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_4318709
_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            'C51 H61 F2 Ir3 Li N3 O6'
_chemical_formula_weight         1433.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.438(2)
_cell_length_b                   15.100(3)
_cell_length_c                   17.742(4)
_cell_measurement_reflns_used    3521
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      21.98375
_cell_measurement_theta_min      1.47255
_cell_volume                     9762(3)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'marresearch mar345'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'marresearch mar345'
_diffrn_measurement_method
'60 images with deltaphi = 3 deg. and exp. time = 180 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56251
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    8.218
_exptl_absorpt_correction_T_max  0.6070
_exptl_absorpt_correction_T_min  0.1360
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.844
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8511
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0428P)^2^+37.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                6456
_reflns_number_total             8511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025749k_s1_1.cif
_cod_data_source_block           3_LiFHF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
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_cod_database_code               4318709