Microwave versus Traditional Solvothermal Synthesis of Ni7II Discs: Effect of Ligand on Exchange Reaction in Solution Studied by Electrospray Ionization-Mass Spectroscopy and Magnetic Properties
Lian-Qiang Wei; Kun Zhang; Ying-Chun Feng; Yun-Hong Wang; Ming-Hua Zeng; Mohamedally Kurmoo; Inorganic Chemistry 50 (2011) 7274–7283; doi:10.1021/ic200883b

data_4325819
_publ_contact_author_email       ZMH@MAILBOX.GXNU.EDU.CN
_publ_contact_author_name        'Ming-Hua Zeng'
_publ_section_title
;
 Microwave versus Traditional Solvothermal Synthesis of Ni7II Discs:
 Effect of Ligand on Exchange Reaction in Solution Studied by Electrospray
 Ionization-Mass Spectroscopy and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7274
_journal_page_last               7283
_journal_paper_doi               10.1021/ic200883b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C54 H66 Cl2 N6 Ni7 O26'
_chemical_formula_weight         1697.00
_space_group_IT_number           147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   14.043(2)
_cell_length_b                   14.043(2)
_cell_length_c                   9.4780(19)
_cell_measurement_reflns_used    1909
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.252
_cell_measurement_theta_min      2.724
_cell_volume                     1618.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8194
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    2.160
_exptl_absorpt_correction_T_max  0.7862
_exptl_absorpt_correction_T_min  0.6719
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1907
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+9.4524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.2237
_reflns_number_gt                1144
_reflns_number_total             1907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200883b_si_002_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1618.8(5)
_cod_database_code               4325819