Oxidized divinyl oligoacene-bridged diruthenium complexes: bridged localized radical characters and reduced aromaticity in bridge cores.
Ou, Ya-Ping; Zhang, Jing; Hu, Yuxuan; Yin, Jun; Chi, Chunyan; Liu, Sheng Hua; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16877–16886; doi:10.1039/d0dt02883e

data_7705838
_publ_section_title
;
 Oxidized divinyl oligoacene-bridged diruthenium complexes: bridged
 localized radical characters and reduced aromaticity in bridge cores.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16877
_journal_page_last               16886
_journal_paper_doi               10.1039/d0dt02883e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '2(C21 H33.5 Cl O P3 Ru), 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H72 Cl6 O2 P6 Ru2'
_chemical_formula_weight         1233.67
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-21 deposited with the CCDC.	2020-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.255(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.081(4)
_cell_length_b                   13.350(4)
_cell_length_c                   17.656(6)
_cell_measurement_reflns_used    7192
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.28
_cell_volume                     2839.7(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19432
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.690
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.9052
_exptl_absorpt_correction_T_min  0.8543
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ,
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.247
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4971
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.392
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.1141
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3160
_refine_ls_wR_factor_ref         0.2402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3181
_reflns_number_total             4971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02883e2.cif
_cod_data_source_block           mo_111220f_0m
_cod_database_code               7705838
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.854
_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
2. Restrained distances
 C19-C23 = C22-C28 = C23-C21 = C28-C18 = C21-C19
 2.42 with sigma of 0.01
 C19-C22 = C22-C23 = C28-C21 = C21-C18
 1.39 with sigma of 0.01
 C11-C20 = C20-C19 = C19-C18 = C18-C17 = C17-C16
 1.39 with sigma of 0.01
 C16-C18 = C17-C19 = C18-C20 = C19-C21 = C20-C16
 2.42 with sigma of 0.01
 P3-C7 = P3-C8 = P3-C9 = P3-C7' = P3-C8' = P3-C9'
 1.73 with sigma of 0.01
 C7-C8 = C7-C9 = C8-C9 = C7'-C8' = C7'-C9' = C8'-C9'
 2.75 with sigma of 0.02
 C22-C29 = C21-C31
 1.51 with sigma of 0.01
 C32-C31
 1.2 with sigma of 0.02
 C23-C29 \\sim C19-C29
 with sigma of 0.01
 C18-C31 \\sim C28-C31
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C7') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) = Uanis(C7')
4. Others
 Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(H7'C)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=
 Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: C11(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5)
 C15(0.5) H15(0.5) C16(0.5) C17(0.5) H17(0.5) C18(0.5) C19(0.5) C20(0.5)
 H20(0.5) C21(0.5) C22(0.5) C23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5)
 C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5) C29(0.5) H29(0.5) C30(0.5)
 H30(0.5) C31(0.5) H31(0.5) C32(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C20(H20), C24(H24),
 C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31)
5.c Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C23(C24,C25,C26,C27,C28)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C7'(H7'A,H7'B,H7'C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C)
;
_shelx_res_checksum              52513
_olex2_submission_special_instructions 'No special instructions were received'