Synthesis and crystal structure of Li[{Ca7(μ3-OH)8I6(thf)12}2(μ-I)]·3THF, a unique H-bound dimer of a Ca7-cluster on the way to sol‒gels
Fromm, Katharina M.; Chemical Communications  (1999) 1659–; doi:10.1039/a904560k

data_7110617
_publ_section_title
;
 Synthesis and crystal structure of
 Li[{Ca7(\m3-OH)8I6(thf)12}2(\m-I)]&#x00B7;3THF, a unique H-bound dimer of
 a Ca7-cluster on the way to sol--gels
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1659
_journal_paper_doi               10.1039/a904560k
_journal_year                    1999
_chemical_formula_moiety         'C108 H232 Ca14 I13 O43'
_chemical_formula_sum            'C54 H116 Ca7 I6.5 O21.5'
_chemical_formula_weight         2214.88
_chemical_name_common            Ca7-Cluster-Dimer
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.592(3)
_cell_length_b                   21.592(3)
_cell_length_c                   36.839(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_volume                     14874(4)
_computing_molecular_graphics    'SCHAKAL (E.Keller, Uni Freiburg) '
_computing_publication_material  'WORD 97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Enraf-Nonius
_diffrn_measurement_method       omega-scan
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            7165
_diffrn_reflns_theta_full        26.93
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.25
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.447
_exptl_absorpt_correction_type   'face indexation '
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             6579
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+72.2258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.2057
_reflns_number_gt                4307
_reflns_number_total             7165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904560ksup1.cif
_cod_data_source_block           Ca7-Dimer
_cod_original_sg_symbol_H-M      R(-3)
_cod_original_formula_sum        'C54 H116 Ca7 I6.50 O21.50'
_cod_database_code               7110617