#------------------------------------------------------------------------------
#$Date: 2021-09-07 10:13:06 +0300 (Tue, 07 Sep 2021) $
#$Revision: 269006 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/45/1564563.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_1564563
loop_
_publ_author_name
'Yakushev, Ilya A.'
'Stolarov, Igor P.'
'Cherkashina, Natalia V.'
'Churakov, Andrei V.'
'Zubavichus, Yan V.'
'Markov, Alexander A.'
'Gekhman, Alexander E.'
'Vargaftik, Michael N.'
_publ_section_title
;
 Two routes to platinum-based carboxylate-bridged heterometallics
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119631
_journal_paper_doi               10.1016/j.ica.2020.119631
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         'C8 H12 Mn O8 Pt, 0.5(C6 H6)'
_chemical_formula_sum            'C11 H15 Mn O8 Pt'
_chemical_formula_weight         525.26
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 101.16(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.088(3)
_cell_length_b                   8.065(2)
_cell_length_c                   18.647(3)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      4.0
_cell_volume                     1488.4(6)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'MarCCD (Doyle, 2011)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       φ
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.787
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20702
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.991
_diffrn_reflns_theta_max         27.991
_diffrn_reflns_theta_min         2.793
_exptl_absorpt_coefficient_mu    13.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.344
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.980
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0046(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0329
_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)+(0.0075P)²+9.6398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2505
_reflns_number_total             2629
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-508-11963110.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1564563
_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   0.298
_shelx_estimated_absorpt_t_max   0.825
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.52679(2) 0.72963(4) 0.34364(2) 0.04145(15) Uani 1 1 d . . . . .
Mn1 Mn 0.27687(10) 0.72853(16) 0.25794(5) 0.0487(3) Uani 1 1 d . . . . .
O11 O 0.4492(4) 0.6175(6) 0.4226(2) 0.0444(11) Uani 1 1 d . . . . .
O12 O 0.2399(4) 0.6672(5) 0.3613(2) 0.0351(9) Uani 1 1 d . . . . .
O21 O 0.5995(4) 0.8419(7) 0.2629(2) 0.0475(12) Uani 1 1 d . . . . .
O22 O 0.4043(4) 0.7907(5) 0.1862(2) 0.0366(9) Uani 1 1 d . . . . .
O31 O 0.5003(5) 0.9399(7) 0.3959(2) 0.0494(12) Uani 1 1 d . . . . .
O32 O 0.3433(4) 1.0430(7) 0.3078(2) 0.0516(13) Uani 1 1 d . . . . .
O41 O 0.5845(4) 0.5201(7) 0.3029(2) 0.0469(12) Uani 1 1 d . . . . .
O42 O 0.3799(4) 0.4120(7) 0.2700(2) 0.0512(13) Uani 1 1 d . . . . .
C11 C 0.3205(6) 0.6177(8) 0.4162(3) 0.0352(13) Uani 1 1 d . . . . .
C12 C 0.2670(7) 0.5539(10) 0.4800(3) 0.0447(16) Uani 1 1 d . . . . .
H12A H 0.199320 0.467882 0.463579 0.067 Uiso 1 1 calc R U . . .
H12B H 0.225256 0.645030 0.502429 0.067 Uiso 1 1 calc R U . . .
H12C H 0.341222 0.506788 0.515983 0.067 Uiso 1 1 calc R U . . .
C21 C 0.5232(6) 0.8417(8) 0.1999(3) 0.0375(13) Uani 1 1 d . . . . .
C22 C 0.5837(7) 0.9056(10) 0.1379(4) 0.0491(17) Uani 1 1 d . . . . .
H22A H 0.583404 0.817375 0.101794 0.074 Uiso 1 1 calc R U . . .
H22B H 0.676795 0.941514 0.156581 0.074 Uiso 1 1 calc R U . . .
