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_1514762
_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_formula_moiety         'C52 H44 P2 Rh, C40 H24 B O4, 3(C H2 Cl2)'
_chemical_formula_sum            'C95 H74 B Cl6 O4 P2 Rh'
_chemical_formula_weight         1668.01
_chemical_melting_point          ?
_chemical_name_systematic
;
((Bicyclo[2.2.1]hepta-2,5-diene)((rac)-bis-2,2'-(diphenylphosphino)-1,1'
-binaphthalene)rhodium)((rac)-bis-(1,1'-binaphthalen-2,2'-dioxo)boronate).
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.7932(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3718(2)
_cell_length_b                   20.1092(2)
_cell_length_c                   21.5060(2)
_cell_measurement_reflns_used    19378
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     8359.34(14)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
;
'SIR92 (Giacovazzo et al, 1992)'
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            129861
_diffrn_reflns_theta_full        27.478
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         0.78
_refine_diff_density_min         -1.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         19008
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.001264
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +21.54P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1458
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1456
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                14743
_reflns_number_total             19014
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.09
_oxford_diffrn_Wilson_scale      23.61
_oxford_refine_ls_r_factor_ref   0.0703
_oxford_refine_ls_scale          0.19184(8)
_oxford_reflns_number_all        19014
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 5883
_cod_data_source_file            c3sc51096d.txt
_cod_data_source_block           5883
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C95 H74 B1 Cl6 O4 P2 Rh1'
_cod_database_code               1514762