Synthetic and computational study of geminally bis(supermesityl) substituted phosphorus compounds.
Fleming, Conor G. E.; Slawin, Alexandra M. Z.; Athukorala Arachchige, Kasun S.; Randall, Rebecca; Bühl, Michael; Kilian, Petr; Dalton transactions (Cambridge, England : 2003) 42 (2013) 1437–1450; doi:10.1039/c2dt31971c

data_7020774
_publ_section_title
;
 Synthetic and computational study of geminally bis(supermesityl)
 substituted phosphorus compounds.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1437
_journal_page_last               1450
_journal_paper_doi               10.1039/c2dt31971c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C37 H61 O P'
_chemical_formula_sum            'C37 H61 O P'
_chemical_formula_weight         552.86
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.892(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.039(4)
_cell_length_b                   10.854(5)
_cell_length_c                   14.610(6)
_cell_measurement_reflns_used    6582
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.13
_cell_volume                     1719.0(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10779
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             612.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.440
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2339 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.57(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5639
_refine_ls_number_restraints     7
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1006P)^2^+1.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2115
_reflns_number_gt                5048
_reflns_number_total             5639
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2dt31971c.txt
_cod_data_source_block           4
_cod_database_code               7020774