Hydrothermal Synthesis, Structures and Magnetic Studies of Transition Metal Sulfates Containing Hydrazine
Li-Hui Jia; Ru-Yin Li; Zhi-Ming Duan; Shang-Da Jiang; Bing-Wu Wang; Zhe-Ming Wang; Song Gao; Inorganic Chemistry 50 (2011) 144–154; doi:10.1021/ic101488k

data_4324097
_publ_section_title
;
 Hydrothermal Synthesis, Structures and Magnetic Studies of Transition
 Metal Sulfates Containing Hydrazine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              144
_journal_page_last               154
_journal_paper_doi               10.1021/ic101488k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'H5 N2 Ni0.5 O4 S'
_chemical_formula_weight         158.47
_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                90.57(3)
_cell_angle_beta                 105.73(3)
_cell_angle_gamma                98.93(3)
_cell_formula_units_Z            2
_cell_length_a                   5.2667(11)
_cell_length_b                   5.8284(12)
_cell_length_c                   7.3005(15)
_cell_measurement_reflns_used    1169
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     212.77(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3856
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  0.7664
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            Blue-Green
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             162
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.098(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                842
_reflns_number_total             966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101488k_si_002.cif
_cod_data_source_block           last
_cod_original_cell_volume        212.78(8)
_cod_original_formula_sum        'H5 N2 Ni0.50 O4 S'
_cod_database_code               4324097