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_7042920
_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
'C73 H90 N4 Ni4 O14, 2(C H4 O), 2(H2 O) [+ solvent]'
_chemical_formula_sum            'C75 H102 N4 Ni4 O18'
_chemical_formula_weight         1582.44
_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                102.451(2)
_cell_angle_beta                 100.521(2)
_cell_angle_gamma                109.527(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3023(11)
_cell_length_b                   16.2603(14)
_cell_length_c                   22.3585(18)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.29
_cell_volume                     3955.5(6)
_computing_cell_refinement       'Bruker D8 Quest'
_computing_data_collection       'Bruker D8 Quest'
_computing_data_reduction        'Bruker D8 Quest'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            193877
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.269
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       rod
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         19637
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0328P)^2^+3.2951P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14822
_reflns_number_total             19637
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {281f0051-d553-4f4f-83a4-528a392fb097}
_cod_data_source_file            c7dt01579h2.cif
_cod_data_source_block           Cpd2
_cod_depositor_comments
;

2018-03-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C150 H204 N8 Ni8 O36'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     3164.88
_cod_database_code               7042920
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.906
_shelxl_version_number           2013-2
_shelx_res_checksum              75420
_shelx_fab_checksum              17948