Poly[[diaquadeca-μ~2~-cyanido-κ^20^<i>C</i>:<i>N</i>-hexacyanido-κ^6^<i>C</i>-bis(μ~2~-5-methylpyrimidine-κ^2^<i>N</i>:<i>N</i>')bis(5-methylpyrimidine-κ<i>N</i>)tricopper(II)ditungstate(V)] dihydrate]
Tsunobuchi, Yoshihide; Kaneko, Souhei; Nakabayashi, Koji; Ohkoshi, Shin-ichi; Acta Crystallographica Section E 70 (2014) m47–m48; doi:10.1107/S1600536814000166

data_2239002
_publ_section_title
;
 Poly[[diaquadeca-\m~2~-cyanido-\k^20^<i>C</i>:<i>N</i>-hexacyanido-\k^6^<i>C</i>-bis(\m~2~-5-methylpyrimidine-\k^2^<i>N</i>:<i>N</i>')bis(5-methylpyrimidine-\k<i>N</i>)tricopper(II)ditungstate(V)]
 dihydrate]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m47
_journal_page_last               m48
_journal_paper_doi               10.1107/S1600536814000166
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Cu3 W2 (C N)16 (C5 H6 N2)4 (H2 O1)2], 2H2 O1'
_chemical_formula_moiety         'C36 H32 Cu3 N24 O4 W2'
_chemical_formula_sum            'C36 H32 Cu3 N24 O4 W2'
_chemical_formula_weight         1423.19
_chemical_name_systematic
'Poly[[diaquadeca-\m~2~-cyanido-\k^20^<i>C</i>:<i>N</i>-hexacyanido-\k^6^<i>C</i>-bis(\m~2~-5-methylpyrimidine-\k^2^<i>N</i>:<i>N</i>')bis(5-methylpyrimidine-\k<i>N</i>)tricopper(II)ditungstate(V)] dihydrate]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.6140(10)
_cell_angle_beta                 84.824(2)
_cell_angle_gamma                73.0900(10)
_cell_formula_units_Z            1
_cell_length_a                   7.5953(4)
_cell_length_b                   11.8232(7)
_cell_length_c                   14.7017(8)
_cell_measurement_reflns_used    10947
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1241.44(12)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2007)'
_computing_molecular_graphics    '<i>PyMOLWin</i> (DeLano, 2007)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12240
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    5.943
_exptl_absorpt_correction_T_max  0.7716
_exptl_absorpt_correction_T_min  0.4517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             683
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.017
_refine_diff_density_min         -0.862
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5666
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0422P)^2^+0.3667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                5465
_reflns_number_total             5666
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5281sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1241.45(12)
_cod_database_code               2239002
_cod_database_fobs_code          2239002