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_4515195
_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(C264 H136 N48 Ni16 O12)'
_chemical_formula_sum            'C66 H34 N12 Ni4 O3'
_chemical_formula_weight         1277.89
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-26
_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                   28.7935(2)
_cell_length_b                   28.7935(2)
_cell_length_c                   21.0494(3)
_cell_measurement_reflns_used    8359
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      69.2980
_cell_measurement_theta_min      2.5810
_cell_volume                     17451.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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_temperature      253(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -57.00 -27.00   0.50   20.00    --  -45.20  24.00-126.00   60
  2  \w    -22.00  15.00   0.50   20.00    --  -45.20  24.00-126.00   74
  3  \w    -94.00 -18.00   0.50   60.00    -- -100.80  24.00-126.00  152
  4  \w    -83.00  14.00   0.50   20.00    --    5.00 -57.00-120.00  194
  5  \w    -83.00 -52.00   0.50   20.00    --  -45.20 -24.00  68.00   62
  6  \w   -108.00 -14.00   0.50   60.00    -- -100.80  57.00 -60.00  188
  7  \w    -44.00 -11.00   0.50   60.00    -- -100.80  38.00-120.00   66
  8  \w   -129.00-100.00   0.50   60.00    -- -100.80 -57.00   0.00   58
  9  \w   -190.00-135.00   0.50   60.00    -- -100.80 -57.00   0.00  110
 10  \w   -111.00 -76.00   0.50   60.00    -- -100.80  38.00-120.00   70
 11  \w   -114.00 -40.00   0.50   60.00    -- -100.80  72.00 -30.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143732000
_diffrn_orient_matrix_UB_12      -0.0492361000
_diffrn_orient_matrix_UB_13      0.0208310000
_diffrn_orient_matrix_UB_21      -0.0081250000
_diffrn_orient_matrix_UB_22      -0.0177744000
_diffrn_orient_matrix_UB_23      -0.0681324000
_diffrn_orient_matrix_UB_31      0.0508946000
_diffrn_orient_matrix_UB_32      0.0110567000
_diffrn_orient_matrix_UB_33      -0.0167697000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28540
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.044
_diffrn_reflns_theta_max         67.044
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    0.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3317
_refine_ls_wR_factor_ref         0.3406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5840
_reflns_number_total             7954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00021_si_007.cif
_cod_data_source_block           BUT-123
_cod_database_code               4515195
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni C O N'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.939
_reflns_odcompleteness_completeness 99.12
_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. 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
3. 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
4. Others
 Sof(C18B)=Sof(C19B)=1-FVAR(1)
 Sof(C18A)=Sof(C19A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C16(H16), C17(H17), C6(H6), C8(H8), C14(H14), C13(H13), C11(H11),
 C10(H10)
;
_shelx_res_checksum              19039
_shelx_hkl_checksum              11481
_shelx_fab_checksum              26995
_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 1.545
_oxdiff_exptl_absorpt_empirical_full_min 0.720