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]
Mimassi, Lamia; Guyard-Duhayon, Carine; Rager, Marie Noelle; Amouri, Hani; Inorganic Chemistry 43 (2004) 6644–6649; doi:10.1021/ic049361w

data_4331479
_publ_section_title
;
 Chiral Recognition and Resolution of the Enantiomers of Supramolecular
 Triangular Hosts:&#x00A0; Synthesis, Circular Dichroism, NMR, and X-ray
 Molecular Structure of
 [Li&#x2282;(R,R,R)-{Cp*Rh(5-chloro-2,3-dioxopyridine)}3][\D-Trisphat]
;
_journal_issue                   21
_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_absolute_configuration ad
_chemical_compound_source
;
?
;
_chemical_formula_moiety
;
(C45 H51 Cl3 N3 O6 Rh3), (C18 Cl12 O6 P),
3(C7 H8), (C H2 Cl2), 2.5(H2 O) '
;
_chemical_formula_sum            'C85 H82 Cl17 Li N3 O14.5 P Rh3'
_chemical_formula_weight         2326.92
_chemical_name_systematic
;                                                                               
?                                                                               
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-07-01
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.816(4)
_cell_length_b                   22.695(6)
_cell_length_c                   23.105(8)
_cell_measurement_reflns_used    112
_cell_measurement_temperature    180
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      3.8
_cell_volume                     9867(5)
_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 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type
; 
Enraf 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  0.12
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41358
_diffrn_reflns_theta_full        22.772
_diffrn_reflns_theta_max         25.515
_diffrn_reflns_theta_min         2.069
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
 DIFABS (Walker & Stuart, 1983) 
;
_exptl_crystal_colour            ' red '
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             4664.000
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.18
_refine_diff_density_min         -1.33
_refine_ls_abs_structure_details 'Flack, 7025 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1145
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         7956
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.021951
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 0.560 0.611 0.279 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1623
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0850
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7956
_reflns_number_total             17012
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic049361wsup2.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        9867.0(49)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C85 H82 Cl17 Li1 N3 O14.50 P1 Rh3 '
_cod_database_code               4331479