Three microporous metal-organic frameworks assembled from dodecanuclear {NiLn} subunits: synthesis, structure, gas adsorption and magnetism.
Feng, Dan-Dan; Dong, Hui-Ming; Liu, Zheng-Yu; Zhao, Xiao-Jun; Yang, En-Cui; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15344–15352; doi:10.1039/c8dt02816h

data_7047571
_publ_section_title
;
 Three microporous metal-organic frameworks assembled from dodecanuclear
 {NiLn} subunits: synthesis, structure, gas adsorption and magnetism.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15344
_journal_page_last               15352
_journal_paper_doi               10.1039/c8dt02816h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.04(C672 H816 N240 Ni24 O336 Tb48)'
_chemical_formula_sum            'C28 H34 N10 Ni O14 Tb2'
_chemical_formula_weight         1111.20
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-13 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   32.2995(5)
_cell_length_b                   32.2995(5)
_cell_length_c                   32.2995(5)
_cell_measurement_reflns_used    9139
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.36
_cell_volume                     33696.7(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            123673
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         1.261
_exptl_absorpt_coefficient_mu    2.875
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1249 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.8835. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             13008
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+112.1332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5702
_reflns_number_total             6999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02816h2.cif
_cod_data_source_block           n151022a_sq
_cod_depositor_comments
'Adding full bibliography for 7047570--7047572.cif.'
_cod_original_cell_volume        33696.7(16)
_cod_database_code               7047571
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.570
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. Others
 Fixed Sof: H2(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
4.a Riding coordinates:
 O2(H2), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3)
;
_shelx_res_checksum              29799
_shelx_fab_checksum              62029
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'