Chiral Recognition and Resolution of the Enantiomers of Supramolecular Triangular Hosts: Synthesis, Circular Dichroism, NMR, and X-ray Molecular Structure of [Li@(R,R,R)-{Cp*Rh(5-chloro-2,3-dioxopyridine)}3][Δ-Trisphat]
Lamia Mimassi; Carine Guyard-Duhayon; Marie Noelle Rager; Hani Amouri; Inorganic Chemistry 43 (2004) 6644–6649; doi:10.1021/ic049361w

data_4311764
_publ_contact_author_address
; 

Laboratoire de Chimie Inorganique et 

Materiaux Moleculaires, UMR CNRS 7071,

Universite Pierre et Marie Curie,

4 place Jussieu, case 42, 

75252 Paris Cedex 05, France

;
_publ_contact_author_email       amouri@ccr.jussieu.fr
_publ_contact_author_fax         '(33)1 44 27 38 41'
_publ_contact_author_name        'Hani Amouri'
_publ_contact_author_phone       '(33)1 44 27 30 83'
_publ_section_title
;
 Chiral Recognition and Resolution of the Enantiomers of Supramolecular
 Triangular Hosts: Synthesis, Circular Dichroism, NMR, and X-ray Molecular
 Structure of
 [Li@(R,R,R)-{Cp*Rh(5-chloro-2,3-dioxopyridine)}3][\D-Trisphat]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6644
_journal_page_last               6649
_journal_paper_doi               10.1021/ic049361w
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source
;

?

;
_chemical_formula_moiety         'C45 H51 Cl3 N3 O6 Rh3, 3(C1 H1 Cl3)'
_chemical_formula_sum            'C48 H54 Cl12 N3 O6 Rh3'
_chemical_formula_weight         1503.12
_chemical_name_systematic
; 

? 

;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-16-12
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   19.132(2)
_cell_length_b                   19.132(2)
_cell_length_c                   20.4073(17)
_cell_measurement_reflns_used    265
_cell_measurement_temperature    295
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      3.5
_cell_volume                     6469.0(11)
_computing_cell_refinement
; 

'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'

;
_computing_data_collection
; 

 COLLECT (Nonius BV, 1997) 

;
_computing_data_reduction
; 

'EvalCCD (Duisenberg & Schreurs 1990-2000)'

;
_computing_molecular_graphics
; 

 CAMERON (Watkin et al 1996) 

;
_computing_publication_material
; 

 CRYSTALS (Watkin et al 2003) 

;
_computing_structure_refinement
; 

 CRYSTALS (Watkin et al 2003) 

;
_computing_structure_solution
; 

 SIR92 (Altomare et al, 1994) 

;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 

Nonius Kappa CCD 

;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.11
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37120
_diffrn_reflns_theta_full        27.501
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         1.229
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 

 DIFABS (Walker & Stuart, 1983) 

;
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.29
_refine_diff_density_min         -1.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8233
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000360
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 

 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 

 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 

 Method = Robust Weighting (Prince, 1982) 

 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 

 A~i~ are: 

 0.547 0.422 0.312 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1358
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0570
_reflns_limit_h_max              0
_reflns_limit_h_min              -21
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2119
_reflns_number_total             4972
_reflns_threshold_expression     I>1.50u(I)
_cod_data_source_file            ic049361wsi20040517_052049.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6469.1(11)
_cod_original_sg_symbol_H-M      'P -3 c 1 '
_cod_database_code               4311764