Hydroquinone/quinone electro- and photochemical interconversion in isolable polypyridylruthenium(II) complexes.
Oyama, Dai; Kanno, Takatoshi; Takase, Tsugiko; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7759–7767; doi:10.1039/d1dt00678a

data_7707369
_publ_section_title
;
 Hydroquinone/quinone electro- and photochemical interconversion in
 isolable polypyridylruthenium(II) complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7759
_journal_page_last               7767
_journal_paper_doi               10.1039/d1dt00678a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C33 H26 N6 O2 Ru, 0.5(H2 O), 2(F6 P), 0.25(O), 0.25(C H4 O)'
_chemical_formula_sum            'C33.25 H28 F12 N6 O3 P2 Ru'
_chemical_formula_weight         950.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-29 deposited with the CCDC.	2021-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.6880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4452(2)
_cell_length_b                   12.9054(2)
_cell_length_c                   49.4032(7)
_cell_measurement_reflns_used    29325
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      30.6260
_cell_measurement_theta_min      2.2630
_cell_volume                     7925.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'Rigaku Mercury area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00  65.00   0.50   28.00    --  -25.00  45.00   0.00  360
  2  \w   -115.00  65.00   0.50   28.00    --  -25.00  45.00  90.00  360
  3  \w   -115.00  65.00   0.50   28.00    --  -25.00  45.00 180.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0321609000
_diffrn_orient_matrix_UB_12      0.0246586000
_diffrn_orient_matrix_UB_13      -0.0095766000
_diffrn_orient_matrix_UB_21      0.0334309000
_diffrn_orient_matrix_UB_22      0.0205679000
_diffrn_orient_matrix_UB_23      0.0107197000
_diffrn_orient_matrix_UB_31      0.0331836000
_diffrn_orient_matrix_UB_32      -0.0446097000
_diffrn_orient_matrix_UB_33      -0.0003495000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            45972
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.74a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             3804
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol, acetonitrile'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.812
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         11354
_refine_ls_number_restraints     616
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0876
_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^)+(0.0592P)^2^+40.1573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9368
_reflns_number_total             11354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00678a2.cif
_cod_data_source_block           sampler3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Orange' was changed
to 'orange' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7707368--7707369.cif.
;
_cod_database_code               7707369
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ru'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 P2-F10 \\sim P2-F8A
 with sigma of 0.02
 P1-F4 \\sim P1-F5A
 with sigma of 0.02
 P2-F7 \\sim P2-F10A
 with sigma of 0.02
 P1-F1 \\sim P1-F3A
 with sigma of 0.02
 P2-F9 \\sim P2-F7A
 with sigma of 0.02
 P1-F6 \\sim P1-F1A
 with sigma of 0.02
 P2-F8 \\sim P2-F9A
 with sigma of 0.02
 P1-F3 \\sim P1-F6A
 with sigma of 0.02
 P1-F2 \\sim P1-F4A
 with sigma of 0.02
 P1-F5 \\sim P1-F2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P2 \\sim F10 \\sim F7 \\sim F11 \\sim F9 \\sim F8 \\sim F12 \\sim F9A \\sim F7A
\\sim F10A \\sim F8A: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
F12A \\sim P2 \\sim F10 \\sim F7 \\sim F11 \\sim F9 \\sim F8 \\sim F12 \\sim
F10A \\sim F8A \\sim F7A \\sim F9A \\sim F11A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
F5A \\sim P1 \\sim F2A \\sim F3A \\sim F6A \\sim F4A \\sim F1A \\sim F3 \\sim
F5 \\sim F1 \\sim F2 \\sim F6 \\sim F4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 F6A, P1, F3, F5A, F4, F2A, F3A, F5, F6, F4A, F2, F1, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, P2, F10, F8A, F9A, F7A, F12A, F11, F11A, F8, F10A, F12, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) F10(0.5) F7(0.5) F11(0.5) F9(0.5)
 F8(0.5) F12(0.5) F10A(0.5) F8A(0.5) F7A(0.5) F9A(0.5) F12A(0.5) F11A(0.5)
 O4(0.25) F6(0.5) F4(0.5) F1(0.5) F5(0.5) F3(0.5) F2(0.5) F6A(0.5) F4A(0.5)
 F2A(0.5) F5A(0.5) F3A(0.5) F1A(0.5) O3(0.25) H3A(0.25) C34(0.25) H34A(0.25)
 H34B(0.25) H34C(0.25)
6.a Free rotating group:
 O5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C12(H12), C14(H14), C31(H31), C17(H17), C20(H20), C5(H5), C18(H18),
 C22(H22), C10(H10), C24(H24), C19(H19), C23(H23), C9(H9), C4(H4), C29(H29),
 C2(H2A), C3(H3), C7(H7), C8(H8), C28(H28)
6.c Tetrahedral OH refined with riding coordinates:
 O3(H3A)
6.d Idealised Me refined with riding coordinates:
 C34(H34A,H34B,H34C)
6.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
6.f Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_shelx_res_checksum              73025
_shelx_hkl_checksum              28118
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.269
_oxdiff_exptl_absorpt_empirical_full_min 0.843