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_7047572
_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 Gd48 N240 Ni24 O336)'
_chemical_formula_sum            'C28 H34 Gd2 N10 Ni O14'
_chemical_formula_weight         1107.86
_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     dual
_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                   32.6462(5)
_cell_length_b                   32.6462(5)
_cell_length_c                   32.6462(5)
_cell_measurement_reflns_used    3034
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.7750
_cell_measurement_theta_min      5.0510
_cell_volume                     34793.5(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -49.00  -1.00   1.00   27.54    --  -41.49  19.00  30.00   48
  2  \w     35.00 109.00   1.00   40.15    --  107.08 -95.00 150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0322844000
_diffrn_orient_matrix_UB_12      -0.0226594000
_diffrn_orient_matrix_UB_13      -0.0258823000
_diffrn_orient_matrix_UB_21      0.0178551000
_diffrn_orient_matrix_UB_22      0.0414117000
_diffrn_orient_matrix_UB_23      -0.0140442000
_diffrn_orient_matrix_UB_31      0.0294512000
_diffrn_orient_matrix_UB_32      -0.0001986000
_diffrn_orient_matrix_UB_33      0.0368298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11691
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.934
_diffrn_reflns_theta_max         66.934
_diffrn_reflns_theta_min         3.830
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.402
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             12960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0582P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3805
_reflns_number_total             5173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02816h2.cif
_cod_data_source_block           a151118b_sq
_cod_depositor_comments
'Adding full bibliography for 7047570--7047572.cif.'
_cod_original_cell_volume        34793.6(16)
_cod_database_code               7047572
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: H2(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
4.a Riding coordinates:
 O2(H2), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              63800
_shelx_fab_checksum              63956
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.848