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_4329287
_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         'C30 H60 Br Cu N6 O2 P4'
_chemical_formula_sum            'C30 H60 Br Cu N6 O2 P4'
_chemical_formula_weight         804.17
_chemical_name_systematic
; 
 ? 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.645(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8133(10)
_cell_length_b                   26.476(2)
_cell_length_c                   16.7607(15)
_cell_measurement_reflns_used    1954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.23
_cell_volume                     4798.2(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            78026
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.8855
_exptl_absorpt_correction_T_min  0.7667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       Block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
Two regions of electron density appearing to be partially occupied
by significantly disordered lattice dichloromethane molecules on
the basis of trial models were removed with the SQUEEZE option of
PLATON (Spek, 2009) after the trial models preoved unsuccessful.
disordered 
;
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         10620
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0561P)^2^+2.3630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                7713
_reflns_number_total             10620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300541n_si_002_6.cif
_cod_data_source_block           msb447_0m
_cod_original_cell_volume        4798.3(8)
_cod_database_code               4329287