N–C bond formation between two anilines coordinated to a ruthenium center in cis-form affording a 3,5-cyclohexadiene-1,2-diimine moiety
Tomioka, Nozomi; Nanbu, Shinkoh; Misawa-Suzuki, Tomoyo; Nagao, Hirotaka; RSC Advances 11 (2021) 36644–36650; doi:10.1039/D1RA07736H

data_7243926
_publ_section_title
;
 N--C bond formation between two anilines coordinated to a ruthenium
 center in cis-form affording a 3,5-cyclohexadiene-1,2-diimine moiety
;
_journal_issue                   58
_journal_name_full               'RSC Advances'
_journal_page_first              36644
_journal_page_last               36650
_journal_paper_doi               10.1039/D1RA07736H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C34 H34 N6 Ru, 2(C F3 O3 S)'
_chemical_formula_sum            'C36 H34 F6 N6 O6 Ru S2'
_chemical_formula_weight         925.88
_chemical_name_common
'di(4-methylaniline)bis(2,2'-bipyridine)ruthenium bis(trifluoromethanesulfonate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.23880(10)
_cell_length_b                   22.2125(3)
_cell_length_c                   15.9788(2)
_cell_measurement_reflns_used    21405
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      75.2570
_cell_measurement_theta_min      3.3420
_cell_volume                     3988.12(8)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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      298.15
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_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    -23.00  33.00   0.50    0.50    --  -44.30  19.00   0.00  112
  2  \w     -8.00  36.00   0.50    0.50    --  -44.30  19.00-120.00   88
  3  \w    -20.00  33.00   0.50    0.50    --  -44.30  19.00-150.00  106
  4  \w    -43.00 -14.00   0.50    2.00    --  -90.25  45.00  60.00   58
  5  \w    -42.00 -15.00   0.50    2.00    --  -90.25  45.00  90.00   54
  6  \w    -22.00  34.00   0.50    0.50    --  -44.30  19.00 150.00  112
  7  \w     50.00  90.00   0.50    0.50    --   44.30-133.00 158.00   80
  8  \w     53.00  78.00   0.50    2.00    --  109.26-133.00 158.00   50
  9  \w     79.00 104.00   0.50    2.00    --  109.26 -95.00 114.01   50
 10  \w     49.00  74.00   0.50    0.50    --   44.30-135.00 -20.00   50
 11  \w     42.00 116.00   0.50    2.00    --  109.26-135.00 -20.00  148
 12  \w     47.00  72.00   0.50    2.00    --  109.26 -94.00 -60.00   50
 13  \w     43.00 105.00   0.50    2.00    --  109.26 -77.00 -30.00  124
 14  \w     72.00 104.00   0.50    2.00    --  109.26 -99.00-138.77   64
 15  \w     36.00  66.00   0.50    2.00    --  109.26 -61.00 -30.00   60
 16  \w     36.00  88.00   0.50    2.00    --  109.26 -94.00 -30.00  104
 17  \w     33.00 105.00   0.50    2.00    --  109.26-105.00  95.80  144
 18  \w     41.00 108.00   0.50    2.00    --  109.26-125.00  90.00  134
 19  \w     88.00 170.00   0.50    2.00    --  109.26  30.00 120.00  164
 20  \w    110.00 135.00   0.50    2.00    --  109.26 135.00  45.00   50
 21  \w     89.00 178.00   0.50    2.00    --  109.26  61.00 -30.00  178
 22  \w    118.00 144.00   0.50    2.00    --  109.26 133.00-133.00   52
 23  \w     91.00 177.00   0.50    2.00    --  109.26  61.00  30.00  172
 24  \w    -78.00 -53.00   0.50    2.00    --  -90.25 133.00-133.00   50
 25  \w    -87.00 -60.00   0.50    0.50    --  -44.30 133.00-133.00   54
 26  \w   -117.00 -73.00   0.50    0.50    --  -44.30-135.00 -20.00   88
 27  \w   -103.00 -72.00   0.50    2.00    --  -90.25-135.00 -20.00   62
 28  \w   -116.00 -77.00   0.50    0.50    --  -44.30-133.00 158.00   78
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0091775000
_diffrn_orient_matrix_UB_12      -0.0675723000
_diffrn_orient_matrix_UB_13      0.0208876000
_diffrn_orient_matrix_UB_21      -0.0452094000
_diffrn_orient_matrix_UB_22      -0.0155941000
_diffrn_orient_matrix_UB_23      -0.0890797000
_diffrn_orient_matrix_UB_31      0.1290472000
_diffrn_orient_matrix_UB_32      -0.0006520000
_diffrn_orient_matrix_UB_33      -0.0306116000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29966
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.482
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.80411
_refine_diff_density_max         3.087
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0520
_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^)+(0.1058P)^2^+4.8005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6872
_reflns_number_total             8005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07736h2.cif
_cod_data_source_block           4-methylaniline
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'N' was changed to 'n' 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 (97 times).

data item '_geom_angle_publ_flag' value 'Y' was changed to 'y' 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 (4 times).

data item '_geom_bond_publ_flag' value 'N' was changed to 'n' 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 (53 times).

data item '_geom_bond_publ_flag' value 'Y' was changed to 'y' 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 (9 times).

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7243926
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H34F6N6O6S2Ru
_chemical_oxdiff_usercomment     '298 K'
_shelx_estimated_absorpt_t_max   1.00000
_shelx_estimated_absorpt_t_min   0.80411
_diffrn_oxdiff_digest_frames
;
017b5f5a67fb37692e3af5569d495bdbfb000295a4e
;
_diffrn_oxdiff_digest_hkl
;
0143ecd6f679cba7ccda5bde9bb66575f50352
;
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C15(H15), C24(H24), C9(H9), C18(H18), C27(H27), C26(H26), C6(H6),
 C28(H28), C10(H10), C34(H34), C31(H31), C23(H23), C33(H33), C32(H32), C2(H2),
 C22(H22), C16(H16), C13(H13), C5(H5), C21(H21), C12(H12), C17(H17), C3(H3)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
;
_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 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.831