Two lanthanum(III) complexes containing η^2^-pyrazolate and η^2^-1,2,4-triazolate ligands: intramolecular C—H···N/O interactions and coordination geometries
Wang, Yu-Long; Feng, Meng; Tao, Xian; Tang, Qing-Yun; Shen, Ying-Zhong; Acta Crystallographica Section C 69 (2013) 25–28; doi:10.1107/S0108270112049281

data_2018732
_publ_section_title
;
 Two lanthanum(III) complexes containing \h^2^-pyrazolate and
 \h^2^-1,2,4-triazolate ligands: intramolecular
 C---H&#x00B7;&#x00B7;&#x00B7;N/O interactions and coordination geometries
;
_journal_coeditor_code           BI3050
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              25
_journal_page_last               28
_journal_paper_doi               10.1107/S0108270112049281
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[La (C15 H11 N2)3 (C4 H8 O)3] , C4 H8 O'
_chemical_formula_moiety         'C57 H57 La N6 O3, C4 H8 O'
_chemical_formula_sum            'C61 H65 La N6 O4'
_chemical_formula_weight         1085.10
_chemical_name_systematic
;
tris(3,5-diphenylpyrazolato-\k^2^<i>N</i>,<i>N</i>')tris(tetrahydrofuran-
\k<i>O</i>)lanthanum(III) tetrahydrofuran monosolvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.146(3)
_cell_length_b                   16.358(3)
_cell_length_c                   22.856(5)
_cell_measurement_reflns_used    20820
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0572
_cell_measurement_theta_min      2.6078
_cell_volume                     5288.9(19)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn CCD area-detector'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22016
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.338
_refine_ls_abs_structure_details
'Flack (1983), <b>with how many Friedel pairs?</b>'
_refine_ls_abs_structure_Flack   0.450(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         9592
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0219P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                9280
_reflns_number_total             9592
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3050.cif
_cod_data_source_block           I
_cod_original_cell_volume        5288.8(18)
_cod_database_code               2018732
_cod_database_fobs_code          2018732