Cuboidal [Ni4O4] cluster as a precursor to recyclable, carbon-supported nickel nanoparticle reduction catalysts
Yuan, Yan-Qiu; Yuan, Feng-Ling; Li, Fei-Long; Hao, Zhi-Min; Guo, Jun; Young, David James; Zhang, Wen-Hua; Lang, Jian-Ping; Dalton Trans.  (2017) –; doi:10.1039/C7DT01579H

data_7042918
_publ_section_title
;
 Cuboidal [Ni4O4] cluster as a precursor to recyclable, carbon-supported
 nickel nanoparticle reduction catalysts
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01579H
_journal_year                    2017
_chemical_formula_moiety         'C68 H80 N4 Ni4 O14, H2 O'
_chemical_formula_sum            'C68 H82 N4 Ni4 O15'
_chemical_formula_weight         1430.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                76.203(3)
_cell_angle_beta                 84.493(3)
_cell_angle_gamma                88.665(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2603(4)
_cell_length_b                   12.8921(4)
_cell_length_c                   23.0008(8)
_cell_measurement_reflns_used    11263
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.8960
_cell_measurement_theta_min      3.0870
_cell_volume                     3514.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40832
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.415
_diffrn_reflns_theta_min         2.819
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         18299
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0733P)^2^+6.3708P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12527
_reflns_number_total             18299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01579h2.cif
_cod_data_source_block           NI4
_cod_database_code               7042918
_publcif_datablock.id            {902db103-326b-4fbb-9f2a-1c4c9b795c8c}
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.807
_shelxl_version_number           2013-2
_shelx_res_checksum              27394