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_7233223
_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 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-06-19 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.180(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.6743(14)
_cell_length_b                   40.711(6)
_cell_length_c                   20.576(3)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.19
_cell_volume                     8000(2)
_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  0.0377
_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       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            131738
_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         28.700
_diffrn_reflns_theta_min         1.000
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0833 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.8620.
The \l/2 correction factor is Not present.
;
_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    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         20652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0267P)^2^+10.5732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18119
_reflns_number_total             20652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04886c2.cif
_cod_data_source_block           mb_ii_49_r74_fi_abs
_cod_database_code               7233223
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C22(H22), C64(H64), C25(H25), C13(H13), C61(H61), C49(H49), C52(H52), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8A), C42(H42), C19(H19), C3(H3A), C35(H35), C18(H18), C7(H7),
 C59(H59), C74(H74), C20(H20), C30(H30), C6(H6), C58(H58), C38(H38), C77(H77),
 C45(H45), C46(H46), C47(H47), C70(H70), C76(H76), C41(H41), C2(H2), C32(H32),
 C57(H57), C71(H71), C31(H31), C69(H69), C37(H37), C8(H8)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C72(H72A,H72B,H72C), C65(H65A,H65B,
 H65C), C39(H39A,H39B,H39C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C50(H50A,
 H50B,H50C), C78(H78A,H78B,H78C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C66(H66A,H66B,H66C), C63(H63A,H63B,H63C), C62(H62A,H62B,
 H62C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C11(H11A,
 H11B,H11C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              64380
_shelx_fab_checksum              61129
_olex2_submission_special_instructions 'No special instructions were received'