The shiny side of copper: bringing copper(i) light-emitting electrochemical cells closer to application
Keller, Sarah; Prescimone, Alessandro; La Placa, Maria-Grazia; Junquera-Hernández, José M.; Bolink, Henk J.; Constable, Edwin C.; Sessolo, Michele; Ortí, Enrique; Housecroft, Catherine E.; RSC Advances 10 (2020) 22631–22644; doi:10.1039/D0RA03824E

data_7240739
_publ_section_title
;
 The shiny side of copper: bringing copper(i) light-emitting
 electrochemical cells closer to application
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              22631
_journal_page_last               22644
_journal_paper_doi               10.1039/D0RA03824E
_journal_volume                  10
_journal_year                    2020
_chemical_compound_source        'Sarah Keller'
_chemical_formula_moiety         '[C52 H46 Cu1 F6 N2 O1 P3] + 2.33(CH2Cl2)'
_chemical_formula_sum            'C54.33 H50.66 Cl4.66 Cu F6 N2 O P3'
_chemical_formula_weight         1183.30
_chemical_melting_point          ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2018-12-12
_audit_creation_method           CRYSTALS_ver_14.61_build_7031
_audit_update_record
;
2020-01-17 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                113.589(2)
_cell_angle_beta                 92.960(2)
_cell_angle_gamma                108.444(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8055(3)
_cell_length_b                   15.0529(4)
_cell_length_c                   18.6132(5)
_cell_measurement_reflns_used    137380
_cell_measurement_temperature    130
_cell_measurement_theta_max      57.55
_cell_measurement_theta_min      2.31
_cell_volume                     2814.51(15)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      130
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            99434
_diffrn_reflns_theta_full        54.000
_diffrn_reflns_theta_max         57.350
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.312
_exptl_absorpt_correction_T_max  0.7598
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1211.72
_exptl_crystal_recrystallization_method
; 
DCM / Et2O
;
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
this equates to 98 e-/formula unit which can be rationalised with 2.33(CH2Cl2)
per formula unit.
ALL the numbers and formulae have been already modified to keep this result in
account.
;
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.71
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10798
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.0004854
_refine_ls_shift/su_mean         0.0000406
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3222
_refine_ls_wR_factor_gt          0.2929
_refine_ls_wR_factor_ref         0.3106
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6531
_reflns_number_total             10831
_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   0.1239
_oxford_refine_ls_scale          0.3401(8)
_oxford_reflns_number_all        10831
_oxford_structure_analysis_title 'SK213B_130K in P-1'
_cod_data_source_file            d0ra03824e2.cif
_cod_data_source_block           SK213B_130K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7240738--7240744.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C54.33 H50.66 Cl4.66 Cu1 F6 N2 O1 P3'
_cod_database_code               7240739
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)