Resorcinol Based Acyclic Dimeric and Cyclic Di- and Tetrameric Cyclodiphosphazanes: Synthesis, Structural Studies, and Transition Metal Complexes
Guddekoppa S. Ananthnag; Seema Kuntavalli; Joel T. Mague; Maravanji S. Balakrishna; Inorganic Chemistry 51 (2012) 5919–5930; doi:10.1021/ic300541n

data_4329289
_publ_section_title
;
 Resorcinol Based Acyclic Dimeric and Cyclic Di- and Tetrameric
 Cyclodiphosphazanes: Synthesis, Structural Studies, and Transition Metal
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5919
_journal_page_last               5930
_journal_paper_doi               10.1021/ic300541n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C28 H44 N4 O4 P4 Se4'
_chemical_formula_sum            'C28 H44 N4 O4 P4 Se4'
_chemical_formula_weight         940.39
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.451(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0127(6)
_cell_length_b                   13.9234(7)
_cell_length_c                   11.9517(6)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      2.53
_cell_volume                     1873.02(16)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009a)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32446
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    4.126
_exptl_absorpt_correction_T_max  0.5546
_exptl_absorpt_correction_T_min  0.2286
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS  (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       Block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00115(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.7734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                4472
_reflns_number_total             4802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300541n_si_002_8.cif
_cod_data_source_block           msb479_1m
_cod_database_code               4329289