Bulky 4-phosphacyclohexanones: diastereoselective complexations, orthometallations and unprecedented [3.1.1]metallabicycles.
Doherty, Ruth; Haddow, Mairi F.; Harrison, Zoë A; Orpen, A. Guy; Pringle, Paul G.; Turner, Alex; Wingad, Richard L.; Dalton transactions (Cambridge, England : 2003)  (2006) 4310–4320; doi:10.1039/b607490a

data_7007577
_publ_section_title
;
 Bulky 4-phosphacyclohexanones: diastereoselective complexations,
 orthometallations and unprecedented [3.1.1]metallabicycles.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4310
_journal_page_last               4320
_journal_paper_doi               10.1039/b607490a
_journal_year                    2006
_chemical_formula_moiety         'C23 H27 O2 P'
_chemical_formula_sum            'C23 H27 O2 P'
_chemical_formula_weight         366.42
_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                 102.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2849(13)
_cell_length_b                   22.074(4)
_cell_length_c                   14.046(3)
_cell_measurement_reflns_used    1102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.017
_cell_measurement_theta_min      4.006
_cell_volume                     1900.8(7)
_computing_cell_refinement       'Bruker SMART V5.625 (Bruker AXS, 2001)'
_computing_data_collection       'Bruker SMART V5.625 (Bruker AXS, 2001)'
_computing_data_reduction        'Bruker SAINT V7.06 (Bruker AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_publication_material  'Bruker SHELXTL V6.14 (Bruker AXS, 2003)'
_computing_structure_refinement  'SHELXL V6.12 (Bruker 2001)'
_computing_structure_solution    'SHELXS V6.12 (Bruker 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1763
_diffrn_reflns_av_sigmaI/netI    0.1547
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10169
_diffrn_reflns_theta_full        70.01
_diffrn_reflns_theta_max         70.01
_diffrn_reflns_theta_min         3.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.990000
_exptl_absorpt_correction_T_min  0.525841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0828
_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^)+(0.1356P)^2^+0.2261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2561
_reflns_number_gt                1974
_reflns_number_total             3068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b607490a.txt
_cod_data_source_block           rac-CyLb(O)_zahlhsad
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7007577