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#$Date: 2021-08-11 01:17:46 +0300 (Wed, 11 Aug 2021) $
#$Revision: 268012 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564338.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_1564338
loop_
_publ_author_name
'Chen, Qiu-Cheng'
'Fridman, Natalia'
'Tumanskii, Boris L.'
'Gross, Zeev'
_publ_section_title
;
 Chromophore-Supported Structural and Functional Model of Dinuclear Copper
 Enzymes, for Facilitating Mechanism of Action Studies
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02593G
_journal_year                    2021
_chemical_formula_moiety         'C54 H21 F20 N5 Pd2, C7 H16'
_chemical_formula_sum            'C61 H37 F20 N5 Pd2'
_chemical_formula_weight         1432.75
_chemical_name_common            'Gross222b (Chosen)'
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc24wl6v
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-03-25 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.406(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.504(3)
_cell_length_b                   21.031(3)
_cell_length_c                   16.726(3)
_cell_measurement_reflns_used    5355
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.108
_cell_measurement_theta_min      1.526
_cell_volume                     6074.5(17)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23168
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.108
_diffrn_reflns_theta_max         25.108
_diffrn_reflns_theta_min         1.526
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            green-blue
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       plate
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.526
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5355
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0546
_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)+(0.0853P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4626
_reflns_number_total             5355
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc02593g2.cif
_cod_data_source_block           Gross222b
_cod_original_cell_volume        6074.5(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1564338
_shelx_shelxl_version_number     2018/3
_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   0.885
_shelx_estimated_absorpt_t_max   0.940
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.49721(2) 0.46749(2) 0.34865(2) 0.03100(17) Uani 1 1 d . U . . .
F1 F 0.4878(2) 0.66778(17) 0.5028(2) 0.0554(9) Uani 1 1 d . U . . .
F2 F 0.4458(3) 0.7682(2) 0.5857(3) 0.0831(14) Uani 1 1 d . U . . .
F3 F 0.3233(3) 0.8390(2) 0.5242(3) 0.1003(17) Uani 1 1 d . U . . .
F4 F 0.2403(3) 0.8101(2) 0.3783(4) 0.116(2) Uani 1 1 d . U . . .
F5 F 0.2816(3) 0.7102(2) 0.2931(3) 0.0890(15) Uani 1 1 d . U . . .
F6 F 0.1721(3) 0.4048(2) 0.2684(3) 0.0946(15) Uani 1 1 d . U . . .
F7 F 0.0483(3) 0.3543(3) 0.3211(5) 0.150(3) Uani 1 1 d . U . . .
F8 F 0.0587(9) 0.2990(6) 0.4547(16) 0.102(2) Uani 0.58(3) 1 d . U P A 1
F8A F 0.0744(12) 0.3017(9) 0.495(2) 0.102(2) Uani 0.42(3) 1 d . U P A 2
F9 F 0.2074(4) 0.2965(3) 0.5672(3) 0.133(2) Uani 1 1 d . U . . .
F10 F 0.3292(3) 0.3462(2) 0.5125(2) 0.0779(13) Uani 1 1 d . U . . .
N1 N 0.3889(3) 0.5102(2) 0.3482(3) 0.0302(10) Uani 1 1 d . U . . .
N2 N 0.4391(3) 0.3850(2) 0.3024(3) 0.0334(10) Uani 1 1 d . U . . .
N3 N 0.500000 0.6080(3) 0.250000 0.0314(15) Uani 1 2 d S TU P . .
H3 H 0.500001 0.566150 0.250001 0.038 Uiso 1 2 calc R U P . .
C1 C 0.4095(3) 0.6292(2) 0.3502(3) 0.0334(12) Uani 1 1 d . U . . .
C2 C 0.3724(3) 0.5723(3) 0.3671(3) 0.0326(12) Uani 1 1 d . U . . .
C3 C 0.3050(3) 0.5724(3) 0.4047(4) 0.0408(14) Uani 1 1 d . U . . .
H3A H 0.282883 0.608575 0.425984 0.049 Uiso 1 1 calc R U . . .
