Generation of Spirotricyclic Site-Differentiated Cyclotriphosphazenes: A Solvent-Free Approach to Multidentate N/O Donor Ligand Systems
Michael Harmjanz; Ingmar M. Piglosiewicz; Brian L. Scott; Carol J. Burns; Inorganic Chemistry 43 (2004) 642–650; doi:10.1021/ic034990b

data_4310445
_publ_contact_author_address
;
 Los Alamos National Laboratory, MS J514, Los Alamos NM 87544
;
_publ_contact_author_email       mharm@lanl.gov
_publ_contact_author_name
;
 Michael Harmjanz, Ingmar M. Piglosiewicz, Brian, L. Scott, Carol J. Burns
;
_publ_section_title
;
 Generation of Spirotricyclic Site-Differentiated Cyclotriphosphazenes: A
 Solvent-Free Approach to Multidentate N/O Donor Ligand Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              642
_journal_page_last               650
_journal_paper_doi               10.1021/ic034990b
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C21 H36 Fe2 I4 N11 O0.75 P3'
_chemical_formula_weight         1166.82
_chemical_name_common            compound_5
_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                 91.431(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.114(4)
_cell_length_b                   16.681(5)
_cell_length_c                   16.772(5)
_cell_measurement_temperature    203(2)
_cell_volume                     3947(2)
_computing_cell_refinement       'Bruker SAINT 4.05'
_computing_data_collection       'Bruker SMART 4.210'
_computing_data_reduction        'Bruker SAINT 4.05'
_computing_molecular_graphics    'SHELXTL/NT 5.10'
_computing_publication_material  'SHELXTL/NT 5.10'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4/PC'
_diffrn_measurement_method       '\f 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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24663
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    4.016
_exptl_absorpt_correction_T_max  0.7726
_exptl_absorpt_correction_T_min  0.6148
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multifaceted block'
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+12.6369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                6120
_reflns_number_total             7174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034990bsi20031021_052857_3.cif
_cod_data_source_block           5
_cod_original_cell_volume        3948(2)
_cod_database_code               4310445