Formation of a Novel Phenyldiphosphonic Acid Anion Dimer through Metal Assisted Hydrolysis of the P-N Bond
Savariraj Kingsley; Ashwani Vij; Vadapalli Chandrasekhar; Inorganic Chemistry 40 (2001) 6057–6060; doi:10.1021/ic010624l

data_4320543
_publ_contact_author
;
       V. Chandrasekhar
       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       '+91 512 597 435'
_publ_section_title
;
 Formation of a Novel Phenyldiphosphonic Acid Anion Dimer through Metal
 Assisted Hydrolysis of the P-N Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6057
_journal_page_last               6060
_journal_paper_doi               10.1021/ic010624l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(C15 H24 Cl N6 Pd), C12 H11 O5 P2'
_chemical_formula_sum            'C27 H35 Cl N6 O5 P2 Pd'
_chemical_formula_weight         727.42
_chemical_melting_point          149
_chemical_name_common            ringPd
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.351(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5566(50)
_cell_length_b                   15.8960(60)
_cell_length_c                   16.8390(60)
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.5
_cell_volume                     3295(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19299
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.894414
_exptl_absorpt_correction_T_min  0.733326
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+5.3350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                7359
_reflns_number_total             7731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010624l.cif
_cod_data_source_block           RingPd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_calc_flag' value 'Calc' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (28 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3295.3(2)
_cod_original_formula_sum        'C27 H35 Cl1 N6 O5 P2 Pd1'
_cod_database_code               4320543