Tris(ethanol-κ<i>O</i>)tris(picrato-κ^2^<i>O</i>^1^,<i>O</i>^2^)lanthanum(III) tri-2-pyridylamine solvate
Chan, Eric J.; Acta Crystallographica Section E 64 (2008) m984–m985; doi:10.1107/S1600536808019296

data_2219206
_publ_section_title
;Tris(ethanol-\k<i>O</i>)tris(picrato-\k^2^<i>O</i>^1^,<i>O</i>^2^)lanthanum(III)
 tri-2-pyridylamine solvate
;
_journal_coeditor_code           ZL2121
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m984
_journal_page_last               m985
_journal_paper_doi               10.1107/S1600536808019296
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[La (C6 H2 N3 O7)3 (C2 H6 O)3], C15 H12 N4'
_chemical_formula_moiety         'C24 H24 La N9 O24, C15 H12 N4'
_chemical_formula_sum            'C39 H36 La N13 O24'
_chemical_formula_weight         1209.69
_chemical_name_systematic
;Tris(ethanol-\k<i>O</i>)tris(picrato-\k^2^<i>O</i>^1^,<i>O</i>^2^)lanthanum(III)
tri-2-pyridylamine
 solvate
;
_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                101.714(11)
_cell_angle_beta                 111.610(14)
_cell_angle_gamma                90.676(8)
_cell_formula_units_Z            4
_cell_length_a                   15.7554(19)
_cell_length_b                   16.4752(14)
_cell_length_c                   20.427(4)
_cell_measurement_reflns_used    16526
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1501
_cell_measurement_theta_min      2.5872
_cell_volume                     4805.1(13)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics    'XTAL3.7 (Hall <i>et al.</i>,  2001)'
_computing_publication_material  'XTAL3.7 (Hall <i>et al.</i>,  2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       \w
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.1973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58832
_diffrn_reflns_theta_full        26.795
_diffrn_reflns_theta_max         31.16
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.99
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .03
_refine_diff_density_max         2.846
_refine_diff_density_min         -0.750
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1419
_refine_ls_number_reflns         28469
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.031P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                14209
_reflns_number_total             28469
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2121.cif
_cod_data_source_block           I
_cod_database_code               2219206
_cod_database_fobs_code          2219206