#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:51:41 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289487 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/48/7714816.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714816
loop_
_publ_author_name
'Biswas, Mitrali'
'Dey, Sanchaita'
'Dhara, Suman'
'Panda, Sanjib'
'Lahiri, Goutam Kumar'
_publ_section_title
;
 Metal-ligand synergy driven functionalisation of alkylene linked
 bis(aldimine) on a diruthenium(II) platform. Cyclisation versus
 oxygenation.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2167
_journal_page_last               2180
_journal_paper_doi               10.1039/d3dt03730d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C34 H42 N4 O8 Ru2, 2(Cl O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H46 Cl6 N4 O16 Ru2'
_chemical_formula_weight         1205.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-17 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.810(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9403(5)
_cell_length_b                   12.6420(2)
_cell_length_c                   22.9581(7)
_cell_measurement_reflns_used    13879
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      31.2990
_cell_measurement_theta_min      1.9510
_cell_volume                     4726.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ   -100.21 132.59   0.80    4.00  15.81  -9.84 -59.25    --   291
  2  ω   -100.81  15.19   0.80    4.00    --   -9.84 -59.25 -51.92  145
  3  ω   -100.81  15.19   0.80    4.00    --   -9.84 -59.25  92.08  145
  4  ω   -100.81  15.19   0.80    4.00    --   -9.84 -59.25  20.08  145
  5  ω   -100.81  15.19   0.80    4.00    --   -9.84 -59.25 164.08  145
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0038929000
_diffrn_orient_matrix_UB_12      -0.0550362000
_diffrn_orient_matrix_UB_13      0.0065794000
_diffrn_orient_matrix_UB_21      0.0245705500
_diffrn_orient_matrix_UB_22      0.0107353500
_diffrn_orient_matrix_UB_23      0.0328273000
_diffrn_orient_matrix_UB_31      -0.0357928500
_diffrn_orient_matrix_UB_32      0.0014569500
_diffrn_orient_matrix_UB_33      0.0059250000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            67540
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.786
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0413
_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/[σ²(Fo²)+(0.0296P)²+15.4248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6301
_reflns_number_total             8096
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           '[2](ClO4)2_autored'
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714816
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 85.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.71
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C4(H4), C1(H1), C15(H15), C10(H10)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C)
;
_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 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.799
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.30964(2) 0.31122(2) 0.68499(2) 0.02100(6) Uani 1 1 d . . . . .
Cl1 Cl 0.07641(4) 0.70979(5) 0.39606(3) 0.03135(13) Uani 1 1 d . . . . .
Cl2 Cl 0.07491(6) 1.04155(7) 0.47449(5) 0.0563(2) Uani 1 1 d . . . . .
Cl3 Cl 0.02047(7) 1.25776(9) 0.43833(7) 0.0811(4) Uani 1 1 d . . . . .
O1 O 0.38353(11) 0.19795(13) 0.74095(9) 0.0272(4) Uani 1 1 d . . . . .
O2 O 0.30087(11) 0.23744(13) 0.60551(8) 0.0260(3) Uani 1 1 d . . . . .
O3 O 0.32069(11) 0.38487(14) 0.76513(9) 0.0280(4) Uani 1 1 d . . . . .
O4 O 0.21338(11) 0.22566(14) 0.68214(9) 0.0289(4) Uani 1 1 d . . . . .
N1 N 0.23826(12) 0.43038(16) 0.62978(10) 0.0228(4) Uani 1 1 d . . . . .
N2 N 0.39709(12) 0.41136(16) 0.68128(9) 0.0221(4) Uani 1 1 d . . . . .
O6 O 0.15866(13) 0.66947(18) 0.42514(12) 0.0455(5) Uani 1 1 d . . . . .
O8 O 0.07238(17) 0.80590(18) 0.42708(15) 0.0581(7) Uani 1 1 d . . . . .
O5 O 0.02168(15) 0.6350(2) 0.40289(14) 0.0610(7) Uani 1 1 d . . . . .
C5 C 0.28074(14) 0.51158(18) 0.61856(11) 0.0222(4) Uani 1 1 d . . . . .
O7 O 0.05628(18) 0.7306(3) 0.33005(12) 0.0754(9) Uani 1 1 d . . . . .
C6 C 0.36934(15) 0.49643(19) 0.64820(12) 0.0238(5) Uani 1 1 d . . . . .
