Tris(4-methylbenzyl)(1,4,7-trimethyl-1,4,7-triazacyclononane)lanthanum(III)
Bambirra, Sergio; Meetsma, Auke; Bart Hessen, Bart; Acta Crystallographica Section E 63 (2007) m2891–m2891; doi:10.1107/S1600536807053640

data_2216335
_publ_section_title
;
 Tris(4-methylbenzyl)(1,4,7-trimethyl-1,4,7-triazacyclononane)lanthanum(III)
;
_journal_coeditor_code           BV2078
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2891
_journal_page_last               m2891
_journal_paper_doi               10.1107/S1600536807053640
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[La (C8 H9)3 (C9 H21 N3)]'
_chemical_formula_moiety         'C33 H48 La N3'
_chemical_formula_sum            'C33 H48 La N3'
_chemical_formula_weight         625.67
_chemical_name_systematic
;
tris(4-methylbenzyl)(1,4,7-trimethyl-1,4,7-triazacyclononane)lanthanum(III)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.094(2)
_cell_length_b                   13.4720(10)
_cell_length_c                   14.4880(10)
_cell_measurement_reflns_used    5692
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      2.42
_cell_volume                     3141.3(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2006)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF99 (Beurskens <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD area-detector
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23512
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2006).
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.384
_exptl_absorpt_correction_T_max  0.9203
_exptl_absorpt_correction_T_min  0.7575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006))'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.471
_refine_diff_density_min         -0.603
_refine_ls_abs_structure_details
;
Flack & Bernardinelli (1999, 2000), 2909 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6249
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                4265
_reflns_number_total             6249
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bv2078.cif
_cod_data_source_block           I
_cod_database_code               2216335
_cod_database_fobs_code          2216335