Uniting Ruthenium(II) and Platinum(II) Polypyridine Centers in Heteropolymetallic Complexes Giving Strong Two-Photon Absorption.
Shi, Pengfei; Coe, Benjamin J.; Sánchez, Sergio; Wang, Daqi; Tian, Yupeng; Nyk, Marcin; Samoc, Marek; Inorganic chemistry 54 (2015) 11450–11456; doi:10.1021/acs.inorgchem.5b02089

data_4346766
_publ_section_title
;
 Uniting Ruthenium(II) and Platinum(II) Polypyridine Centers in
 Heteropolymetallic Complexes Giving Strong Two-Photon Absorption.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11450
_journal_page_last               11456
_journal_paper_doi               10.1021/acs.inorgchem.5b02089
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C150 H108 N30 Pt6 Ru, 13(F6 P), 10(C2 N), N O3'
_chemical_formula_sum            'C170 H108 F78 N41 O3 P13 Pt6 Ru'
_chemical_formula_weight         5929.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-20
_audit_creation_method
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
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_cell_angle_alpha                90
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_cell_measurement_reflns_used    5272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.0360
_cell_measurement_theta_min      2.8370
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.534
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
  1 omega   82.21  268.21   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8669  124.2087 186

  2 phi    -25.79  333.43   1.0006   59.9980
omega____ theta____ kappa____ phi______ frames
 130.5397  110.0000   73.8669     -     359

  3 phi    -23.50  313.71   1.0006   59.9980
omega____ theta____ kappa____ phi______ frames
-135.7903  111.0000   73.8669     -     337

  4 phi    -25.79  333.43   1.0006   59.9980
omega____ theta____ kappa____ phi______ frames
  91.4694  110.0000   73.8669     -     359

  5 omega  -73.67   56.33   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -45.0000   73.8669    9.2081 130

  6 phi    -25.79  258.39   1.0006   59.9980
omega____ theta____ kappa____ phi______ frames
 114.2097  112.0000   73.8669     -     284

  7 omega  118.99  232.99   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8669   39.2088 114

  8 omega   87.57  210.57   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669 -125.7919 123

  9 omega  -70.42   10.58   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -80.0000   73.8669  174.2088 81

 10 phi     53.79  168.86   1.0006   25.0000
omega____ theta____ kappa____ phi______ frames
   6.0794  -65.0000   73.8669     -     115

 11 omega  -52.90    8.10   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0000   73.8669 -170.7919 61

 12 phi    -25.79   -1.78   1.0006   59.9980
omega____ theta____ kappa____ phi______ frames
-175.7903  113.0000   73.8669     -     24

 13 omega  166.71  198.71   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       95.0000   73.8669  104.2087 32

 14 omega  168.00  203.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   73.8669  -60.7900 35

