Highly soluble fluorine containing Cu(i) AlkylPyrPhos TADF complexes.
Busch, Jasmin M.; Zink, Daniel M.; Di Martino-Fumo, Patrick; Rehak, Florian R.; Boden, Pit; Steiger, Sophie; Fuhr, Olaf; Nieger, Martin; Klopper, Wim; Gerhards, Markus; Bräse, Stefan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15687–15698; doi:10.1039/c9dt02447f

data_7700898
_publ_section_title
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 Highly soluble fluorine containing Cu(i) AlkylPyrPhos TADF complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15687
_journal_page_last               15698
_journal_paper_doi               10.1039/c9dt02447f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C59 H48 Cu2 F6 I2 N P3, C H2 Cl2'
_chemical_formula_sum            'C60 H50 Cl2 Cu2 F6 I2 N P3'
_chemical_formula_weight         1443.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-28 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.373(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1297(5)
_cell_length_b                   12.6256(2)
_cell_length_c                   25.3784(6)
_cell_measurement_reflns_used    97656
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      63.59
_cell_measurement_theta_min      4.31
_cell_volume                     5708.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38804
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        62.495
_diffrn_reflns_theta_max         62.495
_diffrn_reflns_theta_min         4.306
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.566
_exptl_absorpt_correction_T_max  0.0758
_exptl_absorpt_correction_T_min  0.0187
_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.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       needle
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+51.3246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8926
_reflns_number_total             9040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02447f2.cif
_cod_data_source_block           jmb83-15
_cod_depositor_comments
'Adding full bibliography for 7700890--7700898.cif.'
_cod_database_code               7700898
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.119
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H8AA(0.5) H8AB(0.5) H8BC(0.5) H8BD(0.5) C9A(0.5)
 H9AA(0.5) H9AB(0.5) C10A(0.5) H10A(0.5) H10B(0.5) C11A(0.5) H11A(0.5)
 H11B(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) C10B(0.5) H10C(0.5) H10D(0.5) C11B(0.5)
 H11C(0.5) H11D(0.5)
3.a Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8AA,H8AB), C8(H8BC,H8BD), C9A(H9AA,H9AB), C10A(H10A,H10B),
 C11A(H11A,H11B), C9B(H9BA,H9BB), C10B(H10C,H10D), C11B(H11C,H11D), C60(H60A,
 H60B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50),
  C52(H52), C53(H53), C55(H55), C56(H56), C58(H58), C59(H59)
;
_shelx_res_checksum              95144
_olex2_submission_special_instructions 'No special instructions were received'