H6 H 0.405352 0.547240 0.643363 0.029 Uiso 1 1 calc R . . . .
C7 C 0.48631(14) 0.3958(2) 0.71349(11) 0.0246(5) Uani 1 1 d . . . . .
H7A H 0.514556 0.453312 0.701403 0.029 Uiso 1 1 calc R . . . .
H7B H 0.501173 0.327687 0.699895 0.029 Uiso 1 1 calc R . . . .
C11 C 0.31706(16) 0.1378(2) 0.60452(13) 0.0287(5) Uani 1 1 d . . . . .
C2 C 0.11381(16) 0.5242(2) 0.57144(13) 0.0327(6) Uani 1 1 d . . . . .
H2 H 0.055765 0.527835 0.556032 0.039 Uiso 1 1 calc R . . . .
C3 C 0.15662(17) 0.6059(2) 0.55975(13) 0.0316(5) Uani 1 1 d . . . . .
H3 H 0.128241 0.666086 0.535966 0.038 Uiso 1 1 calc R . . . .
C9 C 0.38363(16) 0.1026(2) 0.72214(13) 0.0302(5) Uani 1 1 d . . . . .
C4 C 0.24151(16) 0.5996(2) 0.58301(12) 0.0275(5) Uani 1 1 d . . . . .
H4 H 0.271978 0.654450 0.574730 0.033 Uiso 1 1 calc R . . . .
C1 C 0.15628(15) 0.4364(2) 0.60595(13) 0.0278(5) Uani 1 1 d . . . . .
H1 H 0.126423 0.379393 0.612785 0.033 Uiso 1 1 calc R . . . .
C16 C 0.19123(16) 0.2203(2) 0.72906(15) 0.0319(6) Uani 1 1 d . . . . .
C14 C 0.28797(17) 0.3533(2) 0.80245(13) 0.0329(6) Uani 1 1 d . . . . .
C15 C 0.22697(18) 0.2774(2) 0.78660(14) 0.0356(6) Uani 1 1 d . . . . .
H15 H 0.207169 0.262299 0.818136 0.043 Uiso 1 1 calc R . . . .
C10 C 0.35268(18) 0.0718(2) 0.65796(14) 0.0333(6) Uani 1 1 d . . . . .
H10 H 0.356169 -0.001256 0.649773 0.040 Uiso 1 1 calc R . . . .
C12 C 0.2965(2) 0.0934(2) 0.53889(14) 0.0388(6) Uani 1 1 d . . . . .
H12A H 0.263167 0.144612 0.506320 0.058 Uiso 1 1 calc GR . . . .
H12B H 0.265526 0.027458 0.533448 0.058 Uiso 1 1 calc GR . . . .
H12C H 0.347279 0.079147 0.534059 0.058 Uiso 1 1 calc GR . . . .
C8 C 0.4206(2) 0.0223(2) 0.77470(16) 0.0424(7) Uani 1 1 d . . . . .
H8A H 0.472168 0.049769 0.807506 0.064 Uiso 1 1 calc GR . . . .
H8B H 0.431346 -0.043318 0.756796 0.064 Uiso 1 1 calc GR . . . .
H8C H 0.382241 0.007882 0.794088 0.064 Uiso 1 1 calc GR . . . .
C17 C 0.12110(18) 0.1465(2) 0.71778(16) 0.0399(7) Uani 1 1 d . . . . .
H17A H 0.085494 0.143196 0.671742 0.060 Uiso 1 1 calc GR . . . .
H17B H 0.089477 0.172430 0.740812 0.060 Uiso 1 1 calc GR . . . .
H17C H 0.142478 0.075793 0.733413 0.060 Uiso 1 1 calc GR . . . .
C13 C 0.3177(2) 0.4083(3) 0.86570(14) 0.0434(7) Uani 1 1 d . . . . .
H13A H 0.376846 0.396724 0.889495 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.288901 0.380117 0.890392 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.306750 0.484320 0.858744 0.065 Uiso 1 1 calc GR . . . .
C18 C 0.0651(3) 1.1680(3) 0.5031(2) 0.0661(11) Uani 1 1 d . . . . .
H18A H 0.119892 1.194175 0.532934 0.079 Uiso 1 1 calc R . . . .
H18B H 0.030286 1.163261 0.526914 0.079 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 O4 87.97(7) . . ?
