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_2016586
_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 (C34 H32 N6)] (Cl O4)2 , H2 O'
_chemical_formula_moiety         'C34 H32 N6 Zn 2+ , 2Cl O4 - , H2 O'
_chemical_formula_sum            'C34 H34 Cl2 N6 O9 Zn'
_chemical_formula_weight         806.99
_chemical_name_common            '[Zn(bqbpen)](ClO4)2.H2O'
_chemical_name_systematic
;[N,N'-bis(2-pyridylmethyl)-N,N'-bis(2-quinolmethyl)ethane-1,2-diamine-\k^6^N]-
zinc(II)
 diperchlorate monohydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.891(3)
_cell_length_b                   12.022(3)
_cell_length_c                   23.838(5)
_cell_measurement_reflns_used    8135
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      1.9
_cell_volume                     3407.7(14)
_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  0.064
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28487
_diffrn_reflns_reduction_process 28487
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Siemens, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.15(9)
_refine_diff_density_min         -0.59(9)
_refine_ls_abs_structure_details
;
Rogers factor refined for 2959 Bijvoet pairs where
both members have I > 3\s(I)
For the crystal studied, N1 and N2 have the S configuration
;
_refine_ls_abs_structure_Rogers  0.93(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.0004
_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 = 0.51'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                6872
_reflns_number_total             7803
_reflns_threshold_expression     I>2.5\s(I)
_cod_data_source_file            ga3084.cif
_cod_data_source_block           III
_cod_original_cell_volume        3407.8(14)
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               2016586
_cod_database_fobs_code          2016586