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_7044459
_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         'C23 H23 Cl5 N6 O Ru2'
_chemical_formula_sum            'C23 H23 Cl5 N6 O Ru2'
_chemical_formula_weight         778.86
_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             2017-08-14
_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                77.1190(10)
_cell_angle_beta                 84.0320(10)
_cell_angle_gamma                71.1160(10)
_cell_formula_units_Z            2
_cell_length_a                   9.79250(10)
_cell_length_b                   11.28330(10)
_cell_length_c                   15.4471(2)
_cell_measurement_reflns_used    25740
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9170
_cell_measurement_theta_min      2.1170
_cell_volume                     1573.33(3)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -16.00  68.00   0.50    5.00    --   -4.80  37.00  30.00  168
  2  \w    -26.00  36.00   0.50    5.00    --    3.71 -99.00 -30.00  124
  3  \w    -26.00  36.00   0.50    5.00    --    3.71 -99.00 -90.00  124
  4  \w    -26.00  36.00   0.50    5.00    --    3.71 -99.00-150.00  124
  5  \w    -26.00  27.00   0.50    5.00    --   -4.80 -99.00 -60.00  106
  6  \w    -26.00  27.00   0.50    5.00    --   -4.80 -99.00  30.00  106
  7  \w    -26.00  27.00   0.50    5.00    --   -4.80 -99.00  90.00  106
  8  \w    -68.00  25.00   0.50    5.00    --    3.71 -77.00 -60.00  186
  9  \w    -68.00  62.00   0.50    5.00    --    3.71   0.00  30.00  260
 10  \w    -71.00 -46.00   0.50    5.00    --    3.71 -19.00 120.00   50
 11  \w    -77.00   6.00   0.50    5.00    --   -4.80 -37.00-150.00  166
;
_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      -0.0245956000
_diffrn_orient_matrix_UB_12      -0.0110682000
_diffrn_orient_matrix_UB_13      0.0450182000
_diffrn_orient_matrix_UB_21      0.0688685000
_diffrn_orient_matrix_UB_22      -0.0052519000
_diffrn_orient_matrix_UB_23      0.0139133000
_diffrn_orient_matrix_UB_31      -0.0227941000
_diffrn_orient_matrix_UB_32      0.0667093000
_diffrn_orient_matrix_UB_33      -0.0010737000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37538
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.858
_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_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+1.1927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5645
_reflns_number_total             5961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03085a2.cif
_cod_data_source_block           rju2_abs
_cod_original_cell_volume        1573.34(3)
_cod_database_code               7044459
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Ru2N6Cl5C23H23O
_chemical_oxdiff_usercomment     'Crystallized from DMF/MeOH'
_reflns_odcompleteness_completeness 99.98
_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
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C20(H20),
 C19(H19), C18(H18), C17(H17), C14(H14), C13(H13), C12(H12), C11(H11), C21(H21)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_fab_checksum              87667
_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 1.141
_oxdiff_exptl_absorpt_empirical_full_min 0.906