O1 Ru1 N1 177.76(8) . . ?
O1 Ru1 N2 98.99(8) . . ?
O2 Ru1 O1 91.68(7) . . ?
O2 Ru1 O3 178.93(7) . . ?
O2 Ru1 O4 88.95(7) . . ?
O2 Ru1 N1 89.36(7) . . ?
O2 Ru1 N2 91.07(7) . . ?
O3 Ru1 O1 87.67(7) . . ?
O3 Ru1 O4 91.87(8) . . ?
O3 Ru1 N1 91.26(8) . . ?
O3 Ru1 N2 88.20(8) . . ?
O4 Ru1 N1 94.03(8) . . ?
O4 Ru1 N2 173.04(8) . . ?
N1 Ru1 N2 79.01(8) . . ?
O8 Cl1 O6 109.18(16) . . ?
O8 Cl1 O7 109.28(19) . . ?
O5 Cl1 O6 109.66(16) . . ?
O5 Cl1 O8 109.30(16) . . ?
O5 Cl1 O7 111.20(19) . . ?
O7 Cl1 O6 108.20(15) . . ?
C9 O1 Ru1 123.35(18) . . ?
C11 O2 Ru1 122.57(17) . . ?
C14 O3 Ru1 124.85(18) . . ?
C16 O4 Ru1 123.92(18) . . ?
C5 N1 Ru1 114.72(15) . . ?
C1 N1 Ru1 126.32(17) . . ?
C1 N1 C5 118.9(2) . . ?
C6 N2 Ru1 115.29(16) . . ?
C6 N2 C7 118.6(2) . . ?
C7 N2 Ru1 126.13(15) . . ?
N1 C5 C6 113.5(2) . . ?
N1 C5 C4 122.0(2) . . ?
C4 C5 C6 124.5(2) . . ?
N2 C6 C5 117.4(2) . . ?
N2 C7 C7 109.4(2) . 2_656 ?
O2 C11 C10 126.1(2) . . ?
O2 C11 C12 114.7(2) . . ?
C10 C11 C12 119.2(2) . . ?
C3 C2 C1 119.5(2) . . ?
C2 C3 C4 119.5(2) . . ?
O1 C9 C10 124.2(2) . . ?
O1 C9 C8 115.4(3) . . ?
C10 C9 C8 120.4(2) . . ?
C5 C4 C3 118.5(2) . . ?
N1 C1 C2 121.6(2) . . ?
O4 C16 C15 125.3(2) . . ?
O4 C16 C17 114.6(3) . . ?
C15 C16 C17 120.1(3) . . ?
O3 C14 C15 124.8(3) . . ?
O3 C14 C13 115.2(3) . . ?
C15 C14 C13 119.9(3) . . ?
C14 C15 C16 127.1(3) . . ?
C9 C10 C11 126.5(2) . . ?
Cl2 C18 Cl3 110.4(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 O1 2.0072(17) . ?
Ru1 O2 1.9960(17) . ?
Ru1 O3 1.9963(17) . ?
Ru1 O4 2.0155(17) . ?
Ru1 N1 2.038(2) . ?
Ru1 N2 2.0454(19) . ?
Cl1 O6 1.434(2) . ?
Cl1 O8 1.425(2) . ?
Cl1 O5 1.419(2) . ?
Cl1 O7 1.427(3) . ?
Cl2 C18 1.765(4) . ?
Cl3 C18 1.772(5) . ?
O1 C9 1.281(3) . ?
O2 C11 1.295(3) . ?
O3 C14 1.288(3) . ?
O4 C16 1.297(3) . ?
N1 C5 1.366(3) . ?
N1 C1 1.339(3) . ?
N2 C6 1.290(3) . ?
N2 C7 1.468(3) . ?
C5 C6 1.456(3) . ?
C5 C4 1.385(3) . ?
C7 C7 1.537(5) 2_656 ?
C11 C10 1.397(4) . ?
C11 C12 1.501(4) . ?
C2 C3 1.379(4) . ?
C2 C1 1.390(4) . ?
C3 C4 1.389(4) . ?
C9 C10 1.394(4) . ?
C9 C8 1.502(4) . ?
C16 C15 1.402(4) . ?
C16 C17 1.498(4) . ?
C14 C15 1.384(4) . ?
C14 C13 1.493(4) . ?
