A family of Ru(ii) complexes built on a novel sexipyridine building block: synthesis, photophysical properties and the rare structural characterization of a triruthenium species.
Laramée-Milette, Baptiste; Lussier, Félix; Ciofini, Ilaria; Hanan, Garry S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11551–11561; doi:10.1039/c5dt00631g

data_1519677
_publ_section_title
;
 A family of Ru(ii) complexes built on a novel sexipyridine building
 block: synthesis, photophysical properties and the rare structural
 characterization of a triruthenium species.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11551
_journal_page_last               11561
_journal_paper_doi               10.1039/c5dt00631g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C93 H69 N21 Ru3, 3(C2 H3 N), 6(B F4)'
_chemical_formula_sum            'C99 H78 B6 F24 N24 Ru3'
_chemical_formula_weight         2427.30
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2014-07-31 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8909(7)
_cell_length_b                   13.6566(4)
_cell_length_c                   35.3984(12)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100
_cell_measurement_theta_max      54.195
_cell_measurement_theta_min      2.791
_cell_volume                     11060.0(6)
_computing_cell_refinement
;
SAINT (2013) V8.34A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2013) V8.34A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            230761
_diffrn_reflns_theta_full        56.64
_diffrn_reflns_theta_max         56.64
_diffrn_reflns_theta_min         2.70
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  0.7511
_exptl_absorpt_correction_T_min  0.6004
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1252 before and 0.0748 after correction.
The Ratio of minimum to maximum transmission is 0.7994.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4871
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1559
_refine_ls_number_reflns         22119
_refine_ls_number_restraints     1351
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+27.5002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2174
_reflns_number_gt                15904
_reflns_number_total             22119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00631g2.cif
_cod_data_source_block           BALA40_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1519676--1519677.cif.
;
_cod_database_code               1519677
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C109-N22
 1.22 with sigma of 0.01
 B5-F17 = B5-F18A = B5-F19A = B5-F20A
 1.38 with sigma of 0.01
 B5-F18B = B5-F19B = B5-F20B
 1.38 with sigma of 0.01
 B1-F4A = B1-F4B
 1.38 with sigma of 0.01
 B3-F12A = B3-F12B = B3-F10A = B3-F10B
 1.38 with sigma of 0.01
 B4-F13 = B4-F15B = B4-F15A = B4-F16A = B4-F16B
 1.38 with sigma of 0.01
 B2-F5 = B2-F6A = B2-F6B = B2-F7A = B2-F7B
 1.38 with sigma of 0.01
 B2-F8A = B2-F8B
 1.38 with sigma of 0.01
 C75B-C76B
 1.47 with sigma of 0.02
 C79C-C80B
 1.39 with sigma of 0.02
 C79C-C78C
 1.39 with sigma of 0.02
 C78C-C77C
