Harnessing Structural Dynamics in a 2D Manganese-Benzoquinoid Framework To Dramatically Accelerate Metal Transport in Diffusion-Limited Metal Exchange Reactions.
Liu, Lujia; Li, Liang; DeGayner, Jordan A.; Winegar, Peter H.; Fang, Yu; Harris, T. David; Journal of the American Chemical Society 140 (2018) 11444–11453; doi:10.1021/jacs.8b06774

data_4132814
_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 Mn2 O12, 2(C8 H20 N1)'
_chemical_formula_sum            'C34 H40 Cl6 Mn2 N2 O12'
_chemical_formula_weight         991.26
_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   geom
_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                   14.0315(12)
_cell_length_b                   14.0315(12)
_cell_length_c                   10.2484(17)
_cell_measurement_reflns_used    2695
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.248
_cell_measurement_theta_min      2.600
_cell_volume                     1747.4(4)
_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      99.98
_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       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9151
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.545
_diffrn_reflns_theta_max         22.545
_diffrn_reflns_theta_min         1.676
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0698 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.8269.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.942
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         842
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0680
_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/[\s^2^(Fo^2^)+(0.0962P)^2^+6.6789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.1963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                690
_reflns_number_total             842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06774_si_002.cif
_cod_data_source_block           1
_cod_database_code               4132814
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3
 1.56 with sigma of 0.01
 C3-C4
 1.54 with sigma of 0.01
 N1-C3 \\sim N1-C5
 with sigma of 0.01
 N1-C6 \\sim N1-C4
 with sigma of 0.01
 C3-C6 \\sim C5-C4
 with sigma of 0.01
3. Restrained planarity
 N1, C3, C4, C5, C6
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
N1 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C5 \\sim C6: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C4(0.33333) H4A(0.33333) H4B(0.33333) H4C(0.33333) C3(0.33333)
 H3A(0.33333) H3B(0.33333) C5(0.33333) H5A(0.33333) H5B(0.33333) C6(0.33333)
 H6A(0.33333) H6B(0.33333) H6C(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'