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_2016585
_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 (C30 H30 N6)] (Cl O4)2'
_chemical_formula_moiety         'C30 H30 N6 Zn 2+ , 2Cl O4 -'
_chemical_formula_sum            'C30 H30 Cl2 N6 O8 Zn'
_chemical_formula_weight         738.910
_chemical_name_common            '[Zn(qtpen)](ClO4)2'
_chemical_name_systematic
;
[N,N,N'-tris(2-pyridylmethyl)-N'-(2-quinolmethyl)ethane-1,2-diamine-\k^6^N]-
diperchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 94.634(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.231(2)
_cell_length_b                   15.147(2)
_cell_length_c                   15.167(2)
_cell_measurement_reflns_used    7829
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      1.9
_cell_volume                     3029.7(7)
_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  0.026
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25310
_diffrn_reflns_reduction_process 25310
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Siemens, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.43(7)
_refine_diff_density_min         -1.18(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    78
_refine_ls_number_parameters     402
_refine_ls_number_reflns         4838
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.030
_refine_ls_shift/su_max          0.0013
_refine_ls_shift/su_mean         0.00004
_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 = 5.7'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.035
_reflns_number_gt                4838
_reflns_number_total             6946
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ga3084.cif
_cod_data_source_block           II
_cod_original_cell_volume        3029.5(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C30 H30 Cl2 N6 O8 Zn1'
_cod_database_code               2016585
_cod_database_fobs_code          2016585