Highly emitting near-infrared lanthanide "encapsulated sandwich" metallacrown complexes with excitation shifted toward lower energy.
Trivedi, Evan R.; Eliseeva, Svetlana V.; Jankolovits, Joseph; Olmstead, Marilyn M.; Petoud, Stéphane; Pecoraro, Vincent L.; Journal of the American Chemical Society 136 (2014) 1526–1534; doi:10.1021/ja4113337

data_4121401
_publ_section_title
;
 Highly emitting near-infrared lanthanide &quot;encapsulated
 sandwich&quot; metallacrown complexes with excitation shifted toward
 lower energy.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1526
_journal_page_last               1534
_journal_paper_doi               10.1021/ja4113337
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C200 H136 Dy N40 O32 Zn16, 3(C F3 O3 S), 2(C4 H8 O2)'
_chemical_formula_sum            'C211 H152 Dy F9 N40 O45 S3 Zn16'
_chemical_formula_weight         5443.32
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           75
_space_group_name_Hall           'P 4'
_space_group_name_H-M_alt        'P 4'
_symmetry_space_group_name_Hall  'P 4'
_symmetry_space_group_name_H-M   'P 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'XT (Sheldrick, 2012)'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.4975(19)
_cell_length_b                   30.4975(19)
_cell_length_c                   13.3192(9)
_cell_measurement_reflns_used    9607
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.4
_cell_volume                     12388.2(14)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_publication_material  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            173993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.003
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             5466
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_refine_diff_density_max         3.006
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.330(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1506
_refine_ls_number_reflns         37814
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+8.2231P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                33073
_reflns_number_total             37814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4113337_si_002.cif
_cod_data_source_block           mn2138
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        12388.2(18)
_cod_database_code               4121401
_shelx_estimated_absorpt_t_min   0.615
_shelx_estimated_absorpt_t_max   0.677
_shelxl_version_number           2012-9
_shelx_res_checksum              48438
_shelx_hkl_checksum              32279