A counterion study of a series of [Cu(P^P)(N^N)][A] compounds with bis(phosphane) and 6-methyl and 6,6'-dimethyl-substituted 2,2'-bipyridine ligands for light-emitting electrochemical cells
Meyer, Marco; Mardegan, Lorenzo; Tordera, Daniel; Prescimone, Alessandro; Sessolo, Michele; Bolink, Henk J.; Constable, Edwin C.; Housecroft, Catherine E.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03239A

data_7708686
_publ_section_title
;
 A counterion study of a series of [Cu(P^P)(N^N)][A] compounds with
 bis(phosphane) and 6-methyl and 6,6'-dimethyl-substituted 2,2'-bipyridine
 ligands for light-emitting electrochemical cells
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03239A
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C51 H44 Cu N2 O P2, F6 P'
_chemical_formula_sum            'C51 H44 Cu F6 N2 O P3'
_chemical_formula_weight         971.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-01 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7640(3)
_cell_length_b                   19.7573(3)
_cell_length_c                   22.6092(4)
_cell_measurement_reflns_used    57709
_cell_measurement_temperature    150
_cell_measurement_theta_max      56.78
_cell_measurement_theta_min      2.58
_cell_volume                     8828.5(2)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
X-Area X-Red32 1.65.0.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55800
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         56.649
_diffrn_reflns_theta_min         2.583
_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    3.715
_exptl_absorpt_correction_T_max  0.4593
_exptl_absorpt_correction_T_min  0.0074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SSTOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens 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, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.370(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         17467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+7.9905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                13131
_reflns_number_total             17467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03239a2.cif
_cod_data_source_block           mem042b_150k
_cod_database_code               7708686
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.606
_shelx_estimated_absorpt_t_min   0.482
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.630(6)
 0.370(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C92(H92), C67(H67), C66(H66), C65(H65), C35(H35), C47(H47), C14(H14),
 C16(H16), C69(H69), C15(H15), C71(H71), C68(H68), C81(H81), C88(H88), C75(H75),
  C9(H9), C48(H48), C18(H18), C34(H34), C4(H4), C79(H79), C30(H30), C86(H86),
 C53(H53), C33(H33), C17(H17), C98(H98), C20(H20), C95(H95), C21(H21), C49(H49),
  C41(H41), C50(H50), C51(H51), C80(H80), C28(H28), C29(H29), C24(H24),
 C99(H99), C58(H58), C96(H96), C94(H94), C93(H93), C72(H72), C102(H102),
 C87(H87), C45(H45), C7(H7), C8(H8), C22(H22), C44(H44), C100(H100), C2(H2),
 C55(H55), C54(H54), C59(H59), C73(H73), C42(H42), C60(H60), C3(H3), C101(H101),
  C74(H74), C43(H43), C23(H23)
3.b Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C39(H39A,H39B,H39C), C90(H90A,H90B,H90C), C38(H38A,H38B,
 H38C), C11(H11A,H11B,H11C), C63(H63A,H63B,H63C), C12(H12A,H12B,H12C), C89(H89A,
 H89B,H89C)
;
_shelx_res_checksum              8815
_shelx_hkl_checksum              55128
_olex2_date_sample_data_collection 2021-03-11
_olex2_date_sample_submission    2021-03-04
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
;
The crystal was mounted on a mylar loop in perfluoroether oil
;
_olex2_submission_original_sample_id MEM042
_olex2_submission_special_instructions 'No special instructions were received'