Metal Complexes with a New N4O3 Amine Pendant-Armed Macrocyclic Ligand: Synthesis, Characterization, Crystal Structures, and Fluorescence Studies
Manuel Vicente; Rufina Bastida; Carlos Lodeiro; Alejandro Macías; A. Jorge Parola; Laura Valencia; Sharon E. Spey; Inorganic Chemistry 42 (2003) 6768–6779; doi:10.1021/ic034245z

data_4312323
_publ_section_title
;
 Metal Complexes with a New N4O3 Amine Pendant-Armed Macrocyclic Ligand:
 Synthesis, Characterization, Crystal Structures, and Fluorescence Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6768
_journal_page_last               6779
_journal_paper_doi               10.1021/ic034245z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C24 H36 Cl2 N4 O11 Zn1'
_chemical_formula_sum            'C24 H38 Cl2 N4 O8 Zn'
_chemical_formula_weight         646.85
_chemical_name_systematic
;
 ?
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.104(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.815(2)
_cell_length_b                   14.774(5)
_cell_length_c                   15.133(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.09
_cell_measurement_theta_min      15.92
_cell_volume                     2918.6(13)
_computing_cell_refinement       'CAD4-Express Software (Nonius, 1994)'
_computing_data_collection       'CAD4-Express Software (Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6331
_diffrn_reflns_theta_full        75.89
_diffrn_reflns_theta_max         75.89
_diffrn_reflns_theta_min         3.76
_diffrn_standards_decay_%        6
_diffrn_standards_interval_count 183
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  0.6203
_exptl_absorpt_correction_T_min  0.2594
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.653
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6080
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2340
_reflns_number_gt                3043
_reflns_number_total             6080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034245zsi20030306_112308_3.cif
_cod_data_source_block           '[ZnLCl](ClO4).H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2918.7(13)
_cod_database_code               4312323