 1.39 with sigma of 0.02
 C77C-C76B
 1.39 with sigma of 0.02
 C76B-N15B
 1.39 with sigma of 0.02
 C80B-N15B
 1.39 with sigma of 0.02
 C80B-C79B
 1.39 with sigma of 0.02
 C79B-C78B
 1.39 with sigma of 0.02
 C78B-C77B
 1.39 with sigma of 0.02
 C77B-C76B
 1.39 with sigma of 0.02
 C76B-N15B
 1.39 with sigma of 0.02
 F22-F24 = F24-F23 = F23-F22
 2.24 with sigma of 0.02
 F24-F21 = F23-F21 = F22-F21
 2.24 with sigma of 0.02
 F10B-F11B = F10B-F12B = F11B-F12B
 2.24 with sigma of 0.02
 F10B-F9 = F11B-F9 = F12B-F9
 2.24 with sigma of 0.02
 F10A-F11A = F10A-F12A = F11A-F12A
 2.24 with sigma of 0.02
 F10A-F9 = F11A-F9 = F12A-F9
 2.24 with sigma of 0.02
 F17-F18A = F17-F19A = F17-F20A
 2.24 with sigma of 0.02
 F18A-F19A = F18A-F20A = F19A-F20A
 2.24 with sigma of 0.02
 F17-F18B = F17-F19B = F17-F20B
 2.24 with sigma of 0.02
 F18B-F19B = F18B-F20B = F19B-F20B
 2.24 with sigma of 0.02
 F15A-F16A
 2.24 with sigma of 0.02
 F14B-F16B = F14B-F13 = F16B-F13
 2.24 with sigma of 0.02
 F15B-F14B = F15B-F16B = F15B-F13
 2.24 with sigma of 0.02
 C108-N22
 2.6 with sigma of 0.02
 C75B-N15B
 2.39 with sigma of 0.02
 N16-C76B
 2.39 with sigma of 0.02
 C74B-C76B
 2.5 with sigma of 0.02
 C75B-C77B
 2.5 with sigma of 0.02
 N15B-C79B
 2.38 with sigma of 0.04
 C80B-C78B
 2.38 with sigma of 0.04
 C79B-C77B
 2.38 with sigma of 0.04
 C78B-C76B
 2.38 with sigma of 0.04
 C77B-N15B
 2.38 with sigma of 0.04
 C76B-C80B
 2.38 with sigma of 0.04
 C80B-C78C
 2.38 with sigma of 0.04
 C79C-C77C
 2.38 with sigma of 0.04
 C78C-C76B
 2.38 with sigma of 0.04
 C77C-N15B
 2.38 with sigma of 0.04
 C76B-C80B
 2.38 with sigma of 0.04
 N15B-C79C
 2.38 with sigma of 0.04
 F22-F24 \\sim F22-F23 \\sim F21-F23
 with sigma of 0.02
 F22-F21 \\sim F21-F24 \\sim F24-F23
 with sigma of 0.02
 B6-F22 \\sim B6-F21 \\sim B6-F24 \\sim B6-F23
 with sigma of 0.02
 F5-F7B \\sim F5-F8B \\sim F6B-F8B
 with sigma of 0.02
 F5-F6B \\sim F6B-F7B \\sim F7B-F8B
 with sigma of 0.02
 B2-F5 \\sim B2-F6B \\sim B2-F7B \\sim B2-F8B
 with sigma of 0.02
 F5-F7A \\sim F5-F8A \\sim F6A-F8A
 with sigma of 0.02
 F5-F6A \\sim F6A-F7A \\sim F7A-F8A
 with sigma of 0.02
 B2-F5 \\sim B2-F6A \\sim B2-F7A \\sim B2-F8A
 with sigma of 0.02
3. Restrained planarity
 C74B, C73B, C72B, N16, C75B
 with sigma of 0.1
 C72B, N16, C75B, C74B, C73B
 with sigma of 0.1
 C81A, N14A, C85A, C84A, C82A
 with sigma of 0.1
 N16, C71A, C72A, C73A, C74A, C75A
 with sigma of 0.1
 C75B, C76B, N15B, N16, Ru3
 with sigma of 0.1
 C79C, C78C, C77C, C76B, N15B, C80B
 with sigma of 0.1
4. Rigid bond restraints
 C35, C37, C36, C39, C33, C31, C34, C32, C40, C38, C55, C41, C45, C47, C46,
 C50, C49, C48, C51, C44, C52, C42, C53, C43, C54, C76A, C77A, C78A, C79A, C80A,
  C68, C66, C70, C67, C61, C65, C69, C64, C62, C73A, C74A, C75A, C71A, C72A,
 C63, C16, C15, C11, C12, C13, C14, C20, C10, C9, C1, C6, C8, C7, C4, C2, C3,
 C5, C22, C21, C30, C27, C26, C29, C28, C23, C24, C25, C101, C102, C103, C17,
 C19, C18, C105, C107, C104, C106, C75B, C71B, C72B, C73B, C74B, C109, C108,
 C81A, C85A, C84A, C83A, C82A, C81B, C85B, C84B, C83B, C82B, C60, C56, C57, C58,
