Chiral recognition in contact ion-pairs; observation, characterization and analysis
Raskatov, Jevgenij A.; Thompson, Amber L.; Cowley, Andrew R.; Claridge, Timothy D. W.; Brown, John M.; Chemical Science 4 (2013) 3140–; doi:10.1039/c3sc51096d

data_1514763
_publ_section_title
;
 Chiral recognition in contact ion-pairs; observation, characterization
 and analysis
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3140
_journal_paper_doi               10.1039/c3sc51096d
_journal_volume                  4
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C51 H40 P2 Rh, C40 H24 B O4, C4 H10 O, 3(C H2 Cl2)'
_chemical_formula_sum            'C98 H80 B Cl6 O5 P2 Rh'
_chemical_formula_weight         1726.09
_chemical_melting_point          ?
_chemical_name_systematic
;
((Bicyclo[2.2.1]hepta-2,5-diene)((R)-bis-2,2'-(diphenylphosphino)-1,1'
-binaphthalene)rhodium)((S,S)-bis-(1,1'-binaphthalen-2,2'-dioxo)boronate).
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7224(3)
_cell_length_b                   20.2138(4)
_cell_length_c                   25.7426(6)
_cell_measurement_reflns_used    86469
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     8181.2(3)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution
;
'SIR92 (Giacovazzo et al, 1992)'
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            86469
_diffrn_reflns_theta_full        27.406
_diffrn_reflns_theta_max         27.406
_diffrn_reflns_theta_min         5.091
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       prism
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_thermal_history
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.74
_refine_ls_abs_structure_details 'Flack, 8421 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         11955
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.013974
_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:
0.920 0.171 0.593
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1040
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0578
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                11955
_reflns_number_total             18392
_reflns_threshold_expression     I>3.00u(I)
_oxford_refine_ls_scale          0.13988(18)
_cod_data_source_file            c3sc51096d.txt
_cod_data_source_block           arc1636
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '
Not determined' was changed to '?'
- the value is undefined or not given.

'_symmetry_cell_setting'
value 'Orthorhombic' changed to 'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               1514763