Tris(pyrazolyl)phosphine Oxides. Synthesis and Coordination Chemistry with Copper(I)
Tazelaar, Cornelis G. J.; Lyaskovskyy, Volodymyr; Dijk, Tom van; Broere, Daniël L. J.; Kolfschoten, Ludo A.; Khiar, Rima Osman Hassan; Lutz, Martin; Slootweg, J. Chris; Lammertsma, Koop; Organometallics 31 (2012) 3308–; doi:10.1021/om300051f

data_4078035
_publ_section_title
;
 Tris(pyrazolyl)phosphine Oxides. Synthesis and Coordination Chemistry
 with Copper(I)
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3308
_journal_paper_doi               10.1021/om300051f
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C33 H36 Cu N6 O P2, P F6, 2(C H2 Cl2)'
_chemical_formula_sum            'C35 H40 Cl4 Cu F6 N6 O P3'
_chemical_formula_weight         972.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.223(1)
_cell_angle_beta                 106.463(1)
_cell_angle_gamma                91.278(1)
_cell_formula_units_Z            2
_cell_length_a                   11.0739(3)
_cell_length_b                   12.6624(3)
_cell_length_c                   15.9619(2)
_cell_measurement_reflns_used    17080
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.65
_cell_volume                     2089.69(8)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Pixel15, Twinabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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_measurement_method       '\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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0091
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40560
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Twinabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9572
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+1.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                8587
_reflns_number_total             9572
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300051f_si_002.cif
_cod_data_source_block           s4103a
_cod_database_code               4078035