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#$Date: 2024-10-06 07:56:33 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295092 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/36/7133640.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_7133640
loop_
_publ_author_name
'Gearing, Hayden B.'
'Söhnel, Tilo'
'Young, Paul'
'Lisboa, Lynn'
'Wright, L. James'
'Crowley, James D.'
'Hartinger, Christian G.'
_publ_section_title
;
 Modulating the guest binding ability within mixed-coordination geometry
 [Pd(μ-L)₄RuCl₂]²⁺ and
 [Pd(μ-L)₄Pt]⁴⁺ cage architectures.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10950
_journal_page_last               10953
_journal_paper_doi               10.1039/d4cc03613a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C24 H20 Cl2 N4 O4 Ru'
_chemical_formula_sum            'C24 H20 Cl2 N4 O4 Ru'
_chemical_formula_weight         600.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_Hall           '-P 2ab 2bc'
_space_group_name_H-M_alt        'P n n n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-01 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1800(2)
_cell_length_b                   10.4500(2)
_cell_length_c                   12.4200(2)
_cell_measurement_reflns_used    1011
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      0.845
_cell_measurement_theta_min      0.090
_cell_volume                     1191.46(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'MicroED - Techni G2 F20'
_diffrn_radiation_type           'electron beam'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.5750
_diffrn_reflns_av_unetI/netI     0.2478
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11932
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        0.845
_diffrn_reflns_theta_max         0.845
_diffrn_reflns_theta_min         0.090
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       powder
_exptl_crystal_F_000             214
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       4653(47)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.2986
_refine_ls_R_factor_gt           0.1895
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4163
_refine_ls_wR_factor_ref         0.5053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                433
_reflns_number_total             1011
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03613a2.cif
_cod_data_source_block           a_hage115
_cod_depositor_comments
'Adding full bibliography for 7133640--7133644.cif.'
_cod_original_sg_symbol_H-M      'P n n n'
_cod_database_code               7133640
_shelx_shelxl_version_number     2019/3
_diffrn_oxdiff_scatteringfactors_ed 'Peng, L.M. (1999) Micron 30, 625-648'
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y, 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 -0.250000 0.750000 0.750000 0.056(2) Uani 1 4 d S T P . .
Cl1 Cl 0.0129(11) 0.750000 0.750000 0.064(3) Uani 1 2 d S T P . .
O1 O -0.012(3) 0.6415(18) 0.3439(11) 0.100(6) Uani 1 1 d . . . . .
N1 N -0.2498(18) 0.6086(13) 0.6306(9) 0.071(4) Uani 1 1 d . . . . .
C1 C -0.1767(19) 0.6171(13) 0.5414(9) 0.061(4) Uani 1 1 d . . . . .
H1 H -0.113606 0.686509 0.536223 0.073 Uiso 1 1 calc R U . . .
C2 C -0.180(2) 0.5390(14) 0.4557(10) 0.073(4) Uani 1 1 d . . . . .
C3 C -0.097(2) 0.560(2) 0.3580(11) 0.098(7) Uani 1 1 d . . . . .
H3 H -0.112749 0.503574 0.301418 0.118 Uiso 1 1 calc R U . . .
C4 C -0.280(2) 0.4289(17) 0.4657(11) 0.083(6) Uani 1 1 d . . . . .
H4 H -0.290935 0.369978 0.410197 0.099 Uiso 1 1 calc R U . . .
C5 C -0.352(2) 0.4176(19) 0.5576(11) 0.094(6) Uani 1 1 d . . . . .
H5 H -0.415090 0.348627 0.567206 0.113 Uiso 1 1 calc R U . . .
C6 C -0.337(2) 0.5034(15) 0.6363(11) 0.083(6) Uani 1 1 d . . . . .
H6 H -0.389848 0.490586 0.699358 0.100 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
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0000 0.0000 '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
Cl1 Ru1 Cl1 180.0 . 2_465 ?
N1 Ru1 Cl1 90.1(5) 2_465 . ?
N1 Ru1 Cl1 90.1(5) 3_566 2_465 ?
N1 Ru1 Cl1 89.9(5) . . ?
N1 Ru1 Cl1 90.1(5) . 2_465 ?
N1 Ru1 Cl1 89.9(5) 3_566 . ?
N1 Ru1 Cl1 89.9(5) 4_456 2_465 ?
N1 Ru1 Cl1 89.9(5) 2_465 2_465 ?
N1 Ru1 Cl1 90.1(5) 4_456 . ?
N1 Ru1 N1 89.8(7) 3_566 4_456 ?
N1 Ru1 N1 179.9(9) 4_456 2_465 ?
N1 Ru1 N1 179.9(9) . 3_566 ?
N1 Ru1 N1 90.2(7) . 4_456 ?
N1 Ru1 N1 90.2(7) 3_566 2_465 ?
N1 Ru1 N1 89.8(7) . 2_465 ?
C1 N1 Ru1 123.8(11) . . ?
C1 N1 C6 113.9(13) . . ?
C6 N1 Ru1 122.1(10) . . ?
N1 C1 H1 115.7 . . ?
N1 C1 C2 128.5(16) . . ?
C2 C1 H1 115.7 . . ?
C1 C2 C3 123.9(16) . . ?
C1 C2 C4 115.0(14) . . ?
C3 C2 C4 121.1(13) . . ?
O1 C3 C2 126.1(16) . . ?
O1 C3 H3 117.0 . . ?
C2 C3 H3 117.0 . . ?
C2 C4 H4 121.5 . . ?
C5 C4 C2 117.0(14) . . ?
C5 C4 H4 121.5 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(19) . . ?
C6 C5 H5 119.4 . . ?
N1 C6 H6 117.8 . . ?
C5 C6 N1 124.4(16) . . ?
C5 C6 H6 117.8 . . ?
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 Cl1 2.414(11) 2_465 ?
Ru1 Cl1 2.414(11) . ?
Ru1 N1 2.094(12) . ?
Ru1 N1 2.094(12) 3_566 ?
Ru1 N1 2.094(12) 4_456 ?
Ru1 N1 2.094(12) 2_465 ?
O1 C3 1.17(2) . ?
N1 C1 1.298(18) . ?
N1 C6 1.36(2) . ?
C1 H1 0.9300 . ?
C1 C2 1.342(17) . ?
C2 C3 1.45(2) . ?
C2 C4 1.47(2) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.33(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.33(2) . ?
C6 H6 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ru1 N1 C1 C2 -172.7(14) . . . . ?
Ru1 N1 C6 C5 172.7(15) . . . . ?
N1 C1 C2 C3 177.8(18) . . . . ?
N1 C1 C2 C4 -1(2) . . . . ?
C1 N1 C6 C5 -2(3) . . . . ?
C1 C2 C3 O1 5(3) . . . . ?
C1 C2 C4 C5 -1(2) . . . . ?
C2 C4 C5 C6 1(3) . . . . ?
C3 C2 C4 C5 -179.4(16) . . . . ?
C4 C2 C3 O1 -177(2) . . . . ?
C4 C5 C6 N1 1(3) . . . . ?
C6 N1 C1 C2 2(2) . . . . ?
