Conformationally rigid chelate rings in metal complexes of pyridyloxy-substituted 2,2'-dioxybiphenyl-cyclotetra- and cyclotriphosphazene platforms.
Ainscough, Eric W.; Brodie, Andrew M.; Derwahl, Andreas; Kirk, Steve; Otter, Carl A.; Inorganic chemistry 46 (2007) 9841–9852; doi:10.1021/ic701241v

data_4339681
_publ_section_title
;
 Conformationally rigid chelate rings in metal complexes of
 pyridyloxy-substituted 2,2'-dioxybiphenyl-cyclotetra- and
 cyclotriphosphazene platforms.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9841
_journal_page_last               9852
_journal_paper_doi               10.1021/ic701241v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C38.5 H35.75 Br2 Co N8.25 O6 P3'
_chemical_formula_weight         1021.66
_chemical_name_systematic
; 
 ? 
;
_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                 94.63
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9529(2)
_cell_length_b                   10.58350(10)
_cell_length_c                   31.52860(10)
_cell_measurement_temperature    357(2)
_cell_volume                     4308.06(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Area detector'
_diffrn_measurement_method       'phi and omega 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    0.0336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            23354
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  0.802439
_exptl_absorpt_correction_T_min  0.708432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Acta Cryst., 1995, A51, 33'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2058
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00021(7)
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         7874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0174P)^2^+5.8465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                6690
_reflns_number_total             7874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701241v-file002.cif
_cod_data_source_block           sk50
_cod_original_cell_volume        4308.08(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C38.50 H35.75 Br2 Co N8.25 O6 P3'
_cod_database_code               4339681