1,2,3-Triazolate-Bridged Tetradecametallic Transition Metal Clusters [M14(L)6O6(OMe)18X6] (M = FeIII, CrIII and VIII/IV) and Related Compounds: Ground-State Spins Ranging from S=0 to S=25 and Spin-Enhanced Magnetocaloric Effect
Rachel Shaw; Rebecca H. Laye; Leigh F. Jones; David M. Low; Caytie Talbot-Eeckelaers; Qiang Wei; Constantinos J. Milios; Simon Teat; Madeleine Helliwell; James Raftery; Marco Evangelisti; Marco Affronte; David Collison; Euan K. Brechin; Eric J. L. McInnes; Inorganic Chemistry 46 (2007) 4968–4978; doi:10.1021/ic070320k

data_4308253
_publ_section_title
;
1,2,3-Triazolate-Bridged Tetradecametallic Transition Metal Clusters
[M14(L)6O6(OMe)18X6] (M = FeIII, CrIII and VIII/IV) and Related Compounds:
Ground-State Spins Ranging from S=0 to S=25 and Spin-Enhanced
Magnetocaloric Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4968
_journal_page_last               4978
_journal_paper_doi               10.1021/ic070320k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C34 H83 Cl6 Fe14 N18 O28.5'
_chemical_formula_weight         2194.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.139(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.049(2)
_cell_length_b                   17.069(3)
_cell_length_c                   16.566(3)
_cell_measurement_reflns_used    7892
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.512
_cell_measurement_theta_min      2.313
_cell_volume                     3506.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Station 9.8, SRS, Daresbury'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18509
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         24.22
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    3.117
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_correction_T_min  0.7457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2214
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         18509
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0565P)^2^+5.3010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                13220
_reflns_number_total             18509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070320k-file004.cif
_cod_data_source_block           feta
_cod_depositor_comments
;
 Removing the '_publ_author' data item since it was not found in the core
 CIF dictionary and the same information was already provided in the official
 bibliography data items. No information was lost by removing this data item.

 Antanas Vaitkus,
 2017-03-07
;
_cod_original_formula_sum        'C34 H83 Cl6 Fe14 N18 O28.50'
_cod_database_code               4308253