#------------------------------------------------------------------------------
#$Date: 2019-11-23 15:18:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/92/4349274.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_4349274
loop_
_publ_author_name
'Białek, Michał J'
'Sprutta, Natasza'
'Latos-Grażyński, Lechosław'
_publ_section_title
;
 Coordination-Induced Molecular Tweezing: Ruthenium Clusters Docked at
 Azuliporphyrinogens.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12061
_journal_page_last               12073
_journal_paper_doi               10.1021/acs.inorgchem.6b02228
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C60 H48 S2'
_chemical_formula_weight         833.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 116.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.001(6)
_cell_length_b                   9.234(2)
_cell_length_c                   24.424(5)
_cell_measurement_reflns_used    3095
_cell_measurement_temperature    79.98(13)
_cell_measurement_theta_max      28.7538
_cell_measurement_theta_min      2.7602
_cell_volume                     5435(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      79.98(13)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13069
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.805
_diffrn_reflns_theta_min         2.766
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
;
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0611
_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)+(0.0898P)²+0.8751P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4285
_reflns_number_total             6236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02228_si_002.cif
_cod_data_source_block           Az2S2_Pg
_cod_original_cell_volume        5434(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4349274
_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.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.36403(8) 0.2940(2) 0.18932(9) 0.0216(5) Uani 1 1 d . .
C2 C 0.33062(8) 0.2041(2) 0.20576(9) 0.0215(5) Uani 1 1 d . .
C2C C 0.25349(10) -0.0033(3) 0.23470(11) 0.0355(6) Uani 1 1 d . .
H2C H 0.2265 -0.0680 0.2333 0.043 Uiso 1 1 calc R U
C4 C 0.40192(8) 0.3012(3) 0.29486(9) 0.0232(5) Uani 1 1 d . .
C3 C 0.35545(8) 0.2084(2) 0.27425(9) 0.0219(5) Uani 1 1 d . .
C5 C 0.43921(8) 0.3453(3) 0.36057(9) 0.0233(5) Uani 1 1 d . .
H5 H 0.4433 0.2612 0.3867 0.028 Uiso 1 1 calc R U
C5C C 0.37211(11) 0.7048(3) 0.36732(11) 0.0436(7) Uani 1 1 d . .
H5C H 0.3563 0.7842 0.3419 0.052 Uiso 1 1 calc R U
C8 C 0.57512(9) 0.5128(3) 0.37887(9) 0.0250(5) Uani 1 1 d . .
H8 H 0.5966 0.5947 0.3832 0.030 Uiso 1 1 calc R U
C7 C 0.52040(9) 0.5184(3) 0.37462(9) 0.0251(5) Uani 1 1 d . .
H7 H 0.5029 0.6042 0.3759 0.030 Uiso 1 1 calc R U
C6 C 0.49677(8) 0.3857(3) 0.36858(9) 0.0236(5) Uani 1 1 d . .
C9 C 0.59232(8) 0.3770(2) 0.37598(9) 0.0218(5) Uani 1 1 d . .
C10 C 0.64551(8) 0.3269(2) 0.37549(9) 0.0209(5) Uani 1 1 d . .
H10 H 0.6564 0.2360 0.3986 0.025 Uiso 1 1 calc R U
C10C C 0.76851(10) 0.5235(3) 0.50180(11) 0.0321(6) Uani 1 1 d . .
H10C H 0.7894 0.5163 0.5441 0.038 Uiso 1 1 calc R U
C21 C 0.40652(9) 0.3503(2) 0.24305(9) 0.0247(5) Uani 1 1 d . .
H21 H 0.4342 0.4122 0.2443 0.030 Uiso 1 1 calc R U
C5A C 0.41534(8) 0.4691(3) 0.38275(9) 0.0247(5) Uani 1 1 d . .
C3B C 0.29152(10) 0.0409(3) 0.29345(11) 0.0303(5) Uani 1 1 d . .
H3B H 0.2864 0.0014 0.3255 0.036 Uiso 1 1 calc R U
C3A C 0.33609(9) 0.1360(3) 0.31067(10) 0.0259(5) Uani 1 1 d . .
H3A H 0.3557 0.1536 0.3526 0.031 Uiso 1 1 calc R U
C2B C 0.24999(10) 0.0347(3) 0.17845(11) 0.0339(6) Uani 1 1 d . .
H2B H 0.2210 -0.0075 0.1445 0.041 Uiso 1 1 calc R U
C2A C 0.28416(9) 0.1282(3) 0.16552(10) 0.0276(5) Uani 1 1 d . .
H2A H 0.2743 0.1412 0.1241 0.033 Uiso 1 1 calc R U
S22 S 0.54144(2) 0.25230(6) 0.36756(2) 0.02448(17) Uani 1 1 d . .
