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_4078033
_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         'C23 H36 Cu N7 O P, F6 P, C H2 Cl2'
_chemical_formula_sum            'C24 H38 Cl2 Cu F6 N7 O P2'
_chemical_formula_weight         750.99
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9778(6)
_cell_length_b                   18.8108(7)
_cell_length_c                   10.5559(4)
_cell_measurement_reflns_used    9119
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.21
_cell_volume                     3371.2(2)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0107
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46498
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7748
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0610P)^2^+1.8717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                7525
_reflns_number_total             7748
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300051f_si_002.cif
_cod_data_source_block           l0122a
_cod_database_code               4078033