μ-1,4-Benzenedicarboxylato-bis[<i>trans</i>-aqua(1,4,8,11-tetraazacyclotetradecane)nickel(II)] diperchlorate forms a three-dimensional hydrogen-bonded framework
Zakaria, Choudhury M.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section C 57 (2001) 683–686; doi:10.1107/S0108270101003857

data_2012049
_publ_section_title
;\m-1,4-Benzenedicarboxylato-bis[<i>trans</i>-aqua(1,4,8,11-tetraazacyclotetradecane)nickel(II)]
 diperchlorate forms a three-dimensional hydrogen-bonded framework
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              683
_journal_page_last               686
_journal_paper_doi               10.1107/S0108270101003857
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Ni2 (C10 H24 N4)2 (H2O)2 (C8 H4 O4)] (ClO4)2'
_chemical_formula_moiety         'C28 H56 N8 Ni2 O6 , 2Cl O4'
_chemical_formula_sum            'C28 H56 Cl2 N8 Ni2 O14'
_chemical_formula_weight         917.09
_chemical_name_systematic
;
\m-1,4-Benzenedicarboxylato-bis[trans-aqua(1,4,8,11-tetraazacyclotetradecane
)nickel(II)] diperchlorate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.5220(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2842(3)
_cell_length_b                   14.9172(4)
_cell_length_c                   13.0621(4)
_cell_measurement_reflns_used    7654
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.84
_cell_volume                     1956.21(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .995
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .052
_diffrn_reflns_av_sigmaI/netI    .0852
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13566
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  .9224
_exptl_absorpt_correction_T_min  .8167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .07
_refine_diff_density_max         .70
_refine_diff_density_min         -.44
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .38(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7654
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          .075
_refine_ls_R_factor_gt           .041
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.019P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .097
_reflns_number_gt                5458
_reflns_number_total             7654
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1465.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2012049
_cod_database_fobs_code          2012049