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_4310443
_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            'C44 H56 N5 O12 P3'
_chemical_formula_weight         939.85
_chemical_name_common            'compound 3h'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.527(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.214(9)
_cell_length_b                   11.700(4)
_cell_length_c                   18.977(8)
_cell_measurement_temperature    203(2)
_cell_volume                     4588(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28104
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         0.99
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9561
_exptl_absorpt_correction_T_min  0.9166
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.817
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.817
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0972
_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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                6653
_reflns_number_total             8284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034990bsi20031021_052857_1.cif
_cod_data_source_block           3h
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4310443