Chiral pyridyl phosphinites with large aryl substituents as efficient ligands for the asymmetric iridium-catalyzed hydrogenation of difficult substrates
Woodmansee, David H.; Müller, Marc-André; Neuburger, Marcus; Pfaltz, Andreas; Chemical Science 1 (2010) 72–; doi:10.1039/c0sc00223b

data_1515872
_publ_section_title
;
 Chiral pyridyl phosphinites with large aryl substituents as efficient
 ligands for the asymmetric iridium-catalyzed hydrogenation of difficult
 substrates
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              72
_journal_paper_doi               10.1039/c0sc00223b
_journal_volume                  1
_journal_year                    2010
_chemical_formula_moiety         'C32 H12 B F24, C16 H24 Ir'
_chemical_formula_sum            'C48 H36 B F24 Ir'
_chemical_formula_weight         1271.80
_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
_audit_creation_date             08-03-13
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 98.362(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2952(5)
_cell_length_b                   18.3006(6)
_cell_length_c                   19.3162(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    173
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4649.9(3)
_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 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            96706
_diffrn_reflns_theta_full        34.442
_diffrn_reflns_theta_max         36.641
_diffrn_reflns_theta_min         2.226
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.004
_exptl_absorpt_correction_T_max  0.94
_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            res
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.81
_refine_diff_density_min         -1.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3459
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         11460
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.010890
_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:
0.979 -0.633E-01 0.556
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0718
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0447
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                11460
_reflns_number_total             21462
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2244(2)
_oxford_structure_analysis_title 'dw101_173k_0m in P2(1)/c'
_cod_data_source_file            c0sc00223b.txt
_cod_data_source_block           17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 21/c '
_cod_original_formula_sum        'C48 H36 B1 F24 Ir1'
_cod_database_code               1515872