An enantiomerically pure P-stereogenic bisphosphine: (<i>S</i>,<i>S</i>)-ethylenebis[(2-methylphenyl)phenylphosphine] (<i>o</i>-tolyl-DiPAMP)
Bendzińska-Berus, Wioletta; Kaik-King, Magdalena; King, Gary; Rychlewska, Urszula; Acta Crystallographica Section C 70 (2014) 1174–1177; doi:10.1107/S205322961402542X

data_2019742
_publ_contact_author
;
Urszula Rychlewska
Faculty of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Pozna\'n
Poland
;
_publ_section_title
;
 An enantiomerically pure P-stereogenic bisphosphine:
 (<i>S</i>,<i>S</i>)-ethylenebis[(2-methylphenyl)phenylphosphine]
 (<i>o</i>-tolyl-DiPAMP)
;
_journal_coeditor_code           KU3144
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1174
_journal_page_last               1177
_journal_paper_doi               10.1107/S205322961402542X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C28 H28 P2'
_chemical_formula_moiety         'C28 H28 P2'
_chemical_formula_sum            'C28 H28 P2'
_chemical_formula_weight         426.44
_chemical_name_systematic
;
(<i>S</i>,<i>S</i>)-(Ethane-1,2-diyl)bis[(2-methylphenyl)phenylphosphane]
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.97250(10)
_cell_length_b                   17.0935(2)
_cell_length_c                   22.8179(3)
_cell_measurement_reflns_used    9393
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      76.1334
_cell_measurement_theta_min      2.5828
_cell_volume                     2329.50(6)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006) and XP (Siemens, 1994)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 10.5357
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Agilent SuperNova Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10411
_diffrn_reflns_theta_full        66.58
_diffrn_reflns_theta_max         66.58
_diffrn_reflns_theta_min         4.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.295
_refine_ls_abs_structure_details
;
Flack (1983), 1716 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.007(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0597P)^2^+0.4488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                4013
_reflns_number_total             4101
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ku3144sup1.cif
_cod_data_source_block           I
_cod_database_code               2019742
_cod_database_fobs_code          2019742