#------------------------------------------------------------------------------
#$Date: 2017-05-18 05:46:53 +0300 (Thu, 18 May 2017) $
#$Revision: 196735 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/60/1546063.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_1546063
loop_
_publ_author_name
'Mosquera, Marta Elena Gonzalez'
'Gomez-Sal, Pilar'
'Egido, Irene'
'López López, María'
'Hortelano, Carlos'
_publ_section_title
;
 FDHALO17: Comparison of Halogen Bonding networks with Ru(II) complexes
 and analysis of the influence of the XB interaction on their reactivity
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C7FD00079K
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H38 Br2 N4 O1 Ru1'
_chemical_formula_sum            'C36 H38 Br2 N4 O Ru'
_chemical_formula_weight         803.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2015-07-02T17:41:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-02-22 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.603(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5219(8)
_cell_length_b                   13.6105(10)
_cell_length_c                   17.4958(10)
_cell_measurement_reflns_used    245
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.32
_cell_measurement_theta_min      3.45
_cell_measurement_wavelength     0.71073
_cell_volume                     3517.8(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13040
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.75
_exptl_absorpt_correction_T_max  0.326
_exptl_absorpt_correction_T_min  0.276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0816P)²+43.5619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                2956
_reflns_number_total             4022
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c7fd00079k2.cif
_cod_data_source_block           2b.H2O
_cod_database_code               1546063
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ru1 Ru 0.25 0.75 0.5 0.02125(19) Uani 1 2 d S
Br1 Br 0.10094(5) 0.82389(6) 0.39780(5) 0.0491(3) Uani 1 1 d .
N1 N 0.2043(4) 0.8180(4) 0.6475(3) 0.0290(11) Uani 1 1 d .
N2 N 0.1576(3) 0.5458(3) 0.4909(3) 0.0249(10) Uani 1 1 d .
C1 C 0.2232(4) 0.7921(4) 0.5947(4) 0.0272(12) Uani 1 1 d .
C2 C 0.1845(4) 0.8498(5) 0.7129(4) 0.0287(13) Uani 1 1 d .
C3 C 0.2210(4) 0.7972(5) 0.7888(4) 0.0343(15) Uani 1 1 d .
C4 C 0.2004(6) 0.8330(7) 0.8526(5) 0.051(2) Uani 1 1 d .
H4 H 0.2226 0.8006 0.9049 0.061 Uiso 1 1 calc R
C5 C 0.1482(6) 0.9147(8) 0.8398(7) 0.068(3) Uani 1 1 d .
H5 H 0.1352 0.937 0.8833 0.081 Uiso 1 1 calc R
C6 C 0.1146(5) 0.9646(7) 0.7639(6) 0.054(2) Uani 1 1 d .
H6 H 0.0808 1.0214 0.7573 0.065 Uiso 1 1 calc R
C7 C 0.1299(4) 0.9326(5) 0.6981(5) 0.0411(17) Uani 1 1 d .
C8 C 0.2809(5) 0.7095(5) 0.7996(5) 0.0457(18) Uani 1 1 d .
H8A H 0.3004 0.6823 0.8558 0.069 Uiso 1 1 calc R
H8B H 0.3329 0.7296 0.7925 0.069 Uiso 1 1 calc R
H8C H 0.2478 0.6608 0.7575 0.069 Uiso 1 1 calc R
C9 C 0.0908(6) 0.9848(6) 0.6137(6) 0.067(3) Uani 1 1 d .
H9A H 0.1091 0.9518 0.5754 0.101 Uiso 1 1 calc R
H9B H 0.1122 1.0514 0.6218 0.101 Uiso 1 1 calc R
H9C H 0.0259 0.9845 0.5897 0.101 Uiso 1 1 calc R
C11 C 0.1911(4) 0.6207(4) 0.4946(4) 0.0247(12) Uani 1 1 d .
C12 C 0.1138(4) 0.4556(4) 0.4842(4) 0.0219(11) Uani 1 1 d .
C13 C 0.0928(4) 0.4292(4) 0.5499(4) 0.0254(12) Uani 1 1 d .
C14 C 0.0475(4) 0.3404(5) 0.5404(5) 0.0373(16) Uani 1 1 d .
H14 H 0.0315 0.3198 0.5824 0.045 Uiso 1 1 calc R
C15 C 0.0262(5) 0.2827(5) 0.4692(5) 0.0414(17) Uani 1 1 d .
H15 H -0.0041 0.2237 0.464 0.05 Uiso 1 1 calc R
C16 C 0.0487(4) 0.3105(5) 0.4061(5) 0.0392(16) Uani 1 1 d .
