Single-Crystal Synthesis and Structures of Highly Stable Ni8-Pyrazolate-Based Metal‒Organic Frameworks
Zhang, Yong-Zheng; He, Tao; Kong, Xiang-Jing; Bian, Zhen-Xing; Wu, Xue-Qian; Li, Jian-Rong; ACS Materials Letters 1 (2019) 20–; doi:10.1021/acsmaterialslett.9b00021

data_4515196
_publ_section_title
;
 Single-Crystal Synthesis and Structures of Highly Stable
 Ni8-Pyrazolate-Based Metal--Organic Frameworks
;
_journal_issue                   1
_journal_name_full               'ACS Materials Letters'
_journal_page_first              20
_journal_paper_doi               10.1021/acsmaterialslett.9b00021
_journal_volume                  1
_journal_year                    2019
_chemical_formula_moiety         '0.25(C312 H96 N120 Ni32 O24)'
_chemical_formula_sum            'C78 H24 N30 Ni8 O6'
_chemical_formula_weight         1946.95
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-15
_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                   25.3510(5)
_cell_length_b                   25.3510(5)
_cell_length_c                   25.3510(5)
_cell_measurement_reflns_used    3001
_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      73.8830
_cell_measurement_theta_min      4.8720
_cell_volume                     16292.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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      100(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00  26.00   1.00   15.00    --  -42.36  57.00 -60.00   95
  2  \w    -65.00   1.00   1.00   15.00    --  -42.36  38.00-150.00   66
  3  \w    -60.00 -18.00   1.00   15.00    --  -42.36  57.00  60.00   42
  4  \w    102.00 165.00   1.00   40.00    --  105.96  61.00 150.00   63
  5  \w    100.00 165.00   1.00   40.00    --  105.96 125.00-120.00   65
  6  \w     48.00  98.00   1.00   40.00    --  105.96 -45.00 -60.00   50
  7  \w     39.00 109.00   1.00   40.00    --  105.96 -94.00 -60.00   70
  8  \w    117.00 173.00   1.00   40.00    --  105.96  45.00-120.00   56
  9  \w     94.00 177.00   1.00   40.00    --  105.96 125.00   0.00   83
;
_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      -0.0444931000
_diffrn_orient_matrix_UB_12      -0.0338800000
_diffrn_orient_matrix_UB_13      -0.0238865000
_diffrn_orient_matrix_UB_21      -0.0341280000
_diffrn_orient_matrix_UB_22      0.0497150000
_diffrn_orient_matrix_UB_23      -0.0070273000
_diffrn_orient_matrix_UB_31      0.0235649000
_diffrn_orient_matrix_UB_32      0.0083226000
_diffrn_orient_matrix_UB_33      -0.0553679000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.975
_diffrn_reflns_theta_max         66.975
_diffrn_reflns_theta_min         3.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.794
_exptl_crystal_description       block
_exptl_crystal_F_000             3896
_refine_diff_density_max         1.986
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         793
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0673
_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^)+(0.1646P)^2^+16.6418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                687
_reflns_number_total             793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00021_si_003.cif
_cod_data_source_block           BUT-3
_cod_original_cell_volume        16292.4(10)
_cod_database_code               4515196
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Ni'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4-C5
 1.48 with sigma of 0.02
 C5-N2
 1.14 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Others
 Fixed Sof: C4(0.5) C5(0.125) N2(0.125)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              25369
_shelx_hkl_checksum              73832
_shelx_fab_checksum              61120
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.696
_oxdiff_exptl_absorpt_empirical_full_min 0.837