Lewis Acid Activation of a Hydrogen Bond Donor Metal‒Organic Framework for Catalysis
Hall, Edward A.; Redfern, Louis R.; Wang, Michael H.; Scheidt, Karl A.; ACS Catalysis 6 (2016) 3248–; doi:10.1021/acscatal.6b00424

data_4513872
_publ_section_title
;
 Lewis Acid Activation of a Hydrogen Bond Donor Metal--Organic Framework
 for Catalysis
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              3248
_journal_paper_doi               10.1021/acscatal.6b00424
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         '0.13(C408 H256 N32 O72 Zn16)'
_chemical_formula_sum            'C51 H32 N4 O9 Zn2'
_chemical_formula_weight         975.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           136
_space_group_name_Hall           '-P 4n 2n'
_space_group_name_H-M_alt        'P 42/m n m'
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-28
_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                90
_cell_formula_units_Z            8
_cell_length_a                   36.0683(19)
_cell_length_b                   36.0683(19)
_cell_length_c                   27.0566(12)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      58.736
_cell_measurement_theta_min      2.740
_cell_volume                     35199(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.805
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.805
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            89846
_diffrn_reflns_point_group_measured_fraction_full 0.805
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.975
_diffrn_reflns_theta_min         1.732
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0928 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.7257.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.368
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         13435
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.2038
_refine_ls_R_factor_gt           0.1212
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3688
_refine_ls_wR_factor_ref         0.4101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3862
_reflns_number_total             13435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b00424_si_002.cif
_cod_data_source_block           cx0113_0m
_cod_depositor_comments          'Adding full bibliography for 4513872.cif.'
_cod_original_cell_volume        35199(4)
_cod_database_code               4513872
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.849
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N3-C25_$1 \\sim C26_$1-C25_$1 \\sim C27-C26_$1 \\sim C27-C26 \\sim C26-C25
\\sim N3-C25
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C7(H7), C10(H10), C20(H20), C17(H17), N1(H1), C12(H12), C9(H9),
 C5(H5), C16(H16), C3(H3), C13(H13), C23(H23), C22(H22), C26(H26), C25(H25)
;
_shelx_res_checksum              30439
_shelx_hkl_checksum              94135
_olex2_date_sample_data_collection 2014-10-28
_olex2_date_sample_submission    2014-10-21
_olex2_submission_special_instructions 'No special instructions were received'