Boosting Chemical Stability, Catalytic Activity, and Enantioselectivity of Metal-Organic Frameworks for Batch and Flow Reactions.
Chen, Xu; Jiang, Hong; Hou, Bang; Gong, Wei; Liu, Yan; Cui, Yong; Journal of the American Chemical Society 139 (2017) 13476–13482; doi:10.1021/jacs.7b06459

data_4131528
_publ_section_title
;
 Boosting Chemical Stability, Catalytic Activity, and Enantioselectivity
 of Metal-Organic Frameworks for Batch and Flow Reactions.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13476
_journal_page_last               13482
_journal_paper_doi               10.1021/jacs.7b06459
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C23 H12 F6 Mn O7 P0.5'
_chemical_formula_sum            'C23 H12 F6 Mn O7 P0.5'
_chemical_formula_weight         584.75
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   27.0514(3)
_cell_length_b                   27.0514(3)
_cell_length_c                   23.2766(5)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.96
_cell_measurement_theta_min      2.68
_cell_volume                     14751.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            133153
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.304
_diffrn_reflns_theta_min         1.886
_exptl_absorpt_coefficient_mu    2.744
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    0.790
_exptl_crystal_description       needle
_exptl_crystal_F_000             3510
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.042(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         8954
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0379
_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/[\s^2^(Fo^2^)+(0.0626P)^2^+3.3342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7837
_reflns_number_total             8954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06459_si_002.cif
_cod_data_source_block           ff_sq
_cod_original_cell_volume        14751.3(5)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_original_formula_sum        'C23 H12 F6 Mn O7 P0.50'
_cod_database_code               4131528
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.810
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.958(6)
 0.042(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 F2A-C14 = F1-C14 = F3-C14 = F3A-C14 = F1A-C14 = F2-C14
 1.3 with sigma of 0.02
 F1-F3 \\sim F3-F2
 with sigma of 0.02
 F1-F2 \\sim F2-F3
 with sigma of 0.02
 F1A-F3A \\sim F3A-F2A
 with sigma of 0.02
 F1A-F2A \\sim F2A-F3A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
F1A \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
F3 \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
F3A \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C10 \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
F1 \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
F2A \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
Uanis(F2A) = Uanis(F1A) = Uanis(F3A)
Uanis(F2) = Uanis(F1) = Uanis(F3)
5. Others
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F1)=FVAR(1)
6.a Rotating group:
 O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C19(H19), C13(H13), C21(H21), C9(H9), C4(H4)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              26021
_shelx_hkl_checksum              54082
_shelx_fab_checksum              39059
_olex2_submission_special_instructions 'No special instructions were received'