  C59, C77B, C78B, C79B, C79C, C78C, C77C, C76B, C80B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, N11, N7, N9, N10, N15A, N14, N13, N2, N1, N3, N5, N6, N4, N19, N17, N18,
 N20, N21, N16, N22, N14A, N14B, N12, N15B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B1, B6, B2, B3, B5, B4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F2, F1, F3, F23, F5, F6A, F8B, F7B, F24, F11A, F17, F13, F12A, F10B, F19A,
 F18A, F20B, F22, F15B, F9, F16A, F21, F12B, F10A, F19B, F18B, F20A, F16B, F11B,
  F4A, F15A, F4B, F14B, F6B, F7A, F8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C75B, N16, C71A, C71B, C72A, C72B, C73B, C73A, C74A, C74B, C75A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F23, B6, F24, F22, F21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C80B, C79B, C78B, C77B, C76B, N15B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C79C, C78C, C77C, C76B, N15B, C80B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C109, N22, C108
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C108 \\sim C109 \\sim N22: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
B2 \\sim F5 \\sim F6A \\sim F6B \\sim F7A \\sim F7B \\sim F8A \\sim F8B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
B1 \\sim B6 \\sim B2 \\sim B3 \\sim B5 \\sim B4: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
F2 \\sim F1 \\sim F3 \\sim F23 \\sim F5 \\sim F6A \\sim F8B \\sim F7B \\sim F24
\\sim F11A \\sim F17 \\sim F13 \\sim F12A \\sim F10B \\sim F19A \\sim F18A
\\sim F20B \\sim F22 \\sim F15B \\sim F9 \\sim F16A \\sim F21 \\sim F12B \\sim
F10A \\sim F19B \\sim F18B \\sim F20A \\sim F16B \\sim F11B \\sim F4A \\sim
F15A \\sim F4B \\sim F14B \\sim F6B \\sim F7A \\sim F8A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C35 \\sim C37 \\sim C36 \\sim C39 \\sim C33 \\sim C31 \\sim C34 \\sim C32 \\sim
C40 \\sim C38 \\sim C55 \\sim C41 \\sim C45 \\sim C47 \\sim C46 \\sim C50 \\sim
C49 \\sim C48 \\sim C51 \\sim C44 \\sim C52 \\sim C42 \\sim C53 \\sim C43 \\sim
C54 \\sim C76A \\sim C77A \\sim C78A \\sim C79A \\sim C80A \\sim C68 \\sim C66
\\sim C70 \\sim C67 \\sim C61 \\sim C65 \\sim C69 \\sim C64 \\sim C62 \\sim
C73A \\sim C74A \\sim C75A \\sim C71A \\sim C72A \\sim C63 \\sim C16 \\sim C15
\\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C20 \\sim C10 \\sim C9 \\sim C1
\\sim C6 \\sim C8 \\sim C7 \\sim C4 \\sim C2 \\sim C3 \\sim C5 \\sim C22 \\sim
C21 \\sim C30 \\sim C27 \\sim C26 \\sim C29 \\sim C28 \\sim C23 \\sim C24 \\sim
C25 \\sim C101 \\sim C102 \\sim C103 \\sim C17 \\sim C19 \\sim C18 \\sim C105
\\sim C107 \\sim C104 \\sim C106 \\sim C75B \\sim C71B \\sim C72B \\sim C73B
\\sim C74B \\sim C109 \\sim C108 \\sim C81A \\sim C85A \\sim C84A \\sim C83A
\\sim C82A \\sim C81B \\sim C85B \\sim C84B \\sim C83B \\sim C82B \\sim C60
\\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C77B \\sim C78B \\sim C79B \\sim
C79C \\sim C78C \\sim C77C \\sim C76B \\sim C80B: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C75A \\sim C71B \\sim N16 \\sim C71A \\sim C75B \\sim C74B \\sim C73B \\sim
