Sm and Eu(iii) lanthanide triple helicate cages based on N,N′-methylene-bis(pyridin-4-one)
Shu, Yu-Bo; Tang, Xiao-Liang; Liu, Wei-Sheng; Inorg. Chem. Front. 1 (2014) 226–; doi:10.1039/C3QI00089C

data_4350764
_publ_section_title
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 Sm and Eu(iii) lanthanide triple helicate cages based on
 N,N&#x2032;-methylene-bis(pyridin-4-one)
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_journal_issue                   3
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              226
_journal_paper_doi               10.1039/C3QI00089C
_journal_volume                  1
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H31.98 N12 O25 Sm2'
_chemical_formula_sum            'C33 H31.98 N12 O25 Sm2'
_chemical_formula_weight         1297.41
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.3524(7)
_cell_length_b                   14.3524(7)
_cell_length_c                   19.1378(8)
_cell_measurement_reflns_used    3450
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.67
_cell_measurement_theta_min      2.69
_cell_volume                     3414.1(3)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8084
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.658
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0544 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.9335.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1913.9
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2668
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0389
_reflns_number_gt                2527
_reflns_number_total             2668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00089c.txt
_cod_data_source_block           syb20121027_1_0m
_cod_original_cell_volume        3414.1(4)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4350764
_olex2_refinement_description
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1. Others
 Fixed Sof: H6A(0.33) H3(0.33)
 Fixed U13: Sm2(0) Sm1(0) O6(0)
 Fixed U23: Sm2(0) Sm1(0) O6(0)
 Fixed Uiso: H2(0.039) H11(0.038) H14(0.038) H23(0.042) H25A(0.043)
 H25B(0.043) H9(0.044) H15(0.048) H21(0.048) H1(0.049) H6A(0.098) H3(0.098)
 Fixed X: Sm2(0.3333) Sm1(0.3333) H2(0.3143) H11(-0.0051) H14(0.0969)
 H23(0.2043) H25A(-0.0448) H25B(0.0094) H9(0.1002) H15(0.0647) H21(0.1808)
 H1(0.143) O6(0.3333) H6A(0.3288) H3(0.3935)
 Fixed Y: Sm2(0.6667) Sm1(0.6667) H2(0.4382) H11(0.4388) H14(0.5184)
 H23(0.3576) H25A(0.338) H25B(0.2669) H9(0.2831) H15(0.5277) H21(0.3668)
 H1(0.6162) O6(0.6667) H6A(0.7223) H3(0.6712)
 Fixed Z: H2(0.1302) H11(0.1069) H14(0.2021) H23(0.0382) H25A(0.0082)
 H25B(0.0002) H9(-0.0992) H15(-0.0431) H21(-0.2016) H1(-0.144) H6A(0.4697)
 H3(0.4697)
;