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_4308255
_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            'C67.3 H107.2 Cl2.1 N18 O29.2 V14'
_chemical_formula_weight         2423.32
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.155(2)
_cell_angle_beta                 75.976(2)
_cell_angle_gamma                76.399(2)
_cell_formula_units_Z            1
_cell_length_a                   13.3000(19)
_cell_length_b                   14.938(2)
_cell_length_c                   15.264(2)
_cell_measurement_reflns_used    13284
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.28
_cell_volume                     2658.7(6)
_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 and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         14135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0579
_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^)+(0.1495P)^2^+0.4276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2099
_reflns_number_gt                11021
_reflns_number_total             14135
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic070320k-file006.cif
_cod_data_source_block           rl3
_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        'C67.30 H107.20 Cl2.10 N18 O29.20 V14'
_cod_database_code               4308255