#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:30:35 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242715 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/28/4132816.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_4132816
loop_
_publ_author_name
'Liu, Lujia'
'Li, Liang'
'DeGayner, Jordan A.'
'Winegar, Peter H.'
'Fang, Yu'
'Harris, T. David'
_publ_section_title
;
 Harnessing Structural Dynamics in a 2D Manganese-Benzoquinoid Framework
 To Dramatically Accelerate Metal Transport in Diffusion-Limited Metal
 Exchange Reactions.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11444
_journal_page_last               11453
_journal_paper_doi               10.1021/jacs.8b06774
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C18 Cl6 O12 Zn2, C18 H42 N6 O6 Zn1'
_chemical_formula_sum            'C36 H42 Cl6 N6 O18 Zn3'
_chemical_formula_weight         1255.56
_space_group_crystal_system      trigonal
_space_group_IT_number           162
_space_group_name_Hall           '-P 3 2'
_space_group_name_H-M_alt        'P -3 1 m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2017-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   13.729(2)
_cell_length_b                   13.729(2)
_cell_length_c                   9.580(4)
_cell_measurement_reflns_used    3017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.372
_cell_measurement_theta_min      2.731
_cell_volume                     1563.8(7)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6731
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.136
_diffrn_reflns_theta_max         24.136
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.7887.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.200
_refine_diff_density_min         -2.528
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.711
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         906
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.679
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.1393
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4038
_refine_ls_wR_factor_ref         0.4215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                590
_reflns_number_total             906
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b06774_si_002.cif
_cod_data_source_block           3a
_cod_original_cell_volume        1563.8(8)
_cod_database_code               4132816
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O2, C3, N1, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zn2, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O2 \\sim C3 \\sim N1 \\sim C4 \\sim C5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: O2(0.5) C3(0.5) H3(0.5) N1(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
5.a Free rotating group:
 O2(C3,H3,N1,C4,H4A,H4B,H4C,C5,H5A,H5B,H5C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, 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
Zn1 Zn 0.6667 0.3333 1.0000 0.0527(14) Uani 1 6 d S T P . .
Cl1 Cl 0.6211(4) 0.6211(4) 0.7155(6) 0.078(2) Uani 1 2 d S T P . .
O1 O 0.6481(6) 0.4512(6) 0.8806(9) 0.056(2) Uani 1 1 d . . . . .
C1 C 0.5802(8) 0.4777(8) 0.9303(12) 0.047(3) Uani 1 1 d . . . . .
C2 C 0.5530(11) 0.5530(11) 0.8695(18) 0.052(4) Uani 1 2 d S T P . .
Zn2 Zn 1.0000 1.0000 0.5000 0.103(3) Uani 1 12 d S TU P . .
O2 O 1.030(4) 1.104(3) 0.407(3) 0.241(17) Uani 0.5 1 d . U . A -1
C3 C 1.026(4) 1.184(2) 0.353(3) 0.246(17) Uani 0.5 1 d G U . A -1
H3 H 0.9647 1.1929 0.3762 0.295 Uiso 0.5 1 d G . . A -1
N1 N 1.099(4) 1.256(2) 0.268(3) 0.248(18) Uani 0.5 1 d G U . A -1
C4 C 1.196(4) 1.247(4) 0.229(5) 0.255(19) Uani 0.5 1 d G U . A -1
H4A H 1.2624 1.3188 0.2364 0.382 Uiso 0.5 1 d G . . A -1
H4B H 1.1871 1.2196 0.1351 0.382 Uiso 0.5 1 d G . . A -1
H4C H 1.2016 1.1946 0.2910 0.382 Uiso 0.5 1 d G . . A -1
C5 C 1.093(6) 1.351(3) 0.211(5) 0.253(19) Uani 0.5 1 d G U . A -1
H5A H 1.0260 1.3488 0.2452 0.380 Uiso 0.5 1 d G . . A -1
H5B H 1.0899 1.3459 0.1112 0.380 Uiso 0.5 1 d G . . A -1
H5C H 1.1576 1.4194 0.2396 0.380 Uiso 0.5 1 d G . . A -1
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 O1 96.2(4) 6_557 3_665
O1 Zn1 O1 93.1(3) 5_657 4_667
O1 Zn1 O1 93.1(3) 2_655 .
O1 Zn1 O1 93.1(3) 6_557 5_657
O1 Zn1 O1 93.1(3) 3_665 .
O1 Zn1 O1 78.7(4) 3_665 5_657
O1 Zn1 O1 167.9(4) 3_665 4_667
O1 Zn1 O1 78.7(4) 6_557 2_655
O1 Zn1 O1 167.9(4) 6_557 .
O1 Zn1 O1 93.1(3) 3_665 2_655
O1 Zn1 O1 96.2(4) 5_657 .
O1 Zn1 O1 167.9(4) 5_657 2_655
O1 Zn1 O1 78.7(4) 4_667 .
O1 Zn1 O1 93.1(3) 6_557 4_667
O1 Zn1 O1 96.2(4) 2_655 4_667
C1 O1 Zn1 114.4(7) . .
O1 C1 C1 116.3(6) . 4_667
O1 C1 C2 124.9(11) . .
C2 C1 C1 118.8(7) . 4_667
C1 C2 Cl1 118.8(7) . .
C1 C2 Cl1 118.8(7) 10 .
C1 C2 C1 122.4(15) 10 .
C3 O2 Zn2 160(3) . .
O2 C3 H3 117.4 . .
O2 C3 N1 125.1 . .
N1 C3 H3 117.5 . .
C3 N1 C4 119.4 . .
C3 N1 C5 123.5 . .
C5 N1 C4 117.1 . .
N1 C4 H4A 109.4 . .
N1 C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4B 109.6 . .
H4A C4 H4C 109.4 . .
H4B C4 H4C 109.4 . .
N1 C5 H5A 109.4 . .
N1 C5 H5B 109.4 . .
N1 C5 H5C 109.4 . .
H5A C5 H5B 109.5 . .
H5A C5 H5C 109.4 . .
H5B C5 H5C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.099(8) 6_557
Zn1 O1 2.099(8) 4_667
Zn1 O1 2.099(8) 2_655
Zn1 O1 2.099(8) 3_665
Zn1 O1 2.099(8) 5_657
Zn1 O1 2.099(8) .
Cl1 C2 1.746(17) .
O1 C1 1.251(12) .
C1 C1 1.55(2) 4_667
C1 C2 1.391(13) .
C2 C1 1.391(13) 10
Zn2 O2 1.55(2) .
O2 C3 1.2473 .
C3 H3 0.9298 .
C3 N1 1.2864 .
N1 C4 1.4474 .
N1 C5 1.4469 .
C4 H4A 0.9594 .
C4 H4B 0.9593 .
C4 H4C 0.9601 .
C5 H5A 0.9594 .
C5 H5B 0.9587 .
C5 H5C 0.9603 .
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_4
Zn1 O1 C1 C1 0.1(15) . 4_667
Zn1 O1 C1 C2 -179.3(11) . .
O1 C1 C2 Cl1 -2.4(19) . .
O1 C1 C2 C1 -179.3(9) . 10
C1 C1 C2 Cl1 178.2(11) 4_667 .
C1 C1 C2 C1 1(2) 4_667 10
Zn2 O2 C3 N1 174(7) . .
O2 C3 N1 C4 -0.6 . .
O2 C3 N1 C5 -178.0 . .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.000 0.000 54.6 21.0
2 0.190 0.698 0.500 300.1 56.2
