Libraries of Bisdiazaphospholanes and Optimization of Rhodium-Catalyzed Enantioselective Hydroformylation
Tyler T. Adint; Gene W. Wong; Clark R. Landis; Journal of Organic Chemistry 78 (2013) 4231–4238; doi:10.1021/jo400525w

data_4028215
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Libraries of Bisdiazaphospholanes and Optimization of Rhodium-Catalyzed
 Enantioselective Hydroformylation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4231
_journal_page_last               4238
_journal_paper_doi               10.1021/jo400525w
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C50 H50 N4 O15 P2'
_chemical_formula_sum            'C50 H50 N4 O15 P2'
_chemical_formula_weight         1008.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
manual editing of the CIF file 
created by SHELXTL Ver. 6.10
and processed with modiCIfer-03272007. 
;
_audit_update_record
;
2008-04-02 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.2000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_b                   12.2669(3)
_cell_length_c                   18.5384(4)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      69.1671
_cell_measurement_theta_min      4.1521
_cell_volume                     4875.89(18)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50\% \w and 0.5 \% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            77061
_diffrn_reflns_theta_full        69.94
_diffrn_reflns_theta_max         69.94
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  0.6560
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.939
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         8980
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+4.6039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                8392
_reflns_number_total             8980
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo400525w_si_002.cif
_cod_data_source_block           landis20
_cod_original_sg_symbol_Hall     '-P 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4028215