C5B C 0.39029(10) 0.5879(3) 0.34558(10) 0.0370(6) Uani 1 1 d . .
H5B H 0.3856 0.5890 0.3055 0.044 Uiso 1 1 calc R U
C5D C 0.37713(10) 0.7050(3) 0.42622(11) 0.0330(6) Uani 1 1 d . .
C5E C 0.40204(9) 0.5878(3) 0.46297(10) 0.0302(5) Uani 1 1 d . .
H5E H 0.4062 0.5866 0.5029 0.036 Uiso 1 1 calc R U
C5F C 0.42122(9) 0.4711(3) 0.44211(10) 0.0282(5) Uani 1 1 d . .
H5F H 0.4382 0.3936 0.4682 0.034 Uiso 1 1 calc R U
C5G C 0.35614(11) 0.8323(3) 0.44936(11) 0.0426(7) Uani 1 1 d . .
H5G H 0.3701 0.8250 0.4930 0.064 Uiso 1 1 calc R U
H5H H 0.3163 0.8310 0.4302 0.064 Uiso 1 1 calc R U
H5I H 0.3687 0.9211 0.4394 0.064 Uiso 1 1 calc R U
C10A C 0.69264(8) 0.4348(2) 0.40814(10) 0.0228(5) Uani 1 1 d . .
C10B C 0.72426(9) 0.4296(2) 0.47160(10) 0.0261(5) Uani 1 1 d . .
H10B H 0.7156 0.3620 0.4942 0.031 Uiso 1 1 calc R U
C10D C 0.78205(9) 0.6277(3) 0.46997(12) 0.0322(6) Uani 1 1 d . .
C10E C 0.74900(10) 0.6369(3) 0.40689(12) 0.0350(6) Uani 1 1 d . .
H10E H 0.7563 0.7082 0.3846 0.042 Uiso 1 1 calc R U
C10F C 0.70523(10) 0.5411(3) 0.37660(11) 0.0311(6) Uani 1 1 d . .
H10F H 0.6841 0.5489 0.3343 0.037 Uiso 1 1 calc R U
C10G C 0.83155(11) 0.7272(3) 0.50313(15) 0.0486(8) Uani 1 1 d . .
H10G H 0.8320 0.7999 0.4752 0.073 Uiso 1 1 calc R U
H10H H 0.8652 0.6717 0.5182 0.073 Uiso 1 1 calc R U
H10I H 0.8288 0.7730 0.5369 0.073 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 0.0033 0.0016 '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'
S S 0.1246 0.1234 '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
C21 C1 C2 108.15(18) . .
C21 C1 C10 125.94(19) . 2_655
C2 C1 C10 125.89(19) . 2_655
C2A C2 C1 125.9(2) . .
C2A C2 C3 127.8(2) . .
C1 C2 C3 106.33(18) . .
C2B C2C C3B 129.6(2) . .
C2B C2C H2C 115.2 . .
C3B C2C H2C 115.2 . .
C21 C4 C3 107.53(18) . .
C21 C4 C5 125.6(2) . .
C3 C4 C5 126.85(19) . .
C3A C3 C4 126.5(2) . .
C3A C3 C2 126.5(2) . .
C4 C3 C2 107.02(18) . .
C4 C5 C6 110.71(17) . .
C4 C5 C5A 113.07(17) . .
C6 C5 C5A 109.93(18) . .
C4 C5 H5 107.6 . .
C6 C5 H5 107.6 . .
C5A C5 H5 107.6 . .
C5D C5C C5B 120.9(2) . .
C5D C5C H5C 119.5 . .
C5B C5C H5C 119.5 . .
C9 C8 C7 113.4(2) . .
C9 C8 H8 123.3 . .
C7 C8 H8 123.3 . .
C6 C7 C8 113.2(2) . .
C6 C7 H7 123.4 . .
C8 C7 H7 123.4 . .
C7 C6 C5 129.6(2) . .
C7 C6 S22 110.31(16) . .
C5 C6 S22 120.08(17) . .
C8 C9 C10 129.3(2) . .
C8 C9 S22 110.53(16) . .
C10 C9 S22 120.04(17) . .
C9 C10 C1 110.78(17) . 2_655
C9 C10 C10A 111.52(17) . .
C1 C10 C10A 112.67(17) 2_655 .
C9 C10 H10 107.2 . .
C1 C10 H10 107.2 2_655 .
C10A C10 H10 107.2 . .
C10D C10C C10B 121.2(2) . .
C10D C10C H10C 119.4 . .
C10B C10C H10C 119.4 . .
C1 C21 C4 110.96(19) . .
C1 C21 H21 124.5 . .
C4 C21 H21 124.5 . .