H22C H 0.530397 0.999789 0.114936 0.074 Uiso 1 1 calc R U . . .
C31 C 0.4158(7) 1.0510(10) 0.3701(3) 0.0482(18) Uani 1 1 d . . . . .
C32 C 0.4072(8) 1.1953(10) 0.4196(4) 0.0500(17) Uani 1 1 d . . . . .
H32A H 0.314745 1.238657 0.410181 0.075 Uiso 1 1 calc R U . . .
H32B H 0.469542 1.282386 0.410350 0.075 Uiso 1 1 calc R U . . .
H32C H 0.431831 1.159132 0.470612 0.075 Uiso 1 1 calc R U . . .
C41 C 0.5046(6) 0.4042(10) 0.2752(3) 0.0442(16) Uani 1 1 d . . . . .
C42 C 0.5719(7) 0.2575(9) 0.2489(4) 0.0517(18) Uani 1 1 d . . . . .
H42A H 0.512067 0.209024 0.206342 0.077 Uiso 1 1 calc R U . . .
H42B H 0.591363 0.174680 0.287949 0.077 Uiso 1 1 calc R U . . .
H42C H 0.656548 0.292449 0.234991 0.077 Uiso 1 1 calc R U . . .
C1 C 0.0545(10) 0.9601(12) 0.4411(5) 0.075(3) Uani 1 1 d . . . . .
H1 H 0.091918 0.933733 0.399484 0.090 Uiso 1 1 calc R U . . .
C2 C 0.1369(9) 1.0021(11) 0.5049(5) 0.067(2) Uani 1 1 d . . . . .
H2 H 0.232204 1.002115 0.508664 0.080 Uiso 1 1 calc R U . . .
C3 C 0.0820(10) 1.0443(12) 0.5635(5) 0.070(2) Uani 1 1 d . . . . .
H3 H 0.139195 1.076955 0.607875 0.084 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 0.0046 0.0020 '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 0.0146 0.0077 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3549 0.8831 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -2.7969 9.8935 '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
O41 Pt1 O31 170.09(19) . .
O41 Pt1 O11 94.71(19) . .
O31 Pt1 O11 85.24(19) . .
O41 Pt1 O21 85.4(2) . .
O31 Pt1 O21 94.9(2) . .
O11 Pt1 O21 178.49(16) . .
O41 Pt1 Mn1 94.55(13) . .
O31 Pt1 Mn1 95.36(14) . .
O11 Pt1 Mn1 88.91(12) . .
O21 Pt1 Mn1 89.58(13) . .
O22 Mn1 O12 152.70(17) . .
O22 Mn1 O32 98.70(17) . 2_545
O12 Mn1 O32 100.29(17) . 2_545
O22 Mn1 O42 101.20(17) . 2
O12 Mn1 O42 97.57(17) . 2
O32 Mn1 O42 91.93(19) 2_545 2
O22 Mn1 Pt1 76.06(12) . .
O12 Mn1 Pt1 76.65(11) . .
O32 Mn1 Pt1 134.00(14) 2_545 .
O42 Mn1 Pt1 134.07(15) 2 .
O22 Mn1 O32 81.62(16) . .
O12 Mn1 O32 88.96(16) . .
O32 Mn1 O32 155.57(16) 2_545 .
O42 Mn1 O32 64.28(17) 2 .
Pt1 Mn1 O32 70.03(10) . .
O22 Mn1 O42 90.33(16) . .
O12 Mn1 O42 80.62(15) . .
O32 Mn1 O42 64.11(16) 2_545 .
O42 Mn1 O42 154.91(16) 2 .
Pt1 Mn1 O42 70.20(10) . .
O32 Mn1 O42 140.20(14) . .
C11 O11 Pt1 117.5(4) . .
C11 O12 Mn1 129.0(4) . .
C21 O21 Pt1 116.5(4) . .
C21 O22 Mn1 129.4(4) . .
