Copper(i) ionic complexes based on imidazo[4,5-f][1,10]phenanthrolin diimine chelating ligands: crystal structures, and photo- and electroluminescence properties
Rozhkov, Anton V.; Eliseeva, Svetlana N.; Baykov, Sergey V.; Zelenkov, Lev E.; Goriachiy, Dmitry O.; Taydakov, Ilya V.; New Journal of Chemistry 44 (2020) 110–120; doi:10.1039/C9NJ05109K

data_7059142
_publ_section_title
;
 Copper(i) ionic complexes based on imidazo[4,5-f][1,10]phenanthrolin
 diimine chelating ligands: crystal structures, and photo- and
 electroluminescence properties
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              110
_journal_page_last               120
_journal_paper_doi               10.1039/C9NJ05109K
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C55 H39 Cl Cu N4 O2 P2, C H2 Cl2, B F4'
_chemical_formula_sum            'C56 H41 B Cl3 Cu F4 N4 O2 P2'
_chemical_formula_weight         1120.57
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-20 deposited with the CCDC.	2019-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.279(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4377(5)
_cell_length_b                   15.4971(3)
_cell_length_c                   20.1990(5)
_cell_measurement_reflns_used    10361
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.3730
_cell_measurement_theta_min      3.2560
_cell_volume                     5443.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -21.00   35.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   38.0000 -180.0000 56

  2 omega  -87.00   47.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241    0.0000  -30.0000 134

  3 omega  -49.00   39.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -38.0000  -30.0000 88

  4 omega  -56.00  -23.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241    0.0000  -90.0000 33

  5 omega    3.00   49.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   38.0000   30.0000 46

  6 omega  -97.00  -67.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241 -178.0000   90.0000 30

  7 omega  -98.00  -73.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241 -178.0000    0.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0219559000
_diffrn_orient_matrix_UB_12      -0.0281332000
_diffrn_orient_matrix_UB_13      0.0216550000
_diffrn_orient_matrix_UB_21      -0.0249448000
_diffrn_orient_matrix_UB_22      0.0084764000
_diffrn_orient_matrix_UB_23      0.0254153000
_diffrn_orient_matrix_UB_31      -0.0236494000
_diffrn_orient_matrix_UB_32      -0.0350909000
_diffrn_orient_matrix_UB_33      -0.0111925000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43848
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.615
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         12469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0716P)^2^+15.6689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9940
_reflns_number_total             12469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05109k2.cif
_cod_data_source_block           8344-11196_rav-249
_cod_depositor_comments
;Adding full bibliography for 7059140--7059142.cif.

 Adding full bibliography for 7059140--7059142.cif.
;
_cod_database_code               7059142
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C55 B Cu F4 N4 O2 P2'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C7(H7), C27(H27), C8(H8), C1(H1), C9(H9), C31(H31), C39(H39),
 C28(H28), C49(H49), C2(H2A), C55(H55), C3(H3A), C29(H29), C51(H51), C21(H21),
 C30(H30), C48(H48), C42(H42), C33(H33), C15(H15), C17(H17), C18(H18), C36(H36),
  C53(H53), C54(H54), C52(H52), C25(H25), C45(H45), C40(H40), C34(H34),
 C35(H35), C47(H47), C41(H41), C46(H46), C22(H22), C24(H24), C23(H23)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              12433
_shelx_fab_checksum              33925
_olex2_submission_special_instructions 'No special instructions were received'