Crystal Structures and Magnetic Properties of Two Low-Dimensional Materials Constructed from [MnIII(salen)H2O]+ and [M(CN)8]3-/4- (M = Mo or W) Precursors
Paweł Przychodzeń; Krzysztof Lewiński; Maria Bałanda; Robert Pełka; Michał Rams; Tadeusz Wasiutyński; Carine Guyard-Duhayon; Barbara Sieklucka; Inorganic Chemistry 43 (2004) 2967–2974; doi:10.1021/ic035464n

data_4310940
_publ_contact_author_address
;
Faculty of Chemistry, Jagiellonian University,
Ingardena 3, 
30-060 Krakow, Poland
;
_publ_contact_author_email       siekluck@chemia.uj.edu.pl
_publ_contact_author_fax         '48 12 634 05 15'
_publ_contact_author_name        'Barbara Sieklucka'
_publ_contact_author_phone       '48 12 633 63 77'
_publ_section_title
;
 Crystal Structures and Magnetic Properties of Two Low-Dimensional
 Materials Constructed from [MnIII(salen)H2O]+ and [M(CN)8]3-/4- (M = Mo
 or W) Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2967
_journal_page_last               2974
_journal_paper_doi               10.1021/ic035464n
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'((C N)8 W),  ((C16 H14 N2 O2)(H2 O) Mn)3, (H2 O)'
_chemical_formula_sum            'C56 H50 Mn3 N14 O10 W'
_chemical_formula_weight         1427.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.1290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7210(2)
_cell_length_b                   20.6840(4)
_cell_length_c                   20.6370(2)
_cell_measurement_reflns_used    2322
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      1.0
_cell_volume                     5726.14(15)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with the \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20244
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    2.720
_exptl_absorpt_correction_T_max  0.6858
_exptl_absorpt_correction_T_min  0.3433
_exptl_absorpt_correction_type
'multi-scan (DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00051(4)
_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   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         12388
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+5.5584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                10054
_reflns_number_total             12388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035464nsi20031219_115151_1.cif
_cod_data_source_block           1mnw
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

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_sg_symbol_H-M      'P 21/c'
_cod_database_code               4310940