Synthesis, Structure, and Magnetic Properties of the Single-Molecule Magnet [Ni21(cit)12(OH)10(H2O)10]16-
Stefan T. Ochsenbein; Mark Murrie; Eduard Rusanov; Helen Stoeckli-Evans; Chihiro Sekine; Hans U. Güdel; Inorganic Chemistry 41 (2002) 5133–5140; doi:10.1021/ic020252w

data_4318564
_publ_section_title
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 Synthesis, Structure, and Magnetic Properties of the Single-Molecule
 Magnet [Ni21(cit)12(OH)10(H2O)10]16-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5133
_journal_page_last               5140
_journal_paper_doi               10.1021/ic020252w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C138 H362 N14 Na2 Ni21 O155'
_chemical_formula_weight         5977.31
_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                71.111(9)
_cell_angle_beta                 89.314(9)
_cell_angle_gamma                64.928(8)
_cell_formula_units_Z            1
_cell_length_a                   16.5469(11)
_cell_length_b                   18.9571(15)
_cell_length_c                   25.597(2)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.00
_cell_volume                     6807.2(11)
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53570
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3138
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.861
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         24558
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      2.119
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                16072
_reflns_number_total             24558
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic020252w_1.cif
_cod_data_source_block           g85
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        6807.3(9)
_cod_database_code               4318564