Stabilization of Molecular LiF and LiFHF inside Metallamacrocyclic Hosts
Marie-Line Lehaire; Rosario Scopelliti; Kay Severin; Inorganic Chemistry 41 (2002) 5466–5474; doi:10.1021/ic025749k

data_4318712
_publ_contact_author_address
;
Institut de Chimie Mol\'eculaire et Biologique
Ecole Polytechnique F\'ederale de Lausanne
CH-1015 Lausanne
Switzerland
;
_publ_contact_author_email       kay.severin@epfl.ch
_publ_contact_author_fax         '+4121 693 9305'
_publ_contact_author_name        'Kay Severin'
_publ_contact_author_phone       '+4121 693 9302'
_publ_section_title
;
 Stabilization of Molecular LiF and LiFHF inside Metallamacrocyclic Hosts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5466
_journal_page_last               5474
_journal_paper_doi               10.1021/ic025749k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C52.5 H60.5 F Li N3 O7 Ru3'
_chemical_formula_weight         1174.69
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.783(6)
_cell_angle_beta                 103.291(5)
_cell_angle_gamma                97.565(6)
_cell_formula_units_Z            4
_cell_length_a                   14.8439(11)
_cell_length_b                   18.8894(13)
_cell_length_c                   20.9897(12)
_cell_measurement_reflns_used    7991
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      24.05825
_cell_measurement_theta_min      2.1441
_cell_volume                     4974.1(7)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_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      143(2)
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'CCD Detector KM4CCD/SAPPHIRE'
_diffrn_measurement_method       'phi and omega 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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29404
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_correction_T_min  0.7595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2386
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.211
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         15404
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.652
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+43.7726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2128
_reflns_number_gt                11482
_reflns_number_total             15404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025749k_s1_4.cif
_cod_data_source_block           1_LiF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4974.1(6)
_cod_original_formula_sum        'C52.50 H60.50 F Li N3 O7 Ru3'
_cod_database_code               4318712