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_4071367
_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         'C32 H18 Mo N9 O8 P W, C4 H8 O'
_chemical_formula_sum            'C36 H26 Mo N9 O9 P W'
_chemical_formula_weight         1039.42
_chemical_name_systematic
; 
 ? 
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.052(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.87209(6)
_cell_length_b                   17.3152(2)
_cell_length_c                   29.6070(6)
_cell_measurement_reflns_used    45992
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.82
_cell_volume                     5518.64(13)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs, SQUEEZE'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            103081
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.4298
_exptl_absorpt_correction_T_min  0.1821
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         12685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+7.3148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                10614
_reflns_number_total             12685
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800127h-file001.cif
_cod_data_source_block           s3797a
_cod_original_cell_volume        5518.65(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071367