C5F C5A C5B 117.7(2) . .
C5F C5A C5 120.9(2) . .
C5B C5A C5 121.21(19) . .
C3A C3B C2C 129.0(2) . .
C3A C3B H3B 115.5 . .
C2C C3B H3B 115.5 . .
C3 C3A C3B 129.3(2) . .
C3 C3A H3A 115.3 . .
C3B C3A H3A 115.3 . .
C2C C2B C2A 128.7(2) . .
C2C C2B H2B 115.6 . .
C2A C2B H2B 115.6 . .
C2 C2A C2B 129.1(2) . .
C2 C2A H2A 115.5 . .
C2B C2A H2A 115.5 . .
C6 S22 C9 92.63(11) . .
C5C C5B C5A 121.1(2) . .
C5C C5B H5B 119.5 . .
C5A C5B H5B 119.5 . .
C5E C5D C5C 117.9(2) . .
C5E C5D C5G 121.4(2) . .
C5C C5D C5G 120.6(2) . .
C5D C5E C5F 121.7(2) . .
C5D C5E H5E 119.1 . .
C5F C5E H5E 119.1 . .
C5A C5F C5E 120.6(2) . .
C5A C5F H5F 119.7 . .
C5E C5F H5F 119.7 . .
C5D C5G H5G 109.5 . .
C5D C5G H5H 109.5 . .
H5G C5G H5H 109.5 . .
C5D C5G H5I 109.5 . .
H5G C5G H5I 109.5 . .
H5H C5G H5I 109.5 . .
C10F C10A C10B 117.6(2) . .
C10F C10A C10 121.9(2) . .
C10B C10A C10 120.5(2) . .
C10C C10B C10A 121.2(2) . .
C10C C10B H10B 119.4 . .
C10A C10B H10B 119.4 . .
C10C C10D C10E 117.6(2) . .
C10C C10D C10G 120.8(2) . .
C10E C10D C10G 121.6(2) . .
C10D C10E C10F 121.1(2) . .
C10D C10E H10E 119.5 . .
C10F C10E H10E 119.5 . .
C10A C10F C10E 121.2(2) . .
C10A C10F H10F 119.4 . .
C10E C10F H10F 119.4 . .
C10D C10G H10G 109.5 . .
C10D C10G H10H 109.5 . .
H10G C10G H10H 109.5 . .
C10D C10G H10I 109.5 . .
H10G C10G H10I 109.5 . .
H10H C10G H10I 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C21 1.397(3) .
C1 C2 1.411(3) .
C1 C10 1.515(3) 2_655
C2 C2A 1.385(3) .
C2 C3 1.496(3) .
C2C C2B 1.379(3) .
C2C C3B 1.397(3) .
C2C H2C 0.9300 .
C4 C21 1.402(3) .
C4 C3 1.411(3) .
C4 C5 1.516(3) .
C3 C3A 1.390(3) .
C5 C6 1.523(3) .
C5 C5A 1.527(3) .
C5 H5 0.9800 .
C5C C5D 1.383(3) .
C5C C5B 1.387(3) .
C5C H5C 0.9300 .
C8 C9 1.350(3) .
C8 C7 1.435(3) .
C8 H8 0.9300 .
C7 C6 1.359(3) .
C7 H7 0.9300 .
C6 S22 1.732(2) .
C9 C10 1.514(3) .
C9 S22 1.732(2) .
C10 C1 1.515(3) 2_655
C10 C10A 1.527(3) .
C10 H10 0.9800 .
C10C C10D 1.386(3) .
C10C C10B 1.389(3) .
C10C H10C 0.9300 .
C21 H21 0.9300 .
C5A C5F 1.385(3) .
C5A C5B 1.389(3) .
C3B C3A 1.392(3) .
C3B H3B 0.9300 .
C3A H3A 0.9300 .
C2B C2A 1.400(3) .
C2B H2B 0.9300 .
C2A H2A 0.9300 .
C5B H5B 0.9300 .
C5D C5E 1.372(3) .
C5D C5G 1.520(3) .
C5E C5F 1.388(3) .
C5E H5E 0.9300 .
C5F H5F 0.9300 .
C5G H5G 0.9600 .
C5G H5H 0.9600 .
C5G H5I 0.9600 .
C10A C10F 1.382(3) .
C10A C10B 1.393(3) .
C10B H10B 0.9300 .
C10D C10E 1.392(3) .
C10D C10G 1.520(3) .
C10E C10F 1.392(3) .
C10E H10E 0.9300 .
C10F H10F 0.9300 .
C10G H10G 0.9600 .
C10G H10H 0.9600 .
C10G H10I 0.9600 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.181 681 81 ' '
2 0.000 0.500 0.253 681 81 ' '
