#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:52:50 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229981 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/67/7046701.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_7046701
loop_
_publ_author_name
'Sengupta, Gargi'
'Pandey, Pragati'
'De, Subhabrata'
'Ramapanicker, Ramesh'
'Bera, Jitendra K.'
_publ_section_title
;
 A bromo-capped diruthenium(i,i) N-heterocyclic carbene compound for in
 situ bromine generation with NBS: catalytic olefin aziridination
 reactions.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11917
_journal_page_last               11924
_journal_paper_doi               10.1039/c8dt01851k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C36 H36 I2 N8 O4 Ru2'
_chemical_formula_sum            'C36 H36 I2 N8 O4 Ru2'
_chemical_formula_weight         1100.67
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-05-07 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.118(2)
_cell_length_b                   21.118(2)
_cell_length_c                   17.870(3)
_cell_measurement_reflns_used    5941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.90
_cell_measurement_theta_min      2.23
_cell_volume                     6901.8(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2467
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57918
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.040
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       needle
_exptl_crystal_F_000             3204
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6499
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0720
_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/[σ²(Fo²)+(0.0911P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2358
_reflns_number_total             4063
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01851k2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7046701.cif.'
_cod_original_cell_volume        6901.7(18)
_cod_database_code               7046701
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.651
_exptl_absorpt_special_details   SADABS
_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 Ternary CH refined with riding coordinates:
 C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C6(H6), C9(H9)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, 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
Ru1 Ru 0.38772(4) 0.04999(4) 0.18902(5) 0.0401(3) Uani 1 1 d .
I1 I 0.43823(5) 0.14213(4) 0.06710(4) 0.0639(3) Uani 1 1 d .
N1 N 0.2715(5) -0.0793(4) 0.0824(5) 0.051(2) Uani 1 1 d .
N2 N 0.3815(4) -0.0594(4) 0.0851(4) 0.043(2) Uani 1 1 d .
C1 C 0.2769(6) -0.1280(6) 0.0323(6) 0.055(3) Uani 1 1 d .
H1 H 0.238621 -0.163423 0.001861 0.066 Uiso 1 1 calc R
C3 C 0.3447(7) -0.1157(6) 0.0351(6) 0.061(3) Uani 1 1 d .
H3 H 0.364202 -0.140721 0.007979 0.074 Uiso 1 1 calc R
C2 C 0.3365(6) -0.0361(5) 0.1163(5) 0.045(3) Uani 1 1 d .
N3 N 0.4719(4) 0.0236(4) 0.1609(4) 0.0311(18) Uani 1 1 d .
C11 C 0.5437(5) 0.0574(5) 0.1842(5) 0.038(2) Uani 1 1 d .
C4 C 0.4548(6) -0.0263(5) 0.1093(6) 0.045(3) Uani 1 1 d .
C5 C 0.5033(6) -0.0456(6) 0.0787(5) 0.053(3) Uani 1 1 d .
H5 H 0.487405 -0.081932 0.040843 0.063 Uiso 1 1 calc R
C14 C 0.2053(6) -0.0750(6) 0.0978(6) 0.061(3) Uani 1 1 d .
H14 H 0.213062 -0.046248 0.144756 0.073 Uiso 1 1 calc R
C16 C 0.1390(7) -0.1513(7) 0.1082(7) 0.088(4) Uani 1 1 d .
H16A H 0.134354 -0.181720 0.064783 0.132 Uiso 1 1 calc GR
H16B H 0.094768 -0.147632 0.112994 0.132 Uiso 1 1 calc GR
H16C H 0.145477 -0.173616 0.153561 0.132 Uiso 1 1 calc GR
C15 C 0.1943(7) -0.0341(8) 0.0322(7) 0.105(6) Uani 1 1 d .
H15A H 0.238884 0.013247 0.025067 0.158 Uiso 1 1 calc GR
H15B H 0.153313 -0.026247 0.043380 0.158 Uiso 1 1 calc GR
H15C H 0.183741 -0.063250 -0.013561 0.158 Uiso 1 1 calc GR
N4 N 0.5604(4) 0.1106(4) 0.2375(4) 0.046(2) Uani 1 1 d .
C6 C 0.5728(6) -0.0126(6) 0.1030(6) 0.056(3) Uani 1 1 d .
H6 H 0.606070 -0.025829 0.082538 0.067 Uiso 1 1 calc R
C9 C 0.6797(6) 0.1286(6) 0.2386(7) 0.058(3) Uani 1 1 d .
H9 H 0.727704 0.155435 0.258614 0.069 Uiso 1 1 calc R
C7 C 0.5959(6) 0.0409(5) 0.1582(5) 0.045(3) Uani 1 1 d .
C8 C 0.6669(5) 0.0778(6) 0.1884(6) 0.051(3) Uani 1 1 d .
C10 C 0.6268(5) 0.1462(5) 0.2648(6) 0.046(3) Uani 1 1 d .
C12 C 0.7237(6) 0.0593(7) 0.1616(7) 0.070(4) Uani 1 1 d .
