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_4078034
_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         'C32 H30 Cu N7 O P, F6 P'
_chemical_formula_sum            'C32 H30 Cu F6 N7 O P2'
_chemical_formula_weight         768.11
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.357(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6120(3)
_cell_length_b                   23.4829(9)
_cell_length_c                   17.3556(6)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.63
_cell_volume                     3311.5(2)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0097
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57072
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.051
_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     468
_refine_ls_number_reflns         7613
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+2.5110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                6889
_reflns_number_total             7613
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300051f_si_002.cif
_cod_data_source_block           l0123a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078034