Intrinsically chiral paddlewheel diruthenium complexes
Coloma, Isabel; Herrero, Santiago; Cortijo, Miguel; CrystEngComm 26 (2024) 6739–6747; doi:10.1039/D4CE01040J

data_7249577
_publ_section_title
;
 Intrinsically chiral paddlewheel diruthenium complexes
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6739
_journal_page_last               6747
_journal_paper_doi               10.1039/D4CE01040J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C38 H40 Cl N6 O6 Ru2, C3 H6'
_chemical_formula_sum            'C41 H46 Cl N6 O6 Ru2'
_chemical_formula_weight         956.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                93.766(2)
_cell_angle_beta                 109.216(3)
_cell_angle_gamma                112.885(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9823(4)
_cell_length_b                   13.7386(4)
_cell_length_c                   14.3812(4)
_cell_measurement_reflns_used    16502
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      68.1420
_cell_measurement_theta_min      3.3290
_cell_volume                     2175.45(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.98a 64-bit (release 24-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_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     34.00  70.00   0.50    0.42    --  105.13-125.00 120.00   72
  2  \w     86.00 111.00   0.50    0.42    --  105.13-125.00 120.00   50
  3  \w     55.00 104.00   0.50    0.42    --  105.13-125.00  60.00   98
  4  \w     59.00  96.00   0.50    0.42    --  105.13 -95.00 -90.00   74
  5  \w     62.00  87.00   0.50    0.42    --  105.13 -95.00-150.00   50
  6  \w     33.00 111.00   0.50    0.42    --  105.13-125.00 -90.00  156
  7  \w     38.00  68.00   0.50    0.42    --  105.13 -95.00  60.00   60
  8  \w     43.00  75.00   0.50    0.42    --  105.13 -61.00 120.00   64
  9  \w     36.00  73.00   0.50    0.42    --  105.13 -61.00  90.00   74
 10  \w     36.00  61.00   0.50    0.42    --  105.13 -61.00 -30.00   50
 11  \w     27.00  52.00   0.50    0.42    --  105.13 -45.00  30.00   50
 12  \w     40.00  65.00   0.50    0.42    --  105.13 -61.00 -90.00   50
 13  \w    -29.00  32.00   0.50    0.22    --   48.48 -48.00-178.00  122
 14  \w     28.00  53.00   0.50    0.42    --  105.13 -48.00-178.00   50
 15  \w     27.00  53.00   0.50    0.42    --  105.13 -45.00 -90.00   52
 16  \w     27.00  54.00   0.50    0.42    --  105.13 -45.00 -30.00   54
 17  \w     28.00  53.00   0.50    0.42    --  105.13 -45.00  60.00   50
 18  \w     53.00  79.00   0.50    0.22    --   48.48  48.00 -30.00   52
 19  \w    109.00 135.00   0.50    0.42    --  105.13  48.00 -30.00   52
 20  \w     90.00 138.00   0.50    0.42    --  105.13  30.00 -90.00   96
 21  \w    129.00 168.00   0.50    0.42    --  105.13  45.00 -90.00   78
 22  \w    110.00 178.00   0.50    0.42    --  105.13  45.00-180.00  136
 23  \w    -23.00  29.00   0.50    0.22    --  -49.98  19.00 120.00  104
 24  \w    -41.00 -15.00   0.50    0.42    --  -87.78  45.00  60.00   52
 25  \w   -102.00 -35.00   0.50    0.42    --  -87.78  77.00 120.00  134
 26  \w    -42.00 -10.00   0.50    0.42    --  -87.78  45.00 150.00   64
 27  \w    -49.00  28.00   0.50    0.22    --  -49.98  48.00 -30.00  154
 28  \w    -44.00 -15.00   0.50    0.42    --  -87.78  45.00  30.00   58
 29  \w    -43.00 -17.00   0.50    0.42    --  -87.78  48.00 -30.00   52
 30  \w    -67.00 -30.00   0.50    0.42    --  -87.78  61.00 -90.00   74
 31  \w    -46.00 -16.00   0.50    0.42    --  -87.78  45.00-180.00   60
 32  \w   -124.00 -25.00   0.50    0.42    --  -95.50 142.00 -91.76  198
 33  \w   -108.00 -48.00   0.50    0.42    --  -95.50 108.00 160.54  120
 34  \w   -145.00 -79.00   0.50    0.42    --  -87.78 -30.00  60.00  132
 35  \w   -159.00 -85.00   0.50    0.42    --  -87.78-125.00 150.00  148
 36  \w   -160.00 -71.00   0.50    0.42    --  -87.78 -48.00-178.00  178
 37  \w   -123.00 -48.00   0.50    0.22    --  -49.98 -48.00-178.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0931085000
_diffrn_orient_matrix_UB_12      0.0338015000
_diffrn_orient_matrix_UB_13      0.0181060000
_diffrn_orient_matrix_UB_21      -0.0229479000
_diffrn_orient_matrix_UB_22      -0.0827293000
_diffrn_orient_matrix_UB_23      0.0668046000
_diffrn_orient_matrix_UB_31      0.1014397000
_diffrn_orient_matrix_UB_32      0.0871599000
_diffrn_orient_matrix_UB_33      0.0935263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25322
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.072
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.603
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.100a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       prism
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         8721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0708P)^2^+2.6225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8206
_reflns_number_total             8721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01040j2.cif
_cod_data_source_block           ic176c
_cod_depositor_comments
'Adding full bibliography for 7249576--7249579.cif.'
_cod_original_cell_volume        2175.45(12)
_cod_database_code               7249577
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C37H40N6O34Ru2Cl
_chemical_oxdiff_usercomment     'IC176C 150K'
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.446
_diffrn_oxdiff_digest_frames     0153373d3283418857a8999d28a92af1db03268f633
_diffrn_oxdiff_digest_hkl        011e52d3f4bd9689465f26a677924c1974f37b
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H18A)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=
 Sof(H22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(O3B)=1-FVAR(1)
 Sof(H18)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(O3A)=FVAR(1)
 Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=
 Sof(H42C)=Sof(H42D)=Sof(H40C)=Sof(H40D)=Sof(H43C)=Sof(H43D)=Sof(H44C)=
 Sof(H44D)=0.5*(1-FVAR(3))
 Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C42A)=
 Sof(H42A)=Sof(H42B)=Sof(H40A)=Sof(H40B)=Sof(H43A)=Sof(H43B)=Sof(H44A)=
 Sof(H44B)=0.5*FVAR(3)
 Fixed Sof: C40(0.5) C43(0.5) C44(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C39A(H39A,H39B), C41A(H41A,H41B), C42A(H42A,H42B), C39B(H39C,H39D), C41B(H41C,
 H41D), C42B(H42C,H42D), C40(H40A,H40B), C40(H40C,H40D), C43(H43A,H43B),
 C43(H43C,H43D), C44(H44A,H44B), C44(H44C,H44D)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C18(H18A), C18(H18), C19A(H19A), C21A(H21A), C22A(H22A),
 C19B(H19B), C21B(H21B), C22B(H22B), C25(H25), C26(H26), C28(H28), C29(H29),
 C34(H34), C35(H35), C36(H36)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C23A(H23A,H23B,H23C), C23B(H23D,H23E,
 H23F), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              4180
_shelx_hkl_checksum              46576
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.889