H12A H 0.770824 0.092382 0.185156 0.105 Uiso 1 1 calc GR
H12B H 0.728565 0.064867 0.107101 0.105 Uiso 1 1 calc GR
H12C H 0.708505 0.008707 0.175121 0.105 Uiso 1 1 calc GR
C13 C 0.6467(6) 0.2041(5) 0.3221(6) 0.058(3) Uani 1 1 d .
H13A H 0.673022 0.252212 0.298143 0.086 Uiso 1 1 calc GR
H13B H 0.677986 0.200158 0.360116 0.086 Uiso 1 1 calc GR
H13C H 0.602153 0.198058 0.345789 0.086 Uiso 1 1 calc GR
O1 O 0.2656(4) 0.0822(4) 0.2100(4) 0.066(2) Uani 1 1 d .
C17 C 0.3121(7) 0.0674(5) 0.2043(6) 0.058(3) Uani 1 1 d .
O2 O 0.4713(4) 0.1791(4) 0.2948(4) 0.056(2) Uani 1 1 d .
C18 C 0.4429(6) 0.1272(6) 0.2547(6) 0.048(3) Uani 1 1 d .
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'
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'
I I -0.4742 1.8119 '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_3
I1 Ru1 Ru1 177.00(4) 4
C2 Ru1 Ru1 89.5(3) 4
C2 Ru1 I1 88.4(3) .
C2 Ru1 N3 76.2(3) .
N3 Ru1 Ru1 91.96(17) 4
N3 Ru1 I1 85.46(18) .
C17 Ru1 Ru1 89.9(3) 4
C17 Ru1 I1 92.6(3) .
C17 Ru1 C2 98.4(4) .
C17 Ru1 N3 174.3(4) .
C17 Ru1 C18 87.6(4) .
C18 Ru1 Ru1 90.3(3) 4
C18 Ru1 I1 91.6(3) .
C18 Ru1 C2 174.0(4) .
C18 Ru1 N3 97.8(4) .
C1 N1 C14 126.2(9) .
C2 N1 C1 110.6(9) .
C2 N1 C14 123.3(9) .
C3 N2 C2 112.2(9) .
C3 N2 C4 129.2(10) .
C2 N2 C4 118.6(8) .
C3 C1 N1 107.8(10) .
C1 C3 N2 106.5(10) .
N1 C2 Ru1 142.1(8) .
N1 C2 N2 103.0(8) .
N2 C2 Ru1 114.8(7) .
C11 N3 Ru1 128.8(6) .
C4 N3 Ru1 116.0(6) .
C4 N3 C11 114.8(8) .
N3 C11 C7 125.0(9) .
N4 C11 N3 113.5(8) .
N4 C11 C7 121.5(9) .
N3 C4 N2 114.0(9) .
N3 C4 C5 124.5(10) .
C5 C4 N2 121.4(9) .
C6 C5 C4 119.7(10) .
N1 C14 C16 110.7(9) .
N1 C14 C15 107.9(9) .
C16 C14 C15 111.6(10) .
C10 N4 C11 119.4(9) .
C5 C6 C7 120.0(10) .
C8 C9 C10 124.7(10) .
C11 C7 C8 119.4(9) .
C6 C7 C11 116.1(10) .
C6 C7 C8 124.5(10) .
C9 C8 C7 116.1(10) .
C9 C8 C12 124.0(10) .
C7 C8 C12 119.9(10) .
N4 C10 C9 118.9(10) .
N4 C10 C13 120.7(10) .
C9 C10 C13 120.4(9) .
O1 C17 Ru1 175.2(10) .
O2 C18 Ru1 171.4(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 Ru1 2.8448(16) 4
Ru1 I1 2.7560(11) .
Ru1 C2 2.049(10) .
Ru1 N3 2.172(7) .
Ru1 C17 1.829(14) .
Ru1 C18 1.869(11) .
N1 C1 1.411(13) .
N1 C2 1.354(12) .
N1 C14 1.471(13) .
N2 C3 1.375(12) .
N2 C2 1.385(12) .
N2 C4 1.412(12) .
C1 C3 1.322(15) .
N3 C11 1.377(11) .
N3 C4 1.308(11) .
C11 N4 1.377(12) .
C11 C7 1.393(13) .
C4 C5 1.389(14) .
C5 C6 1.343(14) .
C14 C16 1.529(15) .
C14 C15 1.541(14) .
N4 C10 1.310(11) .
C6 C7 1.391(14) .
C9 C8 1.319(14) .
C9 C10 1.421(14) .
C7 C8 1.407(13) .
C8 C12 1.513(15) .
C10 C13 1.485(13) .
O1 C17 1.174(13) .
O2 C18 1.190(11) .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.000 -0.227 853.7 87.6
2 0.333 0.667 0.928 184.4 40.0
3 0.333 0.667 0.428 184.4 44.7
4 0.667 0.333 0.572 184.4 38.7
5 0.667 0.333 0.072 184.4 43.4
