#------------------------------------------------------------------------------
#$Date: 2017-04-04 16:01:23 +0300 (Tue, 04 Apr 2017) $
#$Revision: 194809 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/52/4345266.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_4345266
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            'Cl3 H15 N5 Ru'
_chemical_formula_weight         292.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3791(12)
_cell_length_b                   10.5086(8)
_cell_length_c                   6.7456(6)
_cell_measurement_reflns_used    3761
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      3.05
_cell_volume                     948.40(14)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10229
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         3.045
_exptl_absorpt_coefficient_mu    2.438
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_description       Needle
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0241
_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)+(0.0342P)²+0.3268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1166
_reflns_number_total             1288
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b03108_si_002.cif
_cod_data_source_block           '[Ru(NH3)5Cl]Cl2'
_cod_depositor_comments
'Adding full bibliography for 4345265--4345267.cif.'
_cod_database_code               4345266
_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   0.442
_shelx_estimated_absorpt_t_max   0.888
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Ru Ru 0.39817(2) 0.2500 0.31881(3) 0.01618(9) Uani 1 2 d S T P
Cl1 Cl 0.52978(6) 0.2500 0.54938(12) 0.02357(16) Uani 1 2 d S T P
Cl2 Cl 0.64895(4) 0.49841(5) 0.16580(8) 0.02549(14) Uani 1 1 d . . .
N1 N 0.2814(2) 0.2500 0.1149(4) 0.0259(6) Uani 1 2 d S T P
H1A H 0.2708 0.1710 0.0723 0.039 Uiso 0.5 1 calc R U P
H1B H 0.2972 0.2995 0.0126 0.039 Uiso 0.5 1 calc R U P
H1C H 0.2262 0.2795 0.1727 0.039 Uiso 0.5 1 calc R U P
N2 N 0.5012(2) 0.2500 0.0818(4) 0.0247(6) Uani 1 2 d S T P
H2A H 0.5518 0.3017 0.1103 0.037 Uiso 0.5 1 calc R U P
H2B H 0.4709 0.2768 -0.0280 0.037 Uiso 0.5 1 calc R U P
H2C H 0.5242 0.1715 0.0631 0.037 Uiso 0.5 1 calc R U P
N3 N 0.2928(2) 0.2500 0.5508(4) 0.0272(6) Uani 1 2 d S T P
H3A H 0.3159 0.2038 0.6514 0.041 Uiso 0.5 1 calc R U P
H3B H 0.2356 0.2167 0.5078 0.041 Uiso 0.5 1 calc R U P
H3C H 0.2823 0.3295 0.5912 0.041 Uiso 0.5 1 calc R U P
N4 N 0.39888(14) 0.44982(19) 0.3196(3) 0.0236(4) Uani 1 1 d . . .
H4A H 0.3536 0.4784 0.2337 0.035 Uiso 1 1 calc R U .
H4B H 0.4592 0.4778 0.2848 0.035 Uiso 1 1 calc R U .
H4C H 0.3841 0.4779 0.4405 0.035 Uiso 1 1 calc R U .
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'
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_1
_geom_angle_site_symmetry_3
N1 Ru N4 90.29(5) . .
N1 Ru N4 90.29(5) . 7_565
N4 Ru N4 179.41(10) . 7_565
N1 Ru N3 89.33(12) . .
N4 Ru N3 90.07(5) . .
N4 Ru N3 90.07(5) 7_565 .
N1 Ru N2 89.40(12) . .
N4 Ru N2 89.94(5) . .
N4 Ru N2 89.94(5) 7_565 .
N3 Ru N2 178.74(11) . .
N1 Ru Cl1 179.90(8) . .
N4 Ru Cl1 89.71(5) . .
N4 Ru Cl1 89.71(5) 7_565 .
N3 Ru Cl1 90.57(9) . .
N2 Ru Cl1 90.69(8) . .
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 N1 2.082(3) .
Ru N4 2.100(2) .
Ru N4 2.100(2) 7_565
Ru N3 2.107(3) .
Ru N2 2.111(3) .
Ru Cl1 2.3494(8) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N4 H4C 0.8900 .
