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_7233226
_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'
_chemical_formula_sum            'C39 H49 Cu F6 N5 P'
_chemical_formula_weight         796.34
_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                 105.029(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.788(3)
_cell_length_b                   10.7257(15)
_cell_length_c                   19.777(3)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.24
_cell_volume                     3849.0(10)
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58630
_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         1.737
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1338 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.6519.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.127
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9548
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0508P)^2^+3.4600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7926
_reflns_number_total             9548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04886c2.cif
_cod_data_source_block           kg_1_75_fi_abs_r75
_cod_original_cell_volume        3849.1(9)
_cod_database_code               7233226
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.899
_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. Restrained distances
 C37-C38 \\sim C37-C39 \\sim C37A-C38A \\sim C37A-C39A
 with sigma of 0.02
3. Others
 Fixed Sof: C37(0.5) H37(0.5) C37A(0.5) H37A(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5) C38A(0.5) H38D(0.5) H38E(0.5) H38F(0.5) C39(0.5) H39A(0.5) H39B(0.5)
 H39C(0.5) C39A(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
4.a Ternary CH refined with riding coordinates:
 C18(H18), C25(H25), C34(H34), C37(H37), C37A(H37A)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C21(H21), C22(H22), C23(H23), C30(H30), C31(H31), C32(H32)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C39(H39A,H39B,H39C),
 C39A(H39D,H39E,H39F)
;
_olex2_submission_special_instructions 'No special instructions were received'