C31 O31 Pt1 124.0(4) . .
C31 O32 Mn1 131.1(5) . 2
C31 O32 Mn1 115.1(5) . .
Mn1 O32 Mn1 112.13(16) 2 .
C41 O41 Pt1 124.7(4) . .
C41 O42 Mn1 131.9(5) . 2_545
C41 O42 Mn1 114.4(5) . .
Mn1 O42 Mn1 111.71(17) 2_545 .
O12 C11 O11 124.5(6) . .
O12 C11 C12 119.2(5) . .
O11 C11 C12 116.3(5) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O22 C21 O21 125.1(6) . .
O22 C21 C22 118.3(6) . .
O21 C21 C22 116.6(5) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
O32 C31 O31 123.2(7) . .
O32 C31 C32 121.4(7) . .
O31 C31 C32 115.5(6) . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
O42 C41 O41 123.0(7) . .
O42 C41 C42 122.1(7) . .
O41 C41 C42 114.9(6) . .
C41 C42 H42A 109.5 . .
C41 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C41 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C2 C1 C3 120.1(8) . 3_576
C2 C1 H1 120.0 . .
C3 C1 H1 120.0 3_576 .
C1 C2 C3 119.4(9) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C2 C3 C1 120.5(9) . 3_576
C2 C3 H3 119.8 . .
C1 C3 H3 119.8 3_576 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 O41 1.986(5) .
Pt1 O31 2.000(5) .
Pt1 O11 2.011(4) .
Pt1 O21 2.013(5) .
Pt1 Mn1 2.7112(13) .
Mn1 O22 2.088(4) .
Mn1 O12 2.091(4) .
Mn1 O32 2.153(5) 2_545
Mn1 O42 2.154(5) 2
Mn1 O32 2.739(6) .
Mn1 O42 2.749(6) .
O11 C11 1.281(7) .
O12 C11 1.245(7) .
O21 C21 1.273(8) .
O22 C21 1.247(7) .
O31 C31 1.266(9) .
O32 C31 1.249(8) .
O41 C41 1.276(9) .
O42 C41 1.245(8) .
C11 C12 1.490(8) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C21 C22 1.499(9) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C31 C32 1.498(10) .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C41 C42 1.494(10) .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C1 C2 1.356(13) .
C1 C3 1.364(13) 3_576
C1 H1 0.9500 .
C2 C3 1.360(12) .
C2 H2 0.9500 .
C3 H3 0.9500 .
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
Mn1 O12 C11 O11 10.7(9) . . . .
Mn1 O12 C11 C12 -169.5(5) . . . .
Pt1 O11 C11 O12 7.7(8) . . . .
Pt1 O11 C11 C12 -172.2(5) . . . .
Mn1 O22 C21 O21 11.8(10) . . . .
Mn1 O22 C21 C22 -169.4(5) . . . .
Pt1 O21 C21 O22 6.4(9) . . . .
Pt1 O21 C21 C22 -172.4(5) . . . .
Mn1 O32 C31 O31 -166.1(5) 2 . . .
Mn1 O32 C31 O31 30.1(8) . . . .
Mn1 O32 C31 C32 14.0(9) 2 . . .
Mn1 O32 C31 C32 -149.7(5) . . . .
Pt1 O31 C31 O32 -2.7(9) . . . .
Pt1 O31 C31 C32 177.2(4) . . . .
Mn1 O42 C41 O41 -169.4(4) 2_545 . . .
Mn1 O42 C41 O41 28.2(7) . . . .
Mn1 O42 C41 C42 10.9(9) 2_545 . . .
Mn1 O42 C41 C42 -151.5(5) . . . .
Pt1 O41 C41 O42 1.0(9) . . . .
Pt1 O41 C41 C42 -179.3(4) . . . .
C3 C1 C2 C3 -1.9(16) 3_576 . . .
C1 C2 C3 C1 1.9(16) . . . 3_576
