#------------------------------------------------------------------------------
#$Date: 2020-05-06 00:10:26 +0300 (Wed, 06 May 2020) $
#$Revision: 251768 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/48/4134897.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_4134897
loop_
_publ_author_name
'Danowski, Wojciech'
'Castiglioni, Fabio'
'Sardjan, Andy'
'Krause, Simon'
'Pfeifer, Lukas'
'Roke, Diederik'
'Comotti, Angiolina'
'Browne, Wesley R.'
'Feringa, Ben L.'
_publ_section_title
;
 Visible Light Driven Rotation of Molecular Motors in a Dual-Function
 Metal Organic Framework Enabled by Energy Transfer.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03063
_journal_year                    2020
_chemical_formula_sum            'C12 H6 N1.5 O2 Pd0.25 Zn0.5'
_chemical_formula_weight         262.47
_space_group_crystal_system      tetragonal
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5927(19)
_cell_length_b                   16.5927(19)
_cell_length_c                   22.318(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.23
_cell_measurement_theta_min      2.66
_cell_volume                     6144.5(17)
_computing_cell_refinement       'Bruker SAINT 8.37A'
_computing_data_collection       'Bruker APEX3 V2016.1-0'
_computing_data_reduction        'Bruker SAINT 8.37A'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(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           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2393
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        39.958
_diffrn_reflns_theta_max         39.958
_diffrn_reflns_theta_min         2.663
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            clear_dark_red
_exptl_crystal_density_diffrn    0.284
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.369
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1149
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.1238
_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)+(0.1696P)²+52.5070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3295
_refine_ls_wR_factor_ref         0.3715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                755
_reflns_number_total             1149
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c03063_si_004.cif
_cod_data_source_block           cu_lp18039_0m_sq
_cod_original_cell_volume        6144.7(19)
_cod_original_formula_sum        'C12 H6 N1.50 O2 Pd0.25 Zn0.50'
_cod_database_code               4134897
_shelx_shelxl_version_number     2018/1
_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   0.840
_shelx_estimated_absorpt_t_max   0.948
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
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 0.000000 0.000000 0.500000 0.153(3) Uani 1 16 d S TU P . .
Zn1 Zn 0.500000 0.500000 0.4377(4) 0.123(3) Uani 1 8 d S TU P . .
O1 O 0.4150(6) 0.4150(6) 0.4520(9) 0.134(6) Uani 1 2 d S TU P . .
N1 N 0.1198(13) 0.000000 0.500000 0.152(9) Uani 1 4 d S TU P . .
C1 C 0.2550(11) 0.0392(10) 0.500000 0.160(10) Uani 1 2 d S TU P . .
H1 H 0.300592 0.073801 0.500000 0.192 Uiso 1 2 calc R U P . .
N2 N 0.500000 0.500000 0.352(2) 0.138(11) Uani 1 8 d S TU P . .
C2 C 0.1715(10) 0.0625(11) 0.500000 0.151(8) Uani 1 2 d S TU P . .
C3 C 0.1462(11) 0.1462(11) 0.500000 0.156(10) Uani 1 4 d S TU P . .
C4 C 0.2134(12) 0.2134(12) 0.500000 0.129(9) Uani 1 4 d S TU P . .
C5 C 0.2415(10) 0.2415(10) 0.4425(14) 0.170(9) Uani 1 2 d S TU P . .
H5 H 0.220840 0.220840 0.405848 0.204 Uiso 1 2 calc R U P . .
C6 C 0.3021(9) 0.3021(9) 0.4442(14) 0.145(8) Uani 1 2 d S TU P . .
H6 H 0.324522 0.324522 0.408725 0.174 Uiso 1 2 calc R U P . .
C7 C 0.3262(13) 0.3262(13) 0.500000 0.119(8) Uani 1 4 d S TU P . .
C8 C 0.3949(16) 0.3949(16) 0.500000 0.114(9) Uani 1 4 d S TU P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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
N1 Pd1 N1 90.000(1) . 11_556 ?
N1 Pd1 N1 180.0 . 9_556 ?
N1 Pd1 N1 90.000(4) 11_556 9_556 ?
N1 Pd1 N1 90.000(4) . 3 ?
N1 Pd1 N1 180.0 11_556 3 ?
N1 Pd1 N1 90.000(2) 9_556 3 ?
N2 Zn1 O1 99.1(6) . 2_665 ?
N2 Zn1 O1 99.1(6) . 4_565 ?
O1 Zn1 O1 88.6(2) 2_665 4_565 ?
N2 Zn1 O1 99.1(6) . 3_655 ?
O1 Zn1 O1 88.6(2) 2_665 3_655 ?
O1 Zn1 O1 161.9(12) 4_565 3_655 ?
N2 Zn1 O1 99.1(6) . . ?
O1 Zn1 O1 161.9(12) 2_665 . ?
O1 Zn1 O1 88.6(2) 4_565 . ?
O1 Zn1 O1 88.6(2) 3_655 . ?
N2 Zn1 Zn1 180.0 . 9_666 ?
O1 Zn1 Zn1 80.9(6) 2_665 9_666 ?
O1 Zn1 Zn1 80.9(6) 4_565 9_666 ?
O1 Zn1 Zn1 80.9(6) 3_655 9_666 ?
O1 Zn1 Zn1 80.9(6) . 9_666 ?
C8 O1 Zn1 123(3) . . ?
C2 N1 C2 101(2) . 13 ?
C2 N1 Pd1 129.6(10) . . ?
C2 N1 Pd1 129.6(10) 13 . ?
C1 C1 C2 105.6(10) 13 . ?
N1 C2 C1 114.0(16) . . ?
N1 C2 C3 123.5(16) . . ?
C1 C2 C3 122.5(16) . . ?
C2 C3 C2 124(2) 7_556 . ?
C2 C3 C4 118.1(11) 7_556 . ?
C2 C3 C4 118.1(11) . . ?
C5 C4 C5 126(3) 10_556 . ?
C5 C4 C3 117.2(16) 10_556 . ?
C5 C4 C3 117.2(16) . . ?
C6 C5 C4 116(3) . . ?
C7 C6 C5 116(3) . . ?
C6 C7 C6 131(4) 10_556 . ?
C6 C7 C8 114.4(18) 10_556 . ?
C6 C7 C8 114.4(18) . . ?
O1 C8 O1 133(4) 10_556 . ?
O1 C8 C7 114(2) 10_556 . ?
O1 C8 C7 114(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 N1 1.99(2) . ?
Pd1 N1 1.99(2) 11_556 ?
Pd1 N1 1.99(2) 9_556 ?
Pd1 N1 1.99(2) 3 ?
Zn1 N2 1.91(4) . ?
Zn1 O1 2.019(13) 2_665 ?
Zn1 O1 2.019(13) 4_565 ?
Zn1 O1 2.019(13) 3_655 ?
Zn1 O1 2.019(13) . ?
Zn1 Zn1 2.780(18) 9_666 ?
O1 C8 1.171(17) . ?
N1 C2 1.35(2) . ?
N1 C2 1.35(2) 13 ?
C1 C1 1.30(3) 13 ?
C1 C2 1.44(2) . ?
C2 C3 1.45(2) . ?
C3 C4 1.58(4) . ?
C4 C5 1.44(3) 10_556 ?
C4 C5 1.44(3) . ?
C5 C6 1.42(3) . ?
C6 C7 1.37(2) . ?
C7 C8 1.61(5) . ?
