Going against the flow: Os(II)-to-Ru(II) energy transfer in rod-like polypyridyl chromophore
Laramee-Milette, Baptiste; Hanan, Garry; Chem. Commun.  (2017) –; doi:10.1039/C7CC03541A

data_7120512
_publ_section_title
;
 Going against the flow: Os(II)-to-Ru(II) energy transfer in rod-like
 polypyridyl chromophore
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03541A
_journal_year                    2017
_chemical_formula_moiety         'C55 H43 N11 Ru, 2(F6 P)'
_chemical_formula_sum            'C55 H43 F12 N11 P2 Ru'
_chemical_formula_weight         1249.01
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                97.096(4)
_cell_angle_beta                 100.183(5)
_cell_angle_gamma                92.627(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3351(18)
_cell_length_b                   12.808(3)
_cell_length_c                   23.398(5)
_cell_measurement_reflns_used    1532
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      37.67
_cell_measurement_theta_min      3.27
_cell_volume                     2725.8(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.2343
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6455
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        44.482
_diffrn_reflns_theta_max         44.482
_diffrn_reflns_theta_min         3.032
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.422
_exptl_absorpt_correction_T_max  0.7487
_exptl_absorpt_correction_T_min  0.4528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.6048.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     584
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.2783
_refine_ls_R_factor_gt           0.1470
_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^)+(0.1860P)^2^+25.2260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3280
_refine_ls_wR_factor_ref         0.4138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2473
_reflns_number_total             5501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03541a2.cif
_cod_data_source_block           matrix_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2725.9(9)
_cod_database_code               7120512
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-C7
 1.31 with sigma of 0.02
 C7-N2
 1.35 with sigma of 0.02
 N2-C3
 1.46 with sigma of 0.02
 C3-C2
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
 C1-N1
 1.47 with sigma of 0.02
 N3-C8
 1.39 with sigma of 0.02
 C7-N3
 1.41 with sigma of 0.02
 N3-C6
 1.49 with sigma of 0.02
 C6-C5
 1.51 with sigma of 0.02
 C5-C4
 1.53 with sigma of 0.02
 C4-N2
 1.48 with sigma of 0.02
 C14-C13
 1.38 with sigma of 0.02
 C13-C12
 1.38 with sigma of 0.02
 C12-C11
 1.38 with sigma of 0.02
 F3B-P1
 1.6273 with sigma of 0.02
 F2B-P1
 1.6273 with sigma of 0.02
 F2A-P1
 1.6273 with sigma of 0.02
 F5B-P1
 1.6273 with sigma of 0.02
 F5A-P1
 1.6273 with sigma of 0.02
 P1-F4B
 1.6273 with sigma of 0.02
 F1-P1
 1.6273 with sigma of 0.02
 P1-F6
 1.6273 with sigma of 0.02
 F7-P2
 1.6273 with sigma of 0.02
 F12-P2
 1.6273 with sigma of 0.02
 F10B-P2
 1.6273 with sigma of 0.02
 F10A-P2
 1.6273 with sigma of 0.02
 F11A-P2
 1.6273 with sigma of 0.02
 P2-F8A
 1.6273 with sigma of 0.02
 F9B-P2
 1.6273 with sigma of 0.02
 F9A-P2
 1.6273 with sigma of 0.02
 P2-F8B
 1.6273 with sigma of 0.02
 F3A-P1
 1.6273 with sigma of 0.02
 F4A-P1
 1.6273 with sigma of 0.02
 F11B-P2
 1.6273 with sigma of 0.02
 N1-C2
 2.43 with sigma of 0.04
 C1-C3
 2.43 with sigma of 0.04
 C1-C7
 2.34 with sigma of 0.04
 N1-N2
 2.37 with sigma of 0.04
 C7-C3
 2.45 with sigma of 0.04
 N2-C2
 2.45 with sigma of 0.04
 C8-C7
 2.48 with sigma of 0.04
 N1-N3
 2.36 with sigma of 0.04
 C7-C6
 2.44 with sigma of 0.04
 N3-C5
 2.42 with sigma of 0.04
 C6-C4
 2.42 with sigma of 0.04
 C5-N2
 2.51 with sigma of 0.04
 C7-C4
 2.51 with sigma of 0.04
 N2-N3
 2.32 with sigma of 0.04
 C6-C8
 2.46 with sigma of 0.04
 N3-C9
 2.31 with sigma of 0.04
 C18-C13
 2.38 with sigma of 0.04
 C12-C14
 2.38 with sigma of 0.04
 C13-C11
 2.38 with sigma of 0.04
 C12-C19
 2.38 with sigma of 0.04
 F4A-F3A
 2.3014 with sigma of 0.04
 F3A-F2A
 2.3014 with sigma of 0.04
 F2A-F5A
 2.3014 with sigma of 0.04
 F4A-F5A
 2.3014 with sigma of 0.04
 F4B-F3B
 2.3014 with sigma of 0.04
 F3B-F2B
 2.3014 with sigma of 0.04
