Fluoride Bridges as Structure-Directing Motifs in 3d-4f Cluster Chemistry
Torben Birk; Kasper S. Pedersen; Christian Aa. Thuesen; Thomas Weyhermüller; Magnus Schau-Magnussen; Stergios Piligkos; Högni Weihe; Susanne Mossin; Marco Evangelisti; Jesper Bendix; Inorganic Chemistry 51 (2012) 5435–5443; doi:10.1021/ic300421x

data_4329135
_publ_contact_author_address
;
Department of Chemistry, University of Copenhagen
Universitetsparken 5
DK-2100 Copenhagen
Denmark
;
_publ_contact_author_email       bendix@kiku.dk
_publ_contact_author_fax         '+45 35320212'
_publ_contact_author_name        'Jesper Bendix'
_publ_contact_author_phone       '+45 35320101'
_publ_section_title
;
 Fluoride Bridges as Structure-Directing Motifs in 3d-4f Cluster Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5435
_journal_page_last               5443
_journal_paper_doi               10.1021/ic300421x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C46 H48 Cr2 F45 Ho3 N6 O12, 7(C2 H3 N) '
_chemical_formula_sum            'C60 H69 Cr2 F45 Ho3 N13 O12'
_chemical_formula_weight         2618.07
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.042(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.242(2)
_cell_length_b                   15.402(2)
_cell_length_c                   24.956(4)
_cell_measurement_reflns_used    52837
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.55
_cell_volume                     9312(2)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0966
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            164089
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    2.893
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       plate
_exptl_crystal_F_000             5080
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.857
_refine_diff_density_min         -1.381
_refine_diff_density_rms         .216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         16428
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+90.5644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                13173
_reflns_number_total             16428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300421x_si_001_3.cif
_cod_data_source_block           11_Cr2Ho3_kcd678
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329135