Synthesis, Structure, and Magnetic Properties of Amine-Templated Open-Framework Nickel(II) Sulfates
J. N. Behera; K. V. Gopalkrishnan; C. N. R. Rao; Inorganic Chemistry 43 (2004) 2636–2642; doi:10.1021/ic035488u

data_4310877
_publ_section_title
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 Synthesis, Structure, and Magnetic Properties of Amine-Templated
 Open-Framework Nickel(II) Sulfates
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2636
_journal_page_last               2642
_journal_paper_doi               10.1021/ic035488u
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        NiO+H2SO4+1,3-DAP+EG+H2O+HF
_chemical_formula_sum            'C3 H18 F2 N2 Ni3 O15 S3'
_chemical_formula_weight         632.50
_chemical_name_common            'Layered NiSo4 with 1,3-DAP'
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0120(7)
_cell_length_b                   7.3584(5)
_cell_length_c                   9.9143(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      1.71
_cell_volume                     867.74(9)
_computing_cell_refinement       SAINT(Siemens,1996)
_computing_data_collection       SMART(Siemens,1996)
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL v5.0'
_computing_publication_material  'SHELXTL v5.0'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens CCD-diffractometer'
_diffrn_measurement_method       \W
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3447
_diffrn_reflns_theta_max         23.21
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    3.683
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.787021
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.335
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_coef       0.0245(18)
_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_all   1.084
_refine_ls_goodness_of_fit_obs   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      0.938
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1280
_refine_ls_wR_factor_obs         0.0999
_reflns_number_observed          1881
_reflns_number_total             2259
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic035488usi20040131_085404_3.cif
_cod_data_source_block           I_1,3-DAP
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4310877