Cyclotriphosphazene Hydrazides as Efficient Multisite Coordination Ligands. η3-fac-non-geminal-N3 Coordination of spiro-N3P3[O2C12H8][N(Me)NH2]4(L) in L2CoCl3 and L2M(NO3)2 (M = Ni, Zn, Cd)
Vadapalli Chandrasekhar; Venkatasubbaiah Krishnan; Alexander Steiner; Jamie F. Bickley; Inorganic Chemistry 43 (2004) 166–172; doi:10.1021/ic034561d

data_4310296
_publ_section_title
;
 Cyclotriphosphazene Hydrazides as Efficient Multisite Coordination
 Ligands. \h3-fac-non-geminal-N3 Coordination of
 spiro-N3P3[O2C12H8][N(Me)NH2]4(L) in L2CoCl3 and L2M(NO3)2 (M = Ni, Zn,
 Cd)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              166
_journal_page_last               172
_journal_paper_doi               10.1021/ic034561d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C34 H64 Cl3 Co N22 O6 P6'
_chemical_formula_weight         1228.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.920(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1714(12)
_cell_length_b                   21.337(3)
_cell_length_c                   16.404(2)
_cell_measurement_temperature    213(2)
_cell_volume                     2849.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       /w-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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18118
_diffrn_reflns_theta_full        24.20
_diffrn_reflns_theta_max         24.20
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         8566
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      3.391
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+1.0959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                7595
_reflns_number_total             8566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034561dsi20030806_120741_1.cif
_cod_data_source_block           compound_4
_cod_original_cell_volume        2849.7(7)
_cod_database_code               4310296