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_7243922
_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         'C32 H26 N6 Ru, 2(F6 P)'
_chemical_formula_sum            'C32 H26 F12 N6 P2 Ru'
_chemical_formula_weight         885.60
_chemical_name_common
'N1-phenylcyclohexa-3,5-diene-1,2-diiminebis(2,2'-bipyridine)ruthenium hexafulolophosphate'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-16 deposited with the CCDC.	2021-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.31180(10)
_cell_length_b                   18.79730(10)
_cell_length_c                   13.97790(10)
_cell_measurement_reflns_used    18776
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      75.5780
_cell_measurement_theta_min      3.3310
_cell_volume                     3468.37(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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    -80.00 -42.00   0.50    0.15    --  -42.55 113.00 150.00   76
  2  \w     52.00  78.00   0.50    0.15    --   42.55-113.00  58.00   52
  3  \w   -116.00 -91.00   0.50    0.60    --  -90.25-113.00  58.00   50
  4  \w    -81.00 -42.00   0.50    0.60    --  -90.25 113.00 150.00   78
  5  \w     70.00  98.00   0.50    0.60    --  109.88-113.00  58.00   56
  6  \w    105.00 152.00   0.50    0.60    --  109.88 113.00 150.00   94
  7  \w    -21.00  37.00   0.50    0.15    --  -42.55  19.00-180.00  116
  8  \w    -22.00  36.00   0.50    0.15    --  -42.55  19.00  60.00  116
  9  \w    -22.00  32.00   0.50    0.15    --  -42.55  19.00 -90.00  108
 10  \w    -33.00  32.00   0.50    0.15    --  -42.55  37.00 -60.00  130
 11  \w     95.00 120.00   0.50    0.15    --   42.55 178.00-120.00   50
 12  \w    -41.00 -14.00   0.50    0.60    --  -90.25  45.00-120.00   54
 13  \w    -43.00 -18.00   0.50    0.60    --  -90.25  45.00  60.00   50
 14  \w    -42.00 -15.00   0.50    0.60    --  -90.25  45.00   0.00   54
 15  \w    -43.00 -17.00   0.50    0.60    --  -90.25  45.00 -90.00   52
 16  \w    -41.00 -14.00   0.50    0.60    --  -90.25  45.00 -30.00   54
 17  \w    -43.00 -18.00   0.50    0.60    --  -90.25  45.00 -60.00   50
 18  \w    -43.00 -17.00   0.50    0.60    --  -90.25  45.00  90.00   52
 19  \w     34.00  59.00   0.50    0.60    --  109.88 -45.00 -90.00   50
 20  \w     34.00  59.00   0.50    0.60    --  109.88 -45.00-120.00   50
 21  \w     34.00  59.00   0.50    0.60    --  109.88 -45.00 -60.00   50
 22  \w     46.00  79.00   0.50    0.60    --  109.88 -61.00   0.00   66
 23  \w     38.00  64.00   0.50    0.60    --  109.88 -61.00  90.00   52
 24  \w     35.00  61.00   0.50    0.60    --  109.88 -45.00-150.00   52
 25  \w     35.00  61.00   0.50    0.60    --  109.88 -45.00 -30.00   52
 26  \w     91.00 151.00   0.50    0.60    --  109.88  30.00-120.00  120
 27  \w     37.00 109.00   0.50    0.60    --  109.88 -77.00  90.00  144
 28  \w     39.00  78.00   0.50    0.60    --  109.88 -61.00-150.00   78
 29  \w     34.00  61.00   0.50    0.60    --  109.88 -45.00 120.00   54
 30  \w     40.00 101.00   0.50    0.60    --  109.88 -94.00 -60.00  122
 31  \w     34.00  59.00   0.50    0.60    --  109.88 -45.00 150.00   50
 32  \w     53.00 104.00   0.50    0.60    --  109.88 -94.00  90.00  102
 33  \w     36.00  61.00   0.50    0.60    --  109.88 -45.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534730000
_diffrn_orient_matrix_UB_12      -0.0199646000
_diffrn_orient_matrix_UB_13      0.0876338000
_diffrn_orient_matrix_UB_21      -0.0321749000
_diffrn_orient_matrix_UB_22      0.0781098000
_diffrn_orient_matrix_UB_23      0.0097059000
_diffrn_orient_matrix_UB_31      -0.0986435000
_diffrn_orient_matrix_UB_32      -0.0146895000
_diffrn_orient_matrix_UB_33      -0.0676570000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25055
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.608
_diffrn_reflns_theta_min         3.348
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93290
_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 blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.93290
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0532P)^2^+1.8550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6425
_reflns_number_total             6959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07736h2.cif
_cod_data_source_block           exp_14
_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 (101 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 (6 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 (49 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 (10 times).

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7243922
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H26F12N6P2Ru
_chemical_oxdiff_usercomment     '298 K'
_diffrn_oxdiff_digest_frames
;
012453944d8e9f8c05bbf566d29a4d71e8000410b70
;
_diffrn_oxdiff_digest_hkl
;
019a6e6e2700455525ffb7962a37564e3e8d37
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C29(H23), C32(H26), C6(H5), C5(H4), C3(H2), C22(H18), C30(H24), C4(H3),
 C31(H25), C12(H10), C8(H6), C26(H22), C19(H15), C13(H11), C23(H19), C11(H9),
 C21(H17), C14(H12), C24(H20), C25(H21), C16(H14), C15(H13), C10(H8), C20(H16),
 C9(H7)
;
_shelx_res_checksum              6475
_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 1.154
_oxdiff_exptl_absorpt_empirical_full_min 0.883