Tuning the photophysical properties of lanthanide(iii)/zinc(ii) 'encapsulated sandwich' metallacrowns emitting in the near-infrared range.
Eliseeva, Svetlana V.; Nguyen, Tu N.; Kampf, Jeff W.; Trivedi, Evan R.; Pecoraro, Vincent L.; Petoud, Stéphane; Chemical science 13 (2022) 2919–2931; doi:10.1039/d1sc06769a

data_1566278
_publ_section_title
;
 Tuning the photophysical properties of lanthanide(iii)/zinc(ii)
 'encapsulated sandwich' metallacrowns emitting in the near-infrared
 range.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2919
_journal_page_last               2931
_journal_paper_doi               10.1039/d1sc06769a
_journal_volume                  13
_journal_year                    2022
_chemical_formula_sum            'C187 H120 F9 N62 Nd O57.5 S3 Zn16'
_chemical_formula_weight         5612.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.7978(4)
_cell_length_b                   29.7978(4)
_cell_length_c                   27.5410(19)
_cell_measurement_reflns_used    129624
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      73.4200
_cell_measurement_theta_min      2.9480
_cell_volume                     24453.9(17)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            472686
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.076
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    4.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             11056
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         12397
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1476P)^2^+15.3928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11558
_reflns_number_total             12397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06769a2.cif
_cod_data_source_block           tn1177a_sq
_cod_depositor_comments
'Adding full bibliography for 1566278--1566279.cif.'
_cod_original_cell_volume        24453.9(18)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C187 H120 F9 N62 Nd O57.50 S3 Zn16'
_cod_database_code               1566278
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.493
_shelx_estimated_absorpt_t_max   0.597
_shelx_res_checksum              57558
_shelx_hkl_checksum              24771
_shelx_fab_checksum              87916