A hexaaza macrocyclic ligand containing acetohydrazide pendants for Ln(iii) complexation in aqueous solution. Solid-state and solution structures and DFT calculations
Núñez, Cristina; Bastida, Rufina; Macías, Alejandro; Mato-Iglesias, Marta; Platas-Iglesias, Carlos; Valencia, Laura; Dalton Transactions  (2008) 3841–3850; doi:10.1039/b800953h

data_7003876
_publ_section_title
;
 A hexaaza macrocyclic ligand containing acetohydrazide pendants for
 Ln(iii) complexation in aqueous solution. Solid-state and solution
 structures and DFT calculations
;
_journal_issue                   29
_journal_name_full               'Dalton Transactions'
_journal_page_first              3841
_journal_page_last               3850
_journal_paper_doi               10.1039/b800953h
_journal_year                    2008
_chemical_formula_moiety         '[La(C26H42N14O4)]Br1.5(NO3)1.5(H2O)6'
_chemical_formula_sum            'C26 H54 Br1.5 La N15.5 O14.5'
_chemical_formula_weight         1074.57
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 123.1460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.656(2)
_cell_length_b                   10.6477(10)
_cell_length_c                   21.655(2)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.54
_cell_measurement_theta_min      2.19
_cell_volume                     4180.8(7)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'BRUKER Shelxtl'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker CCD SMART1000'
_diffrn_measurement_method       'omega and phi 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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15902
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  0.8627
_exptl_absorpt_correction_T_min  0.4457
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0775P)^2^+11.1164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                3656
_reflns_number_total             4217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800953h.txt
_cod_data_source_block           .onoccn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4180.9(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C26 H54 Br1.50 La N15.50 O14.50'
_cod_database_code               7003876