Synthesis and derivatization of highly-functionalized ?5-phospholes
Javier Ruiz; Marta P. Gonzalo; Marilin Vivanco; Santiago; Garcia-Grand; Chem.Commun. 50 (2014) 5597–; doi:10.1039/C4CC02089H

data_7113324
_publ_section_title
;
 Synthesis and derivatization of highly-functionalized ?5-phospholes
;
_journal_name_full               Chem.Commun.
_journal_page_first              5597
_journal_paper_doi               10.1039/C4CC02089H
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H37 N O4 P2, C4 H8 O'
_chemical_formula_sum            'C40 H45 N O5 P2'
_chemical_formula_weight         681.71
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.518(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4539(10)
_cell_length_b                   11.1081(5)
_cell_length_c                   20.2140(9)
_cell_measurement_reflns_used    6789
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      69.48
_cell_measurement_theta_min      3.74
_cell_volume                     3565.7(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0581595
_diffrn_orient_matrix_UB_12      -0.0311037
_diffrn_orient_matrix_UB_13      0.0290628
_diffrn_orient_matrix_UB_21      -0.0027442
_diffrn_orient_matrix_UB_22      0.0302612
_diffrn_orient_matrix_UB_23      0.0455588
_diffrn_orient_matrix_UB_31      -0.0239876
_diffrn_orient_matrix_UB_32      -0.0788747
_diffrn_orient_matrix_UB_33      0.0060185
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6644
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         72.20
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
Absolute Configuration of C3 = R
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.8590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                4547
_reflns_number_total             6644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02089h2.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7113324