Phospha-Scorpionate Complexes by Click Chemistry using Phenyl Azide and Ethynylphosphine Oxides
van Assema, Sander G. A.; Tazelaar, Cornelis G. J.; de Jong, G. Bas; van Maarseveen, Jan H.; Schakel, Marius; Lutz, Martin; Spek, Anthony L.; Slootweg, J. Chris; Lammertsma, Koop; Organometallics 27 (2008) 3210–; doi:10.1021/om800127h

data_4071366
_publ_section_title
;
 Phospha-Scorpionate Complexes by Click Chemistry using Phenyl Azide and
 Ethynylphosphine Oxides
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3210
_journal_paper_doi               10.1021/om800127h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C29 H18 N9 O5 P W, C4 H8 O'
_chemical_formula_sum            'C33 H26 N9 O6 P W'
_chemical_formula_weight         859.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.452(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.6093(5)
_cell_length_b                   20.4105(5)
_cell_length_c                   13.53985(18)
_cell_measurement_reflns_used    29211
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.62
_cell_volume                     6945.6(2)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            78673
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    3.430
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0211P)^2^+22.3521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                5893
_reflns_number_total             7986
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800127h-file001.cif
_cod_data_source_block           s3595a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4071366