Three overcrowded zinc(II) complexes with potentially hexadentate polypyridyl ligands
Hazell, Alan; Mønsted, Ole; Rasmussen, Jens Christian; Toftlund, Hans; Acta Crystallographica Section C 64 (2008) m185–m189; doi:10.1107/S0108270108007014

data_2016584
_publ_section_title
;
 Three overcrowded zinc(II) complexes with potentially hexadentate
 polypyridyl ligands
;
_journal_coeditor_code           GA3084
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m185
_journal_page_last               m189
_journal_paper_doi               10.1107/S0108270108007014
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zn (C26 H28 N6)] (Cl O4)2 , 0.67H2 O'
_chemical_formula_moiety         'C26 H28 N6 Zn 2+ , 2Cl O4 - , 0.67H2 O'
_chemical_formula_sum            'C78 H88 Cl6 N18 O26 Zn3'
_chemical_formula_weight         700.86
_chemical_name_common            '[Zn(tpen)](ClO4)2 2/3H2O'
_chemical_name_systematic
;
[N,N,N',N'-tetrakis(2-pyridylmethyl)ethane-1,2-diamine-\k^6^N]zinc(II)
diperchlorate 0.67-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 107.625(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            12
_cell_length_a                   41.064(3)
_cell_length_b                   9.3590(7)
_cell_length_c                   23.785(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      1.8
_cell_volume                     8711.9(12)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
ORTEPIII (Burnett and Johnson, 1996), KRYSTAL (Hazell, 1995) and
PLATON (Spek,
2003)
;
_computing_publication_material  'KRYSTAL (Hazell, 1995)'
_computing_structure_refinement
;
ORFLS (Busing <i>et al.</i>,  1962; modified) and KRYSTAL (Hazell,
1995)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1997) and KRYSTAL (Hazell, 1995)
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device       'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41218
_diffrn_reflns_reduction_process 41218
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Siemens, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4328.0
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.55(4)
_refine_diff_density_min         -0.35(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     591
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/{[\s~cs~(F^2^)+B +(1+A)F^2^]^1/2^-|F|}^2^ where A = 0.03 and B = 0.5'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                6179
_reflns_number_total             10019
_reflns_threshold_expression     I>2.5\s(I)
_cod_data_source_file            ga3084.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016584
_cod_database_fobs_code          2016584