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_4323834
_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            'C30 H42 Cl2 Cu I N15 P3 Zn'
_chemical_formula_weight         1032.41
_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                 93.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.876(5)
_cell_length_b                   21.599(4)
_cell_length_c                   9.117(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4496.1(16)
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5326
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.959
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             2072
_refine_diff_density_max         1.702
_refine_diff_density_min         -1.065
_refine_diff_density_rms         .204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   0.998
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         5166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      0.998
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_obs          0.0700
_refine_ls_shift/esd_max         -0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1498P)^2^+36.8094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2645
_refine_ls_wR_factor_obs         0.2006
_reflns_number_observed          3806
_reflns_number_total             5166
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950907b_5.cif
_cod_data_source_block           P3N3(3,5-Me2C3N2H)6(ZnCl2)(CuI)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1498P)^2^+36.8094P] 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^)+( 0.1498P)^2^+36.8094P]
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        4495.8(16)
_cod_database_code               4323834