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_4325818
_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            'C86 H114 Cl2 N8 Ni8 O30'
_chemical_formula_weight         2280.43
_space_group_IT_number           2
_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                67.9210(10)
_cell_angle_beta                 78.6370(10)
_cell_angle_gamma                89.7840(10)
_cell_formula_units_Z            1
_cell_length_a                   10.7335(8)
_cell_length_b                   14.7471(10)
_cell_length_c                   16.7834(12)
_cell_measurement_reflns_used    8891
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.942
_cell_measurement_theta_min      2.358
_cell_volume                     2406.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17538
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    1.667
_exptl_absorpt_correction_T_max  0.7210
_exptl_absorpt_correction_T_min  0.5481
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         8516
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0527
_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^)+(0.1169P)^2^+3.7538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                7513
_reflns_number_total             8516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200883b_si_002_1.cif
_cod_data_source_block           4
_cod_database_code               4325818