A new lanthanum coordination polymer built from a semi-rigid tripodal carboxylic acid ligand: synthesis, crystal structure and properties
Zhou, Lian; Shi, Pei-Dong; Guo, Xiao-Kun; Feng, Xiu-Cun; Wang, Lin-Lin; Zhang, Jun; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619011240

data_2021747
_publ_section_title
;
 A new lanthanum coordination polymer built from a semi-rigid tripodal
 carboxylic acid ligand: synthesis, crystal structure and properties
;
_journal_coeditor_code           YP3192
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619011240
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[La (C33 H27 O9) (C3 H7 N O)2], 4C3 H7 N O, 0.25H2 O'
_chemical_formula_moiety         'C39 H41 La N2 O11, 4(C3 H7 N O), 0.25(H2 O)'
_chemical_formula_sum            'C51 H69.5 La N6 O15.25'
_chemical_formula_weight         1149.53
_chemical_name_systematic
;Poly[[bis(dimethylformamide)(\m~6~-4,4',4''-{[(2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene)]tris(oxy)}tribenzoato)lanthanum(III)]
dimethylformamide tetrasolvate 0.25-hydrate]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                77.482(3)
_cell_angle_beta                 73.859(3)
_cell_angle_gamma                85.101(2)
_cell_formula_units_Z            2
_cell_length_a                   12.947(3)
_cell_length_b                   13.889(3)
_cell_length_c                   16.2890(11)
_cell_measurement_reflns_used    1570
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      20.458
_cell_measurement_theta_min      2.197
_cell_volume                     2745.8(9)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      291.15
_diffrn_detector                 'Bruker APEXII area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23526
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.502
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.8354
_exptl_absorpt_correction_T_min  0.7972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1193
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.685
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         11881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1470
_reflns_number_gt                8526
_reflns_number_total             11881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3192sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C51 H69.50 La N6 O15.25'
_cod_database_code               2021747
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.835
_shelx_hkl_checksum              55551
_shelx_res_checksum              59311
_cod_database_fobs_code 2021747