Polymorph Selective Growth of Sodium Tetrakis(2-pyridinecarboxylato) Lanthanides and Their Structure Sensitive Properties
Hong, Jung Hoon; Oh, Yunghee; Kim, Youngmee; Kang, Sung Kwon; Choi, Jungkweon; Kim, Wan Seop; Lee, Jong In; Kim, Sung-Jin; Hur, Nam Hwi; Crystal Growth & Design 8 (2008) 1364–; doi:10.1021/cg7012705

data_4503535
_publ_section_title
;
 Polymorph Selective Growth of Sodium Tetrakis(2-pyridinecarboxylato)
 Lanthanides and Their Structure Sensitive Properties
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1364
_journal_paper_doi               10.1021/cg7012705
_journal_volume                  8
_journal_year                    2008
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C24 H20 N4 Na O10 Tb'
_chemical_formula_sum            'C24 H20 N4 Na O10 Tb'
_chemical_formula_weight         706.36
_chemical_name_common            unknown
_chemical_name_systematic        unknown
_space_group_IT_number           179
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      179
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   12.5255(5)
_cell_length_b                   12.5255(5)
_cell_length_c                   59.758(5)
_cell_measurement_reflns_used    5434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      0.2
_cell_volume                     8119.3(8)
_computing_cell_refinement       'Bruker SMART program'
_computing_data_collection       'Bruker SMART program'
_computing_data_reduction        'Bruker SMART program'
_computing_molecular_graphics    'Ortep-3 Ver.1.08'
_computing_publication_material  'enCIFer 1.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'transmittance with Laue geometry'
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            45922
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX CCD'
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         15
_exptl_absorpt_coefficient_mu    2.691
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal rod'
_exptl_crystal_F_000             4176.0
_exptl_crystal_recrystallization_method 'solvent evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                2569
_reflns_number_total             3295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg7012705-file003.cif
_cod_data_source_block           2(Tb)100K
_cod_depositor_comments
;
  Moved the _audit_creation_method data item out of the loop.

  Antanas Vaitkus,
  2019-03-01
;
_cod_database_code               4503535