Mono- and Dinuclear d10 Metal Complexes of Hexakis(3,5-dimethylpyrazolyl)cyclotriphosphazene. Synthesis, Structures, and Unusual Solution Dynamic Behavior
Younghun Byun; Dongwon Min; Junghwan Do; Hoseop Yun; Youngkyu Do; Inorganic Chemistry 35 (1996) 3981–3989; doi:10.1021/ic950907b

data_4323832
_publ_section_title
;
 Mono- and Dinuclear d10 Metal Complexes of
 Hexakis(3,5-dimethylpyrazolyl)cyclotriphosphazene. Synthesis, Structures,
 and Unusual Solution Dynamic Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3981
_journal_page_last               3989
_journal_paper_doi               10.1021/ic950907b
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C31 H44 Cd2 Cl6 N15 P3'
_chemical_formula_weight         1157.22
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.71(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.585(5)
_cell_length_b                   17.585(4)
_cell_length_c                   14.404(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4592.1(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4456
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.423
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             2312
_refine_diff_density_max         1.043
_refine_diff_density_min         -.950
_refine_diff_density_rms         .095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         4286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_obs          0.0365
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0528P)^2^+13.7294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_obs         0.0886
_reflns_number_observed          3814
_reflns_number_total             4286
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950907b_3.cif
_cod_data_source_block           P3N3(3,5-Me2C3N2H)6(CdCl2)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0528P)^2^+13.7294P] 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^)+( 0.0528P)^2^+13.7294P]
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        4592.0(19)
_cod_database_code               4323832