A novel POMos-based hybrid with penta-coordinated Mo in trigonal bipyramid: structure and an efficient precursor for hydrodesulfurization catalyst
Liang, Ji-Lei; Lu, Yu-Kun; Zhao, Jin-chong; Li, Xue-Hui; Pan, Yuan; Wu, Meng-Meng; Liu, Yun-Qi; Liu, Chen-Guang; RSC Advances 4 (2014) 27787–; doi:10.1039/c4ra02696a

data_7216865
_publ_section_title
;
 A novel POMos-based hybrid with penta-coordinated Mo in trigonal
 bipyramid: structure and an efficient precursor for hydrodesulfurization
 catalyst
;
_journal_issue                   53
_journal_name_full               'RSC Advances'
_journal_page_first              27787
_journal_paper_doi               10.1039/c4ra02696a
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C15 H12 Mo2 N3 Ni O7'
_chemical_formula_sum            'C15 H12 Mo2 N3 Ni O7'
_chemical_formula_weight         596.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.021(8)
_cell_angle_beta                 90.098(6)
_cell_angle_gamma                106.227(8)
_cell_formula_units_Z            2
_cell_length_a                   7.1747(5)
_cell_length_b                   11.1258(13)
_cell_length_c                   11.4017(8)
_cell_measurement_temperature    293(2)
_cell_volume                     864.53(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4971
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.138
_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     256
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                2291
_reflns_number_total             3110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra02696a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        864.53(13)
_cod_database_code               7216865