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_1514764
_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
;
'(R),(R,R)'
;
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C52 H44 P2 Rh, C40 H24 B O4, 4( C H2 Cl2 ) '
_chemical_formula_sum            'C96 H76 B Cl8 O4 P2 Rh'
_chemical_formula_weight         1752.94
_chemical_melting_point          ?
_chemical_name_systematic
;
((Bicyclo[2.2.1]hepta-2,5-diene)((R)-bis-2,2'-(diphenylphosphino)-1,1'-binaphthalene)rhodium)
((R,R)-bis-(1,1'-binaphthalen-2,2'-dioxo)boronate).
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 111.9738(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8286(2)
_cell_length_b                   25.5279(4)
_cell_length_c                   14.3047(2)
_cell_measurement_reflns_used    38581
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     4005.65(11)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.060
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38581
_diffrn_reflns_theta_full        27.478
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         5.118
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' orange-yellow '
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_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         0.75
_refine_diff_density_min         -1.12
_refine_ls_abs_structure_details 'Flack, 6867 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         10962
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.029637
_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:
0.294 0.754E-01 0.775E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0814
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0464
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              29
_reflns_limit_k_min              -33
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                10962
_reflns_number_total             16161
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            c3sc51096d.txt
_cod_data_source_block           arc1456
_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 'Monoclinic' changed to 'monoclinic' 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 1 21 1 '
_cod_original_formula_sum        ' C96 H76 B Cl8 O4 P2 Rh '
_cod_database_code               1514764