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_4312321
_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_sum            'C24 H44 Cl2 N4 O14'
_chemical_formula_weight         683.53
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(14)
_cell_angle_beta                 90.000(12)
_cell_angle_gamma                71.895(12)
_cell_formula_units_Z            2
_cell_length_a                   9.650(7)
_cell_length_b                   10.244(7)
_cell_length_c                   17.201(12)
_cell_measurement_temperature    150(2)
_cell_volume                     1616(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1422
_diffrn_reflns_av_sigmaI/netI    0.1206
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8150
_diffrn_reflns_theta_full        28.13
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1672P)^2^+0.0137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2297
_refine_ls_wR_factor_ref         0.2720
_reflns_number_gt                4162
_reflns_number_total             6614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034245zsi20030306_112308_1.cif
_cod_data_source_block           '[H2L](ClO4)2.3H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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        1616.2(19)
_cod_database_code               4312321