Nature of Magnetic Interactions in 3D {[MII(pyrazole)4]2[NbIV(CN)8].4H2O}n (M = Mn, Fe, Co, Ni) Molecular Magnets
Dawid Pinkowicz; Robert Pełka; Olga Drath; Wojciech Nitek; Maria Bałanda; Anna Małgorzata Majcher; Giordano Poneti; Barbara Sieklucka; Inorganic Chemistry 49 (2010) 7565–7576; doi:10.1021/ic100937h

data_4316278
_publ_contact_author_address
;
Department of Chemistry
Jagiellonian University
Ingardena 3, 30-060 Cracow
Poland
;
_publ_contact_author_email       pinkowic@chemia.uj.edu.pl
_publ_contact_author_fax         00(000)0000000
_publ_contact_author_name        'Pinkowicz, Dawid'
_publ_contact_author_phone       '0048 12 6632051'
_publ_section_title
;
 Nature of Magnetic Interactions in 3D
 {[MII(pyrazole)4]2[NbIV(CN)8].4H2O}n (M = Mn, Fe, Co, Ni) Molecular
 Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7565
_journal_page_last               7576
_journal_paper_doi               10.1021/ic100937h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C32 H40 Mn2 N24 Nb O4'
_chemical_formula_weight         1027.67
_chemical_name_common            OD13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-12-10T23:46:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8528(4)
_cell_length_b                   21.8528(4)
_cell_length_c                   9.6461(2)
_cell_measurement_reflns_used    10815
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     4606.45(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0435012
_diffrn_orient_matrix_UB_12      0.0131189
_diffrn_orient_matrix_UB_13      0.0054195
_diffrn_orient_matrix_UB_21      -0.0088676
_diffrn_orient_matrix_UB_22      0.0114735
_diffrn_orient_matrix_UB_23      0.043405
_diffrn_orient_matrix_UB_31      0.0251119
_diffrn_orient_matrix_UB_32      -0.0958556
_diffrn_orient_matrix_UB_33      0.0304685
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20882
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.8834
_exptl_absorpt_correction_T_min  0.7557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0028(2)
_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   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+1.4936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                2387
_reflns_number_total             3363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100937h_si_002.cif
_cod_data_source_block           od13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4606.42(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4316278