Exposed Equatorial Positions of Metal Centers via Sequential Ligand Elimination and Installation in MOFs.
Yuan, Shuai; Zhang, Peng; Zhang, Liangliang; Garcia-Esparza, Angel T; Sokaras, Dimosthenis; Qin, Jun-Sheng; Feng, Liang; Day, Gregory S.; Chen, Wenmiao; Drake, Hannah F.; Elumalai, Palani; Madrahimov, Sherzod T.; Sun, Daofeng; Zhou, Hong-Cai; Journal of the American Chemical Society 140 (2018) 10814–10819; doi:10.1021/jacs.8b04886

data_4132564
_publ_section_title
;
 Exposed Equatorial Positions of Metal Centers via Sequential Ligand
 Elimination and Installation in MOFs.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10814
_journal_page_last               10819
_journal_paper_doi               10.1021/jacs.8b04886
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.5(C144 H96 N24 Ni6 O64 Zr12)'
_chemical_formula_sum            'C72 H48 N12 Ni3 O32 Zr6'
_chemical_formula_weight         2316.67
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.365
_cell_length_b                   29.365
_cell_length_c                   29.365
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      77.8860
_cell_measurement_theta_min      4.2584
_cell_volume                     25321.534
_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      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 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     1.54184
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            95874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.784
_diffrn_reflns_theta_min         4.258
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.608
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         1416
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1876P)^2^+87.8949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.2594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1296
_reflns_number_total             1416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04886_si_002.cif
_cod_data_source_block           PCN160Ni
_cod_original_cell_volume        25321.0(16)
_cod_database_code               4132564
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C3-C2 = C3-C4 = C4-N1
 1.4 with sigma of 0.005
 C4_$1-C4
 2.2 with sigma of 0.005
 C3_$1-C3
 2.2 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N1) = Uanis(C4) = Uanis(C3) = Uanis(C2)
4. Others
 Fixed Sof: Ni1(0.0625)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              75670
_shelx_hkl_checksum              24112
_shelx_fab_checksum              24343
_olex2_submission_special_instructions 'No special instructions were received'