Highly Stable Red-Light-Emitting Electrochemical Cells.
Ertl, Cathrin D.; Momblona, Cristina; Pertegás, Antonio; Junquera-Hernández, José M; La-Placa, Maria-Grazia; Prescimone, Alessandro; Ortí, Enrique; Housecroft, Catherine E.; Constable, Edwin C.; Bolink, Henk J.; Journal of the American Chemical Society 139 (2017) 3237–3248; doi:10.1021/jacs.6b13311

data_4125560
_publ_section_title
;
 Highly Stable Red-Light-Emitting Electrochemical Cells.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3237
_journal_page_last               3248
_journal_paper_doi               10.1021/jacs.6b13311
_journal_volume                  139
_journal_year                    2017
_chemical_compound_source        'Cathrin Ertl'
_chemical_formula_moiety         '[C34 H24 F6 Ir1 N4 P1 S1].1.5CH2Cl2'
_chemical_formula_sum            'C35.5 H27 Cl3 F6 Ir N4 P S'
_chemical_formula_weight         985.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-13
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 106.359(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4951(15)
_cell_length_b                   13.7676(14)
_cell_length_c                   18.7348(19)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    123
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3
_cell_volume                     3587.4(6)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33781
_diffrn_reflns_theta_full        66.530
_diffrn_reflns_theta_max         66.534
_diffrn_reflns_theta_min         3.177
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.8
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.82
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_recrystallization_method
; 
DCM / Et2O 
;
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
this makes 253 e-/cell: it equates to 63.25 e-/formula unit.
it corresponds to 1.5 DCM per formula.
all the numbers and formulae have been corrected to take account for this result
;
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.0007993
_refine_ls_shift/su_mean         0.0000289
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.11 6.21 2.97 0.757 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0547
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0547
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6169
_reflns_number_total             6209
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0244
_oxford_refine_ls_scale          0.057516(5)
_oxford_reflns_number_all        6184
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'ce352_123K_0m in P2(1)/c'
_cod_data_source_file            ja6b13311_si_001.cif
_cod_data_source_block           CE352_123K
_cod_depositor_comments          'Adding full bibliography for 4125560.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C35.50 H27 Cl3 F6 Ir1 N4 P1 S1'
_cod_database_code               4125560