Dinuclear ruthenium acetylide complexes with diethynylated anthrahydroquinone and anthraquinone frameworks: a multi-stimuli-responsive organometallic switch.
Oyama, Yousuke; Kawano, Reo; Tanaka, Yuya; Akita, Munetaka; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7432–7441; doi:10.1039/c9dt01255a

data_7049784
_publ_section_title
;
 Dinuclear ruthenium acetylide complexes with diethynylated
 anthrahydroquinone and anthraquinone frameworks: a
 multi-stimuli-responsive organometallic switch.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7432
_journal_page_last               7441
_journal_paper_doi               10.1039/c9dt01255a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C136 H122 P8 Ru2 Si2'
_chemical_formula_sum            'C136 H122 P8 Ru2 Si2'
_chemical_formula_weight         2262.41
_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     dual
_audit_creation_date             2019-04-12
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.383(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.758(5)
_cell_length_b                   12.1471(19)
_cell_length_c                   18.658(3)
_cell_measurement_reflns_used    5476
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.38
_cell_volume                     6477.3(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      87(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30233
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.425
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1041 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.8340.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       plate
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.610
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         11447
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6550
_reflns_number_total             11447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01255a2.cif
_cod_data_source_block           3Cl4
_cod_depositor_comments
'Adding full bibliography for 7049783--7049784.cif.'
_cod_original_cell_volume        6477.5(18)
_cod_database_code               7049784
_shelx_shelxl_version_number     2018/3
_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
 Si1A-C66A
 1.85 with sigma of 0.02
 Si1A-C68A
 1.85 with sigma of 0.02
 Si1A-C67A
 1.85 with sigma of 0.02
 Si1-C66
 1.85 with sigma of 0.02
 Si1-C67
 1.85 with sigma of 0.02
 Si1-C68
 1.85 with sigma of 0.02
 C68A-C66A
 2.6 with sigma of 0.04
 C66A-C67A
 2.6 with sigma of 0.04
 C67A-C68A
 2.6 with sigma of 0.04
 C66-C67
 2.6 with sigma of 0.04
 C67-C68
 2.6 with sigma of 0.04
 C68-C66
 2.6 with sigma of 0.04
 Si1-C53 \\sim Si1A-C53
 with sigma of 0.02
 Si1-C66 \\sim Si1A-C66A
 with sigma of 0.02
 Si1-C67 \\sim Si1A-C67A
 with sigma of 0.02
 Si1-C68 \\sim Si1A-C68A
 with sigma of 0.02
 C53-C66 \\sim C53-C66A
 with sigma of 0.04
 C53-C67 \\sim C53-C67A
 with sigma of 0.04
 C53-C68 \\sim C53-C68A
 with sigma of 0.04
 C66-C67 \\sim C66A-C67A
 with sigma of 0.04
 C66-C68 \\sim C66A-C68A
 with sigma of 0.04
 C67-C68 \\sim C67A-C68A
 with sigma of 0.04
3. Rigid bond restraints
 C66, C67, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68A, C66, C66A, C67, C67A, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C66 \\sim C67 \\sim C68: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C68A \\sim C68 \\sim C67A \\sim C66 \\sim C66A \\sim C67: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67A)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(Si1A) \\sim Ueq,
Uanis(Si1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=Sof(Si1A)=Sof(C68A)=Sof(H68D)=
 Sof(H68E)=Sof(H68F)=Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=1-FVAR(1)
 Sof(Si1)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=Sof(H67B)=
 Sof(H67C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C51(H51A,H51B), C26(H26A,H26B), C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C30(H30), C23(H23), C41(H41), C20(H20), C18(H18), C6(H6), C2(H2),
 C24(H24), C60(H60), C40(H40), C46(H46), C32(H32), C9(H9), C34(H34), C38(H38),
 C37(H37), C22(H22), C31(H31), C29(H29), C21(H21), C12(H12), C5(H5), C49(H49),
 C11(H11), C28(H28), C36(H36), C44(H44), C14(H14), C50(H50), C16(H16), C42(H42),
  C35(H35), C10(H10), C15(H15), C43(H43), C3(H3), C4(H4), C47(H47), C65(H65),
 C62(H62), C48(H48), C17(H17), C64(H64)
6.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C66A(H66D,H66E,
 H66F), C68A(H68D,H68E,H68F), C67A(H67D,H67E,H67F)
;
_olex2_submission_special_instructions 'No special instructions were received'