C4 C 0.2780(3) 0.5126(3) 0.4049(4) 0.0408(14) Uani 1 1 d . U . . .
H4 H 0.232678 0.499026 0.424473 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3307(3) 0.4732(3) 0.3700(3) 0.0340(12) Uani 1 1 d . U . . .
C6 C 0.3229(3) 0.4072(3) 0.3621(3) 0.0350(13) Uani 1 1 d . U . . .
C7 C 0.3713(3) 0.3668(3) 0.3277(3) 0.0366(13) Uani 1 1 d . U . . .
C8 C 0.3598(4) 0.3001(3) 0.3120(3) 0.0418(14) Uani 1 1 d . U . . .
H8 H 0.317904 0.275224 0.324353 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4188(4) 0.2788(3) 0.2766(4) 0.0478(16) Uani 1 1 d . U . . .
H9 H 0.426891 0.236480 0.259834 0.057 Uiso 1 1 calc R U . . .
C10 C 0.4671(3) 0.3330(3) 0.2694(4) 0.0388(14) Uani 1 1 d . U . . .
C11 C 0.4780(3) 0.7099(3) 0.2794(4) 0.0428(15) Uani 1 1 d . U . . .
H11 H 0.461065 0.746731 0.304368 0.051 Uiso 1 1 calc R U . . .
C12 C 0.4606(3) 0.6446(2) 0.2986(3) 0.0323(12) Uani 1 1 d . U . . .
C13 C 0.3854(3) 0.6856(2) 0.3956(4) 0.0350(12) Uani 1 1 d . U . . .
C14 C 0.4261(4) 0.7020(3) 0.4706(4) 0.0406(13) Uani 1 1 d . U . . .
C15 C 0.4056(4) 0.7534(3) 0.5133(4) 0.0499(15) Uani 1 1 d . U . . .
C16 C 0.3427(4) 0.7887(3) 0.4813(5) 0.0620(18) Uani 1 1 d . U . . .
C17 C 0.3013(4) 0.7754(3) 0.4073(5) 0.065(2) Uani 1 1 d . U . . .
C18 C 0.3225(4) 0.7233(3) 0.3654(4) 0.0545(17) Uani 1 1 d . U . . .
C19 C 0.2539(2) 0.3774(2) 0.3895(3) 0.0439(14) Uani 1 1 d G U . . .
C20 C 0.1817(3) 0.3791(2) 0.3405(3) 0.0658(19) Uani 1 1 d G U . . .
C21 C 0.1176(2) 0.3531(3) 0.3678(4) 0.089(2) Uani 1 1 d G U . . .
C22 C 0.1258(3) 0.3253(2) 0.4441(4) 0.102(2) Uani 1 1 d G U . . .
C23 C 0.1980(3) 0.3236(2) 0.4931(3) 0.079(2) Uani 1 1 d G U . . .
C24 C 0.2620(2) 0.3496(2) 0.4658(2) 0.0551(17) Uani 1 1 d G U . . .
C25 C 0.6131(4) 0.4318(3) 0.3788(4) 0.0481(16) Uani 1 1 d . U . . .
H25A H 0.617(4) 0.405(3) 0.437(4) 0.07(2) Uiso 1 1 d . . . . .
H25B H 0.624(4) 0.402(4) 0.328(5) 0.09(3) Uiso 1 1 d . . . . .
C26 C 0.6147(3) 0.4974(3) 0.3737(4) 0.0479(15) Uani 1 1 d . U . . .
H26 H 0.638977 0.518364 0.330335 0.057 Uiso 1 1 calc R U . . .
C27 C 0.5709(3) 0.5329(3) 0.4190(4) 0.0453(15) Uani 1 1 d . U . . .
H27A H 0.563417 0.578283 0.404048 0.054 Uiso 1 1 calc R U . . .
H27B H 0.580581 0.525500 0.478202 0.054 Uiso 1 1 calc R U . . .
C28 C 0.1993(10) 0.5605(10) 0.1778(12) 0.264(12) Uani 1 1 d D U . . .
