Lanthanide complexes of a new nonadentate ligand derived from 1,4,7-triazacyclononane: synthesis, structural characterisation and NMR spectroscopic studies
Tei, Lorenzo; Baum, Gerhard; Blake, Alexander J.; Fenske, Dieter; Schröder, Martin; Journal of the Chemical Society, Dalton Transactions  (2000) 2793–; doi:10.1039/b002794o

data_7009698
_publ_section_title
;
 Lanthanide complexes of a new nonadentate ligand derived from
 1,4,7-triazacyclononane: synthesis, structural characterisation and
 NMR spectroscopic studies
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2793
_journal_paper_doi               10.1039/b002794o
_journal_year                    2000
_chemical_formula_moiety         'C21 H33 N6 O6 Sm, 3CH~3~OH, 0.5(H~2~O)'
_chemical_formula_sum            'C24 H46 N6 O9.5 Sm'
_chemical_formula_weight         721.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier method'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   28.337(4)
_cell_length_b                   28.337(4)
_cell_length_c                   23.405(5)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     16276(5)
_computing_cell_refinement       'Stoe IPDS'
_computing_data_collection       'Stoe IPDS'
_computing_data_reduction        'Stoe IPDS'
_computing_molecular_graphics    'SHELXTL/PL (version 5-03)(Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.306
_diffrn_measured_fraction_theta_max 0.306
_diffrn_measurement_device_type  'Stoe IPDS image plate'
_diffrn_measurement_method       'area detector'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15155
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_type   'empirical (Habitus)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             6660
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.920
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.112
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+11.2710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                6483
_reflns_number_total             8051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002794o.txt
_cod_data_source_block           n3pvsm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+11.2710P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+11.2710P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'placed geometrically' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C24 H46 N6 O9.50 Sm'
_cod_database_code               7009698