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_4337104
_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(C41 H42 N4 Pt), 0.5(C H2 Cl2), 0.5(C5 H12)'
_chemical_formula_sum            'C85 H91 Cl N8 Pt2'
_chemical_formula_weight         1650.28
_chemical_name_systematic
;
bis(Phenylethynyl)-(1,1'-dipentyl-3,3'-methylene-bis(benzimidazoline)
-2,2'-diylidene)-platinum(II) dichloromethane pentane solvate 4/1/1
;
_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
_audit_creation_date             2013-07-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.494(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9885(7)
_cell_length_b                   25.6500(8)
_cell_length_c                   19.5345(9)
_cell_measurement_reflns_used    11787
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.9
_cell_measurement_theta_min      2.7
_cell_volume                     7746.2(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0863
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60100
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.691
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.442
_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    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.953
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         15828
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0518P)^2^+62.9050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                11015
_reflns_number_total             15828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401841n_si_002.cif
_cod_data_source_block           1b_ccdc950235
_cod_database_code               4337104
_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
2. Restrained distances
 C84-C85 = C85-C86 = C86-C87 = C87-C88
 1.52 with sigma of 0.01
 C78-C79A = C78-C79B = C79A-C80A = C79B-C80B
 1.52 with sigma of 0.01
 C80A-C81A = C80B-C81B = C81A-C82A = C81B-C82B
 1.52 with sigma of 0.01
 C73-C74A = C73-C74B = C74A-C75A = C74B-C75B
 1.52 with sigma of 0.01
 C75A-C76A = C76A-C77A = C75B-C76B = C76B-C77B
 1.52 with sigma of 0.01
 C84-C86 = C85-C87 = C86-C88
 2.53 with sigma of 0.02
 C78-C80A = C78-C80B = C79A-C81A = C80A-C82A = C79B-C81B = C80A-C82B
 2.53 with sigma of 0.02
 C73-C75A = C73-C75B = C74A-C76A = C74B-C76B
 2.53 with sigma of 0.02
 C75A-C77A = C75B-C77B
 2.53 with sigma of 0.02
 C74A-C75A \\sim C75A-C76A \\sim C76A-C77A
 with sigma of 0.005
 C73-C75A \\sim C74A-C76A \\sim C75A-C77A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 3A with sigma of
 0.005 and sigma for terminal atoms of 0.01
C83 \\sim Cl1 \\sim Cl2: within 3A with sigma of 0.005 and sigma for terminal
 atoms of 0.01
Uiso(C3B) = Uiso(C4B) = Uiso(C5B) = Uiso(C6B) = Uiso(C7B) = Uiso(C8B)
Uiso(C2A) = Uiso(C2B)
Uiso(C3A) = Uiso(C4A) = Uiso(C5A) = Uiso(C6A) = Uiso(C7A) = Uiso(C8A)
Uiso(C79A) = Uiso(C79B) = Uiso(C80A) = Uiso(C80B) = Uiso(C81A) = Uiso(C81B) =
 Uiso(C82A) = Uiso(C82B)
Uiso(C84) = Uiso(C85) = Uiso(C86) = Uiso(C87) = Uiso(C88)
Uiso(C74A) = Uiso(C74B)
Uiso(C75A) = Uiso(C75B)
Uiso(C76A) = Uiso(C76B)
Uiso(C77A) = Uiso(C77B)
4. Others
 Sof(H78C)=Sof(H78D)=Sof(C79B)=Sof(H79C)=Sof(H79D)=Sof(C80B)=Sof(H80C)=
 Sof(H80D)=Sof(C81B)=Sof(H81C)=Sof(H81D)=Sof(C82B)=Sof(H82D)=Sof(H82E)=
 Sof(H82F)=1-FVAR(1)
 Sof(H78A)=Sof(H78B)=Sof(C81A)=Sof(H81A)=Sof(H81B)=Sof(C82A)=Sof(H82A)=
 Sof(H82B)=Sof(H82C)=Sof(C80A)=Sof(H80A)=Sof(H80B)=Sof(C79A)=Sof(H79A)=
 Sof(H79B)=FVAR(1)
 Sof(H73C)=Sof(H73D)=Sof(C77B)=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C76B)=
 Sof(H76C)=Sof(H76D)=Sof(C75B)=Sof(H75C)=Sof(H75D)=Sof(C74B)=Sof(H74C)=
 Sof(H74D)=1-FVAR(2)
 Sof(H73A)=Sof(H73B)=Sof(C74A)=Sof(H74A)=Sof(H74B)=Sof(C75A)=Sof(H75A)=
 Sof(H75B)=Sof(C76A)=Sof(H76A)=Sof(H76B)=Sof(C77A)=Sof(H77A)=Sof(H77B)=
 Sof(H77C)=FVAR(2)
 Sof(C3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=
 Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C2B)=1-FVAR(3)
 Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=FVAR(3)
 Fixed Sof: Cl1(0.5) Cl2(0.5) C83(0.5) H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5)
 H84B(0.5) H84C(0.5) C85(0.5) H85A(0.5) H85B(0.5) C86(0.5) H86A(0.5) H86B(0.5)
 C87(0.5) H87A(0.5) H87B(0.5) C88(0.5) H88A(0.5) H88B(0.5) H88C(0.5)
5.a :
 C3A(C4A,C5A,C6A,C7A,C8A,C9,C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,C21,
 C22,C23,C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,C35,C36,C37,C38,C39,C40,
 C41,C42,C43,C44,C45,C46,C47,C48,C49,C50,C51,C52,C53,C54,C55,C56,C57,C58,C59,
 C60,C61,C62,C63,C64,C65,C66,C67,C68,C69,C70,C71,C72,C73,C74A,C75A,C76A,C77A,
 C78,C81A,C82A,C80A,N1,N2,N3,N4,N5,N6,N7,N8,Pt1,Pt2,Cl1,Cl2,C83,C84,C85,C86,C87,
 C88,C79A,C79B,C80B,C81B,C82B,C77B,C76B,C75B,C74B), C3B(C4B,C5B,C6B,C7B,C8B,C2B)
5.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C65(H65A,H65B), C73(H73A,H73B), C73(H73C,H73D), C74A(H74A,H74B), C75A(H75A,
 H75B), C76A(H76A,H76B), C78(H78A,H78B), C78(H78C,H78D), C81A(H81A,H81B),
 C80A(H80A,H80B), C83(H83A,H83B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C79A(H79A,H79B), C79B(H79C,H79D), C80B(H80C,H80D), C81B(H81C,H81D),
 C76B(H76C,H76D), C75B(H75C,H75D), C74B(H74C,H74D)
5.c Me refined with riding coordinates:
 C82A(H82A,H82B,H82C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C)
5.d Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27),
  C28(H28), C29(H29), C30(H30), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C60(H60), C61(H61),
  C62(H62), C63(H63), C68(H68), C69(H69), C70(H70), C71(H71), C4B(H4B),
 C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B)
5.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C77A(H77A,H77B,H77C), C82B(H82D,
 H82E,H82F), C77B(H77D,H77E,H77F)
;
_shelxl_version_number           2013-4