#------------------------------------------------------------------------------
#$Date: 2017-04-04 16:01:23 +0300 (Tue, 04 Apr 2017) $
#$Revision: 194809 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/52/4345265.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_4345265
loop_
_publ_author_name
'Nathan, Sarah R.'
'Pino, Nicholas W.'
'Arduino, Daniela M.'
'Perocchi, Fabiana'
'MacMillan, Samantha N.'
'Wilson, Justin J.'
_publ_section_title
;
 Synthetic Methods for the Preparation of a Functional Analogue of Ru360,
 a Potent Inhibitor of Mitochondrial Calcium Uptake.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3123
_journal_page_last               3126
_journal_paper_doi               10.1021/acs.inorgchem.6b03108
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'Cl4 H26 N8 O3 Ru2'
_chemical_formula_weight         530.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.612(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2808(5)
_cell_length_b                   11.7183(7)
_cell_length_c                   9.0833(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.85
_cell_volume                     875.55(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      223(2)
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32732
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         2.849
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       Block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0265
_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)+(0.0339P)²+1.2644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1995
_reflns_number_total             2171
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b03108_si_002.cif
_cod_data_source_block           '[(OH)(NH3)4Ru(?-O)Ru(NH3)4(OH2)]Cl4'
_cod_depositor_comments
'Adding full bibliography for 4345265--4345267.cif.'
_cod_database_code               4345265
_shelx_shelxl_version_number     2014/7
_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_min   0.720
_shelx_estimated_absorpt_t_max   0.853
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ru Ru -0.03061(3) 0.03091(2) -0.19781(2) 0.01860(8) Uani 1 1 d . . .
O1 O -0.0706(3) 0.06308(19) -0.4197(2) 0.0319(5) Uani 1 1 d D . .
H100 H -0.073(5) 0.1280(18) -0.439(4) 0.048 Uiso 1 1 d D U .
O2 O 0.0000 0.0000 0.0000 0.0199(5) Uani 1 2 d S . P
N1 N -0.2713(3) 0.0826(2) -0.1811(3) 0.0306(5) Uani 1 1 d . . .
H1A H -0.2707 0.1436 -0.1207 0.046 Uiso 1 1 calc R U .
H1B H -0.3260 0.0251 -0.1439 0.046 Uiso 1 1 calc R U .
H1C H -0.3201 0.1013 -0.2716 0.046 Uiso 1 1 calc R U .
N2 N 0.0547(3) 0.1985(2) -0.1609(3) 0.0258(5) Uani 1 1 d . . .
H2A H 0.1591 0.1968 -0.1202 0.039 Uiso 1 1 calc R U .
H2B H -0.0060 0.2343 -0.0990 0.039 Uiso 1 1 calc R U .
H2C H 0.0477 0.2363 -0.2476 0.039 Uiso 1 1 calc R U .
N3 N 0.2079(3) -0.0223(2) -0.2236(3) 0.0279(5) Uani 1 1 d . . .
H3A H 0.2182 -0.0973 -0.2031 0.042 Uiso 1 1 calc R U .
H3B H 0.2793 0.0173 -0.1611 0.042 Uiso 1 1 calc R U .
H3C H 0.2279 -0.0097 -0.3175 0.042 Uiso 1 1 calc R U .
N4 N -0.1178(3) -0.1349(2) -0.2501(3) 0.0271(5) Uani 1 1 d . . .
H4A H -0.1976 -0.1520 -0.1944 0.041 Uiso 1 1 calc R U .
H4B H -0.0361 -0.1854 -0.2315 0.041 Uiso 1 1 calc R U .
H4C H -0.1569 -0.1381 -0.3466 0.041 Uiso 1 1 calc R U .
Cl1 Cl 0.41270(10) 0.16380(7) 0.03199(9) 0.03832(18) Uani 1 1 d . . .
Cl2 Cl 0.32985(11) 0.20169(7) 0.58345(8) 0.03969(19) 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
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'
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_3
O2 Ru O1 178.45(7) .
O2 Ru N2 91.28(6) .
O1 Ru N2 89.91(9) .
O2 Ru N1 90.66(7) .
O1 Ru N1 88.32(10) .
N2 Ru N1 91.33(10) .
O2 Ru N4 92.52(6) .
O1 Ru N4 86.30(9) .
N2 Ru N4 176.20(9) .
N1 Ru N4 88.80(10) .
O2 Ru N3 91.43(7) .
O1 Ru N3 89.58(10) .
N2 Ru N3 89.56(10) .
N1 Ru N3 177.72(10) .
N4 Ru N3 90.18(10) .
Ru O1 H100 114(3) .
Ru O2 Ru 180.000(12) 3
Ru N1 H1A 109.5 .
Ru N1 H1B 109.5 .
H1A N1 H1B 109.5 .
Ru N1 H1C 109.5 .
H1A N1 H1C 109.5 .
H1B N1 H1C 109.5 .
Ru N2 H2A 109.5 .
Ru N2 H2B 109.5 .
H2A N2 H2B 109.5 .
Ru N2 H2C 109.5 .
H2A N2 H2C 109.5 .
H2B N2 H2C 109.5 .
Ru N3 H3A 109.5 .
Ru N3 H3B 109.5 .
H3A N3 H3B 109.5 .
Ru N3 H3C 109.5 .
H3A N3 H3C 109.5 .
H3B N3 H3C 109.5 .
Ru N4 H4A 109.5 .
Ru N4 H4B 109.5 .
H4A N4 H4B 109.5 .
Ru N4 H4C 109.5 .
H4A N4 H4C 109.5 .
H4B N4 H4C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru O2 1.8218(2) .
Ru O1 2.039(2) .
Ru N2 2.102(2) .
Ru N1 2.105(2) .
Ru N4 2.108(2) .
Ru N3 2.110(2) .
O1 H100 0.782(18) .
O2 Ru 1.8219(2) 3
N1 H1A 0.9000 .
N1 H1B 0.9000 .
N1 H1C 0.9000 .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N2 H2C 0.9000 .
N3 H3A 0.9000 .
N3 H3B 0.9000 .
N3 H3C 0.9000 .
N4 H4A 0.9000 .
N4 H4B 0.9000 .
N4 H4C 0.9000 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H100 Cl1 0.782(18) 2.455(19) 3.231(2) 173(4) 4_565
N1 H1A Cl2 0.90 2.66 3.521(3) 161.0 4_565
N1 H1B Cl1 0.90 2.57 3.451(3) 165.7 3
N2 H2B Cl2 0.90 2.38 3.273(2) 170.4 4_565
N2 H2C Cl1 0.90 2.47 3.319(2) 156.9 4_565
N3 H3A Cl2 0.90 2.64 3.503(3) 160.0 2_545
N3 H3C Cl2 0.90 2.80 3.375(3) 123.1 1_554
N4 H4A Cl1 0.90 2.44 3.334(3) 170.2 3
N4 H4B Cl2 0.90 2.44 3.288(3) 157.5 2_545
N4 H4C Cl2 0.90 2.55 3.412(2) 159.5 3
