Solution and solid state structures of binuclear zinc(II) complexes of bis(pentadentate) ligands derived from bis(1,4,7-triazacyclononane) macrocycles
J. Brudenell, Suzanne; Spiccia, Leone; C. R. Hockless, David; R. T. Tiekink, Edward; Journal of the Chemical Society, Dalton Transactions  (1999) 1475–; doi:10.1039/a809946d

data_7027235
_publ_contact_author
;
 Dr ERT TIEKINK,
 Department of Chemistry,
 The University of Adelaide,
 AUSTRALIA 5005
;
_publ_section_title
;
 Solution and solid state structures of binuclear zinc(II) complexes of
 bis(pentadentate) ligands derived from bis(1,4,7-triazacyclononane)
 macrocycles
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1475
_journal_paper_doi               10.1039/a809946d
_journal_year                    1999
_chemical_formula_sum            'C39 H54 Cl3 N10 O13.5 Zn2'
_chemical_formula_weight         1116.03
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Wed Feb 10 16:03:15 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.863(9)
_cell_length_b                   19.011(5)
_cell_length_c                   12.663(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    220
_cell_measurement_theta_max      41.5
_cell_measurement_theta_min      32.3
_cell_volume                     4541(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      220
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.03699
_diffrn_orient_matrix_UB_12      -0.03496
_diffrn_orient_matrix_UB_13      0.02111
_diffrn_orient_matrix_UB_21      -0.01907
_diffrn_orient_matrix_UB_22      0.00013
_diffrn_orient_matrix_UB_23      -0.07369
_diffrn_orient_matrix_UB_31      0.03284
_diffrn_orient_matrix_UB_32      -0.03931
_diffrn_orient_matrix_UB_33      -0.01901
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5840
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -9.11
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       multifaceted
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.65
_refine_ls_abs_structure_details
;
refinement of opp. hand gave sig.
greater values of R and Rw, i.e. 0.078 and 0.073, resp.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.107
_refine_ls_hydrogen_treatment    'incl. in calc. positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         3195
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0715
_refine_ls_shift/esd_max         0.0315
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0665
_reflns_number_observed          3195
_reflns_number_total             5840
_reflns_observed_criterion       I>2.0sigma(I)
_cod_data_source_file            809946dsup1.cif
_cod_data_source_block           '[C39H54Cl3N10O13.5Zn2]'
_cod_original_cell_volume        4540(2)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C39 H54 Cl3 N10 O13.50 Zn2 '
_cod_database_code               7027235