Efficient Photoswitch System Combining a Dimethyldihydropyrene Pyridinium Core and Ruthenium(II) Bis-Terpyridine Entities.
Jacquet, Margot; Lafolet, Frédéric; Cobo, Saioa; Loiseau, Frédérique; Bakkar, Assil; Boggio-Pasqua, Martial; Saint-Aman, Eric; Royal, Guy; Inorganic chemistry 56 (2017) 4357–4368; doi:10.1021/acs.inorgchem.6b02861

data_4345796
_publ_section_title
;
 Efficient Photoswitch System Combining a Dimethyldihydropyrene Pyridinium
 Core and Ruthenium(II) Bis-Terpyridine Entities.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4357
_journal_page_last               4368
_journal_paper_doi               10.1021/acs.inorgchem.6b02861
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety
'C80 H70 N8, 1(B2 F8), 0.7(C2 H3 N), 0.5(H2 O)'
_chemical_formula_sum            'C81.4 H73.1 B2 F8 N8.7 O0.5'
_chemical_formula_weight         1354.80
_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   mixed
_audit_creation_date             2016-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                112.18(2)
_cell_angle_beta                 97.06(3)
_cell_angle_gamma                96.59(3)
_cell_formula_units_Z            1
_cell_length_a                   9.411(3)
_cell_length_b                   13.294(3)
_cell_length_c                   16.113(5)
_cell_measurement_reflns_used    26157
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.535
_cell_volume                     1823.9(10)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaCCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26157
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.535
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.473165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1649 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.4732.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       needle
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         6332
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0927
_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^)+(0.1397P)^2^+2.1281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4490
_reflns_number_total             6332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02861_si_002.cif
_cod_data_source_block           nanny
_cod_original_formula_sum        'C81.40 H73.10 B2 F8 N8.70 O0.50'
_cod_database_code               4345796
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C45-N46
 1.2 with sigma of 0.02
 C44-C45
 1.5 with sigma of 0.02
 C44-N46
 2.8 with sigma of 0.02
 F4B-B1B
 1.37 with sigma of 0.02
 B1B-F3B
 1.37 with sigma of 0.02
 B1B-F2B
 1.37 with sigma of 0.02
 B1B-F1B
 1.37 with sigma of 0.02
 F1A-B1A
 1.37 with sigma of 0.02
 B1A-F4A
 1.37 with sigma of 0.02
 B1A-F2A
 1.37 with sigma of 0.02
 B1A-F3A
 1.37 with sigma of 0.02
 F2B-F1B
 2.24 with sigma of 0.02
 F1B-F3B
 2.24 with sigma of 0.02
 F2B-F3B
 2.24 with sigma of 0.02
 F4B-F2B
 2.24 with sigma of 0.02
 F4B-F1B
 2.24 with sigma of 0.02
 F4B-F3B
 2.24 with sigma of 0.02
 F4A-F3A
 2.24 with sigma of 0.02
 F3A-F2A
 2.24 with sigma of 0.02
 F2A-F4A
 2.24 with sigma of 0.02
 F1A-F4A
 2.24 with sigma of 0.02
 F1A-F3A
 2.24 with sigma of 0.02
 F1A-F2A
 2.24 with sigma of 0.02
 C8B-C7
 1.5 with sigma of 0.02
 C10B-C7
 1.5 with sigma of 0.02
 C7-C9B
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C8A, C8B, C9A, C9B, C10A, C10B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F2B, B1B, F3B, F4B, F1B, F2A, B1A, F1A, F4A, F3A, F2C, F3C, B1C, F4C, F1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C8B \\sim C9B \\sim C10B \\sim C10A \\sim C9A \\sim C8A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F2A \\sim B1A \\sim F1A \\sim F4A \\sim F3A \\sim F2B \\sim B1B \\sim F3B \\sim
F4B \\sim F1B \\sim F2C \\sim F3C \\sim B1C \\sim F4C \\sim F1C: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(B1B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uanis(C9A) = Uanis(C10B)
Uanis(C10A) = Uanis(C8B)
5. Others
 Sof(C3B)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C3A)=FVAR(1)
 Sof(F2A)=Sof(B1A)=Sof(F1A)=Sof(F4A)=Sof(F3A)=0.6*(1-FVAR(3))
 Sof(B1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F1B)=0.6*FVAR(3)
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=1-FVAR(3)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(3)
 Fixed Sof: F3C(0.4) F4C(0.4) F1C(0.4) B1C(0.4) C45(0.35) N46(0.35) C44(0.35)
 H44A(0.35) H44B(0.35) H44C(0.35) O1(0.25) H1A(0.25) H1B(0.25) F2C(0.4)
6.a Riding coordinates:
 O1(H1A,H1B)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C19(H19), C12(H12), C15(H15), C1(H1), C16(H16), C39(H39), C28(H28),
 C18(H18), C22(H22), C23(H23), C31(H31), C42(H42), C26(H26), C25(H25), C40(H40),
  C36(H36), C41(H41), C34(H34), C35(H35), C33(H33)
6.d Idealised Me refined with riding coordinates:
 C9B(H9BA,H9BB,H9BC)
6.e Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C13A(H13A,
 H13B,H13C), C13B(H13D,H13E,H13F), C44(H44A,H44B,H44C), C10B(H10D,H10E,H10F),
 C8B(H8BA,H8BB,H8BC)
;
_shelx_res_checksum              12030
_shelx_hkl_checksum              66069
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'