H28A H 0.179314 0.536622 0.128505 0.396 Uiso 1 1 calc R U . . .
H28B H 0.222795 0.531018 0.220140 0.396 Uiso 1 1 calc R U . . .
H28C H 0.238398 0.590994 0.166171 0.396 Uiso 1 1 calc R U . . .
C29 C 0.1341(8) 0.5956(8) 0.2062(11) 0.215(8) Uani 1 1 d D U . . .
H29A H 0.113230 0.626273 0.163274 0.258 Uiso 1 1 calc R U . . .
H29B H 0.156518 0.620778 0.254385 0.258 Uiso 1 1 calc R U . . .
C30 C 0.0669(10) 0.5589(7) 0.2280(18) 0.35(2) Uani 1 1 d D U . . .
H30A H 0.086850 0.530808 0.274165 0.426 Uiso 1 1 calc R U . . .
H30B H 0.046800 0.531102 0.181505 0.426 Uiso 1 1 calc R U . . .
C31 C 0.000000 0.5958(10) 0.250000 0.214(11) Uani 1 2 d DS TU P . .
H31A H 0.020124 0.623704 0.296305 0.257 Uiso 0.5 1 calc R U P . .
H31B H -0.020124 0.623706 0.203697 0.257 Uiso 0.5 1 calc R U P . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/chem.202002682 2020
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
N2 Pd1 N1 88.23(17) . . ?
N2 Pd1 C27 164.3(2) . . ?
N1 Pd1 C27 101.1(2) . . ?
N2 Pd1 C26 135.6(2) . . ?
N1 Pd1 C26 135.9(2) . . ?
C27 Pd1 C26 38.1(2) . . ?
N2 Pd1 C25 100.5(2) . . ?
N1 Pd1 C25 166.1(2) . . ?
C27 Pd1 C25 68.1(2) . . ?
C26 Pd1 C25 37.8(2) . . ?
C5 N1 C2 106.3(4) . . ?
C5 N1 Pd1 117.7(4) . . ?
C2 N1 Pd1 128.7(3) . . ?
C10 N2 C7 106.7(4) . . ?
C10 N2 Pd1 129.4(4) . . ?
C7 N2 Pd1 120.5(3) . . ?
C12 N3 C12 112.3(6) . 2_655 ?
C12 C1 C2 133.7(5) . . ?
C12 C1 C13 113.2(5) . . ?
C2 C1 C13 113.0(5) . . ?
N1 C2 C1 129.3(5) . . ?
N1 C2 C3 108.7(5) . . ?
C1 C2 C3 121.9(5) . . ?
C4 C3 C2 108.5(5) . . ?
C3 C4 C5 106.8(5) . . ?
N1 C5 C6 126.9(5) . . ?
N1 C5 C4 109.6(5) . . ?
C6 C5 C4 123.5(5) . . ?
C7 C6 C5 126.1(5) . . ?
C7 C6 C19 116.7(5) . . ?
C5 C6 C19 117.2(5) . . ?
N2 C7 C6 124.9(5) . . ?
N2 C7 C8 108.5(5) . . ?
C6 C7 C8 126.6(5) . . ?
C9 C8 C7 108.1(5) . . ?
C8 C9 C10 106.1(5) . . ?
N2 C10 C10 124.4(3) . 2_655 ?
N2 C10 C9 110.6(5) . . ?
C10 C10 C9 125.0(4) 2_655 . ?
C11 C11 C12 109.1(3) 2_655 . ?
C1 C12 N3 132.3(5) . . ?
C1 C12 C11 122.8(5) . . ?
N3 C12 C11 104.7(5) . . ?
C14 C13 C18 116.8(5) . . ?
C14 C13 C1 120.6(5) . . ?
C18 C13 C1 122.6(6) . . ?
F1 C14 C15 118.5(6) . . ?
F1 C14 C13 119.7(5) . . ?
C15 C14 C13 121.9(6) . . ?
F2 C15 C16 120.1(6) . . ?
