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_4350765
_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 Eu2 N12 O25'
_chemical_formula_sum            'C33 H31.98 Eu2 N12 O25'
_chemical_formula_weight         1300.63
_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             2013-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.359(2)
_cell_length_b                   14.359(2)
_cell_length_c                   19.115(4)
_cell_measurement_reflns_used    805
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.00
_cell_measurement_theta_min      2.69
_cell_volume                     3413.1(10)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5775
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.834
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0576 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.8486.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1919.9
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2690
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+162.9368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                2014
_reflns_number_total             2690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00089c.txt
_cod_data_source_block           syb121208a_0m
_cod_original_cell_volume        3413.1(14)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4350765
_olex2_refinement_description
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1. Others
 Fixed Sof: H3A(0.33) H3(0.33)
 Fixed U13: Eu2(0) Eu1(0) O3(0)
 Fixed U23: Eu2(0) Eu1(0) O3(0)
 Fixed Uiso: H1(0.07) H2(0.099) H4(0.136) H5(0.098) H6A(0.061) H6B(0.061)
 H7(0.083) H8(0.115) H10(0.112) H11(0.07) H3A(0.116) H3(0.116)
 Fixed X: H1(0.503) H2(0.5225) H4(0.2302) H5(0.2159) H6A(0.2679) H6B(0.393)
 H7(0.4718) H8(0.4626) H10(0.1904) H11(0.1786) Eu2(0.3333) Eu1(0.3333)
 O3(0.3333) H3A(0.3874) H3(0.3407)
 Fixed Y: H1(0.9676) H2(0.895) H4(0.8213) H5(0.9029) H6A(0.9854) H6B(1.0578)
 H7(1.0307) H8(0.9423) H10(0.6973) H11(0.803) Eu2(0.6667) Eu1(0.6667)
 O3(0.6667) H3A(0.6593) H3(0.7281)
 Fixed Z: H1(0.4615) H2(0.3588) H4(0.2946) H5(0.3925) H6A(0.4919) H6B(0.5005)
 H7(0.5996) H8(0.7016) H10(0.6349) H11(0.5464) H3A(0.0304) H3(0.0304)
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