Photoisomerization and thermal isomerization of ruthenium aqua complexes with chloro-substituted asymmetric bidentate ligands
Hirahara, Masanari; Goto, Hiroki; Yamamoto, Rei; Yagi, Masayuki; Umemura, Yasushi; RSC Advances 9 (2019) 2002–; doi:10.1039/C8RA08943D

data_7232177
_publ_section_title
;
 Photoisomerization and thermal isomerization of ruthenium aqua complexes
 with chloro-substituted asymmetric bidentate ligands
;
_journal_issue                   4
_journal_name_full               'RSC Advances'
_journal_page_first              2002
_journal_paper_doi               10.1039/C8RA08943D
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C29 H20 Cl2 N5 Ru, F6 P'
_chemical_formula_sum            'C29 H20 Cl2 F6 N5 P Ru'
_chemical_formula_weight         755.45
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2016-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 137.909(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.524(4)
_cell_length_b                   8.2372(14)
_cell_length_c                   25.346(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    296
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      2.46
_cell_volume                     2872.3(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.9767
_diffrn_measured_fraction_theta_max 0.9763
_diffrn_measurement_device_type
'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            15826
_diffrn_reflns_theta_full        27.4573
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.4333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, G. M., 1996)'
_exptl_crystal_colour            'lusterous dark purple'
_exptl_crystal_density_diffrn    1.7469
_exptl_crystal_description       block
_exptl_crystal_F_000             1504.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.2139
_refine_diff_density_min         -0.9923
_refine_diff_density_rms         0.2099
_refine_ls_d_res_high            0.7707
_refine_ls_d_res_low             13.7573
_refine_ls_goodness_of_fit_ref   0.9724
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.9642
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+6.6230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -26
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                3066
_reflns_number_total             6426
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra08943d2.cif
_cod_data_source_block           6clru
_cod_original_cell_volume        2872.2(9)
_cod_database_code               7232177
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6 \\sim P1-F8
\\sim P1-F9 \\sim P1-F10 \\sim P1-
 F11 \\sim P1-F12 \\sim P1-F13
 with sigma of 0.02
 F3-F12 \\sim F3-F11 \\sim F3-F5 \\sim F3-F9 \\sim F9-F11 \\sim F9-F12 \\sim
F9-F13 \\sim F13-F11 \\sim F13-
 F12 \\sim F13-F5
 with sigma of 0.02
 F5-F11 \\sim F5-F12
 with sigma of 0.02
 F2-F1 \\sim F2-F4 \\sim F2-F8 \\sim F2-F6 \\sim F6-F1 \\sim F6-F4 \\sim F6-F10
\\sim F10-F1 \\sim F10-F4 ~
 F10-F8 \\sim F8-F1 \\sim F8-F4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(F3)=Sof(F5)=Sof(F9)=Sof(F11)=Sof(F12)=Sof(F13)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F4)=Sof(F6)=Sof(F8)=Sof(F10)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'