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_4318713
_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            'C54 H65 F Li N3 O7 Rh3'
_chemical_formula_weight         1202.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   44.177(9)
_cell_length_b                   12.390(3)
_cell_length_c                   20.164(4)
_cell_measurement_reflns_used    '463 spots from first image'
_cell_measurement_temperature    143(2)
_cell_volume                     10201(4)
_computing_cell_refinement       'marresearch marHKL, 1.9.1'
_computing_data_collection       'marresearch mar345, 1.2.11'
_computing_data_reduction        'marresearch marHKL'
_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 0.879
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'mar345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 degrees 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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29489
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.562
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00242(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         10389
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0809P)^2^+22.2495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                9206
_reflns_number_total             10389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025749k_s1_5.cif
_cod_data_source_block           2_LiF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4318713