Tuning the Luminescent Properties of Pt(II) Acetylide Complexes through Varying the Electronic Properties of N-Heterocyclic Carbene Ligands.
Zhang, Yuzhen; Clavadetscher, Jessica; Bachmann, Michael; Blacque, Olivier; Venkatesan, Koushik; Inorganic chemistry 53 (2014) 756–771; doi:10.1021/ic401841n

data_4337105
_publ_section_title
;
 Tuning the Luminescent Properties of Pt(II) Acetylide Complexes through
 Varying the Electronic Properties of N-Heterocyclic Carbene Ligands.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              756
_journal_page_last               771
_journal_paper_doi               10.1021/ic401841n
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C31 H34 F2 N6 Pt), 3(C H4 O)'
_chemical_formula_sum            'C65 H80 F4 N12 O3 Pt2'
_chemical_formula_weight         1543.59
_chemical_name_systematic
;
bis(4-Fluorophenylethynyl)-(1,1'-dipentyl-3,3'-methylene-bis(1,2,4-triazoline)
-2,2'-diylidene)-platinum(II) methanol solvate 2/3
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-07-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                82.817(3)
_cell_angle_beta                 69.071(4)
_cell_angle_gamma                73.626(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8528(6)
_cell_length_b                   15.5714(5)
_cell_length_c                   17.8630(6)
_cell_measurement_reflns_used    10205
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.5
_cell_volume                     3451.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL2013, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS97, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9908
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34609
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.543
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.110
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12649
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0462P)^2^+3.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                8899
_reflns_number_total             12649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401841n_si_002.cif
_cod_data_source_block           2a_ccdc950236
_cod_database_code               4337105
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-C63 = O2-C64 = O3-C65 = O4-C66
 1.43 with sigma of 0.01
 C29-C30 = C30-C31
 1.53 with sigma of 0.01
 C58-C59 \\sim C59-C60
 with sigma of 0.005
 C60-C61A \\sim C60-C61B \\sim C61A-C62A \\sim C61B-C62B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C26 \\sim C25 \\sim C24: within 3A with sigma of 0.005 and sigma for terminal atoms of 0.01
C28 \\sim C29 \\sim C30: within 3A with sigma of 0.005 and sigma for terminal atoms of 0.01
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47: within 3A with sigma of 0.005 and sigma for terminal atoms of 0.01
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 3A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(C62A) = Uiso(C62B)
Uiso(C61A) = Uiso(C61B)
4. Others
 Fixed Sof: H60A(0.5) H60B(0.5) H60C(0.5) H60D(0.5) C61A(0.5) H61A(0.5)
 H61B(0.5) C61B(0.5) H61C(0.5) H61D(0.5) C62A(0.5) H62A(0.5) H62B(0.5)
 H62C(0.5) C62B(0.5) H62D(0.5) H62E(0.5) H62F(0.5) O3(0.75) H3(0.75) O4(0.5)
 H4A(0.5) C65(0.75) H65A(0.75) H65B(0.75) H65C(0.75) C66(0.5) H66A(0.5)
 H66B(0.5) H66C(0.5) O1(0.75) H1(0.75) C63(0.75) H63A(0.75) H63B(0.75)
 H63C(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C50(H50A,H50B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
  C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C60(H60C,H60D), C61A(H61A,
 H61B), C61B(H61C,H61D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16),
 C18(H18), C21(H21), C35(H35), C36(H36), C38(H38), C39(H39), C43(H43), C44(H44),
  C46(H46), C47(H47), C49(H49), C52(H52)
5.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O3(H3), O4(H4A), O1(H1)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C57(H57A,H57B,H57C), C62A(H62A,H62B,
 H62C), C62B(H62D,H62E,H62F), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C63(H63A,H63B,H63C)
;
_shelxl_version_number           2013-4