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_4128908
_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         'C64 Cl22 N16 Ni14 O47 Zr6'
_chemical_formula_sum            'C64 Cl22 N16 Ni14 O47 Zr6'
_chemical_formula_weight         3893.68
_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'
_audit_creation_date             2019-07-18
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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
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_cell_formula_units_Z            2
_cell_length_a                   31.4535(18)
_cell_length_b                   19.6380(12)
_cell_length_c                   21.9912(13)
_cell_measurement_reflns_used    9151
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.406
_cell_measurement_theta_min      2.809
_cell_volume                     13583.6(14)
_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      100.04
_diffrn_measured_fraction_theta_full 0.986
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_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.986
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42413
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_diffrn_reflns_theta_full        50.629
_diffrn_reflns_theta_max         50.629
_diffrn_reflns_theta_min         2.810
_exptl_absorpt_coefficient_mu    5.132
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            GREEN
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_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3693
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_exptl_crystal_size_mid          0.1
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_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
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_reflns_number_gt                5314
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_cod_data_source_block           HUST-2
_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               4128908
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C7 = C7-C2 = C1-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 0.01
 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 0.01
 C2-O1 = C2-O2
 2.45 with sigma of 0.01
 C1-O1 = C1-O2
 1.25 with sigma of 0.01
 C9-O3 = C9-O4
 2.45 with sigma of 0.01
 C8-O3 = C8-O4
 1.25 with sigma of 0.01
 C5-C15
 1.45 with sigma of 0.02
 C15-C4 = C15-C6
 2.45 with sigma of 0.02
 C12-C16
 1.45 with sigma of 0.02
 C16-C11 = C16-C13
 2.45 with sigma of 0.02
 N1-N2 = N2-C15 = C15-N3 = N3-N4 = N4-C16 = C16-N2
 1.25 with sigma of 0.01
 N2-N3 = C15-N4 = N3-C16 = N4-N2 = C16-C15
 2.25 with sigma of 0.01
 N1-C15 = N1-C16
 2.25 with sigma of 0.02
 C5-N2 = C5-N3
 2.25 with sigma of 0.02
 C12-N2 = C12-N4
 2.25 with sigma of 0.02
 O9_$2-O9 = O8_$1-O8
 3.5 with sigma of 0.02
 Ni0A-Cl2A
 2.4 with sigma of 0.02
 Ni0A-Cl1A
 2.4 with sigma of 0.02
2. Restrained planarity
 C2, C3, C4, C5, C6, C7
 with sigma of 0.075
 C1, C2, C3, C7
 with sigma of 0.075
 O1, O2, C1, C2
 with sigma of 0.075
 C9, C10, C11, C12, C13, C14
 with sigma of 0.075
 C8, C9, C10, C14
 with sigma of 0.075
 O3, O4, C8, C9
 with sigma of 0.075
 C5, C4, C6, C15
 with sigma of 0.075
 C11, C12, C13, C16
 with sigma of 0.075
 N1, C15, N2, C16
 with sigma of 0.075
 N1, N2, N3, N4, C15, C16
 with sigma of 0.075
 C5, N2, N3, C15
 with sigma of 0.075
 C12, C16, N2, N4
 with sigma of 0.075
3. Rigid bond restraints
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, O6, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni0A, Cl2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni0A, Cl1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zr02, O7, Zr01
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni2, Cl12, Ni3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2A, Ni0A, Cl1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni2, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni3, O15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
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
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
O7 \\sim O5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O6 \\sim O7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Ni3 \\sim O15: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C15) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C16) \\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(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2A) = Uanis(Cl1A)
;
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_olex2_submission_special_instructions 'No special instructions were received'