H16 H 0.034 0.2698 0.359 0.047 Uiso 1 1 calc R
C17 C 0.0933(4) 0.3991(4) 0.4114(4) 0.0286(13) Uani 1 1 d .
C18 C 0.1157(5) 0.4340(6) 0.3422(5) 0.0437(17) Uani 1 1 d .
H18A H 0.1463 0.4961 0.3582 0.066 Uiso 1 1 calc R
H18B H 0.0609 0.4414 0.2901 0.066 Uiso 1 1 calc R
H18C H 0.1543 0.3869 0.3338 0.066 Uiso 1 1 calc R
C19 C 0.1189(4) 0.4907(5) 0.6279(4) 0.0349(14) Uani 1 1 d .
H19A H 0.1494 0.5488 0.6233 0.052 Uiso 1 1 calc R
H19B H 0.1585 0.4539 0.6774 0.052 Uiso 1 1 calc R
H19C H 0.0655 0.5092 0.6332 0.052 Uiso 1 1 calc R
O1 O 0 0.6518(8) 0.25 0.099(4) Uani 1 2 d S
H1W H 0.0569 0.68 0.2599 0.114 Uiso 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -4 -2 0.149
-4 1 5 0.217
15 10 -1 0.2
3 -1 -4 0.178
1 1 -4 0.113
0 -1 2 0.174
5 -7 4 0.162
-2 2 1 0.274
-2 1 0 0.218
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
C1 Ru1 C1 180.00(14) 7_566 .
C1 Ru1 C11 90.4(2) 7_566 7_566
C1 Ru1 C11 89.6(2) . 7_566
C1 Ru1 C11 89.6(2) 7_566 .
C1 Ru1 C11 90.4(2) . .
C11 Ru1 C11 180.0000(10) 7_566 .
C1 Ru1 Br1 92.04(17) 7_566 .
C1 Ru1 Br1 87.96(17) . .
C11 Ru1 Br1 89.02(17) 7_566 .
C11 Ru1 Br1 90.98(17) . .
C1 Ru1 Br1 87.96(17) 7_566 7_566
C1 Ru1 Br1 92.04(17) . 7_566
C11 Ru1 Br1 90.98(17) 7_566 7_566
C11 Ru1 Br1 89.02(17) . 7_566
Br1 Ru1 Br1 180.0000(10) . 7_566
C1 N1 C2 178.2(6) . .
C11 N2 C12 178.0(6) . .
N1 C1 Ru1 177.3(6) . .
C3 C2 N1 117.7(6) . .
C3 C2 C7 124.3(6) . .
N1 C2 C7 118.0(6) . .
C2 C3 C4 115.4(7) . .
C2 C3 C8 120.6(6) . .
C4 C3 C8 124.0(7) . .
C5 C4 C3 121.1(8) . .
C6 C5 C4 121.1(7) . .
C7 C6 C5 121.0(8) . .
C6 C7 C2 117.0(8) . .
C6 C7 C9 121.4(8) . .
C2 C7 C9 121.6(7) . .
N2 C11 Ru1 179.2(5) . .
C13 C12 C17 124.4(5) . .
C13 C12 N2 117.9(5) . .
C17 C12 N2 117.7(5) . .
C12 C13 C14 116.5(6) . .
C12 C13 C19 122.4(5) . .
C14 C13 C19 121.1(6) . .
C15 C14 C13 120.6(6) . .
C16 C15 C14 121.4(6) . .
C15 C16 C17 120.8(6) . .
C12 C17 C16 116.3(6) . .
C12 C17 C18 121.2(6) . .
C16 C17 C18 122.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C1 1.982(6) 7_566
Ru1 C1 1.982(6) .
Ru1 C11 1.993(6) 7_566
Ru1 C11 1.993(6) .
Ru1 Br1 2.5159(8) .
Ru1 Br1 2.5159(8) 7_566
N1 C1 1.154(8) .
N1 C2 1.393(8) .
N2 C11 1.148(7) .
N2 C12 1.403(7) .
C2 C3 1.387(10) .
C2 C7 1.393(9) .
C3 C4 1.393(10) .
C3 C8 1.507(11) .
C4 C5 1.363(14) .
C5 C6 1.368(15) .
C6 C7 1.356(11) .
C7 C9 1.500(13) .
C12 C13 1.388(8) .
C12 C17 1.394(8) .
C13 C14 1.391(8) .
C13 C19 1.491(9) .
C14 C15 1.377(11) .
C15 C16 1.367(11) .
C16 C17 1.394(9) .
C17 C18 1.494(9) .