 15 phi    237.77  312.82   1.0006   59.9980
omega____ theta____ kappa____ phi______ frames
 124.2097  111.0000   73.8669     -     75
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'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
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_diffrn_orient_matrix_UB_31      -0.1277987500
_diffrn_orient_matrix_UB_32      -0.0024983500
_diffrn_orient_matrix_UB_33      0.0061847500
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1882
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.534
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
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_diffrn_reflns_number            85718
_diffrn_reflns_point_group_measured_fraction_full 0.534
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         50.436
_diffrn_reflns_theta_min         2.868
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64229
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
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_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       block
_exptl_crystal_F_000             11392
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
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_refine_diff_density_max         2.061
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_refine_ls_extinction_coef       0.000043(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         10920
_refine_ls_number_restraints     1227
_refine_ls_restrained_S_all      1.894
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.1352
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3260
_refine_ls_wR_factor_ref         0.3556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7073
_reflns_number_total             10920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02089_si_005.cif
_cod_data_source_block           '[5][NO3][PF6]13.10MeCN'
_cod_original_cell_volume        22609(3)
_cod_database_code               4346766
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 91.46
_reflns_odcompleteness_iscentric 1
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O10-N24 = O95-N24 = O15-N24
 1.2 with sigma of 0.02
 P36-F3 = P36-F40 = P36-F41 = P36-F51 = P36-F77 = P36-F29
 1.5 with sigma of 0.02
 F29-F51
 2.2 with sigma of 0.02
 F29-F77
 2.2 with sigma of 0.02
 F29-F3
 2.2 with sigma of 0.02
 F40-F29
 2.2 with sigma of 0.02
 F77-F51
 2.2 with sigma of 0.02
 F77-F3
 2.2 with sigma of 0.02
 F41-F51
 2.2 with sigma of 0.02
 F41-F3
 2.2 with sigma of 0.02
 F41-F77
 2.2 with sigma of 0.02
 F41-F40
 2.2 with sigma of 0.02
 F40-F3
 2.2 with sigma of 0.02
 F40-F51
 2.2 with sigma of 0.02
 F40-F51
 2.2 with sigma of 0.02
 F40-F3
 2.2 with sigma of 0.02
 N73-C56 = N4-C1H
 2.5 with sigma of 0.02
 N99-C10
 2.5 with sigma of 0.02
 N4-C79
 1.1 with sigma of 0.02
 C64-N99
 1.1 with sigma of 0.02
 C91-N26
 1.1 with sigma of 0.02
 O10-N24 \\sim O15-N24 \\sim O95-N24
 with sigma of 0.02
 O15-O10 \\sim O10-O95 \\sim O95-O15
 with sigma of 0.02
3. Restrained planarity
 N24, O95, O15, O10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C24 \\sim C97 \\sim C61 \\sim C9 \\sim N68 \\sim C60: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
Uiso(O95) = Uiso(O10) = Uiso(O15) = Uiso(N24)
Uanis(C13) = Uanis(N45) = Uanis(C5) = Uanis(C22) = Uanis(C12) = Uanis(C14)
Uanis(N83) = Uanis(N46)
Uanis(C47) = Uanis(C3)
Uanis(N39) = Uanis(C11) = Uanis(C1) = Uanis(C138) = Uanis(C16) = Uanis(C71)
Uanis(C48) = Uanis(C110) = Uanis(C1C) = Uanis(C107)
5. Rigid body (RIGU) restrains
 C27, C30, C38, C49, C74, N2, C17, C34, C43, N46, C80, C127, Ru4, N83, C92,
 C28, C111, C6, C85, N19, C67, C86, C96, C4, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Pt2, N9, C57, C133, C20, C7, C45, C52, C72, C121, N1, C18, C1F, C15, C81, C44,
  C108, N48, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P2, F10, F35, F31, F23, F117, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, N24, O95, O15
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N21, C129, C94
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F5, F65, F114, F131, P1, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F104, F50, F119, P8, F106, F11, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Pt1, C5, N6, C12, C13, C14, C22, C24, N45, C59, C60, C61, C66, N68, C69, C97,
 C9, C1A, C1D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Ru4, N39, C1, C16, C71, C138, C11, C21, C84, C8, N11, C26, C102
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F9, P7, F120, F6, F37, F89, F25
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P36, F40, F51, F77, F3, F29, F41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P5, F20, F42, F88, F8, F1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Pt3, N28, C58, C125, C50, C118, C1B, N1D, C19, C1E, C1G, C3, C47, C48, C110,
 C1C, C107, C29, N128
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F87, F19, P3, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F42(0.5) F88(0.5) O95(0.5) F8(0.5) O10(0.5) O15(0.5) N24(0.5)
 F1(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C57(H57), C133(H133), C20(H20), C7(H7), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C22(H22), C26(H26), C27(H27), C30(H30), C34(H34), C49(H49),
  C2(H2), C18(H18), C121(H121), C59(H59), C66(H66), C24(H24), C97(H97),
 C61(H61), C74(H74), C28(H28), C6(H6), C85(H85), C84(H84), C96(H96), C32(H32),
 C86(H86), C4(H4), C102(H102), C127(H127), C138(H138), C1(H1), C8(H8), C1A(H1A),
  C118(H118), C50(H50), C58(H58), C1E(H1E), C1G(H1G), C3(H3), C47(H47),
 C1D(H1D), C15(H15), C81(H81), C44(H44), C108(H108), C48(H48), C110(H110),
 C1C(H1C), C107(H107)
7.b Fitted hexagon refined as free rotating group:
 N9(C57,C133,C20,C7,C45), C52(C2,C18,C121,C72,N1), N68(C60,C24,C97,C61,C9),
 N83(C92,C28,C111,C6,C85), C96(C67,C32,C86,N19,C4), C1B(C118,C50,C58,C125,N28),
 N1D(C19,C1E,C1G,C3,C47), C1F(C15,C81,C44,C108,N48), C48(C110,C1C,C107,C29,N128)
;
_shelx_res_checksum              31101
_shelx_hkl_checksum              36357
_olex2_submission_special_instructions 'No special instructions were received'