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_4128909
_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 Ni3 O26 Zr3, 5(Br)'
_chemical_formula_sum            'C32 H16 Br5 N8 Ni3 O26 Zr3'
_chemical_formula_weight         1777.76
_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
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.698(7)
_cell_length_b                   18.590(4)
_cell_length_c                   22.055(4)
_cell_measurement_reflns_used    6111
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      50.406
_cell_measurement_theta_min      2.809
_cell_volume                     12996(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.76
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0000
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38925
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        51.122
_diffrn_reflns_theta_max         51.122
_diffrn_reflns_theta_min         2.441
_exptl_absorpt_coefficient_mu    4.505
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    0.909
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3404
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
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_refine_diff_density_min         -1.209
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     355
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_refine_ls_R_factor_gt           0.1587
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3818
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_reflns_number_gt                3354
_reflns_number_total             7000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06711_si_004.cif
_cod_data_source_block           HUST-3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'NONE' was changed
to 'none' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4128909
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C7 = C7-C2
 1.45 with sigma of 0.01
 C2-C4 = C3-C5 = C4-C6 = C5-C7 = C6-C2 = C7-C3
 2.45 with sigma of 0.01
 C1-C3 = C1-C7
 2.45 with sigma of 0.02
 C1-O1 = C1-O2
 1.25 with sigma of 0.02
 O1-O2
 2.24 with sigma of 0.02
 C2-O1 = C2-O2
 2.45 with sigma of 0.02
 C8-C9 = C9-C10 = C10-C11 = C11-C12 = C12-C13 = C13-C14 = C14-C9
 1.45 with sigma of 0.01
 C9-C11 = C10-C12 = C11-C13 = C12-C14 = C13-C9 = C14-C10
 2.45 with sigma of 0.01
 C8-C10 = C8-C14
 2.45 with sigma of 0.02
 C8-O3 = C8-O4
 1.25 with sigma of 0.02
 O3-O4
 2.24 with sigma of 0.02
 C9-O3 = C9-O4
 2.45 with sigma of 0.02
 C12-C16
 1.45 with sigma of 0.02
 N1-N2 = N2-C15 = C15-N3 = N3-N4 = N4-C16 = C16-N2
 1.3 with sigma of 0.02
 N2-N3 = C15-N4 = N3-C16 = N4-N2 = C16-C15
 2.3 with sigma of 0.02
 N1-C15 = N1-C16
 2.45 with sigma of 0.02
 Ni1-O10
 2.1 with sigma of 0.02
 O10-Ni2
 2.1 with sigma of 0.02
 Ni2-O15
 2.1 with sigma of 0.02
 Ni2-O14
 2.1 with sigma of 0.02
 Ni1-O12
 2.1 with sigma of 0.02
 Ni1-O11
 2.1 with sigma of 0.02
 O13-Ni1
 2.1 with sigma of 0.02
 C15-C4
 2.45 with sigma of 0.01
 O16-Ni2
 2.2 with sigma of 0.02
 O9-Zr02
 2.2 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C7
 with sigma of 0.025
 C2, C3, C4, C5, C6, C7
 with sigma of 0.025
 O1, O2, C1, C2
 with sigma of 0.05
 C8, C9, C10, C14
 with sigma of 0.05
 C9, C10, C11, C12, C13, C14
 with sigma of 0.05
 O3, O4, C8, C9
 with sigma of 0.05
 C11, C12, C13, C16
 with sigma of 0.05
 N1, N2, N3, N4, C15, C16
 with sigma of 0.05
 C12, C16, N2, N4
 with sigma of 0.05
 C15, C5, C4, C6
 with sigma of 0.05
4. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, N2, N3, N4, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni1, O10, Ni2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O11, Ni1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N1 \\sim N2 \\sim N3 \\sim N4 \\sim C15 \\sim C16: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O10 \\sim Ni1 \\sim Ni2: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O11 \\sim Ni1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br4) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br1)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C3(H3), C11(H11), C7(H7), C4(H4), C10(H10), C13(H13)
;
_shelx_res_checksum              78778
_shelx_hkl_checksum              43446
_shelx_fab_checksum              88119
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'