Structural characterization, DFT studies and luminescent properties of dinuclear copper(I)-diimine complexes with the S-shape configurations
Zheng, Dan; Huang, Ting-Hong; Luo, Cheng; Tang, Jing; Inorganica Chimica Acta 529 (2022) 120639–; doi:10.1016/j.ica.2021.120639

data_1565969
_publ_section_title
;
 Structural characterization, DFT studies and luminescent properties of
 dinuclear copper(I)-diimine complexes with the S-shape configurations
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120639
_journal_paper_doi               10.1016/j.ica.2021.120639
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C94 H76 Cu2 N4 P4, 2(B F4)'
_chemical_formula_sum            'C94 H76 B2 Cu2 F8 N4 P4'
_chemical_formula_weight         1686.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_cell_angle_alpha                61.869(10)
_cell_angle_beta                 70.792(11)
_cell_angle_gamma                66.806(11)
_cell_formula_units_Z            1
_cell_length_a                   13.074(8)
_cell_length_b                   14.786(9)
_cell_length_c                   14.943(9)
_cell_measurement_reflns_used    2346
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.54
_cell_measurement_theta_min      2.53
_cell_volume                     2305(2)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.1186
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14199
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.405
_diffrn_reflns_theta_min         1.570
_diffrn_source_current           30.0
_diffrn_source_power             1.44
_diffrn_source_voltage           48.0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10566
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1840
_refine_ls_R_factor_gt           0.0827
_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^)+(0.1755P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2472
_refine_ls_wR_factor_ref         0.3117
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4421
_reflns_number_total             10566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1-complex1.cif
_cod_data_source_block           1
_cod_database_code               1565969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F3A
 1.32 with sigma of 0.02
3. Rigid bond restraints
 F4, B1, F2, F3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C39(H39), C40(H40), C42(H42), C43(H43), C46(H46), C47(H47)
;
_shelx_res_checksum              16335
_shelx_hkl_checksum              56886
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20