C72A \\sim C72B \\sim C73A \\sim C74A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
N16 \\sim C71A \\sim C71B \\sim C72A \\sim C72B \\sim C73A \\sim C73B \\sim
C74A \\sim C75A \\sim C75B \\sim C74B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
F23 \\sim B6 \\sim F24 \\sim F22 \\sim F21: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C77B \\sim C78B \\sim C79B \\sim C76B \\sim N15B \\sim C80B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C79C \\sim C78C \\sim C77C \\sim C76B \\sim N15B \\sim C80B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N22 \\sim C109 \\sim C108: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(N14A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N14A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C50) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N14A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N22) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Fixed Sof: H76A(0.5) H80A(0.5) C73A(0.5) H73A(0.5) C74A(0.5) H74A(0.5)
 C75A(0.5) C71A(0.5) H71A(0.5) C72A(0.5) H72A(0.5) C75B(0.5) C71B(0.5)
 H71B(0.5) C72B(0.5) H72B(0.5) C73B(0.5) H73B(0.5) C74B(0.5) H74B(0.5) F6A(0.5)
 F8B(0.5) F7B(0.5) F11A(0.5) F12A(0.5) F10B(0.5) F19A(0.5) F18A(0.5) F20B(0.5)
 F15B(0.5) F16A(0.5) F12B(0.5) F10A(0.5) F19B(0.5) F18B(0.5) F20A(0.5)
 F16B(0.5) F11B(0.5) F15A(0.5) F4B(0.5) F6B(0.5) F7A(0.5) F8A(0.5) C81A(0.5)
 N14A(0.5) C85A(0.5) H85A(0.5) C84A(0.5) H84A(0.5) C83A(0.5) H83A(0.5)
 C82A(0.5) H82A(0.5) C81B(0.5) N14B(0.5) C85B(0.5) H85B(0.5) C84B(0.5)
 H84B(0.5) C83B(0.5) H83B(0.5) C82B(0.5) H82B(0.5) C77B(0.5) H77B(0.5)
 C78B(0.5) H78B(0.5) C79B(0.5) H79B(0.5) C79C(0.5) H79C(0.5) C78C(0.5)
 H78C(0.5) C77C(0.5) H77C(0.5) H76B(0.5) H80B(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C39(H39), C33(H33), C31(H31), C34(H34), C32(H32), C40(H40),
 C41(H41), C47(H47), C50(H50), C49(H49), C48(H48), C51(H51), C44(H44), C52(H52),
  C42(H42), C53(H53), C43(H43), C54(H54), C76A(H76A), C77A(H77A), C78A(H78A),
 C79A(H79A), C80A(H80A), C70(H70), C67(H67), C61(H61), C69(H69), C64(H64),
 C62(H62), C73A(H73A), C74A(H74A), C71A(H71A), C72A(H72A), C63(H63), C11(H11),
 C12(H12), C13(H13), C14(H14), C20(H20), C10(H10), C9(H9), C1(H1), C7(H7),
 C4(H4), C2(H2), C3(H3), C22(H22), C21(H21), C30(H30), C27(H27), C29(H29),
 C28(H28), C23(H23), C24(H24), C17(H17), C19(H19), C18(H18), C71B(H71B),
 C72B(H72B), C73B(H73B), C74B(H74B), C85A(H85A), C84A(H84A), C83A(H83A),
 C82A(H82A), C85B(H85B), C84B(H84B), C83B(H83B), C82B(H82B), C60(H60), C57(H57),
  C58(H58), C59(H59), C77B(H77B), C78B(H78B), C79B(H79B), C79C(H79C),
 C78C(H78C), C77C(H77C), C76B(H76B), C80B(H80B)
7.b Fitted hexagon refined as free rotating group:
 C47(C46,N10,C50,C49,C48), N15A(C76A,C77A,C78A,C79A,C80A), C75B(N16,C71B,C72B,
 C73B,C74B), C81A(N14A,C85A,C84A,C83A,C82A), C81B(N14B,C85B,C84B,C83B,C82B),
 C60(N12,C56,C57,C58,C59), C79C(C78C,C77C,C76B,N15B,C80B)
7.c Idealised Me refined as rotating group:
 C104(H10A,H10B,H10C), C106(H10D,H10E,H10F), C108(H10G,H10H,H10I)
;
_olex2_submission_special_instructions 'No special instructions were received'