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_7700895
_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         'C54 H40 Cu2 F6 I2 N P3, C5 H12'
_chemical_formula_sum            'C59 H52 Cu2 F6 I2 N P3'
_chemical_formula_weight         1362.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2019-05-28 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 102.080(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9997(6)
_cell_length_b                   12.9197(5)
_cell_length_c                   23.7991(6)
_cell_measurement_reflns_used    50057
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      73.18
_cell_measurement_theta_min      3.34
_cell_volume                     5712.6(3)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_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  0.1121
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22256
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        64.000
_diffrn_reflns_theta_max         64.000
_diffrn_reflns_theta_min         3.340
_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    10.677
_exptl_absorpt_correction_T_max  0.3089
_exptl_absorpt_correction_T_min  0.0177
_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.
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    1.585
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.411
_refine_diff_density_min         -4.412
_refine_diff_density_rms         0.413
_refine_ls_extinction_coef       0.00124(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         9312
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.1216
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2920
_refine_ls_wR_factor_ref         0.2999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7879
_reflns_number_total             9312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02447f2.cif
_cod_data_source_block           jmb057
_cod_depositor_comments
'Adding full bibliography for 7700890--7700898.cif.'
_cod_database_code               7700895
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.675
_shelx_estimated_absorpt_t_min   0.280
_olex2_refinement_description
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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
 C56-C55 = C57-C56 = C58-C57 = C59-C58
 1.54 with sigma of 0.02
 C55-C57
 2.51 with sigma of 0.02
 C56-C58
 2.51 with sigma of 0.02
 C57-C59
 2.51 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
3.b Me refined with riding coordinates:
 C55(H55A,H55B,H55C), C59(H59A,H59B,H59C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), 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), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33),
 C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45),
  C47(H47), C48(H48), C50(H50), C51(H51), C53(H53), C54(H54)
3.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
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_shelx_res_checksum              41800
_olex2_submission_special_instructions 'No special instructions were received'