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_4329286
_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
' C36 H69 Cu4 I4 N9 O2 P4,  0.06(C4 H8 Cl8), C2 H3 N'
_chemical_formula_sum            'C38.25 H72.5 Cl0.5 Cu4 I4 N10 O2 P4'
_chemical_formula_weight         1607.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.582(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.942(5)
_cell_length_b                   11.0604(13)
_cell_length_c                   32.778(4)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.22
_cell_volume                     12278(3)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            52953
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.7813
_exptl_absorpt_correction_T_min  0.5635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       Needle
_exptl_crystal_F_000             6276
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.788
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         14523
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+44.8960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                12514
_reflns_number_total             14523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300541n_si_002_5.cif
_cod_data_source_block           msb410_0m
_cod_original_formula_sum        'C38.25 H72.50 Cl0.50 Cu4 I4 N10 O2 P4'
_cod_database_code               4329286