Dual Supermesityl Stabilization: 1-Alkyl-1H-[1,2,4]triphospholes, with Among the Most Planar and Least Sterically Hindered σ3,λ3-Phosphorus Atoms, and Novel C2P3S4Folded Heterocycles†
Ionkin, Alex S.; Marshall, William J.; Fish, Brian M.; Marchione, Alexander A.; Howe, Laurie A.; Davidson, Fredric; McEwen, Charles N.; Organometallics 27 (2008) 5118–; doi:10.1021/om800528g

data_4072023
_publ_section_title
;
 Dual Supermesityl Stabilization: 1-Alkyl-1H-[1,2,4]triphospholes, with
 Among the Most Planar and Least Sterically Hindered \s3,\l3-Phosphorus
 Atoms, and Novel C2P3S4Folded Heterocycles&#x2020;
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5118
_journal_paper_doi               10.1021/om800528g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C39 H61 P3'
_chemical_formula_weight         622.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   21.285(4)
_cell_length_b                   12.164(2)
_cell_length_c                   29.355(5)
_cell_measurement_temperature    293(2)
_cell_volume                     7600(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            83073
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ireg.block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          3.118
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1330P)^2^+10.8328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2429
_refine_ls_wR_factor_ref         0.2802
_reflns_number_gt                4270
_reflns_number_total             6511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800528g_si_001.cif
_cod_data_source_block           07139
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7601(2)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4072023