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_4329285
_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
'8(C30 H60 Cl Cu N6 O2 P4), 4(C2 H3 N), C2 H4 Cl4'
_chemical_formula_sum            'C250 H496 Cl12 Cu8 N52 O16 P32'
_chemical_formula_weight         6411.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   19.742(2)
_cell_length_b                   13.3563(16)
_cell_length_c                   33.573(4)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.37
_cell_volume                     8852.5(17)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I 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  0.0916
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            74797
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3404
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         20067
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0619P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                14031
_reflns_number_total             20067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300541n_si_002_4.cif
_cod_data_source_block           msb407a_0m
_cod_original_cell_volume        8852.6(18)
_cod_database_code               4329285