Synthesis, characterization, and photoluminescent studies of three-coordinate Cu(i)‒NHC complexes bearing unsymmetrically-substituted dipyridylamine ligands
Glinton, Kwame; Latifi, Reza; Cockrell, David S.; Bardeaux, Matthew; Nguyen, Bachkhoa; Tahsini, Laleh; RSC Advances 9 (2019) 22417–; doi:10.1039/C9RA04886C

data_7233225
_publ_section_title
;
 Synthesis, characterization, and photoluminescent studies of
 three-coordinate Cu(i)--NHC complexes bearing unsymmetrically-substituted
 dipyridylamine ligands
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              22417
_journal_paper_doi               10.1039/C9RA04886C
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C39 H49 Cu N5, F6 P, 0.5(C2 H3 N)'
_chemical_formula_sum            'C40 H50.5 Cu F6 N5.5 P'
_chemical_formula_weight         816.87
_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             2018-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-06 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2600(10)
_cell_length_b                   28.112(3)
_cell_length_c                   12.5861(11)
_cell_measurement_reflns_used    9500
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.32
_cell_volume                     3981.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            78856
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.449
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0930 before and 0.0494 after correction.
The Ratio of minimum to maximum transmission is 0.8451.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+4.4235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8336
_reflns_number_total             9866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04886c2.cif
_cod_data_source_block           kg_i_73_abs_fi_r75
_cod_original_cell_volume        3981.3(6)
_cod_original_formula_sum        'C40 H50.50 Cu F6 N5.50 P'
_cod_database_code               7233225
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: N6(0.5) C40(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C25(H25), C22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C32(H32), C30(H30), C29(H29), C36(H36), C37(H37), C38(H38), C3(H3A),
 C2(H2), C8(H8), C7(H7), C6(H6), C20(H20), C19(H19), C18(H18)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C39(H39A,H39B,H39C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C41(H41A,H41B,H41C)
;
_olex2_submission_special_instructions 'No special instructions were received'