Crystallographic Visualization of Postsynthetic Nickel Clusters into Metal-Organic Framework.
Wang, Xiao-Ning; Zhang, Peng; Kirchon, Angelo; Li, Jia-Luo; Chen, Wen-Miao; Zhao, Yu-Meng; Li, Bao; Zhou, Hong-Cai; Journal of the American Chemical Society 141 (2019) 13654–13663; doi:10.1021/jacs.9b06711

data_4128910
_publ_section_title
;
 Crystallographic Visualization of Postsynthetic Nickel Clusters into
 Metal-Organic Framework.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13654
_journal_page_last               13663
_journal_paper_doi               10.1021/jacs.9b06711
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C32 H16 N8 O16 Zr3'
_chemical_formula_sum            'C32 H16 N8 O16 Zr3'
_chemical_formula_weight         1042.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-18
_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                   31.368(3)
_cell_length_b                   19.7030(16)
_cell_length_c                   22.4548(19)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.46
_cell_measurement_theta_min      3.60
_cell_volume                     13878(2)
_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      99.99
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            77571
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        50.537
_diffrn_reflns_theta_max         50.537
_diffrn_reflns_theta_min         3.602
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORESS
_exptl_crystal_density_diffrn    0.499
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.638
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7418
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1313
_refine_ls_R_factor_gt           0.1077
_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^)+(0.1493P)^2^+138.2032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2728
_refine_ls_wR_factor_ref         0.2952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5508
_reflns_number_total             7418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06711_si_002.cif
_cod_data_source_block           HUST-1
_cod_database_code               4128910
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-N2 = N2-C9 = C9-N3 = N3-N4 = N4-C8 = C8-N2
 1.25 with sigma of 0.01
 N2-N3 = C9-N4 = N3-C8 = N4-N2 = C8-C9
 2.25 with sigma of 0.01
 N1-C8 = N1-C9
 2.25 with sigma of 0.02
 C5-N2 = C5-N4
 2.25 with sigma of 0.02
 C10-N2 = C10-N3
 2.25 with sigma of 0.02
3. Restrained planarity
 O1, C1, O2, C2
 with sigma of 0.01
 C2, C3, C4, C5, C6, C7
 with sigma of 0.01
 C8, C5, C4, C6
 with sigma of 0.01
 N2, C9, N3, N4, C8, N1
 with sigma of 0.01
 C5, C8, N2, N4
 with sigma of 0.01
 C10, C9, N2, N3
 with sigma of 0.01
 C11, C10, C9, C15
 with sigma of 0.01
 C11, C12, C13, C14, C15, C10
 with sigma of 0.01
 O3, O4, C16, C13
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C7(H7), C3(H3), C11(H11), C6(H6), C14(H14), C4(H4), C15(H15)
;
_shelx_res_checksum              87107
_shelx_hkl_checksum              15853
_shelx_fab_checksum              78623
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'