolo[3,4-<i>d</i>]pyrimidin-6-olato]disodium]--diethyl ether--methanol (1/1/2)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.2130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1721(7)
_cell_length_b                   8.1249(5)
_cell_length_c                   28.8799(18)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.5
_cell_volume                     2580.0(3)
_computing_cell_refinement
;
SAINT (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics    'please specify'
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1995)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'CCD scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            27638
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.816
_diffrn_reflns_theta_min         1.864
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0325P)^2^+4.0979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                5149
_reflns_number_total             6097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4018sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2023-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C16 H7 Cl3 N5 Na O2), C4 H10 O, 6(C H4 O)'
_cod_original_formula_iupac
'[Na2 (C16 H7 Cl3 N5 O2)2 (C H4 O)4], C4 H10 O, 2C H4 O'
_cod_original_formula_sum        'C42 H48 Cl6 N10 Na2 O11'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1127.58
_cod_database_code               1543663
_cod_database_fobs_code          1543663
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.925
_shelx_hkl_checksum              87133
_shelx_res_checksum              72937