<i>catena</i>-Poly[[[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)nickel(II)]-μ-oxido-[dioxidotungstate(VI)]-μ-oxido] tetrahydrate]
Ou, Guang-Chuan; Yuan, Xian-You; Li, Zhi-Zhang; Acta Crystallographica Section E 68 (2012) m1173–; doi:10.1107/S1600536812034538

data_2236545
_publ_section_title
;
 <i>catena</i>-Poly[[[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)nickel(II)]-\m-oxido-[dioxidotungstate(VI)]-\m-oxido]
 tetrahydrate]
;
_journal_coeditor_code           PV2574
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1173
_journal_paper_doi               10.1107/S1600536812034538
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni W O4 (C16 H36 N4)], 4H2 O'
_chemical_formula_moiety         'C16 H36 N4 Ni O4 W, 4(H2 O)'
_chemical_formula_sum            'C16 H44 N4 Ni O8 W'
_chemical_formula_weight         663.11
_chemical_name_systematic
;
<i>catena</i>-Poly[[[(5,5,7,12,12,14-hexamethyl-1,4,8,11-
tetraazacyclotetradecane-\k^4^<i>N</i>)nickel(II)]-\m-oxido-
[dioxidotungstate(VI)]-\m-oxido] tetrahydrate]
;
_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           SHELXL97
_cell_angle_alpha                107.163(2)
_cell_angle_beta                 102.529(3)
_cell_angle_gamma                104.984(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8402(14)
_cell_length_b                   11.7653(18)
_cell_length_c                   13.931(2)
_cell_measurement_reflns_used    3766
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      1.93
_cell_volume                     1268.1(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7631
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.318
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_correction_T_min  0.2894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.484
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                4330
_reflns_number_total             5397
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2574.cif
_cod_data_source_block           I
_cod_database_code               2236545
_cod_database_fobs_code          2236545