A Congestedin,in-Diphosphine
Zong, Jie; Mague, Joel T.; Kraml, Christina M.; Pascal, Robert A.; Organic Letters 15 (2013) 2179–; doi:10.1021/ol400728m

data_1511952
_publ_section_title
;
 A Congestedin,in-Diphosphine
;
_journal_issue                   9
_journal_name_full               'Organic Letters'
_journal_page_first              2179
_journal_paper_doi               10.1021/ol400728m
_journal_volume                  15
_journal_year                    2013
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C39 H30 O6 P2 S3, 1.5(C2 H6 O S)'
_chemical_formula_sum            'C42 H39 O7.5 P2 S4.5'
_chemical_formula_weight         869.94
_chemical_name_common
;
 in,in-bis(triarylphosphine) hexaoxide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2012.12-0'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7602(7)
_cell_length_b                   10.5542(4)
_cell_length_c                   21.7285(8)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      64.9839
_cell_measurement_theta_min      4.0691
_cell_volume                     4072.9(3)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'FLIPPER 25 (Spek, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60991
_diffrn_reflns_theta_full        65.10
_diffrn_reflns_theta_max         65.10
_diffrn_reflns_theta_min         4.07
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_exptl_absorpt_coefficient_mu    3.556
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2012b)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.827
_refine_diff_density_min         -0.492
_refine_ls_abs_structure_details
; 
 The crystal is a racemic twin with a twin ratio of 52/48
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         6947
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1452P)^2^+13.3714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2269
_refine_ls_wR_factor_ref         0.2412
_reflns_number_gt                5756
_reflns_number_total             6947
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol400728m_si_002.cif
_cod_data_source_block           rap046_1m
_cod_original_formula_sum        'C42 H39 O7.50 P2 S4.50'
_cod_database_code               1511952