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_7700892
_publ_section_title
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 Highly soluble fluorine containing Cu(i) AlkylPyrPhos TADF complexes.
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_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         'C60 H39 Cu2 F18 I2 N P3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C60.5 H40 Cl Cu2 F18 I2 N P3'
_chemical_formula_weight         1632.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2019-05-28 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
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_cell_angle_alpha                90.236(4)
_cell_angle_beta                 106.170(5)
_cell_angle_gamma                116.415(4)
_cell_formula_units_Z            2
_cell_length_a                   15.2045(10)
_cell_length_b                   15.6811(6)
_cell_length_c                   15.7442(10)
_cell_measurement_reflns_used    44303
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      59.49
_cell_measurement_theta_min      2.57
_cell_volume                     3192.9(4)
_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                 EIGER4M
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0150
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24934
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        52.991
_diffrn_reflns_theta_max         52.991
_diffrn_reflns_theta_min         2.976
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              Metaljet
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    9.932
_exptl_absorpt_correction_T_max  0.6070
_exptl_absorpt_correction_T_min  0.2013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.665
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00015(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         10843
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0655P)^2^+7.2791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9479
_reflns_number_total             10843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02447f2.cif
_cod_data_source_block           jmb053
_cod_depositor_comments
'Adding full bibliography for 7700890--7700898.cif.'
_cod_original_cell_volume        3192.9(3)
_cod_original_formula_sum        'C60.50 H40 Cl Cu2 F18 I2 N P3'
_cod_database_code               7700892
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.219
_shelx_estimated_absorpt_t_min   0.199
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-Cl2
 2.9 with sigma of 0.02
 Cl1-C61 = Cl2-C61
 1.76 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl1 \\sim C61: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Fixed Sof: F4A(0.5) F5A(0.5) F6A(0.5) F7A(0.5) F8A(0.5) F9A(0.5) F10A(0.5)
 F11A(0.5) F12A(0.5) F4B(0.5) F5B(0.5) F6B(0.5) F7B(0.5) F8B(0.5) F9B(0.5)
 F10B(0.5) F11B(0.5) F12B(0.5) Cl2(0.5) C61(0.5) H61A(0.5) H61B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
  C27(H27), C28(H28), C30(H30), C31(H31), C34(H34), C35(H35), C37(H37),
 C38(H38), C41(H41), C42(H42), C44(H44), C45(H45), C48(H48), C49(H49), C51(H51),
  C52(H52), C55(H55), C56(H56), C58(H58), C59(H59)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
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_shelx_res_checksum              59954
_olex2_submission_special_instructions 'No special instructions were received'