Dinuclear nitrido-bridged ruthenium complexes bearing diimine ligands
Urgiles, Julie; Nathan, Sarah R.; MacMillan, Samantha N.; Wilson, Justin J.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03085A

data_7044460
_publ_section_title
;
 Dinuclear nitrido-bridged ruthenium complexes bearing diimine ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03085A
_journal_year                    2017
_chemical_formula_moiety         'C27 H31 Cl5 N6 O5 Ru2'
_chemical_formula_sum            'C27 H31 Cl5 N6 O5 Ru2'
_chemical_formula_weight         898.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-10
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_audit_update_record
;
2017-08-17 deposited with the CCDC.
2017-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                98.4980(10)
_cell_angle_beta                 106.815(2)
_cell_angle_gamma                111.247(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2823(3)
_cell_length_b                   12.5160(2)
_cell_length_c                   15.2094(2)
_cell_measurement_reflns_used    16874
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.7990
_cell_measurement_theta_min      3.0960
_cell_volume                     2000.61(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  72.00   0.50    1.00    --   47.80 -83.00  94.00  190
  2  \w     60.00  85.00   0.50    2.50    --  107.75 -83.00  94.00   50
  3  \w     78.00 103.00   0.50    2.50    --  107.75 -94.00  60.00   50
  4  \w     94.00 130.00   0.50    2.50    --  107.75 -77.00  60.00   72
  5  \w     84.00 117.00   0.50    2.50    --  107.75-125.00   0.00   66
  6  \w     76.00 106.00   0.50    2.50    --  107.75 -94.00  30.00   60
  7  \w     94.00 122.00   0.50    2.50    --  107.75 -61.00 -30.00   56
  8  \w     65.00  91.00   0.50    2.50    --  107.75 -61.00 -30.00   52
  9  \w     65.00  96.00   0.50    2.50    --  107.75 -77.00 -60.00   62
 10  \w     88.00 120.00   0.50    2.50    --  107.75-125.00-120.00   64
 11  \w     63.00 113.00   0.50    2.50    --  107.75 -30.00-150.00  100
 12  \w    105.00 131.00   0.50    2.50    --  107.75  30.00-180.00   52
 13  \w    137.00 163.00   0.50    2.50    --  107.75  30.00-180.00   52
 14  \w    149.00 178.00   0.50    2.50    --  107.75  45.00-180.00   58
 15  \w     99.00 178.00   0.50    2.50    --  107.75  30.00-150.00  158
 16  \w     89.00 178.00   0.50    2.50    --  107.75  83.00-144.00  178
 17  \w    104.00 132.00   0.50    2.50    --  107.75  15.00  90.00   56
 18  \w    137.00 166.00   0.50    2.50    --  107.75  15.00  90.00   58
 19  \w    110.00 177.00   0.50    2.50    --  107.75  77.00 120.00  134
 20  \w     97.00 177.00   0.50    2.50    --  107.75  30.00 150.00  160
 21  \w     95.00 120.00   0.50    2.50    --  107.75-125.00 150.00   50
 22  \w     67.00  99.00   0.50    2.50    --  107.75 -94.00  90.00   64
 23  \w     46.00 119.00   0.50    2.50    --  107.75-125.00  60.00  146
 24  \w     37.00 108.00   0.50    2.50    --  107.75 -94.00 -90.00  142
 25  \w     46.00  72.00   0.50    2.50    --  107.75 -94.00-180.00   52
 26  \w     41.00  88.00   0.50    2.50    --  107.75 -94.00-150.00   94
 27  \w     37.00 120.00   0.50    2.50    --  107.75-125.00 -60.00  166
 28  \w     38.00  94.00   0.50    2.50    --  107.75 -61.00  90.00  112
 29  \w     48.00  79.00   0.50    2.50    --  107.75-125.00 150.00   62
 30  \w     39.00  65.00   0.50    2.50    --  107.75 -94.00  90.00   52
 31  \w     38.00  64.00   0.50    2.50    --  107.75 -94.00  60.00   52
 32  \w     47.00 116.00   0.50    2.50    --  107.75 -45.00 120.00  138
 33  \w     39.00  65.00   0.50    2.50    --  107.75 -94.00  30.00   52
 34  \w     38.00 115.00   0.50    2.50    --  107.75 -45.00-120.00  154
 35  \w     34.00  80.00   0.50    1.00    --   47.80-125.00-150.00   92
 36  \w     35.00 109.00   0.50    2.50    --  107.75 -15.00-150.00  148
 37  \w     55.00  97.00   0.50    1.00    --   47.80  83.00-144.00   84
 38  \w    -58.00  15.00   0.50    1.00    --  -47.80  37.00 -30.00  146
 39  \w    -65.00  24.00   0.50    1.00    --  -47.80  83.00-144.00  178
 40  \w    -58.00  13.00   0.50    1.00    --  -47.80  19.00-150.00  142
 41  \w    -69.00 -44.00   0.50    2.50    --  -86.25  83.00-144.00   50
 42  \w    -62.00 -32.00   0.50    2.50    --  -86.25  45.00  60.00   60
 43  \w    -91.00 -66.00   0.50    1.00    --  -47.80 -83.00  94.00   50
 44  \w   -118.00 -80.00   0.50    1.00    --  -47.80-125.00 -90.00   76
 45  \w   -134.00-109.00   0.50    2.50    --  -86.25 -83.00  94.00   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      0.0115597000
_diffrn_orient_matrix_UB_12      0.0888580000
_diffrn_orient_matrix_UB_13      0.0876876000
_diffrn_orient_matrix_UB_21      -0.1435143000
_diffrn_orient_matrix_UB_22      -0.0409029000
_diffrn_orient_matrix_UB_23      -0.0406812000
_diffrn_orient_matrix_UB_31      -0.0169804000
_diffrn_orient_matrix_UB_32      -0.0969144000
_diffrn_orient_matrix_UB_33      0.0531826000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27775
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.072
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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            'clear red'
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+1.4263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7119
_reflns_number_total             7570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03085a2.cif
_cod_data_source_block           rju1_abs
_cod_original_cell_volume        2000.61(7)
_cod_database_code               7044460
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Ru2N6Cl5C27H31O5
_chemical_oxdiff_usercomment     'Crystallized from DMF/MeOH'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C17(H17), C19(H19), C20(H20), C21(H21)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_fab_checksum              33350
_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 1.549
_oxdiff_exptl_absorpt_empirical_full_min 0.684