F2 C15 C14 120.7(6) . . ?
C16 C15 C14 119.1(6) . . ?
F3 C16 C17 120.1(7) . . ?
F3 C16 C15 118.4(7) . . ?
C17 C16 C15 121.5(6) . . ?
F4 C17 C16 120.0(6) . . ?
F4 C17 C18 121.4(7) . . ?
C16 C17 C18 118.5(6) . . ?
F5 C18 C13 119.4(6) . . ?
F5 C18 C17 118.4(6) . . ?
C13 C18 C17 122.2(7) . . ?
C20 C19 C24 120.0 . . ?
C20 C19 C6 120.6(4) . . ?
C24 C19 C6 119.4(4) . . ?
F6 C20 C21 118.4(4) . . ?
F6 C20 C19 121.6(4) . . ?
C21 C20 C19 120.0 . . ?
F7 C21 C20 120.4(5) . . ?
F7 C21 C22 119.6(5) . . ?
C20 C21 C22 120.0 . . ?
F8 C22 C21 109.6(12) . . ?
F8 C22 C23 130.1(11) . . ?
C21 C22 C23 120.0 . . ?
C21 C22 F8A 135.6(14) . . ?
C23 C22 F8A 104.0(14) . . ?
F9 C23 C24 118.9(5) . . ?
F9 C23 C22 121.1(5) . . ?
C24 C23 C22 120.0 . . ?
F10 C24 C23 118.6(4) . . ?
F10 C24 C19 121.4(4) . . ?
C23 C24 C19 120.0 . . ?
C26 C25 Pd1 70.4(4) . . ?
C27 C26 C25 119.0(6) . . ?
C27 C26 Pd1 70.3(4) . . ?
C25 C26 Pd1 71.8(4) . . ?
C26 C27 Pd1 71.7(4) . . ?
C28 C29 C30 119.4(14) . . ?
C29 C30 C31 117.9(9) . . ?
C30 C31 C30 117.8(17) 2 . ?
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
Pd1 N2 2.094(4) . ?
Pd1 N1 2.096(4) . ?
Pd1 C27 2.108(6) . ?
Pd1 C26 2.126(6) . ?
Pd1 C25 2.144(6) . ?
F1 C14 1.335(7) . ?
F2 C15 1.334(8) . ?
F3 C16 1.352(7) . ?
F4 C17 1.319(8) . ?
F5 C18 1.331(8) . ?
F6 C20 1.307(6) . ?
F7 C21 1.331(7) . ?
F8 C22 1.337(11) . ?
F8A C22 1.424(19) . ?
F9 C23 1.348(6) . ?
F10 C24 1.303(6) . ?
N1 C5 1.378(6) . ?
N1 C2 1.385(7) . ?
N2 C10 1.353(7) . ?
N2 C7 1.378(7) . ?
N3 C12 1.383(6) . ?
N3 C12 1.383(6) 2_655 ?
C1 C12 1.379(7) . ?
C1 C2 1.412(7) . ?
C1 C13 1.506(7) . ?
C2 C3 1.424(7) . ?
C3 C4 1.343(8) . ?
C4 C5 1.434(7) . ?
C5 C6 1.400(7) . ?
C6 C7 1.388(8) . ?
C6 C19 1.498(6) . ?
C7 C8 1.437(8) . ?
C8 C9 1.349(8) . ?
C9 C10 1.435(8) . ?
C10 C10 1.413(11) 2_655 ?
C11 C11 1.343(11) 2_655 ?
C11 C12 1.454(7) . ?
C13 C14 1.381(8) . ?
C13 C18 1.383(8) . ?
C14 C15 1.375(8) . ?
C15 C16 1.364(10) . ?
C16 C17 1.358(10) . ?
C17 C18 1.383(9) . ?
C19 C20 1.3900 . ?
C19 C24 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C25 C26 1.383(9) . ?
C26 C27 1.381(9) . ?
C28 C29 1.5000(11) . ?
C29 C30 1.5000(11) . ?
C30 C31 1.5001(11) . ?