 F2B-F5B
 2.3014 with sigma of 0.04
 F5B-F4B
 2.3014 with sigma of 0.04
 F4B-F6
 2.3014 with sigma of 0.04
 F4A-F6
 2.3014 with sigma of 0.04
 F3B-F6
 2.3014 with sigma of 0.04
 F6-F3A
 2.3014 with sigma of 0.04
 F6-F2B
 2.3014 with sigma of 0.04
 F6-F5A
 2.3014 with sigma of 0.04
 F6-F5B
 2.3014 with sigma of 0.04
 F6-F2A
 2.3014 with sigma of 0.04
 F1-F4A
 2.3014 with sigma of 0.04
 F4B-F1
 2.3014 with sigma of 0.04
 F1-F3B
 2.3014 with sigma of 0.04
 F3A-F1
 2.3014 with sigma of 0.04
 F2B-F1
 2.3014 with sigma of 0.04
 F2A-F1
 2.3014 with sigma of 0.04
 F5B-F1
 2.3014 with sigma of 0.04
 F5A-F1
 2.3014 with sigma of 0.04
 F8A-F11A
 2.3014 with sigma of 0.04
 F11A-F10A
 2.3014 with sigma of 0.04
 F10A-F9A
 2.3014 with sigma of 0.04
 F8B-F11B
 2.3014 with sigma of 0.04
 F11B-F10B
 2.3014 with sigma of 0.04
 F10B-F9B
 2.3014 with sigma of 0.04
 F8B-F9B
 2.3014 with sigma of 0.04
 F9A-F8A
 2.3014 with sigma of 0.04
 F11B-F12
 2.3014 with sigma of 0.04
 F11A-F12
 2.3014 with sigma of 0.04
 F12-F10B
 2.3014 with sigma of 0.04
 F12-F10A
 2.3014 with sigma of 0.04
 F12-F9B
 2.3014 with sigma of 0.04
 F12-F9A
 2.3014 with sigma of 0.04
 F12-F8B
 2.3014 with sigma of 0.04
 F8A-F12
 2.3014 with sigma of 0.04
 F7-F8A
 2.3014 with sigma of 0.04
 F7-F8B
 2.3014 with sigma of 0.04
 F7-F9A
 2.3014 with sigma of 0.04
 F7-F9B
 2.3014 with sigma of 0.04
 F7-F10A
 2.3014 with sigma of 0.04
 F10B-F7
 2.3014 with sigma of 0.04
 F11A-F7
 2.3014 with sigma of 0.04
 F11B-F7
 2.3014 with sigma of 0.04
 F8A-F7
 2.3014 with sigma of 0.04
3. Restrained planarity
 C12, C13, C14, C18, C19, C11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
P2 \\sim F12 \\sim F8A \\sim F7 \\sim F8B \\sim F11B \\sim F9A \\sim F10A \\sim
F11A \\sim F9B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F12 \\sim P2 \\sim F8A \\sim F7 \\sim F8B \\sim F11B \\sim F9A \\sim F10A \\sim
F11A \\sim F9B \\sim F10B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F6 \\sim P1 \\sim F1 \\sim F3B \\sim F5B: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N11 \\sim C55 \\sim C51 \\sim C54 \\sim C52 \\sim C53: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N10 \\sim C46 \\sim C49 \\sim C47 \\sim C50 \\sim C48: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N9 \\sim C45 \\sim C41 \\sim C42 \\sim C44 \\sim C43: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C35 \\sim C40 \\sim C36 \\sim C38 \\sim C37 \\sim C39: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N7 \\sim C29 \\sim C26 \\sim C27 \\sim C28 \\sim C25: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N8 \\sim C33 \\sim C30 \\sim C34 \\sim C31 \\sim C32: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N6 \\sim C20 \\sim C22 \\sim C21 \\sim C23 \\sim C24: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
P1 \\sim F2B \\sim F5B \\sim F1 \\sim F6 \\sim F3B \\sim F4B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 P1, F6, F1, F3B, F5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N2, C7, C3, C1, C2, N3, C5, C4, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C9, C8, N4, C19, C11, C14, C18, N5, C17, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C14, C18, C19, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F6, F1, F3B, F5B, F4B, F2B, F5A, F2A, F3A, F4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C20, C24, Ru1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F11B, P2, F12, F8A, F7, F8B, F9A, F10A, F11A, F9B, F10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F3B(0.5) F8A(0.5) F8B(0.5) F11B(0.5) F9A(0.5) F5B(0.5) F10A(0.5)
 F11A(0.5) F9B(0.5) F10B(0.5) F4B(0.5) F2B(0.5) F5A(0.5) F2A(0.5) F3A(0.5)
 F4A(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C4(H4A,H4B), C6(H6A,H6B)
7.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C40(H40), C49(H49), C47(H47), C26(H26), C33(H33), C22(H22),
 C21(H21), C34(H34), C36(H36), C28(H28), C37(H37), C23(H23), C31(H31), C39(H39),
  C32(H32), C17(H17), C16(H16), C15(H15), C55(H55), C54(H54), C41(H41),
 C52(H52), C42(H42), C44(H44), C43(H43), C53(H53), C10(H10), C9(H9), C13(H13),
 C12(H12)
7.c Fitted hexagon refined as free rotating group:
 C14(C18,N5,C17,C16,C15), C10(C9,C8,N4,C19,C11)
;
_olex2_submission_special_instructions 'No special instructions were received'