Rigid, Perdeuterated Lanthanoid Cryptates: Extraordinarily Bright Near-IR Luminophores.
Christine Doffek; Nicola Alzakhem; Mariusz Molon; Michael Seitz; Inorganic Chemistry 51 (2012) 4539–4545; doi:10.1021/ic202376k

data_4328895
_publ_section_title
;
 Rigid, Perdeuterated Lanthanoid Cryptates: Extraordinarily Bright Near-IR
 Luminophores.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4539
_journal_page_last               4545
_journal_paper_doi               10.1021/ic202376k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C36 H30 Cl Lu N8 O2, 2(Cl), C H4 O, C4 H10 O'
_chemical_formula_sum            'C41 H44 Cl3 Lu N8 O4'
_chemical_formula_weight         994.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            18
_cell_length_a                   37.0817(8)
_cell_length_b                   37.0817(8)
_cell_length_c                   16.1486(5)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    107.5
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.91
_cell_volume                     19230.2(8)
_computing_cell_refinement       'CrysAlis RED 171_33_34d, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 171_33_34d, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 171_33_34d, Oxford Diffraction'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      107.5
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur^TM^2, Oxford Diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27369
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   abspack
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       needle
_exptl_crystal_F_000             9000
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_platon_squeeze_details
; 
 The unit cell contains voids with highly disordered solvent molecules. 
 The residual electron density, as well as the volume, suggest the 
 presence of one methanol and one diethylether molecule per formula unit.  
 These solvents have been treated as diffuse contribution to the scattering 
 without the assignent of precise positional parameters by the SQUEEZE 
 routine of PLATON 
;
_refine_diff_density_max         3.636
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0601
_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^)+(0.1188P)^2^+169.7072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1900
_reflns_number_gt                5875
_reflns_number_total             7564
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202376k_si_002.cif
_cod_data_source_block           bpy3o2-lu
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4328895