Water-Soluble Organometallic Compounds. 6.1Synthesis, Spectral Properties, and Crystal Structures of Complexes of 1,3,5-Triaza-7-phosphaadamantane with Group 10 Metals
Donald J. Darensbourg; Tara J. Decuir; Nicole White Stafford; Jeffrey B. Robertson; Jennifer D. Draper; Joseph H. Reibenspies; Agnes Kathó; Ferenc Joó; Inorganic Chemistry 36 (1997) 4218–4226; doi:10.1021/ic970238x

data_4324023
_publ_section_title
;
 Water-Soluble Organometallic Compounds. 6.1Synthesis, Spectral
 Properties, and Crystal Structures of Complexes of
 1,3,5-Triaza-7-phosphaadamantane with Group 10 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4218
_journal_page_last               4226
_journal_paper_doi               10.1021/ic970238x
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C48 H114.67 Cl8 N24 O5.34 P8 Pd2'
_chemical_formula_weight         1857.82
_chemical_name_systematic
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;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.813(3)
_cell_length_b                   21.578(6)
_cell_length_c                   14.425(4)
_cell_measurement_temperature    163(2)
_cell_volume                     3945.0(19)
_computing_cell_refinement       'CTR (MSC, 1990)'
_computing_data_collection       'CTR (MSC, 1990)'
_computing_data_reduction        'PROCESS (MSC, 1990)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measurement_device       'Rigaku AFC5'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3088
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         4.05
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.189
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.5047
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             1923
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_obs          0.0630
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0490P)^2^+32.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1582
_refine_ls_wR_factor_obs         0.1416
_reflns_number_observed          2083
_reflns_number_total             2952
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970238x_3.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0490P)^2^+32.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0490P)^2^+32.0000P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3945.0(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4324023