Tethered Pyrazolyl Phosphinate: Pyrazolyl-N- and Phosphoryl-O-Metal Coordination in Ph2P(O){OCH2CH2(3,5-Me2Pz)}
Savariraj Kingsley; Vadapalli Chandrasekhar; Christopher D. Incarvito; Matthew K. Lam; Arnold L. Rheingold; Inorganic Chemistry 40 (2001) 5890–5896; doi:10.1021/ic010454c

data_4320480
_publ_contact_author
;
       Chandrasekhar. V
       Department of Chemistry
       IIT, Kanpur 208 016
       India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91 512 597 436'
_publ_contact_author_phone       '+91 512 597 617'
_publ_section_title
;
 Tethered Pyrazolyl Phosphinate: Pyrazolyl-N- and Phosphoryl-O-Metal
 Coordination in Ph2P(O){OCH2CH2(3,5-Me2Pz)}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5890
_journal_page_last               5896
_journal_paper_doi               10.1021/ic010454c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C38 H42 Cl2 N4 O4 P2 Pd'
_chemical_formula_sum            'C38 H42 Cl2 N4 O4 P2 Pd'
_chemical_formula_weight         858.02
_chemical_melting_point          170
_chemical_name_common            Pdopp2epz(5)
_chemical_name_systematic
;

   ?

;
_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                97.551(18)
_cell_angle_beta                 90.000(10)
_cell_angle_gamma                106.87(8)
_cell_formula_units_Z            1
_cell_length_a                   7.671(16)
_cell_length_b                   11.487(2)
_cell_length_c                   11.763(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     983(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    0.0168
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3717
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                3215
_reflns_number_total             3433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010454c_5.cif
_cod_data_source_block           PdOPP2EPZ
_cod_original_cell_volume        982(2)
_cod_database_code               4320480