Synthesis, Structure, and Magnetic Properties of the Low-Symmetry Tetranuclear Cubane-like Nickel Complex [Ni4(pypentO)(pym)(μ3-OH)2(μ-Oac)2(NCS)2(OH2)]
Juan M. Clemente-Juan; Benoît Chansou; Bruno Donnadieu; Jean-Pierre Tuchagues; Inorganic Chemistry 39 (2000) 5515–5519; doi:10.1021/ic0005442

data_4321608
_publ_contact_author             ' J.P.Tuchagues'
_publ_contact_author_email       tuchague@lcctoul.lcc-toulouse.fr
_publ_contact_author_fax         '(33) (0) 5 61 55 20 03 '
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of the Low-Symmetry
 Tetranuclear Cubane-like Nickel Complex
 [Ni4(pypentO)(pym)(\m3-OH)2(\m-Oac)2(NCS)2(OH2)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5515
_journal_page_last               5519
_journal_paper_doi               10.1021/ic0005442
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C61 H88 N14 Ni8 O25.5 S4'
_chemical_formula_weight         2023.37
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 110.619(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9375(14)
_cell_length_b                   20.6604(18)
_cell_length_c                   16.6684(19)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      1.45
_cell_volume                     4492.3(9)
_computing_cell_refinement
;
Stoe and Cie (1996) IPDS Manual. Version 2.75
Stoe and Cie, Darmstadt, Germany
;
_computing_data_collection
;
Stoe and Cie (1996) IPDS Manual. Version 2.75
Stoe and Cie, Darmstadt, Germany
;
_computing_data_reduction
;
Stoe and Cie (1996) IPDS Manual. Version 2.75
Stoe and Cie, Darmstadt, Germany
;
_computing_molecular_graphics
;
Zsolnai,L.(1997). ZORTEP.Molecular Graphics Program.
University of Heidelberg, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
Altomare, A., Cascarano, G., Giacovazzo G.,
Guagliardi A., Burla M.C., Polidori, G.  & Camalli, M. (1994) SIR92 - a
program for automatic solution of crystal structures by direct methods.
J. Appl. Cryst. (27), 435
;
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Stoe and Cie (1996) IPDS Manual. Version 2.75. 
Stoe and Cie, Darmstadt, Germany
;
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29349
_diffrn_reflns_theta_full        22.21
_diffrn_reflns_theta_max         22.21
_diffrn_reflns_theta_min         2.36
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.805
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            light_blue
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         11209
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.784
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                10049
_reflns_number_total             11209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0005442.cif
_cod_data_source_block           C61H88N14O25.5S4N8
_cod_depositor_comments
;
 Correcting the _chemical_formula_sum data item value by changing it from
 'C61 H88 N14 Ni8 O25.5 S4' to 'C61 H88 N14 Ni8 O25.5 S4'.

 Antanas Vaitkus,
 2017-09-22

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
;
_cod_original_cell_volume        4492.3(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        C61H88N14O25.5S4N8
_cod_database_code               4321608